Analysis of Plastics

Rapra Review Reports

Expert overviews covering the science and technology of rubber and plastics

ISSN: 0889-3144

Analysis of Plastics

Report 149

Volume 13, Number 5, 2002

Martin J. Forrest

RAPRA REVIEW REPORTS

A Rapra Review Report comprises three sections, as follows:

1. A commissioned expert review, discussing a key topic of current interest, and referring to the References andAbstracts section. Reference numbers in brackets refer to item numbers from the References and Abstractssection. Where it has been necessary for completeness to cite sources outside the scope of the Rapra Abstractsdatabase, these are listed at the end of the review, and cited in the text as a.1, a.2, etc.

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Item 1Macromolecules

33, No.6, 21st March 2000, p.2171-83EFFECT OF THERMAL HISTORY ON THE RHEOLOGICALBEHAVIOR OF THERMOPLASTIC POLYURETHANESPil Joong Yoon; Chang Dae HanAkron,University

The effect of thermal history on the rheological behaviour of ester- andether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714from B.F.Goodrich) was investigated. It was found that the injectionmoulding temp. used for specimen preparation had a marked effect on thevariations of dynamic storage and loss moduli of specimens with timeobserved during isothermal annealing. Analysis of FTIR spectra indicatedthat variations in hydrogen bonding with time during isothermal annealingvery much resembled variations of dynamic storage modulus with timeduring isothermal annealing. Isochronal dynamic temp. sweep experimentsindicated that the thermoplastic PUs exhibited a hysteresis effect in theheating and cooling processes. It was concluded that the microphaseseparation transition or order-disorder transition in thermoplastic PUs couldnot be determined from the isochronal dynamic temp. sweep experiment.The plots of log dynamic storage modulus versus log loss modulus variedwith temp. over the entire range of temps. (110-190C) investigated. 57 refs.

GOODRICH B.F.USA

Accession no.771897

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Previous Titles Still AvailableVolume 1Report 3 Advanced Composites, D.K. Thomas, RAE, Farnborough.

Report 4 Liquid Crystal Polymers, M.K. Cox, ICI, Wilton.

Report 5 CAD/CAM in the Polymer Industry, N.W. Sandlandand M.J. Sebborn, Cambridge Applied Technology.

Report 8 Engineering Thermoplastics, I.T. Barrie, Consultant.

Report 11 Communications Applications of Polymers,R. Spratling, British Telecom.

Report 12 Process Control in the Plastics Industry,R.F. Evans, Engelmann & Buckham Ancillaries.

Volume 2Report 13 Injection Moulding of Engineering Thermoplastics,

A.F. Whelan, London School of Polymer Technology.

Report 14 Polymers and Their Uses in the Sports and LeisureIndustries, A.L. Cox and R.P. Brown, RapraTechnology Ltd.

Report 15 Polyurethane, Materials, Processing andApplications, G. Woods, Consultant.

Report 16 Polyetheretherketone, D.J. Kemmish, ICI, Wilton.

Report 17 Extrusion, G.M. Gale, Rapra Technology Ltd.

Report 18 Agricultural and Horticultural Applications ofPolymers, J.C. Garnaud, International Committee forPlastics in Agriculture.

Report 19 Recycling and Disposal of Plastics Packaging,R.C. Fox, Plas/Tech Ltd.

Report 20 Pultrusion, L. Hollaway, University of Surrey.

Report 21 Materials Handling in the Polymer Industry,H. Hardy, Chronos Richardson Ltd.

Report 22 Electronics Applications of Polymers, M.T.Goosey,Plessey Research (Caswell) Ltd.

Report 23 Offshore Applications of Polymers, J.W.Brockbank,Avon Industrial Polymers Ltd.

Report 24 Recent Developments in Materials for FoodPackaging, R.A. Roberts, Pira Packaging Division.

Volume 3Report 25 Foams and Blowing Agents, J.M. Methven, Cellcom

Technology Associates.

Report 26 Polymers and Structural Composites in CivilEngineering, L. Hollaway, University of Surrey.

Report 27 Injection Moulding of Rubber, M.A. Wheelans,Consultant.

Report 28 Adhesives for Structural and EngineeringApplications, C. O’Reilly, Loctite (Ireland) Ltd.

Report 29 Polymers in Marine Applications, C.F.Britton,Corrosion Monitoring Consultancy.

Report 30 Non-destructive Testing of Polymers, W.N. Reynolds,National NDT Centre, Harwell.

Report 31 Silicone Rubbers, B.R. Trego and H.W.Winnan,Dow Corning Ltd.

Report 32 Fluoroelastomers - Properties and Applications,D. Cook and M. Lynn, 3M United Kingdom Plc and3M Belgium SA.

Report 33 Polyamides, R.S. Williams and T. Daniels,T & N Technology Ltd. and BIP Chemicals Ltd.

Report 34 Extrusion of Rubber, J.G.A. Lovegrove, NovaPetrochemicals Inc.

Report 35 Polymers in Household Electrical Goods, D.Alvey,Hotpoint Ltd.

Report 36 Developments in Additives to Meet Health andEnvironmental Concerns, M.J. Forrest, RapraTechnology Ltd.

Volume 4Report 37 Polymers in Aerospace Applications, W.W. Wright,

University of Surrey.

Report 39 Polymers in Chemically Resistant Applications,D. Cattell, Cattell Consultancy Services.

Report 41 Failure of Plastics, S. Turner, Queen Mary College.

Report 42 Polycarbonates, R. Pakull, U. Grigo, D. Freitag, BayerAG.

Report 43 Polymeric Materials from Renewable Resources,J.M. Methven, UMIST.

Report 44 Flammability and Flame Retardants in Plastics,J. Green, FMC Corp.

Report 45 Composites - Tooling and Component Processing,N.G. Brain, Tooltex.

Report 46 Quality Today in Polymer Processing, S.H. Coulson,J.A. Cousans, Exxon Chemical International Marketing.

Report 47 Chemical Analysis of Polymers, G. Lawson, LeicesterPolytechnic.

Volume 5Report 49 Blends and Alloys of Engineering Thermoplastics,

H.T. van de Grampel, General Electric Plastics BV.

Report 50 Automotive Applications of Polymers II,A.N.A. Elliott, Consultant.

Report 51 Biomedical Applications of Polymers, C.G. Gebelein,Youngstown State University / Florida Atlantic University.

Report 52 Polymer Supported Chemical Reactions, P. Hodge,University of Manchester.

Report 53 Weathering of Polymers, S.M. Halliwell, BuildingResearch Establishment.

Report 54 Health and Safety in the Rubber Industry, A.R. Nutt,Arnold Nutt & Co. and J. Wade.

Report 55 Computer Modelling of Polymer Processing,E. Andreassen, Å. Larsen and E.L. Hinrichsen, Senter forIndustriforskning, Norway.

Report 56 Plastics in High Temperature Applications,J. Maxwell, Consultant.

Report 57 Joining of Plastics, K.W. Allen, City University.

Report 58 Physical Testing of Rubber, R.P. Brown, RapraTechnology Ltd.

Report 59 Polyimides - Materials, Processing and Applications,A.J. Kirby, Du Pont (U.K.) Ltd.

Report 60 Physical Testing of Thermoplastics, S.W. Hawley,Rapra Technology Ltd.

Volume 6Report 61 Food Contact Polymeric Materials, J.A. Sidwell,

Rapra Technology Ltd.

Report 62 Coextrusion, D. Djordjevic, Klöckner ER-WE-PA GmbH.

Report 63 Conductive Polymers II, R.H. Friend, University ofCambridge, Cavendish Laboratory.

Report 64 Designing with Plastics, P.R. Lewis, The Open University.

Report 65 Decorating and Coating of Plastics, P.J. Robinson,International Automotive Design.

Report 66 Reinforced Thermoplastics - Composition, Processingand Applications, P.G. Kelleher, New Jersey PolymerExtension Center at Stevens Institute of Technology.

Report 67 Plastics in Thermal and Acoustic Building Insulation,V.L. Kefford, MRM Engineering Consultancy.

Report 68 Cure Assessment by Physical and ChemicalTechniques, B.G. Willoughby, Rapra Technology Ltd.

Report 69 Toxicity of Plastics and Rubber in Fire, P.J. Fardell,Building Research Establishment, Fire Research Station.

Report 70 Acrylonitrile-Butadiene-Styrene Polymers,M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. Englandand D.N. Schissel, General Electric Corporate Researchand Development Center.

Report 71 Rotational Moulding, R.J. Crawford, The Queen’sUniversity of Belfast.

Report 72 Advances in Injection Moulding, C.A. Maier,Econology Ltd.

Volume 7

Report 73 Reactive Processing of Polymers, M.W.R. Brown,P.D. Coates and A.F. Johnson, IRC in Polymer Scienceand Technology, University of Bradford.

Report 74 Speciality Rubbers, J.A. Brydson.

Report 75 Plastics and the Environment, I. Boustead, BousteadConsulting Ltd.

Report 76 Polymeric Precursors for Ceramic Materials,R.C.P. Cubbon.

Report 77 Advances in Tyre Mechanics, R.A. Ridha, M. Theves,Goodyear Technical Center.

Report 78 PVC - Compounds, Processing and Applications,J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd.

Report 79 Rubber Compounding Ingredients - Need, Theoryand Innovation, Part I: Vulcanising Systems,Antidegradants and Particulate Fillers for GeneralPurpose Rubbers, C. Hepburn, University of Ulster.

Report 80 Anti-Corrosion Polymers: PEEK, PEKK and OtherPolyaryls, G. Pritchard, Kingston University.

Report 81 Thermoplastic Elastomers - Properties and Applications,J.A. Brydson.

Report 82 Advances in Blow Moulding Process Optimization,Andres Garcia-Rejon,Industrial Materials Institute,National Research Council Canada.

Report 83 Molecular Weight Characterisation of SyntheticPolymers, S.R. Holding and E. Meehan, RapraTechnology Ltd. and Polymer Laboratories Ltd.

Report 84 Rheology and its Role in Plastics Processing,P. Prentice, The Nottingham Trent University.

Volume 8

Report 85 Ring Opening Polymerisation, N. Spassky, UniversitéPierre et Marie Curie.

Report 86 High Performance Engineering Plastics,D.J. Kemmish, Victrex Ltd.

Report 87 Rubber to Metal Bonding, B.G. Crowther, RapraTechnology Ltd.

Report 88 Plasticisers - Selection, Applications and Implications,A.S. Wilson.

Report 89 Polymer Membranes - Materials, Structures andSeparation Performance, T. deV. Naylor, The SmartChemical Company.

Report 90 Rubber Mixing, P.R. Wood.

Report 91 Recent Developments in Epoxy Resins, I. Hamerton,University of Surrey.

Report 92 Continuous Vulcanisation of Elastomer Profiles,A. Hill, Meteor Gummiwerke.

Report 93 Advances in Thermoforming, J.L. Throne, SherwoodTechnologies Inc.

Report 94 Compressive Behaviour of Composites,C. Soutis, Imperial College of Science, Technologyand Medicine.

Report 95 Thermal Analysis of Polymers, M. P. Sepe, Dickten &Masch Manufacturing Co.

Report 96 Polymeric Seals and Sealing Technology, J.A. Hickman,St Clair (Polymers) Ltd.

Volume 9

Report 97 Rubber Compounding Ingredients - Need, Theoryand Innovation, Part II: Processing, Bonding, FireRetardants, C. Hepburn, University of Ulster.

Report 98 Advances in Biodegradable Polymers, G.F. Moore &S.M. Saunders, Rapra Technology Ltd.

Report 99 Recycling of Rubber, H.J. Manuel and W. Dierkes,Vredestein Rubber Recycling B.V.

Report 100 Photoinitiated Polymerisation - Theory andApplications, J.P. Fouassier, Ecole Nationale Supérieurede Chimie, Mulhouse.

Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. FullerCompany.

Report 102 Plastics in Pressure Pipes, T. Stafford, RapraTechnology Ltd.

Report 103 Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.

Report 104 Plastics Profile Extrusion, R.J. Kent, TangramTechnology Ltd.

Report 105 Rubber Extrusion Theory and Development,B.G. Crowther.

Report 106 Properties and Applications of ElastomericPolysulfides, T.C.P. Lee, Oxford Brookes University.

Report 107 High Performance Polymer Fibres, P.R. Lewis,The Open University.

Report 108 Chemical Characterisation of Polyurethanes,M.J. Forrest, Rapra Technology Ltd.

Volume 10

Report 109 Rubber Injection Moulding - A Practical Guide,J.A. Lindsay.

Report 110 Long-Term and Accelerated Ageing Tests on Rubbers,R.P. Brown, M.J. Forrest and G. Soulagnet,Rapra Technology Ltd.

Report 111 Polymer Product Failure, P.R. Lewis,The Open University.

Report 112 Polystyrene - Synthesis, Production and Applications,J.R. Wünsch, BASF AG.

Report 113 Rubber-Modified Thermoplastics, H. Keskkula,University of Texas at Austin.

Report 114 Developments in Polyacetylene - Nanopolyacetylene,V.M. Kobryanskii, Russian Academy of Sciences.

Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky,University of Hamburg.

Report 116 Compounding in Co-rotating Twin-Screw Extruders,Y. Wang, Tunghai University.

Report 117 Rapid Prototyping, Tooling and Manufacturing,R.J.M. Hague and P.E. Reeves, Edward MackenzieConsulting.

Report 118 Liquid Crystal Polymers - Synthesis, Properties andApplications, D. Coates, CRL Ltd.

Report 119 Rubbers in Contact with Food, M.J. Forrest andJ.A. Sidwell, Rapra Technology Ltd.

Report 120 Electronics Applications of Polymers II, M.T. Goosey,Shipley Ronal.

Volume 11

Report 121 Polyamides as Engineering Thermoplastic Materials,I.B. Page, BIP Ltd.

Report 122 Flexible Packaging - Adhesives, Coatings andProcesses, T.E. Rolando, H.B. Fuller Company.

Report 123 Polymer Blends, L.A. Utracki, National ResearchCouncil Canada.

Report 124 Sorting of Waste Plastics for Recycling, R.D. Pascoe,University of Exeter.

Report 125 Structural Studies of Polymers by Solution NMR,H.N. Cheng, Hercules Incorporated.

Report 126 Composites for Automotive Applications, C.D. Rudd,University of Nottingham.

Report 127 Polymers in Medical Applications, B.J. Lambert andF.-W. Tang, Guidant Corp., and W.J. Rogers, Consultant.

Report 128 Solid State NMR of Polymers, P.A. Mirau,Lucent Technologies.

Report 129 Failure of Polymer Products Due to Photo-oxidation,D.C. Wright.

Report 130 Failure of Polymer Products Due to Chemical Attack,D.C. Wright.

Report 131 Failure of Polymer Products Due to Thermo-oxidation,D.C. Wright.

Report 132 Stabilisers for Polyolefins, C. Kröhnke and F. Werner,Clariant Huningue SA.

Volume 12

Report 133 Advances in Automation for Plastics InjectionMoulding, J. Mallon, Yushin Inc.

Report 134 Infrared and Raman Spectroscopy of Polymers,J.L. Koenig, Case Western Reserve University.

Report 135 Polymers in Sport and Leisure, R.P. Brown.

Report 136 Radiation Curing, R.S. Davidson, DavRad Services.

Report 137 Silicone Elastomers, P. Jerschow, Wacker-Chemie GmbH.

Report 138 Health and Safety in the Rubber Industry, N. Chaiear,Khon Kaen University.

Report 139 Rubber Analysis - Polymers, Compounds andProducts, M.J. Forrest, Rapra Technology Ltd.

Report 140 Tyre Compounding for Improved Performance,M.S. Evans, Kumho European Technical Centre.

Report 141 Particulate Fillers for Polymers, Professor R.N.Rothon, Rothon Consultants and ManchesterMetropolitan University.

Report 142 Blowing Agents for Polyurethane Foams, S.N. Singh,Huntsman Polyurethanes.

Report 143 Adhesion and Bonding to Polyolefins, D.M. Brewisand I. Mathieson, Institute of Surface Science &Technology, Loughborough University.

Report 144 Rubber Curing Systems, R.N. Datta, Flexsys BV.

Volume 13

Report 145 Multi-Material Injection Moulding, V. Goodship andJ.C. Love, The University of Warwick.

Report 146 In-Mould Decoration of Plastics, J.C. Love andV. Goodship, The University of Warwick

Report 147 Rubber Product Failure, Roger P. Brown

Report 148 Plastics Waste – Feedstock Recycling, ChemicalRecycling and Incineration, A. Tukker, TNO


ISBN 1-85957-333-9

Martin J. Forrest

(Rapra Technology Limited)


1

Contents

1. Introduction .............................................................................................................................................. 3

2. Analytical Techniques ............................................................................................................................. 3

2.1 Wet Chemistry Techniques ............................................................................................................. 3

2.2 Spectroscopic Techniques ............................................................................................................... 4

2.2.1 Infrared Spectroscopy (IR) ................................................................................................. 42.2.2 Ultraviolet Light Spectroscopy (UV) ................................................................................. 42.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) ......................................................... 42.2.4 Atomic Absorption Spectroscopy (AAS) ........................................................................... 42.2.5 X-Ray Fluorescence Spectroscopy (XRF) ......................................................................... 52.2.6 Raman Spectroscopy .......................................................................................................... 5

2.3 Chromatographic Techniques ......................................................................................................... 5

2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) ......................................................... 52.3.2 Gas Chromatography (GC) ................................................................................................ 62.3.3 High Performance Liquid Chromatography (HPLC) ......................................................... 62.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) ..................................................... 62.3.5 Gel Permeation Chromatography (GPC) ........................................................................... 62.3.6 Thin Layer Chromatography (TLC) ................................................................................... 7

2.4 Thermal Techniques ........................................................................................................................ 7

2.4.1 Differential Scanning Calorimetry (DSC) ......................................................................... 72.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) ........................................................... 82.4.3 Thermogravimetric Analysis (TGA) .................................................................................. 9

2.5 Elemental Techniques ................................................................................................................... 12

2.6 Microscopy Techniques ................................................................................................................ 12

2.7 Miscellaneous Techniques ............................................................................................................ 12

3. Determination of Molecular Weight and Microstructure of Plastic Polymers ................................ 12

3.1 Determination of Molecular Weight ............................................................................................. 12

3.1.1 Gel Permeation Chromatography (GPC) ......................................................................... 133.1.2 Viscosity ........................................................................................................................... 143.1.3 Osmometry ....................................................................................................................... 143.1.4 Light Scattering ................................................................................................................ 143.1.5 Other Methods .................................................................................................................. 15

3.2 Monomer Types and Microstructure ............................................................................................ 15

4. Determination of Polymer Type ........................................................................................................... 15

5. Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19

5.1 Determination of Plasticiser ......................................................................................................... 19

5.2 Determination of Fillers ................................................................................................................ 19

5.2.1 Particulate Fillers .............................................................................................................. 195.2.2 Fibrous Fillers ................................................................................................................... 20

6. Determination of Stabilisers in a Plastics Compound ....................................................................... 21

6.1 UV Stabilisers ............................................................................................................................... 21

6.2 Antioxidants .................................................................................................................................. 22


2

The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those ofRapra Technology Limited or the editor. The series is published on the basis that no responsibility orliability of any nature shall attach to Rapra Technology Limited arising out of or in connection with anyutilisation in any form of any material contained therein.

7. Determination of Functional Additives ............................................................................................... 24

7.1 Process Aids and Lubricants ......................................................................................................... 24

7.2 Slip Additives ................................................................................................................................ 25

7.3 Pigments ........................................................................................................................................ 25

7.4 Antistatic Agents ........................................................................................................................... 25

7.5 Crosslinking Agents and Co-Agents............................................................................................. 26

7.6 Blowing Agents ............................................................................................................................. 27

7.7 Flame Retardants .......................................................................................................................... 28

7.8 Impact Modifiers ........................................................................................................................... 28

8. Analysis of Plastics for Food Contact Use ........................................................................................... 28

8.1 Global Migration Tests ................................................................................................................. 29

8.2 Specific migration and residual monomer tests............................................................................ 30

9. Determination of Stabilisers in PVC ................................................................................................... 31

10. Analysis of Plastic Laminates and Fibres ............................................................................................ 32

11. Surface Analysis of Plastics ................................................................................................................... 34

11.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................................................... 34

11.2 Laser Induced Mass Analysis (LIMA) ......................................................................................... 34

11.3 Secondary Ion Mass Spectroscopy (SIMS) .................................................................................. 36

12. Failure Diagnosis ................................................................................................................................... 36

12.1 Common Compositional Problems ............................................................................................... 36

12.2 Environmental Stress Cracking .................................................................................................... 37

12.3 Contamination Problems .............................................................................................................. 37

12.4 Odour and Emissions Problems .................................................................................................... 37

13. Conclusions ............................................................................................................................................. 38

Additional References ................................................................................................................................... 39

Appendix 1. Solubility Parameters of Plastics, Plasticisers and Typical Solvents .................................. 41

Appendix 2. Specific Gravities of Plastics and Compound Ingredients .................................................. 43

Abbreviations and Acronyms ....................................................................................................................... 45

Abstracts from the Polymer Library Database .......................................................................................... 47

Subject Index ............................................................................................................................................... 133


3

1 Introduction

Plastics present chemical analysts with one of their mostdifficult, but satisfying, challenges. In order to obtainuseful products that perform under a variety ofdemanding conditions, the plastic matrix can be tailormade by the bringing together of a wide range ofpolymers and additives. There is a very wide range ofpolymer types available and in some cases they areblended together. The technology of plastics is thereforea mature one, allowing fine tuning of a compound to fita number of design criteria and product requirements.

The choice of materials available means that plasticscan be used in many applications, ranging fromreplacement windows to packaging materials, andfrom mundane products such as disposable cutlery tohighly specialised components in electrical andaerospace products.

The plastics analyst has therefore to bear in mind thepossible complexity of the system that confronts himand the potential interferences that may be broughtinto play. When reverse engineering a plasticcompound a considerable number of elemental,spectroscopic, chromatographic and thermaltechniques have to be used in an integrated andstructured approach in order to accumulate and crosscheck the data necessary for an accurate result. Withsufficient experience and access to the necessaryinstrumental techniques, it should be possible for theanalyst to successfully elucidate a formulation. Thedetermination of the particular ‘grade’ of plastic,although a consistent request, is however rarelypossible. This is mainly due to the fact that a numberof manufacturers produce very similar, if not identical,products or that the material has been speciallycompounded for a particular purpose. Commercialconfidentiality can also restrict the ability to use theanalytical data to identify a particular manufacturer’sproduct as a significant amount of compositionalinformation may not be disclosed.

The objective of this review is to present, as fully as ispossible within this format, an introduction to thetechniques and methods that are used to characteriseand carry out quality control work on plastics; toinvestigate the failure of plastic products; and todeformulate plastic compounds.

With respect to the last category, the analyst’s job whencharacterising ‘unknowns’ is always made much easierif at least some information is available on the sampleand the types of species that may be present in it. Armedwith this knowledge they can work much more

efficiently and obtain better results. To assist in theacquisition of this knowledge opportunities have beentaken within the text to not only detail the analyticalmethods, but provide examples of the species that theymay be used to detect and quantify. In other words, inorder to have a full understanding of the principlesbehind and surrounding the analytical methods andapproaches it is vital to have an understanding of plastictechnology itself.

Relevant books and academic papers are citedthroughout the review, but there are also a number ofgeneral texts which will provide useful further reading(79, 199, 315, 377, 387, 398, a.1-a7).

The appendices provide useful additional information.Appendix 1 gives solubility parameters of a range ofmaterials. Appendix 2 lists the specific gravities of arange of plastics and compounding ingredients.

2 Analytical Techniques

2.1 Wet Chemistry Techniques

Before the advent of modern instrumental techniques,plastic analysis relied on a sequence of wet chemistryreactions to determine information such as the genericpolymer type of a material.

The amount of wet chemistry carried out in the modernpolymer analysis laboratory in the 21st Century isminimal. There are some tests which can still begrouped under this heading, although even some ofthese can employ an instrumental technique to providethe final answer.

One such method is the oxygen flask combustionmethod, which can be used on PVC products todetermine the amount of PVC in the formulation byquantifying the chlorine present.

The oxygen flask method (ISO 6528.1-1992 and BS7164 Section 23.1- 1993) uses an initial burn in oxygen(although the sample is trapped between two platinumgauge ‘flags’) and trapping of the volatile products inan absorbing solution comprising 1-5 ml of 0.05Mpotassium hydroxide, 0.2 ml of 30% hydrogen peroxideand 10 ml of distilled water. Once the volatiles havebeen trapped there is a choice of analytical method. Atitration can be performed, or ion chromatography canbe used to quantify the chloride ion.


4

2.2 Spectroscopic Techniques

2.2.1 Infrared Spectroscopy (IR)

Infrared spectroscopy (IR) is used extensively in theanalysis of plastics. It is a very good, relatively quicktechnique for the determination of the polymer presentin a plastic product. Unlike rubbers, where the majorityof compounds contain additives such as carbon blackand plasticisers that can interfere with the infrared dataobtained, it is normally possible to record infrared spectradirectly from the plastic sample using either a surfacetechnique (e.g., attenuated total reflectance (ATR)spectroscopy) or in transmission through the samplefrom a film produced by pressing a specimen above itsglass transition or melting point.

Some plasticised plastics products (e.g., PVC or nylon11) will need to be extracted with a solvent (e.g.,methanol) first to remove the plasticiser. Products thatare filled (e.g., polypropylene/talc kettle bodies) willrequire a pyrolysis technique where a pyrolysiscondensates infrared library, such as the one publishedby Rapra Technology, needs to be available.

It is also possible with amorphous plastics that are solublein conventional solvents (e.g., chloroform) at roomtemperature to record infrared spectra from films castfrom solution. This approach has the drawback that allthe solvent needs to be removed from the film ifinterference bands are to be avoided.

Analysis of the solvent extract obtained to prepare theplastic sample for an IR technique can be used to identifythe plasticiser present in a compound. IR analysis of anash of the compound obtained by heating at 550 °C canhelp to identify inorganic fillers. IR can also be used toidentify specialist additives such as fire retardants.

2.2.2 Ultraviolet Light Spectroscopy (UV)

Although not as universally used as IR, UV is anotherspectroscopic technique which has a role to play in the

analysis of plastics. It is used in the qualitative andquantitative analysis of additives, particularlyantioxidants and UV stabilisers.

2.2.3 Nuclear Magnetic Resonance Spectroscopy(NMR)

NMR is a powerful tool for the determination ofpolymer structure. It is at its most sensitive when usedon analytes in solution. Table 1 gives examples ofsolvents used for NMR. Amorphous plastics, such aspolystyrene can be dissolved in deuterated chloroform,whereas for the less soluble semi-crystalline plastics(e.g., PET) solvents such as trichloroacetic acid haveto be used. Of the conventional instruments, both protonand carbon 13 instruments have been used in plasticsanalysis. Combinations of two solvents can be used toachieve a good degree of solubility and elevatedtemperatures (e.g., 70 °C) are also common. The protonNMR solvents can be used for carbon 13 experiments,but the reverse is rarely the case.

Techniques are available for work on a specific plastictype, e.g., in the analysis of polyvinylidene fluoride,fluorine 19 NMR can be used. In this case a solventsuch as dimethylformamide is employed.

The 13C NMR spectrum for a polypropylene-polyethylene copolymer is shown in Figure 1. Thespectrum was obtained at 90 °C in a solution of ortho-dichlorobenzene. The major peaks at 21, 27 and 46ppm are due to the polypropylene, with the other, minorpeaks being due to polyethylene.

2.2.4 Atomic Absorption Spectroscopy (AAS)

This technique, and the related inductively coupledplasma (ICP), are used where it is necessary to quantifymetals in a plastic compound. Although not oftenrequired it can be of use in the analysis of flameretardant systems, where additives such as antimonytrioxide and zinc borate have been used.

scitsalpnokrowRMNnidesustnevlosfoselpmaxE1elbaT

RMNnotorP RMN31nobraC

mroforolhcdetaretueD ohtrO enezneborolhcid

dicacitecaoroulfirT enezneborolhcirT

eneznebdetaretueD enatpeh,.g.e,snobracordyhcitahpilA

enahtedetaretued-orolhcarteT-2,2,1,1


5

2.2.5 X-Ray Fluorescence Spectroscopy (XRF)

This technique is very useful for obtaining semi-quantitative elemental data from plastic compounds andtheir ashes. Among other things, it helps to identifyinorganic fillers and pigments in samples. Thetechnique is usually used in conjunction with IR.

When it comes to analysing small samples, samplesurfaces or contaminants in samples, the scanningelectron microscope (SEM)/XRF combination(sometimes referred to as energy dispersive analysis(Edax)) can be a very valuable tool.

2.2.6 Raman Spectroscopy

Until 1986 Raman spectrometers were either dispersivelong focal length double monochromators or shorterfocal length triple monochromators and required highlytrained scientists to obtain good quality data. The adventof the Fourier Transform (FT)-Raman technique in 1986significantly reduced data acquisition times and alsobrought the technical advantage of suppressing any laserinduced fluorescence within the sample. Furtherdevelopments have enabled smaller, low cost, highperformance, quality instruments to be produced and

have led to the development of the Raman microscope -an instrument analogous to the IR microscope.

This has enabled Raman spectroscopy to be usedroutinely for the identification of polymer types andthe analysis of contaminants within polymer samples.

2.3 Chromatographic Techniques

2.3.1 Gas Chromatography-Mass Spectrometry(GC-MS)

This powerful, versatile technique can be used toobtain a significant amount of compositionalinformation on plastic samples. It is particularly usefulin identifying minor components of the sample suchas the stabiliser, antistatic agent and, whereappropriate, the crosslinking system.

It can also be used to investigate the polymer fractionwithin a sample when the instrument is fitted with apyrolysis unit set at around 600 °C.

The technique also plays a role in failure diagnosis bybeing able to provide information on odours, and

Figure 113C NMR spectrum of polypropylene-polyethylene copolymer


6

organic contaminants that may have degraded theplastic matrix.

There are a variety of ways that the sample or fractionsof the sample (e.g., an extract) can be analysed by GC-MS. These include static headspace, dynamicheadspace, solution injection and pyrolysis.

2.3.2 Gas Chromatography (GC)

This technique can also be used to obtain polymer typeinformation by use of a pyrolysis approach, althoughthe technique is less powerful because of the absenceof a mass spectrometer, and a pyrogram ‘fingerprint’has to be used and a comparison made against a libraryof known standards.

This technique is also used for the identification andquantification of additives such as antioxidants and,where sufficient volatility exists, plasticisers andorganic flame retardants.

2.3.3 High Performance Liquid Chromatography(HPLC)

HPLC can be used to identify and quantify additivesthat are either too involatile or insufficiently stable tobe determined by GC/GC-MS. This is particularly thecase with antioxidants such as Irganox 1010 and 1036.

HPLC also comes into its own in the quantification ofplasticisers such as dioctyl phthalate (DOP).

2.3.4 Liquid Chromatography-Mass Spectroscopy(LC-MS)

This instrument is essentially a coupling of an HPLCwith a mass selective detector and as such offers asignificant enhancement in performance to the polymerchemist. Although such combinations have been aroundfor many years, they were complex and expensive (i.e.,effectively research tools only), and it is only withinthe last five years or so that single quadrupole benchtopLC-MS systems have become reasonably commonplace due to their relative ease of use and cost.

A mass spectrometer can be the ideal detector forliquid chromatography because it offers bothuniversality and the required selectivity for complexanalytical problems. For many years developmentwork has concentrated particular on the design of

the interface between the chromatograph and thedetector. Today, the two most popular types ofinterface for the benchtop single quadrupole LC-MSare the particle beam interface and the atmosphericpressure ionisation (API) interface. The particlebeam interface is used to generate electron ionisation(EI) spectra and the API interface is used to generateeither electrospray (ESI) or atmospheric pressurechemical ionisation (APCI) spectra. A furthercomplexity is that the API interface can generateeither positive (i .e. , molecular ion plus onehydrogen) spectra or negative (i.e., molecular ionminus one hydrogen) spectra.

The particle beam interface is very good forqualitative work because the 70 eV spectra containa significant amount of structural information andcan be searched against conventional mass spectralibraries. However, in the full scan mode thesensitivity is restricted to the low nanogram levels.

In the case of the API interface, both the electrosprayand APCI modes are soft ionisation techniques whichleave the molecular ion (or pseudomolecular ion)intact without much fragmentation. The interfacetherefore offers more sensitivity and is ideal forquantitative work at low levels (e.g., contaminationof drug and food matrices by polymer additives/breakdown products).

2.3.5 Gel Permeation Chromatography (GPC)

For this technique to be successful the sample mustbe readily soluble in an organic solvent. It has a wideapplication in the analysis of plastic samples. It ispossible to obtain molecular weight data on bothamorphous plastics and semi-crystalline plastics. Inthe amorphous case (e.g., polystyrene), the systemused is set around ambient temperature (30 °C) andsolvents such as THF, chloroform and toluene areused. With semi-crystalline plastics (e.g.,polyolefins), more aggressive solvents such as ortho-dichlorobenzene and meta-cresol are used at elevated(140 °C) temperatures.

In the case of some complex plastic systems (e.g.,blends), the development of interfaces such as theLab Connections LC Transform, have proved veryuseful in increasing the amount of information thatcan be obtained in a GPC analysis by enabling IRdata to be recorded on the resultant chromatogram.Hence, with the correct choice of separating column,polymer blends can be separated and identified aswell as plasticisers.


7

2.3.6 Thin Layer Chromatography (TLC)

TLC is a relatively simple technique that can be usedfor both the separation and identification of additivessuch as antioxidants and UV stabilisers. A number ofapproaches are possible using different developingsolvents and spraying agents.

It is also the case that TLC can be used in a preparativeway for the isolation of sample fractions for subsequentchromatographic or spectroscopic analysis.

TLC does have the image of being somewhat oldfashioned and it is to be expected that the marketpenetration of LC-MS systems will further erode thestanding of this technique in the modern analyticallaboratory.

2.4 Thermal Techniques

2.4.1 Differential Scanning Calorimetry (DSC)

DSC is used extensively in the analysis of plastics,particularly those that are semi-crystalline - polyolefins,nylons, polyesters, etc. It is sensitive enough to

differentiate between different polyethylenes (i.e.,LDPE, LLDPE, HDPE, etc.) from their melting pointsand the appearance of their melting endotherms as wellas being able to detect and, with appropriate standardmaterials, quantify plastic blends, e.g., PP/PE and nylon6/nylon 6,6.

The DSC trace for a quenched sample of PET is shownin Figure 2. This trace shows the Tg (around 75 °C) ofthe material, the exothermic formation of the crystallinephase (at 156.9 °C) and the endotherm due to themelting of this phase (at 255 °C).

The DSC trace of a plastic blend is shown in Figure 3.The data obtained has been compared to standards andthe material has been shown to be a blend of ethylene-vinyl acetate copolymer (EVA) and LDPE. Theapproximate proportions of each is EVA 15-20%/LDPE20-25%. In addition the EVA copolymer is thought tocontain around 20-25% of vinyl acetate (VA).

Although not as sensitive as dynamic mechanicalthermal analysis (DMTA) to glass transitions, DSC canbe used to identify a plastic from the glass transition inits thermogram. The glass transition (Tg) and crystallinemelting temperatures (Tm) of a range of plastics aregiven in Table 2.

Figure 2

DSC trace for a quenched sample of PET


8

Figure 3

DSC trace of a blend of EVA and LDPE

It is also possible to use DSC to provide quality controlfingerprint thermograms from which deviations in thecomposition of a plastic compound can be detected.One reason for this is that although the technique isnot capable of determining the molecular weight of aplastic, differences in molecular weight will be apparentin the melting endotherm region.

Using appropriate standard materials it is alsopossible to use DSC to quantify the level of certainadditives, e.g., peroxides, in a sample.

DSC can also be used in thermal stability studies ofthe plastic compound, and to investigate theeffectiveness of antidegradants and fire retardants.

2.4.2 Dynamic Mechnanical Thermal Analysis(DMTA)

DMTA is very useful for generating modulus versustemperature data on plastic compounds. The effects

of temperature on this important material property canbe obtained over a wide temperature range (typically–150 °C to +200 °C), along with the glass transitiontemperature and information on thermal stability.

The use of DMTA to differentiate between plasticsamples that have a similar chemical composition, butvery different physical properties is shown inFigure 4. Both of these samples are polymethyl-methacrylate (PMMA), but the top one is crosslinkedhaving been prepared with a small amount ofdifunctional monomer and the bottom sample is thestandard thermoplastic material. It can be seen thatthe crosslinked sample does not melt and the modulusdoes not fall away significantly until thermaldegradation occurs.

The sensitivity of DMTA to glass transitiontemperatures (approximately 1,000 times greater thanDSC which measures heat capacity changes rather thanmodulus) is very useful in the analysis of plastics andtheir blends.


9

2.4.3 Thermogravimetric Analysis (TGA)

This technique is useful in the analysis of compoundedplastic samples. It is possible to obtain accuratequantifications of the principal compound constituentssuch as plasticiser, polymer and inorganic species.This data can be obtained on small (e.g., 10 mg)samples in a relatively short time (around 45 minutes).By the use of the temperature maxima at which weightevents occur it is also possible to use the technique toobtain some qualitative assignments for the plasticiserand polymer.

A typical TGA programme would be:

Heat from ambient to 550 °C in a nitrogen atmosphereat 20 °C/min until no further weight loss occurs. Then,reduce the heat to 300 °C, change the atmosphere toair and heat at 20 °C/min to 1,000 °C.

It is common to plot the weight loss derivative inconjunction with the weight loss, and this can be usedto detect the presence of a polymer blend of two or morecomponents. Thermal decomposition temperatures of arange of plastics are shown in Table 3.

T(noitisnartssalG2elbaT g T(serutarepmetgnitlemenillatsyrcdna) m scitsalpfoegnarafo)

epyTscitsalP Tg (° )C Tm (° )C

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)EPDL(501

)EPDM(511

)EPDH(531

enelyporpyloP 5 061

ene-1-tubyloP 02– 021

ene-1-tnepyloP 42 07

EFTP 511 723

)EFTCP(enelyhteoroulfirtorolhcyloP 25 122

lohoclalynivyloP 07 TwolebsesopmoceD g

edirolhclynivyloP 08 -

edirolhcenedilynivyloP 81– 091

elirtinolyrcayloP 041ot08 -

enerytsylopcitcatA 59 -

enerytsylopcitcatosI 001 032

TEP 76 652

etalyrcahtemlyhteM 001 -

AlonehpsibfoetanobracyloP 051 522

AlonehpsibfoenoflusyloP 591 -

6nolyN 05 512

6,6nolyN 06 662

edixoenelyhteyloP 55– 66

edixoenelyporpyloP 26– 56

rehtelyhtemlynivyloP 13– 441

rehtelyhtelynivyloP - 68

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10

Figure 4

DMTA results for (a) crosslinked and (b) standard grades of PMMA


11

Other uses for the technique include the production ofcompositional fingerprints for quality control purposesand the investigation of thermal stability and the effectsthat additives such as flame retardants and antioxidantshave on it.

It is possible to interface modern TGA instruments directlyto IR instruments or mass spectrometers, thus obtainingboth quantitative and qualitative data in one analytical step.

The introduction of high resolution TGA instrumentshas enabled more accurate quantifications of minorweight loss events to be made. For example, the use ofhigh resolution TGA to quantify the amount of residualmonomer in a sample of polymethylmethacrylate isshown in Figure 5. The residual monomer weight lossevent peaks at 297.5 °C.

scitsalpfoegnarafoserutarepmetnoitisopmocedlamrehT3elbaT

epyTcitsalP (*noitisopmoced%05eveihcaoterutarepmeT ° )C

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Figure 5

High resolution TGA of polymethylmethacrylate


12

2.5 Elemental Techniques

The determination of the concentration of certainelements can be very useful in plastic analysis work.In particular, it is often necessary to determine theamount of nitrogen or a halogen such as chlorine orfluorine in the calculation of polymer content orpolymer blend proportions. Also, the targeting ofspecific elements can enable the quantity of aparticular additive (e.g., phosphate flame retardant ortitanium dioxide pigment) to be calculated.

The determination of nitrogen is usually done usingcarbon/hydrogen/nitrogen analysers and the techniqueis relatively simple and uses small amounts (e.g., 20-50 mg) of sample.

With the other elements, the technique will varyaccording to the element being quantified. Sulfur andchlorine, for example, can be determined usingoxygen combustion followed by ion chromatographyanalysis of the products.

2.6 Microscopy Techniques

High magnification (e.g., 150x) optical microscopycan be used to examine the dispersion of fillers withinthe plastic matrix. The success of this operation isusually dependent on the generation of high qualitymicrotome sections of the sample.

The technique of scanning electron microscopy hasalready been briefly mentioned in Section 2.2.5 inrelation to the elemental analysis of surfaces inconjunction with XRF. It can also be used in its ownright, where its high magnification powers can beemployed to determine the particle size of fillers andin the detailed examination of fracture surfaces.

Transmission electron microscopy (TEM) can be usedto investigate the phase morphology of polymerblends and the dispersion of fillers.

For other spectroscopic techniques see Section 2.2.

2.7 Miscellaneous Techniques

There are a number of other analytical techniques thatcan be used to characterise plastic samples and manyof these feature in the abstracts at the back of thisReview Report. These include X-ray diffraction(XRD) to identify between different crystalline forms

of inorganic additives (e.g., rutile and anatase formsof titanium dioxide) and direct probe massspectroscopy (for the determination of high molecularweight antioxidants).

Surface analysis techniques such as secondary ion massspectrometry (SIMS), laser induced mass analysis(LIMA) and X-ray photoelectron spectroscopy (XPS)are used for failure diagnosis work associated with suchthings as poor bonding to substrates and for surfacecharacterisation work.

A chromatography technique that achieved prominencein the research literature around ten to fifteen yearsago for the determination of relative high molecularweight additives (e.g., antioxidants) and the study ofplastic oligomers is supercritical fluid chromatography(SFC). This is essentially a liquid chromatographytechnique that uses similar analytical columns to HPLCbut where the mobile phase is a substance (e.g., carbondioxide) that is kept in a supercritical state by a suitablecombination of temperature and pressure. One of thebenefits of the technique is that the analytes can beeasily separated from the mobile phase once thechromatography has taken place so, for example, theycan be deposited on infrared transparent substrates foranalysis using an infrared microscope. The relativelyexpensive nature of the instrumentation and thedevelopment of other techniques (e.g., LC-MS) haverestricted its market penetration.

3 Determination of Molecular Weightand Microstructure of Plastic

Polymers

This section covers analytical techniques that can beapplied both to uncompounded plastic resins andcompounded materials.

3.1 Determination of Molecular Weight

In common with other polymers, plastics have adistribution of molecular weights. This distribution willbe widest for polymers produced by free radicalpolymerisation (e.g., polystyrene) and narrowest forplastics produced using specialised catalyst systemssuch as metallocenes.

There are a number of ways in which the molecularweight distribution of a plastic can be expressed:


13

Mn = Number average molecular weight = Sum nMSum n

Mw = Weight average molecular weight = Sum nM2Sum nM

Mz = Z average molecular weight = Sum nM3Sum nM2

where n = the number of molecules of molar mass M.

The Z average is very sensitive to high molecularweight molecules within the polymer. The weightaverage is always of greater value than the numberaverage. A measure of the breadth of the moleculardistribution of the polymer can be obtained by dividingthe weight average by the number average:

Polydispersity = MwMn

As the polymer tends to monodispersity thepolydispersity approaches unity.

There are a wide variety of methods that can be usedto obtain molecular weights. The principal ones areas follows.

3.1.1 Gel Permeation Chromatography (GPC)

This is the pre-eminent technique and has been refinedand developed extensively over the past 30 years.

It is possible to use it on both uncompounded resinsand plastic compounds and Mn, Mw and Mz valuescan be obtained. GPC is essentially a liquidchromatography technique where the sample isdissolved in a suitable solvent (e.g., THF forpolystyrene) and injected into a system where themolecules are separated according to their molecularsize by a column that contains a swollen, particulate,porous gel packing.

Figure 6 shows the GPC chromatograms for twopolymers that have different molecular weightdistributions but similar calculated molecular weightaverages.

The standard detector for GPC systems is the refractiveindex (RI) detector, but a feature of developments overthe past 10 years is the development of double (RI andviscosity) or triple detector systems (RI, viscosity andlight scattering). These multiple detection systemsprovide measures of ‘true’ molecular weight byobtaining the actual Mark-Houwink parameters (in thecase of the viscosity detector) for the polymer being

Figure 6

GPC chromatograms for two polymers with different molecular weight distributions but similarmolecular weight averages


14

analysed, as opposed to the polystyrene equivalentmolecular weight from the use of monodispersepolystyrene calibrants alone. An inherent property ofthe light scattering detector is that it provides ‘true’molecular weight data.

It is also possible to use spectroscopic detectors suchas infrared and ultraviolet. One practical use of thelatter is to determine if chemical modifiers (e.g., silanecoupling agents) are bound to polymer molecules.This is done by measuring the molecular weightdistribution of the modified plastic at a UVwavelength where the polymer itself does notcontribute to the absorbance and comparing this tothe distribution of the unmodified plastic.

The use of the LC transform module with GPC hasextended its capabilities by allowing IR data to begenerated on the species during the course of an analysis.This is done by impinging the species onto a germaniumdisc which is then placed into a module fitted into thesample compartment of an IR bench. IR data is collectedon the entire chromatogram using continuous collectionsoftware, which enables the IR spectrum of any particularsection to be viewed. This technique is very useful forplastic blends and highly compounded plastics such atPVC, as it allows the polymers in the blend to beidentified, as well as relatively high molecular weightadditives such as plasticisers.

3.1.2 Viscosity

This is a standard procedure for molecular weightdeterminations and involves the use of speciallydesigned viscometers to accurately measure theviscosity of a polymer solution. From this the intrinsicviscosity is determined and hence the molecular weight.The time taken for the polymer solution to pass betweentwo marks on the viscometer is compared to that ofpure solvent and the ratio is the viscosity of the solution.Successive dilutions give a range of concentrations andtimes from which the intrinsic viscosity can becalculated. The value for this is then entered into theMark-Houwink equation:

Intrinsic viscosity = KMX

where K and X are constants for the particular solventbeing used and are referred to as the Mark-Houwinkparameters.

Depending on the source of the Mark-Houwinkparameters the molecular weight can be expressed aseither the number or weight average.

3.1.3 Osmometry

There are two principal osmometry techniques: vapourpressure osmometry and membrane osmometry.

Vapour pressure osmometry involves the indirectmeasuring of the lowering of the vapour pressure of asolvent due to the presence of a solute. It is based on themeasurement of the temperature difference betweendroplets of pure solvent and of polymer solutionmaintained in an isothermal atmosphere saturated withthe solvent vapour. Calibration is by the analysis ofstandards of known molecular weight and should be overthe entire range of molecular weights of interest to ensurethe best results. The technique is useful for polymersthat have molecular weights in the 500-50,000 range.

Membrane osmometry involves the use of amembrane between the solvent and the polymersolution that is permeable to the solvent moleculesbut not to the solvated polymer molecules. This isthe major restriction on the technique and means thatit cannot be used for low molecular weight polymers(< approximately 50,000).

3.1.4 Light Scattering

Recent developments in instrumentation have led to aresurgence of this technique where the weight averagemolecular weight is obtained from the light scatteringbehaviour of polymer solutions. These developmentshave centred around low angle laser light scattering(LALLS), multi-angle laser light scattering (MALLS)and evaporative light scattering (ELS). As well as beingstand alone instruments, light scattering detectors havebeen developed for GPC systems. MALLS detectorscan provide direct information on the branching ratioof a polymer (a.8).

Care has to be taken to ensure that the polymer solutionis clear (to reduce variability) and low cell volumes(0.1 μl) and dilute solutions help this. Solvent choiceis also critical, with the best results being with solventsthat have a very different refractive index to thepolymer, and that are low-scattering themselves.

Evaporative light scattering involves the removal ofthe solvent from the solvated polymer as it elutes downa drift tube and the isolated polymer particles thenscatter light from the light source.

Light scattering can produce precise data and has beenused successfully on polymers with molecular weightsranging from 10,000 to 10,000,000.


15

3.1.5 Other Methods

Other methods include end group analysis (Mn),ultracentrifugation (Mw) and, indirectly by determiningglass transition temperatures, DSC/DTA.

A review of the determination of the molecular weightof polymers has been produced by Holding andMeehan (396).

3.2 Monomer Types and Microstructure

The use of transmission IR, pyrolysis IR and pyrolysisGC to determine the polymer type of a plastic is coveredin Section 2.1. Where appropriate standards areavailable, it is also possible to use IR to quantify theamounts of monomers in copolymers and terpolymers.

Another technique that is very effective at identifyingthe monomers present in a plastic materials is NMR.The NMR technique will also provide information onthe proportions of the various monomers in copolymersand tripolymers. In contrast to IR this information canbe obtained without having to analyse standards ofknown monomer composition; the areas under thediagnostic chemical shifts being used.

NMR instruments can also be used to obtainfundamental structural information on polymers suchas end group chemistry, branch points and structuralisomerism. It is also possible to use IR for the latter,although some of the isomeric structures have relativelyweak absorptions which makes detection difficult whenthey are at a low concentration.

4 Determination of Polymer Type

One of the most basic and useful tests to carry out on aplastic sample is to determine its polymer type.

Due to their relative simplicity, it is usually possible tocarry out an infrared analysis of the plastic material inthe as received state and identify the plastic by referenceto a standards database. The advent of the single bounceattenuated total reflectance (ATR) accessories forFourier transform infrared spectroscopy (FTIR)instruments enables this operation to be carried out ina matter of minutes on a sample a few millimetres insize. Some care should be taken as the relativeintensities of the bands present in ATR spectra can vary

compared to conventional transmission spectra(historically used to compile databases) and there is aslight shifting in the absorption wavenumber value ofthe bands.

If more traditional spectra are required, the usualapproach is to press a thin film of the samples using atemperature which is above the Tg or Tm and to recorda transmission spectrum. A transmission infraredspectrum of polypropylene produced from a filmpressed at 170 °C is shown in Figure 7. Anothertechnique that can be used to obtain transmissionspectra is to dissolve the sample up using a suitablesolvent and to cast a film. Care has to be taken toremove all of the solvent by drying in an oven otherwiseit can influence the data obtained. A transmissioninfrared spectrum of PVC produced from a film castfrom a solution in THF is shown in Figure 8.

For those plastic compounds that contain a plasticiserand/or organic flame retardant, a certain amount ofpreparation work is required to effectively remove theinterference of these constituents. After milling orcomminuting the sample to increase surface area, asolvent extraction is performed to remove these organicspecies. It is then usually possible to record the infraredspectrum using either an ATR technique or bytransmission through a hot pressed film.

One of the most comprehensive databases availableof plastic infrared spectra has been produced byHummel (a.9).

Where the plastic sample contains both a major organicadditive and a filler, it is necessary to pyrolyse theextracted portion of the sample and then record aninfrared spectrum of the collected pyrolysiscondensates. Providing that an extensive database ofpyrolysate spectra is available (234), this method isvery successful in identifying generic polymer typesand polymer blends. In the case of blends, it is alsopossible to express the results semi-quantitatively ifthe appropriate standards are available.

If the plastic only contains a filler, the pyrolysisapproach can be employed without using the initialsolvent extraction step.

The pyrolysate infrared spectra of nylon 6 and lowdensity polyethylene are shown in Figures 9 and 10,respectively.

Another method which enables the polymer type withina plastic sample to be identified is pyrolysis gaschromatography. This method can be applied to either


16

Figure 7

Transmission infrared spectrum of polypropylene produced from a film pressed at 170 °C

Figure 8

Transmission infrared spectrum of unplasticised PVC produced from a film cast from a THF solution


17

Figure 9

Pyrolysate infrared spectrum of nylon 6

Figure 10

Pyrolysate infrared spectrum of low density polyethylene


18

the extracted portion of the sample or the sample asreceived. In the former case any relatively low molecularweight plasticiser elutes early on and does not have asignificant influence on the pyrogram as a whole. Aswith pyrolysis IR, a database of standards needs to beput together and then the pyrogram fingerprints ofunknowns can be matched. The temperature that thepyrolysis unit is set at, and the design of the unit (e.g.,Curie point or microfurnace), will affect the pyrogramsproduced from a particular sample. Again, it is possibleto identify and quantify blends and blend ratios.

Typical experimental conditions for pyrolysis GCexperiments are as follows:

Sample weights 0.1-5.0 mg

Pyrolysis temperatures 400-800 °C (microfurnaceand Curie point)

800-1200 °C (platinumfilament)

Microfurnace type pyrolyser - specific example usingan SGE Pyrojector

Weight of sample 0.4 mg

Pyrolysis temperature 600 °C

Pyrolysis gas Helium at 0.10 MPa

GC column 5% Diphenyl siloxane 30m x 0.25 mm, 1.0 μm film

GC column temperature 2 min at 50 °C followedprogram by 10 °C/min to 280 °C

and then 10 min at 280 °C

GC carrier gas Helium at 0.06 MPa

GC injector temperature 320 °C

Detector Flame ionisation detector(FID) at 350 °C

Adding a mass spectrometer into the system, so thatthe technique becomes pyrolysis GC-MS, furtherincreases the usefulness of the method and theinformation that can be obtained.

The principal diagnostic pyrolysis species which canbe detected in pyrograms of plastics are shown inTable 4.

It can be seen from the above list that certain plastics‘unzip’ to regenerate their monomers whereas otherundergo decomposition reactions to generatecharacteristic breakdown products. In reality, acertain amount of both types of reaction take placefor the majority of polymers and it is the one thatpredominates that determines what the majorpyrolysis products will be.

With respect to the quantification of the polymercomponent within a plastic compound, the easiesttechnique to use is TGA. It is also possible to detect ablend of polymers with TGA and to often obtain asemi-quantification of the blend ratio by reference tothe splitting of the weight loss derivative.Unfortunately, some plastic types (e.g., PVC) undergotwo stage weight loss processes when heated and thefirst stage (loss of hydrogen chloride) will overlapwith the volatilisation of organics (e.g., plasticiser)stage. It is therefore not possible to use TGA alone todetermine the polymer content of these samples.

Another complicating factor is that a number of plastics(e.g., halogenated, polyamides, polyurethanes,polyesters, other heteroatom containing systems) donot completely pyrolyse during the nitrogenatmosphere region and leave a carbonaceous residuewhich essentially oxidises to carbon dioxide in the airregion. This carbonaceous residue, which may to anextent overlap with any weight loss due to a carbonblack pigment, has to be included in order to obtain anaccurate polymer content.

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19

5 Determination of the Plasticiser andFiller in a Plastic Compound

5.1 Determination of Plasticiser

Mention has already been made in Section 4 of theisolation of plasticisers from a plastic matrix bysolvent extraction. Careful choice of solvent isrequired to ensure that the polymer itself doesn’tundergo dissolution and that the plasticiser isselectively isolated. A solvent which has been foundto be useful for polymers such as PVC is methanol.The extraction is carried out under Soxhletconditions with the weight of extract being obtainedfrom the weight gain of the conditioned solventreservoir flask once the solvent has been dried offat 105 °C.

Having quantified the plasticiser present byextraction it is then possible to obtain anidentification by the use of transmission IR. Thereis an excellent database available (399) whichenables an identification to be made. Where theplasticisers have distinct IR spectra (e.g., phthalatesand sulfonamides) it is possible to detect thepresence of a blend of plasticisers. If a quantificationof the blend composition is required, though, this isusually easier to achieve by HPLC then IR.

The TGA technique can usually provide a goodquantification of plasticiser content. Plasticisers thathave higher molecular weights (e.g., so calledpolymerised plasticisers) can give problems as theweight loss event due to their volatilisation canmerge with the pyrolysis weight loss event of thepolymer. As mentioned in the above section,polymers that lose small molecules by heatdegradation (e.g., HCl lost by PVC) give morecomplicated TGA traces and will require a solventextraction step to determine their plasticiser level.

5.2 Determination of Fillers

5.2.1 Particulate Fillers

On some occasions, carbonaceous fillers such as aconducting black (acetylene black) or graphite areadded to a plastic to enable it to meet certainconductivity requirements. It is possible to use TGAto quantify these types of fillers. It is also a usefulway of differentiating between these materials and

conventional carbon black; the former having amaximum oxidation weight loss around 700 °C andthe latter around 550 °C.

The TGA trace for an EVA cable covering filled witha conducting black is shown in Figure 11.

The fact that a number of rubbers (e.g., halogenated,nitrile and polyurethane) produce carbonaceousresidues during the nitrogen atmosphere region hasalready been mentioned in Section 4.1, and care mustbe taken to ensure that these do not affect thequantification of the carbonaceous filler in the airatmosphere region. Use of a high resolution TGAinstrument will assist in this as it will improve theseparation of the two weight loss events.

TGA is also convenient for the quantification ofinorganic fillers such as barytes, silica and silicates.The limitation of the technique is that the totalinorganic content of the plastic is obtained, with noindication of the relative proportion if a blend ofinorganic fillers is present. It is therefore commonpractice to complement the TGA data with a least asemi-quantitative elemental technique such as XRFin order to obtain qualitative as well as quantitativedata. A useful exception to this rule is where thecompound contains calcium carbonate (a relativelycommon diluent filler), in which case the carbonatewill undergo quantitative degradation at around 680-700 °C into carbon dioxide and calcium oxide (whichremains as a residue). It is therefore possible toquantity the amount of calcium carbonate in thesample from the carbon dioxide weight loss (whichwill represent 44% of the carbonate by mass) andthe remaining quantity of residue will indicate if anyother inorganics are present.

The other technique commonly used for thequantification and isolation of inorganic materials(both fillers and additives such as glass fibres) isfurnace ashing. This method is described in ISO345-1 (1997) and a temperature of 500-600 °C isusually used.

Once the ash has been obtained, qualitativeinformation on the inorganic species present can beobtained by IR (liquid paraffin mull technique), XRFor, where the quantification of specific species isrequired, ICP.

Some of the principal diagnostic IR absorption bandsfor inorganic fillers are given in Table 5.


20

Figure 11

TGA trace for an EVA cable cover compound showing weight loss and derivative weight loss curves

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5.2.2 Fibrous Fillers

In certain applications it is necessary to impart thestrength required to a plastic part by the use of a fibrousfillers. The following types are among those used:

(1) Glass fibres

(2) Carbon fibres

(3) Synthetic polymer fibres (e.g., nylon)

(4) Wood flour

It is usually obvious whether a plastic contains a fibrousfiller from either a visual inspection or the use of arelatively low powered optical microscope.

Glass fibres can be isolated and gravimetricallydetermined by ashing at 600 °C in a muffle furnace.Higher temperatures (above 700 °C) can cause problemsas the glass will eventually reach its melting point.Confirmation that the fibres are glass can be carried outusing an infrared microscope. The IR microscope willalso give the cellulose spectrum which is expected for


21

the wood flour filler type, and be able to detect the typeof synthetic fibre (e.g., nylon or polypropylene) usedfrom its characteristic transmission spectrum.

TGA will enable the amount of carbon fibres in acomposite to be quantified. The oxidation temperatureof around 700 °C (instead of the 500-600 °Cexperienced with carbon blacks) will also provide aconfirmation of their presence.

As mentioned above, synthetic polymeric fibres can beidentified by the IR microscope once sufficiently isolatedor, by use of their melting point, by the hot stagemicroscope or DSC. In the case of DSC, somequantification data can be obtained from the size of themelting endotherm providing standards are available.

6 Determination of Stabilisers in aPlastics Compound

In common with other polymer systems, to maintainthe physical properties of a plastic compound stabilisersneed to be added to stop, or at least retard, degradationby a number of agencies (e.g., heat and UV light).

The use of an initial solvent extraction/dissolution stepis common in the analysis of a plastic matrix forantidegradants, as these species may not be volatileenough to be removed by heating the sample. In somecases (e.g., butylated hydroxytoluene) heating a sampleliberates enough of the species to enable an identificationto be made using GC-MS; however quantification willusually require removal by a solvent (to as near 100%efficiency as possible). Analysis of the extract can thenbe carried out by HPLC, UV spectroscopy, or GC if thespecies is heat stable and sufficiently volatile. Relativelynon-specific solvents (i.e., having mid-range solubilityparameters) such as chloroform are good extractingsolvents. Another common approach is to dissolve upthe sample in a suitable solvent and then add a non-solvent to precipitate the polymer. The stabiliser willremain in the solvent phase.

If the type of organic antidegradant in a compound iscompletely unknown, analysis of the solvent extractby GC-MS or LC-MS is an excellent method foridentification. Once the identification has beenachieved, a quantification can be carried out using apreferred method and a validated procedure if available.

Where the antidegradant is not volatile enough to beidentified using a GC based technique, direct probemass spectrometry or LC-MS can be used and the

antidegradant identified by reference to its molecularion and a database. The direct probe mass spectroscopytechnique can be carried out on samples in the asreceived state as well as sample extracts, whereas LC-MS is only used for extracts.

6.1 UV Stabilisers

There is a large range of commercial UV stabilisersfor plastic materials and a number of analyticalapproaches can be used for their detection andquantification.

The UV stabilisers can be divided into five differentgroups:

(a) Benzophenone derivatives

(b) Salicyclic acid esters

(c) Resorcinol esters

(d) Benzotriazole compounds

(e) Coumarin drivatives

In a number of cases specific methods have beendeveloped to determine a particular stabiliser within aparticular polymer. Some representative methods areoutlined next.

In some cases (e.g., the determination of 2-hydroxy-4-n-octoxybenzophenone in polyethylene) the stabiliserhas distinctive diagnostic bands and the relativesimplicity of the infrared characteristics of the polymermatrix enables it to be quantified using transmissioninfrared spectroscopy. A thin film of the sample isproduced by hot pressing at 120 °C, along with filmsof virgin polyethylene containing known amounts ofthe stabiliser. The absorbance maxima of the diagnosticband between 15.8 and 16.2 microns in the standardfilms is used to produce a calibration curve from whichthe amount of stabiliser in the unknown is calculated.The method is capable of detecting the stabiliser downto 0.02% w/w with an accuracy of +/- 5%.

A number of methods use the UV absorbing propertiesof the UV stabiliser. For example, Tinuvin 326 can bedetected in polypropylene down to 0.02% w/w by usingan extraction with chloroform under reflux followedby analysis of the extract using a UV/Vis spectrometer.The ultraviolet absorption peak at 355 nm is used anda calibration curve produced by dissolving knownamounts of Tinuvin 326 in chloroform.

Another technique uses the fluorescence of thesecompounds. Uvitex OB can be detected in a chloroform


22

solution (0.8% w/v of polymer) of polystyrene byexcitation at 370 nm and recording the fluorescence at435 nm. Standard solutions at the 0.8 w/v level of virginpolystyrene and known amounts of Uvitex OB are usedas calibrants.

It is also possible to use gas chromatography (e.g.,Tinuvin P, Tinuvin 326, Tinuvin 327 and CyasorbUV531 in toluene extracts of polyethylenes), thin layerchromatography (e.g., benzophenone and salicylic acidtypes in polyethylenes) and HPLC. This latter methodhas been used extensively for the determination ofantioxidants but has not received as much attention inthe literature for UV stabilisers.

It is also the case that the white pigment titaniumdioxide provides protection against UV light and sothis can be added at reasonable high loadings (e.g., 10%or greater) to products such as window frames. Theamount of titanium dioxide in a plastic can bedetermined after acid digestion of the matrix by theuse of an elemental technique such as AAS/ICP.

6.2 Antioxidants

HPLC based techniques have been widely used byanalysts for the determination of antioxidants in plasticsand a review has been provided by Sidwell (400).

The chromatogram obtained for the determination ofIrganox 1076 in an HDPE compound is shown inFigure 12. An extract of the polymer was analysedusing a C18 reverse phase column with UV detection at230 nm and a mobile phase of 70:30 methanol/waterchanging to 100% methanol.

There is a useful HPLC method which can be used onplastics for the detection and quantification of a widerange (20 species) of antidegradants. The sample isdissolved up using a suitable solvent at an elevatedtemperature if necessary. A non-solvent (e.g., methanol)is then added and the extract analysed by HPLC usingthe following conditions:

Injection volume 25 μl

HPLC column Aqua 5 C18 ODS reverse phasecolumn 150 mm x 3.0 mm(or similar)

Mobile phase A= 75:25 Methanol/Water

B= 50:50 Ethyl Acetate/Acetonitrile

Gradient Time %A %B

Initial 90 10

After 25 min 0 100

Flow rate 2.0 ml/min

Figure 12

HPLC chromatogram of HDPE for determining Irganox 1076


23

Detection UV detector set at 270 nm

Temperature 40 °C

The following antioxidants are examples of those thatcan be determined using this technique:

(1) Irganox 1010

(2) Irganox 1098

(3) Irganox 1076

(4) Irganox 1330

(5) Butylated hydroxytoluene

(6) Irgafos 168

(7) Triclosan

The chromatogram obtained using this method toseparate a complex cocktail of antidegradants is shownin Figure 13.

The wide applicability of this method is due to themobile phase mixture.

The capability of HPLC has been greatly extended bythe commercialisation of affordable liquidchromatography-mass spectroscopy (LC-MS)instruments. The mass selective detector enablesunknown samples to be analysed and the antioxidantspresent to be identified. The LC-MS techniquetherefore compliments GC-MS and, with it, enablesthe complete molecular weight/volatility/polarity rangeto be covered.

TLC is comparatively easy and cheap to use and it isboth quick and accurate for the identification of

Figure 13

HPLC chromatogram of a complex mixture of antidegradants


24

antioxidants in plastic extracts. Irrespective of thecomplexity of the extract composition and the amountused, this method can be used to give a sharp separationfor identification purposes. Distinctive Rf values andcolours can be seen for each antioxidant depending onthe stationary phase, the developing solvent used andthe detection agent.

TLC, in addition to being used for identificationpurposes, can be used in a semi quantitative way;the logarithm of the spot area being proportional tothe quantity of the analyte in the spot, and this valuebeing compared to spots containing standardamounts of the analyte.

Gas chromatography has been used for the analysis ofphenolic and amine type antioxidants. Antioxidantswhich have high boiling points cannot be directly byGC but they can be analysed as derivatives such asacetates, trifluoroacetates, trimethyl silyl-ethers, methylethers, etc. Trimethyl silane based antioxidants, forexample, give good separations on standard siliconebased columns (a.10).

Benchtop LC-MS instruments are proving to beexcellent tools in the analysis of plastics of unknowncomposition to identify and, once this is achieved,quantify the antioxidant present. Prior to the adventof LC-MS it was very difficult to use conventionalHPLC for this task because of the large range ofpossible compounds.

Using the general analysis conditions shown below anumber of antioxidants can be detected in toluene orchloroform extracts of plastics:

Sample preparation: Around 5 mg of extract is diluted1/20 with 80% acetonitrile/water

Instrument: Agilant 1100 series LC-MS

Column: Zorbac SB-C18, 5 um,2.1 mm x 150 mm

Mobile phase: A=water, B=acetonitrile

Gradient Time A B

Initially 15% 85%

after 10 min 1% 99%

or Initially 35% 65%

after 10 min 10% 90%

Flow rate: 0.7 ml/min

Injection volume: 5 μl

MS conditions: Atmospheric Pressure ChemicalIonisation (APCI)

Ion mode: Positive or negative

Vapouriser: 300 °C

Scan range: 200-1600 amu

Fragmentor: 70 or 120 volts (The fragmentorvoltage is chosen to modify thedegree of fragmentation andhence sensitivity)

Antioxidants which have been identified in polyolefinsusing the above conditions include:

• Irgafos 168

• Irganox 1076

• Irganox B225 (50:50 mixture of Irganox 1010and Irgafos 168)

7 Determination of FunctionalAdditives

7.1 Process Aids and Lubricants

In PVC technology certain polymeric additives can beconsidered as process aids. These polymers have asimilar composition to those used as impact modifiersin PVC formulations but are more compatible and soare primarily included to ensure more uniform flowand hence improve surface finish. Such process aidsinclude ABS, chlorinated polyethylene, MBS, EVA-PVC graft polymers and acrylate-methacrylatecopolymers. As these are usually found in unplasticisedPVC, direct analysis of the product by IR will usuallyindicate the presence of those that have a distinctivespectrum as no masking by plasticiser will take place.However, even rigid PVC can contain a small amountof phthalate and so it is advisable to carry out a solventextraction to clean up the matrix first. Where theprocess aid (e.g., chlorinated polyethylene) has arelatively bland spectrum, a technique such as NMRwill be required to both detect and quantify it. NMRwill usually be required to quantify the other types aswell, unless the spectrum is very distinctive andstandards of known composition are available.


25

In the case where a relatively large quantity of filler(talc) has to be incorporated into a polymer (e.g.,polypropylene) it is often necessary to use a processaid/lubricant such as a zinc or calcium stearate. Aquantification of the process aid can be achieved bythe analysis of the sample for the metal by aciddigestion-AAS. The stearate can be qualitativelydetected by solvent extraction GC-MS.

7.2 Slip Additives

It is common for aliphatic amides to be incorporatedinto plastics, particularly polyethylenes, to act as slipadditives.

It is possible to use LC-MS to detect these types ofslip additives in plastic samples. Using the LC-MSconditions described in Section 6.2, it is possible todetect Behenamide (mixture of two aliphatic amidesof molecular weight 331 and 339) and erucamide(molecular weight 337) in solvent extracts ofpolyethylene and polypropylene.

It is also possible to use GC and GC-MS to analysethese and another common slip additive oleamide inextracts from plastics as they have sufficient volatilityto elute from the GC column.

7.3 Pigments

Pigments are used extensively in plastic compoundsand can be of one of four main types:

(1) Inorganic compounds

(2) Organo-metallic compounds

(3) Organic compounds

(4) Carbon black

Pigments such as titanium dioxide and iron oxidebelong to the first group and the analysis of these isrelatively easy as they are thermally stable (so can bedetermined in both the sample ash or in the sample inthe as received state) and have a diagnostic metal atomtogether with a simple chemical structure. Analysistechniques used are therefore elemental methods suchas AAS and ICP.

Groups 2 and 3 present the analyst with a greaterchallenge as there is a very wide number commercially

available, they have relatively high molecular weightsand so cannot be easily removed from the matrix bysolvent extraction and can be thermally labile.

One technique which has been used to identify both thesetypes of pigment and inorganic ones is vapour phaseultraviolet absorption spectrometry at 200 nm (a.11). Inthis method the samples are powdered and then directlyvapourised in the heated graphite atomiser. Thermalultraviolet profiles of organic pigments show absorptionbands between 300 °C and 900 °C, while profiles ofinorganic pigments are characterised by absorption bandsat temperatures above 900 °C. Specific assignments aremade with respect to temperature, relative intensity andwidth of the absorption bands.

A relatively unknown technique (laser desorption fouriertransform ion cyclotron resonance mass spectroscopy)has been used (397) to identify dyes in plastics such aspolymethylmethacrylate. A detection limit of 0.1% wasobtained, which compared with a limit of 1-2% usingan ATR infrared spectroscopy technique.

Infrared spectroscopy techniques can be useful,particularly if the plastic matrix itself (e.g., polyethylene)has a relatively simple infrared spectrum and if standardinfrared spectra of a wide range of pigments is available.

Carbon black is used extensively as a black pigment inproducts such as cable sheaths. The amount present isusually less than 2% and so its quantification by TGAcan be difficult due to the small sample size (10 mg)used. The standard method to quantify the amount ofcarbon black in such a product is therefore the tubefurnace as much larger sample sizes can be used (e.g.,2 g) and hence more accurate quantifications obtained.

7.4 Antistatic Agents

Antistatic agents are usually hygroscopic compoundswhich readily attract moisture and so inhibit the buildup of a static charge on the surface of a plastic product.They are used in many applications from the body ofthe humble plastic pen to numerous packagingapplications.

The selection of an antistatic agent depends greatly onthe polymer matrix since a degree of incompatibilityis vital to ensure that migration to the surface of theproduct occurs at a fast rate after manufacture. Exactchemical composition information can be difficult toobtain from suppliers and so analysis for these additivescan be difficult.


26

In the case of polystyrene, quaternary ammoniumcompounds are widely used and for polyethylene,polyethylene glycol alkyl esters can be used.

In the case of the glycol esters, these can of sufficientlylow molecular weight to be extractable by solvents suchas diethyl ether and then identified by a chromatographictechnique such as GC-MS. As in a number of cases it isto be expected that LC-MS will play a role in the analysisof these additives in the future.

7.5 Crosslinking Agents and Co-Agents

For some plastic products (e.g., cable sheathing) itcan be necessary to impart a degree of crosslinkinginto the product to achieve the requisite physicalproperties. This can be achieved by irradiation usinggamma rays. However, some polymers degrade whensubjected to high energy radiation as illustrated inTable 6. Chemical agents such as peroxides are alsoused. These species produce diagnostic breakdownproducts the identification of which will reveal thetype of peroxide used.

The most useful technique for this type of work is GC-MS. There are two possible modes of sampleintroduction: solution injection and dynamicheadspace. In the case of the former a useful methodof sample preparation involves cryogenic grinding of0.3 g of the sample, followed by extraction using 2 mlof diethyl ether in an ultrasonic bath for 30 minutes.The resulting extract is then analysed under thefollowing conditions:

Instrument: Hewlett Packard 6890/5973 GC-MSD

Carrier: Helium @ 2.0 ml/min constant flow

Injection mode: 1 μl splitless (0.75 min; 50 ml/min)

Injection temperature: 320 °C

Column type: RTX5-MS 30 m x 0.25 mm,0.25 μm film thickness

Column temperature: 40 °C for 5 min, 20 °C/minup to 300 °C held for 12 min

MS settings: 20 to 620 Daltons scannedevery 0.33 s

In the case of the dynamic headspace approach arelatively small amount of sample (e.g., 3 mg) is heatedin the oven of a dynamic desorption unit and thevolatiles produced collected in a cryogenically cooledTenax filled trap. The experimental conditions are asfollows:

Dynamic Headspace

Instrument: Perkin Elmer ATD 400

Desorption temperature: 150 °C for 10 min

Desorption flow: Helium @ 20 ml/min

Trap collection temperature: –30 °C

Trap injection temperature: 250 °C

Trap outlet split flow: 9 ml/min

Trap inlet split flow: off

Split: 10:1

GC-MS

The conditions used are the same as for the diethylether method with the exception of the following:

GC Column temperature: –30 °C to 50 °C at 5 °C/min,following by 20 °C/min to300 °C and then held at300 °C for 12 min

Carrier Helium @ 0.07 MPa

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For either analytical approach, identification of thediagnostic cure system breakdown species is byreference to mass spectral libraries such as thoseproduced by the National Institute of Standards andTechnology (USA) (NIST), the Royal Society ofChemistry, Wiley/NBS (a.12) and the USEnvironmental Protection Agency (EPA)/NationalInstitute of Health (NIH). The mass spectra of themajority of species of interest are in these libraries andso, providing the knowledge to reconstruct cure systemsis available, successful attempts can be made.

One problem associated with this task is that a numberof peroxide curing agents breakdown to give more thatone product and a number of these are common to morethan one peroxide species. This is demonstrated inTable 7.

In addition to identifying the type of peroxide used,these GC-MS techniques will also identify the type ofco-agent (e.g., triallyl cyanurate (TAC) or triallylisocyanurate (TAIC)) used.

7.6 Blowing Agents

There are two main types of blowing agent used withpolymer systems in general:

(1) Chemical Chemical compounds (principallyorganic) that undergo chemicaldecomposition at the processingtemperature to form a gaseous species(e.g., nitrogen) which will create thecellular structure.

Examples include azo compounds,nitroso compounds, sulfonyl hydrazidecompounds and sodium bicarbonate.

(2) Physical Low boiling point organic compounds(e.g., dichloromethane or pentane)which volatilise at the processingtemperature to create a cellularstructure.

With plastics, the most widely used type are thephysical blowing agents.

Where it is suspected that a physical type blowingagent has been used to produce a foam, is it possibleto use headspace GC-MS to identify it. Even in theblown state, the high sensitivity of the techniqueenables an assignment to be made from the smallamount of residual blowing agent that will be present.It is usual to use this type of blowing agent inamorphous plastics that have glass transitiontemperatures around 100 °C, e.g., styrenics. Thisenable the expansion of the plastic to be wellcontrolled.

The reactivity of the chemical blowing agent type canmake analysis difficult (e.g., they will decompose inthe injection port of a GC-MS instrument), and theapproach that is used is to indirectly identify them bythe determination of breakdown fragments. The GC-MS instrument is the best choice for this and a libraryof typical breakdown fragments is required.

Quantification of the chemical blowing agent in anunblown product is very difficult as the polarity andreactivity (e.g., hydrogen bonding reactions andthermal instability) can cause problems during isolationfrom the compound and subsequent analysis. In termsof reverse engineering, this is unlikely to be requiredsince the product will invariably be already blown. Forlaboratories that are carrying out quality control work,other properties such density and expansion ration canbe used to determine compound loadings.

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28

7.7 Flame Retardants

As with blowing agents, there are two main categoriesof flame retardant: organic and inorganic.

The amount and type of organic flame retardant presentin a plastic compound can be determined in ananalogous way to the plasticiser, since this type of flameretardant is usually similar in molecular weight andpolarity and, hence, extractability. Once the type oforganic flame retardant has been determined by IR, anaccurate quantification can be obtained by carrying outan elemental analysis for the halogen (or other relevantelement, e.g., phosphorus) on the unextracted sample.The extract value itself will rarely provide a meaningfulquantification as other species, particularly any processaid/plasticiser, will contribute to it as well. In someinstances (e.g., organophosphates) it may be possibleto use an HPLC analysis of the extract to quantify theflame retardant. GC based techniques can also be usedin some cases, but bromide types present problems forthese techniques because of their relatively highmolecular weights (> 900).

Care must be taken over the quantification of inorganicflame retardants, since some of them (e.g., antimonytrioxide) can react with the organic flame retardantpresent, or break down to produce volatile products,under quantitative ashing conditions, and duringanalysis by thermal techniques such as TGA. A goodinitial approach is a semi-quantitative elementalanalysis by XRF, to see which types are present.Accurate quantifications can then be obtained byprecise elemental determinations.

If it is known that hydrated alumina is present in thesample, it is possible to quantify this reasonably wellusing TGA, by making use of the water loss data.Hydrated alumina loses close to 35% of its weight whenit is heated to 550 °C in a TGA experiment.

7.8 Impact Modifiers

The most commonly encountered impact modifiedplastic is high impact polystyrene (HIPS). The impactmodification is achieved by incorporating discreetdomains of a rubber (butadiene) within the polystyrenematrix. The level of butadiene can be varied accordingto the requirements of the end use. A high level canconvert a glassy brittle material into a ductile, toughproduct. The efficiency of the butadiene to improveimpact resistance alone is not solely related toconcentration, but is also dependent on the size and

distribution within the matrix of the domains thatcontain it. Actual impact performance is determinedby physical tests such as the Charpy and Izod impacttests, and the size and distribution of domains isinvestigated by transmission electron microscopy(TEM), but there are a number of chemical tests thatcan be carried out to determine the level of modifier.

(1) IR analysis - this is performed on a pressed filmand the relative size of the absorption bands due tostyrene (700 cm) and butadiene (966 cm) are takenand compared to standards of known styrene-butadiene levels.

(2) NMR - the plastic is dissolved and the level of thetwo polymers determined by specific shift areas.

(3) Classical wet chemistry - the butadiene level isdetermined in solution by reaction of a reagent withthe double bonds.

There are some instances (e.g., rubber impactmodification of nylon) where the chemical propertiesof the two polymers are so dissimilar that solubilitydifferences can be used to isolate and, in this case,quantify the rubber modifier. The test is carried out bytaking an accurately weighed sample and refluxing itin formic acid until the plastic is digested and only therubber phase remains. The rubber is then washed, driedand weighed.

Other plastics which can contain rubber modifiers (orat least modifiers that have lower glass transitiontemperatures than the plastic phase) include PET andPVC. In the case of PVC, acrylates and methacrylatesare common and the normal approach is to use IR todetect the modifier and then NMR to quantify it.

8 Analysis of Plastics for FoodContact Use

For more than 30 years work has been going oninvolving food contact plastics and the effect thatmigrants from plastics products have on food. The firstEuropean Directive (78/142/EEC), which was on thevinyl chloride monomer content of food contact PVC,was published in the late 1970s and this was followedultimately by the more comprehensive PlasticsDirective (90/128/EEC) in 1990. Since 1990, there hasbeen a gradual harmonisation of European testingrequirements through amendments to 90/128/EEC. Theseventh amendment (2002/17/EC) has recently been


29

published and the initial requirements for testing overalland specific monomer migration have now grown toinclude additive (e.g., antioxidant) migration.

In general, there are two types of analytical test thatare carried out on food contact plastics:

(1) Global migration tests - In these, the plastic is putinto contact with an appropriate food simulantunder representative end use conditions and thetotal amount of material that has migrated into thesimulant determined gravimetrically or, in the caseof involatile food simulants such as olive oil, bygas chromatography.

(2) Specific migration tests - Again, the plastic iscontacted with a food simulant but any analyticalwork in targeted on a specific additive and itsconcentration determined using an appropriatechromatographic technique.

In the case of certain plastics materials, e.g., ABS,grades that are intended for food use have to meetcertain residual monomer targets. Direct analysis ofthese polymers is undertaken to determine theconcentration of these monomers.

8.1 Global Migration Tests

The following food simulants are used for food contactplastics:

Distilled water - Aqueous food use

Distilled water 95%:Ethanol 5% - Alcoholicbeverages such as beers and lagers

Distilled water 85%:Ethanol 15% - Wines

Distilled water 60%:Ethanol 40% - Spirits

A solution of 3% w/v acetic acid in distilled water -Acidic aqueous foods

Olive oil* - Fatty foods (also isopropanol or hexane)

(*Isopropanol and Hexane have been introducedas fatty food simulants to circumvent the analyticalproblems that can occur with olive oil due to itspotential variability as a natural product andinvolatility.)

As mentioned, the global migration figure for a particularplastics material is determined gravimetrically. One

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30

approach is to use conditioned glass crucibles and todry off the simulant on a hot plate after the contactexperiment has been performed under the appropriateconditions (time and temperature).

Once the appropriate simulant has been chosen thecontact time and temperature to use are given in ECDirective 82/711/EEC (Table 8).

In addition, for plastics in contact with food for whicha preservation temperature of less than 20 °C is requiredthe test condition will be 10 days at 20 °C.

The overall global migration limit for plastics is statedin the EC Directive 90/128/EEC as being 10 mg/dm2

(surface area of plastic). This limit can be expressed as60 mg/kg of foodstuff in certain situations. To be usedfor food contact a plastics product must meet thisrequirement.

In a number of packaging types, only one side of aplastic film or laminate may contact the food. Specificsingle side migration cells have been developed (e.g.,by PIRA) to enable the migration from a material underthese conditions to be investigated.

8.2 Specific migration and residual monomer tests

In addition to the global migration limit 90/128/EECalso provides a number of specific migration limits(SMLs) for plastic monomers (Table 9).

There are also SMLs for plastic additives, someexamples are shown in Table 10.

In the case of some monomers, 90/128/EEC gives limits(called quantification limit-monomer (Qm)) relating tothe plastic material itself. For example, vinylidenechloride has a QM of 5 mg/kg of plastic.

Over the years, the detection of species migrating fromfood contact materials has advanced hand in hand withthe gradual lowering of analytical detection limitsbrought about by the refinement of the techniques. Forexample, the SML for acrylonitrile is set at notdetectable above 0.02 mg/kg (i.e., 20 parts per billion)and this would not be obtainable on a routine basiswithout the benefits of modern instrumentation.

The development of suitable methods for the detectionof the wide range of monomers and additives used in

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remonoM LMS

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elirtinolyrcA ffutsdoofgk/gm20.0evobaelbatcetedtoN

matcalorpaC ffutsdoofgk/gm51

edyhedlamroF ffutsdoofgk/gm51

dicacilahthpereT ffutsdoofgk/gm5.7

edirolhcenedilyniV ffutsdoofgk/gm50.0evobaelbatcetedtoN

)CEE/821/09(sevitiddacitsalpemosrofsLMS01elbaT

evitiddA LMS

sretseetalahthpdnaetapidA ffutsdoofgk/gm5.1

edixoirtynomitnA ffutsdoofgk/gm10.0

THB ffutsdoofgk/gm0.3

snobracordyhdetanegordyH ffutsdoofgk/gm0.3

snobracordyhlanoitnevnoC ffutsdoofgk/gm3.0

edimaraets/edimaelO esudoofyttafrofdesuebtonnaC


31

food contact materials requires the application of stateof the art analytical techniques. Normally, headspacemethods are preferred for volatile monomers as suchmethods overcome a lot of the problems of sample matrixclean-up. In principle the food contact simulant, foodstuffor plastic material is heated in a sealed vial fitted withan inert septum (usually PTFE coated rubber). The vialis heated to an accurate set temperature normally in therange 80-100 °C, for an equilibrium time of at least onehour. The headspace above the sample is then analysedfor the presence of the analyte. The quantity of analytein the headspace will always be in equilibrium with theamount present in the sample. Standard addition methodsare used to obtain calibration curves, with the calibrantvials being analysed under the same conditions (i.e., time,temperature and ratio of headspace to bulk material(polymer if necessary)) as the samples. To acquiresufficiently low detection limits it is sometimesnecessary to use specific detectors (e.g., a nitrogen/phosphorus detector (NPD)) or, in the case of massselective detectors, a single ion monitoring approach.For species that are too involatile for headspace basedmethods, other chromatographic and spectroscopicmethods are employed.

A summary of the analytical techniques used in foodmigration work is shown in Table 11.

In the cases where HPLC has been assigned, LC-MSwould also be applicable.

9 Determination of Stabilisers in PVC

Although it is one of the bulk thermoplastics, PVCsuffers from relatively poor stability to ageing agenciessuch as heat and UV light. In order to achieve its statusas an important plastic it was therefore necessary todevelop a specific additive group: PVC stabilisers.

These technological developments have resulted in arange of stabilisers being available that are appropriatefor different grades of PVC, products and end uses.Some of the main types are:

(a) Lead stabilisers (e.g., lead carbonate, lead stearate,lead phthalate)

(b) Metallic soaps (e.g., stearates, palmitates,ricinoleates and octoates of cadmium, barium,calcium and zinc)

(c) Organo-tin compounds (e.g., dibutyltin di-iso-octylthioglycollate)

(d) Epoxide stabilisers (e.g., epoxidised oils andbisphenol A epoxide resins).

The analyst has to bear in mind that it is common for anumber of different stabilisers to be used in a PVCcompound in order achieve the optimum ageing resistance.

gnitsetnoitargimnidesuseuqinhcetlacitylanA11elbaT

etylanA euqinhceT

edirolhclyniV CGecapsdaeH

enerytS CLPHdnaCGecapsdaeH

dicacilahthpereT CLPH

locylgenelyhtE CGecapsdaeH

elirtinolyrcA DPNhtiwCGecapsdaeH

eneidatuB )DSM(rotcetedevitcelesssamhtiwCGecapsdaeH

setanaycosI CLPHnoitasitavireD

edyhedlamroF yrtemirolocnoitasitavireD

sdicacinagrO CIroCLPHriapnoI

sresicitsalP CLPH

stnadixoitnA CFSroCG,CLPH

scinagronI PCIroSAA

scinagroraloP siserohportceleyrallipacdnaCLPH


32

It is obvious that a large number of these stabiliserscontain metal atoms and so a cost effective way ofachieving an initial evaluation of the type of stabiliserpresent is to use a semi-quantitative XRF techniqueon the sample in the as received state. Care should betaken with this as some inorganic pigments/fillers(e.g., titanium dioxide) can mask certain key elements(e.g., cadmium).

If it is a case of quantifying a known stabiliser, thenAAS or ICP can be used to quantify the metal and, withknowledge of the compound formula, the result obtained.

The organo-tin compounds are widely used and foranalytical considerations it is convenient to divide theminto those that contain sulfur and those that do not. Tothe first group belong compounds like dialkyltinmercaptides, mercaptoesters and mercaptocarboxylates, to the second, dialkyltin carboxylates andtheir esters. The identification of acids and alcoholspresent in tin stabilisers containing no sulfur and theidentification of alcohols from stabilisers containingmercaptoesters presents little or no difficulty. However,the identification of the thioacid and of the alkyl groupsattached directly to tin can prove more difficult,especially if long chain acids form part of the compoundor if the stabiliser is not pure, e.g., if it containsplasticiser. The thioacid may also tend to decomposeduring hydrolysis procedures. The application of anumber of analytical methods (e.g., NMR, IR and GC)to determine these types of stabiliser in PVC extractshave been described by Udris (a.13).

Some classic methods based on titration and TLC todetermine organo-tin compounds in solvent extractsof PVC include:

• Potentiometric titration of organo-tin in the extractwith standard sodium methoxide in pyridine usingantimony and calomel electrodes (a.14).

• Titration of dialkyltin thiol compounds in benzene/methanol extract with standard silver nitrate (in IPAmedium) using sulfide coated wire electrode (a.13).

• TLC of organo-tin thioacids and thiols usingKielselgel G plates with development withglacial acetic acid and detection with catecholviolet (a.15).

• TLC of organo-tins using Kieselgel GF 254 withdevelopment using butanol/glacial acetic acidand detection with catechol violet and UVirradiation (a.16).

Of the other types of organo-metallic stabilisers,Mal’kova and co-workers (a.17) have described analternating current polarographic method for thedetermination of cadmium, zinc and barium stearatesor laurates in PVC. Other techniques used on PVCextracts include, column chromatography for barium,cadmium and zinc salts of fatty acids, paperchromatography for cadmium, lead and zinc salts offatty acids (a.18) and polarography for cadmium, leadand zinc salts (a.19).

The advent of bench top LC-MS instruments hasenabled the analysis of stabilisers such as the organo-tin type to be re-examined and laboratories such asthe Analysis Division at Rapra Technology Limitedare investigating the capability of this technique inthis area. This could be another area of plasticsanalysis where LC-MS replaces the more traditionaltechniques.

10 Analysis of Plastic Laminates andFibres

Plastic laminates are used extensively from the ordinarycrisp packet to high specification products for medicaland pharmaceutical use. In all these cases, laminatesare used since the application demands a number ofproperties which no single polymer exhibits.

Taking the example of the crisp packet, the innermostlayer must be inert to the product and provide a barrierto air, the outside layer has to be capable of beingprinted onto and the middle layer (or tie layer) has tobe able to stick both of the other two together.

One of the principle analytical techniques for theanalysis of laminates is the infrared microscope. Thisinstrument is capable of recording transmission infraredspectra from sample down to 10 square microns in size.The approach is usually to prepare a section of thelaminate by microtoming a section and then recordinga spectrum of each layer aided by the masking off ofthe other layers. The sectioning is often undertakenobliquely in order to maximise the apparent layerthickness. The microscope also allows the thicknessof each layer to be determined.

It is also possible to use an ATR technique to recordinfrared spectra of the outside layers and reserve theIR microscope for the central layers. This is possiblebecause the ATR technique only penetrates a fewmicrons into the surface of the layers. It is also possibleby choosing the appropriate crystal (e.g., germanium,


33

zinc selenide, etc) to control the depth of penetration.This can be useful if the layers are particularly thin.

Using the knowledge gained by infrared spectroscopyof the generic polymer types present, the assignmentscan be refined by the use of DSC. Due to the fact thatlaminates by their nature are often constructed ofcompletely different plastic types, the completestructure can be analysed in one operation and themelting endotherm transitions obtained used todifferentiate between various grades. For example inthe case of a laminate which had been shown to becomprised of a polyethylene and a nylon, it would bepossible to differentiate between LLDPE, LDPE andHDPE, and nylon 6 from nylon 6,6.

It is also possible to use a Raman microscope to analysethe different layers that are present within a laminate.As with the IR microscope, it has the ability to isolateindividual layers and, given a satisfactory database, thespectra obtained can be used for identification purposes.

The Raman spectra for four common polymer typesare shown in Figure 14.

Examination of the cross section of laminate samplesunder an optical microscope enables the individuallayers to be viewed. Phase contrast microscopes canaid the differentiation of layers of similar refractiveindex. The use of a polarising microscope can also assistin characterising individual layers and is particularlyuseful when heating laminates under a microscope ona hot stage to recognize the characteristic meltingtemperature of the individual layers.

There are a number of synthetic fibres that can be usedto produce both woven and non-woven fabrics. Themost popular include polyamide, polyester and acrylicsand they can be used in products as varied as clothingand life rafts.

Once again, the infrared microscope is ideal atrecording generic polymer identification spectra fromindividual fibres. Once the generic type has beenestablished, further refinement of the assignment canbe obtained by DSC (e.g., specific polyamide type)and, where a number of fibres are available GPC(molecular weight).

Other microscopic techniques, such as optical (aspectratio), SEM (surface morphology) and EDAX(elemental analysis), Raman microscopy and atomicforce microscopy can be used to further characterisethe product.

Figure 14

Raman spectra of (a) polyethylene, (b) PVC, (c)polystyrene and (d) polyethylene terephthalate


34

11 Surface Analysis of Plastics

There are a number of analytical techniques that canbe used to obtain data on the surface of plasticsmaterials or products. Three of the techniques, IR andRaman microscopy and Edax are covered in Sections2.2.1, 2.2.6 and 2.6. It can be argued that thesetechniques have come into being as the logicaldevelopment of the original, general purposetechniques.

There are however a number of analytical instrumentsthat have been developed with the specific intention ofanalysing surfaces. Three of the principal ones will bementioned in this section.

11.1 X-Ray Photoelectron Spectroscopy (XPS)

In this case the surface of the sample is irradiated withsoft X-rays. These X-rays are sufficiently energetic tocause photoemission of electrons from the core levelsof atoms present on the sample surface. Thephotoelectrons generated are collected and passed toan electron energy analyser and detector. The measuredkinetic energy (KE) of an electron is given by :

KE = hv - BE - sigma

where: hv = energy of the X-ray photon

BE = Binding energy

sigma = work function of the spectrometer

The binding energy of a given core electron ischaracteristic of the element and it is this whichenables the elements on the surface of a sample to beidentified. It is also possible to carry out quantitativework by measuring the relative intensities of thephotoemission from each of the elements present. Thebinding energy of a core level depends principally onthe charge on the nucleus of the atom concerned andsmaller changes are induced as a result of chemicalbonding. Although small, such charges are measurableand provide a means of studying the chemistry of thesample surface (a.20, a.21).

Because only electrons from the top few atomic layerswill have sufficient energy to escape, the technique isvery surface specific and results are normally obtainedfrom between 5 and 10 nm depth at a detection limit ofaround 0.1 atom percent. The analysis area is typically3-10 mm2 and all the elements with the only exceptionof hydrogen can be detected.

Because of its ability to determine surface chemistry,XPS can be particularly useful in the analysis ofpolymer surfaces to see if oxidation has taken placeand, if so, what functional groups (e.g., ester, acid,aldehyde) the oxygen is present in.

This ability of XPS to detect oxygen containingfunctional groups is shown in the narrow and broadscan spectra of PET presented in Figure 15.

Another application is the analysis of polymers todetermine if certain surface treatments (e.g., coronadischarge) have been carried out satisfactorily.

In common with the other surface analysis techniques,it can also be used to investigate surfacecontamination problems and to determine thecomposition of the fracture surfaces in adhesionfailures.

11.2 Laser Induced Mass Analysis (LIMA)

In the LIMA technique, the surface of the sample issubjected to a pulsed UV laser which is sufficientlyenergetic to volatilise a small volume (about 1 μmcube) of material. The ionised fragments in thisvolume are then separated and identified by means ofa time of flight mass spectrometer. Both negative andpositive fragment data can be obtained.

The analysis area in a LIMA experiment is typically1-2 μm, the analysis depth 0.25-0.5 μm and thedetection limit 10-100 ppm. The technique has theability to detect all of the elements in a qualitative way.

The technique is very useful for determiningcompounds on the surface by means of these elementsand molecule fragments, but it is very sensitive, andcare must be taken to ensure that the surface is notcontaminated (e.g., by handling without gloves) andthat the representative control samples are availableto assist in the interpretation of the data.

Its sensitivity and surface specificity make it ideal inthe detection of very low levels of contamination/modification. For example, the detection of amonolayer of silicone contamination of a plastic partthat was hampering the wetting of a paint. It can alsobe used to analyse particulate impurities, fibres anddefects in surface coatings.

LIMA is also referred to as laser microprobe massspectroscopy (LAMMS).


35

Figure 15

XPS spectra of PET (a) narrow spectrum (b) broad spectrum

(a)

(b)


36

11.3 Secondary Ion Mass Spectroscopy (SIMS)

In this technique the sample surface is bombarded by aprimary ion beam (positive ions of argon, caesium,oxygen or gallium). These primary ions impart energyto the surface and, as a consequence of the collisionsproduced, ions, atoms and molecular fragments (calledsputtered particles) are ejected. The primary ions maypenetrate several atom layers into the surface, but thesputtered particles only come from the outer 2-3 atomlayers. In common with the other two techniques,therefore, SIMS is very surface specific and it is possibleto restrict it to a single monolayer. The analysis area istypically 150 μm, the detection limit is 1 ppm and allthe elements are detectable.

Two types of SIMS experiment can be carried out: staticSIMS and dynamic SIMS. In the former case, the surfaceis bombarded with low energy ions and molecular andatomic fragments are produced without the experimentchanging the nature of the surface appreciably; thesurface chemistry can therefore be investigated.Dynamic SIMS uses high energy ions to obtain highlysensitive elemental data down to ppb levels, but thestructural information is lost.

In the case of static SIMS, dedicated libraries are requiredto enable the mass spectra of the fragments to beidentified (a.22).

Another application of SIMS is in the study of themigration of additives (e.g., slip additives and antistats)onto the surface of plastics.

It is often the case that complementary surface analysistechniques such as SIMS and XPS can be used togetherin order to successfully solve a failure or characterisationproblem. In such cases, XPS would be used to generatequantitative information, whilst SIMS would providequalitative clues with respect to the chemistry. Anexample of this is where XPS has successfully detectedand quantified silicon on a surface which is notresponding well to bonding with an adhesive, but thechemical form that the silicon is in is not readily apparent,i.e., it could be silica, silicate or silicone. Analysis of thesame surface by static SIMS enables the mass spectrumof the sputtered top layer fragments to be determinedand the presence of m/e ions at 43, 73 and 147 confirmthat a polydimethyl siloxane is present.

12 Failure Diagnosis

It is an unfortunate fact that plastic products fail inservice. One of the major reasons for this is an incorrect

formulation of the product initially, which is atechnological failing, the other is where the formulationis correct for the application, but where there has beena problem in the mixing/processing side, leading to aproduct that does not meet the specification. Analysingthe plastic component can be useful in failure diagnosis.

12.1 Common Compositional Problems

If it is suspected that the composition of the product isnot correct, for example that the antioxidant or correctcure system has not been incorporated into thecompound, then the appropriate species specific teststhat have been discussed earlier can be carried out. Ifpossible, it is advisable to conduct the analysisalongside that of a sample known to be of the correctcomposition. This ensures that no product specificmatrix effects/interference reactions affect the dataobtained and hence the conclusions reached.

A surprisingly large number of failure problems can besolved by carrying out a simple series of tests including apolymer identification check by IR, a bulk compositionalanalysis by TGA and a molecular weight determination.

Molecular weight determination is very important in thecase of plastics because of the wide use (sometimesunauthorised) of regrind material. Unfortunately, thequality of regrind plastic can vary greatly due to thedegradation, and hence reduction in molecular weightand associated physical properties, that a plasticundergoes when it is reground. This depends greatly onthe conditions (e.g., heat and time of heating) that it issubjected to during the regrinding process. Also, if amaterial already contains a proportion of regroundmaterial the onset of degradation can be accelerated bystructural anomalies already present in the polymer. Thewidespread applicability of GPC to determine themolecular weight distribution of the majority of commonplastics makes it the perfect technique to investigate ifregrind is in a sample. Although small amounts (e.g.,5%) of reasonably high quality regrind can be hard tospot, any significant amount will reveal itself by a shiftin the distribution towards the low molecular weight end.As usual with GPC, the availability of reference samplesis important as the technique is mainly comparative.

Most of the failures that are associated with the use ofeither some or too much regrind are related to a reductionin the strength properties of the plastic, but anotherreasonably common type of failure is odour, especiallyin packaging applications. This odour is invariably dueto oxygenated degradation products of the plastic andcan be detected and analysed by headspace GC-MS.


37

12.2 Environmental Stress Cracking

Environmental stress cracking (ESC) is the prematureinitiation of cracking and embrittlement of a plasticdue to the simultaneous action of stress and strain andcontact with specific fluids. It is estimated that 15% ofall plastic component failures are due to ESC. Thesource of stress is often that which is unavoidablyprocessed in during moulding and so an applied stressis not a pre-requisite. The fluid is sometimes that forwhich the component was designed to contain orconduct, but it is often supplied by such agencies asadhesives, paints, cleaning agents and inks.

Because this type of failure is associated with relativelymobile (i.e., low molecular weight) liquids which arenormally present in small concentrations the techniqueof GC-MS is very well suitable to its investigation. Aparticularly effective approach is dynamic headspaceGC where any stress cracking fluid can be removedfrom the plastic matrix without the use of anothersolvent and long heating times enable it to beconcentrated up to aid detection. An area of plastic thathas not stress cracked can be used as a control.

There are cases where stress cracking can occur due tothe migration of a less volatile liquid (e.g., a plasticiser).An example of such a case is the stress cracking ofABS due to the migration of plasticiser from PVC, andthis can be approached by the detection of phthalate inthe ABS matrix by solvent extraction and then analysisof the extract using HPLC.

Where the liquid is relatively non-volatile and complexin composition (such as silicone oil which causescracking of polyethylene) again a solvent extractiontechnique has to be performed with either infraredmicroscopy analysis of a cast micro-film or a liquidchromatography method (i.e., LC-MS or HPLC) as theanalysis technique.

A review of the environmental stress cracking ofplastics has been produced by Wright (315).

12.3 Contamination Problems

Plastic products can fail, both aesthetically andphysically, because of contaminants. Chemicalresistance and electrical failure are less likely causesof failure as this type of contaminant is not usuallypresent at a high enough concentration.

Contamination can enter the product stream either inthe ingredients used in the production, or during the

manufacturing stage (e.g., mixing, extruding ormoulding).

More often than not this contamination is in the formof solid, discreet entities which makes their removalfrom the product relatively easy. Once removed themicroscopic techniques IR and Edax are excellent atobtaining assignment data in a cost effective way.Where enough of the contaminant is obtainable (e.g.,1 mg), and if a mixture of chemicals is suspected, abulk composition by TGA can be obtained. Ifidentification problems are still occurring, moresophisticated techniques such as GC-MS, SIMS andLIMA can be employed. Where the contamination isin a liquid form, a similar analytical regime can be used.A number of plastic products can suffer from solidinclusions, but it is probably most common in extrudedproducts such as car door seals.

It is also possible to use a Raman microscope systemfor the analysis of contaminants in plastic materials(293). One situation where the technique is particularlyuseful is in the identification of very small (e.g., a fewmicrometers in diameter) polymer gel inclusions withinthe same polymer matrix. Often these gels have a higherdegree of crystallinity and Raman spectroscopy withits high spatial resolution and ability to differentiatebetween difference degrees of crystallinity is the idealtechnique to differentiate between these andcontamination by a foreign material.

Contamination of plastics products by a species at alow level (i.e., less than 1% or at ppm levels) cansometimes be important, for example if a product is tobe used in the pharmaceutical industry. If it is suspectedthat the contaminant is, or contains, a metal, then AAScan be employed. If the presence of an organic moleculeis suspected, then headspace GC-MS can be used toidentify and quantify the species. The high sensitivityof this technique normally makes the use of a controlsample extremely important for a quick interpretationof the output, which is often complex.

12.4 Odour and Emissions Problems

The continuing drive to improve customer care and thehigh profile of health and safety issues, has led topressure on the suppliers of plastics components tocertain industries to minimise odours, and volatiles ingeneral, from their products. This is particular true ofthe automotive industry.

There are a number of specific tests that automotivecompanies insist that plastics components manufactured


38

by suppliers have to pass. An example of such a test isthe VW emissions test which involves placing thecomponent in a cell of given dimensions and heatingthe cell for a given time and a specified temperature.Rather than carry out a detailed analysis of thecomponents liberated from the component, the result isexpressed in terms of ppm of total organic compoundsas determined by an organic vapour analyser (OVA).Limits are given as to the permissible concentrations.

For quality control purposes it is the case at presentthat human smell panels will be used in preference toinstrumental analytical techniques which do not yetadequately mimic the human response. There arepractical drawbacks to this approach, leading to a lotof research going into ‘electronic noses’ utilising anumber (e.g., 32) of sensors based on organicconducting polymers. These devices enable fingerprintsof satisfactory products to be recorded which are usedas references for quality checks.

Work has been carried out to determine the additiveswhich contribute the most to the overall odour of plasticproducts. One of the most useful techniques isheadspace GC-MS. It is advisable to use the dynamicform of headspace sampling as this enables the volatilesfrom the sample to be concentrated. This benefit isimportant as some chemical species can cause an odourproblem at very low levels due to the specific sensitivityof the human nose.

For this type of work the dynamic headspace sampler(e.g., the Perkin Elmer ATD 400) is operated in adiffusion mode where the sample is heated at arelatively low temperature (e.g., 50 °C), which helpsto ensure that additional volatile species are notgenerated due to degradation of the sample, for arelatively long period of time (e.g., in excess of 30minutes). The odour species collected in the trap ofthe dynamic headspace sampler can then be analysedunder the following conditions:

Headspace trap injection temperature: 200 °C

GC column type: SGE RTX5 MS 30 m x0.25 mm, 0.25 μm film

GC column temperature –30 °C to 50 °C at 5 °C/min and then 20 °C/min

(cryogenic cooling) to 320 °C.

MS conditions 20 to 450 atomic mass unitsscanned every 0.33 s

13 Conclusion

This review describes the analysis of plastics, plasticcompounds and plastic products in as comprehensivea way as is possible within the format of a RapraReview Report. The abstracts from the RapraPolymer Library and the additional readingreferences provided should greatly assist the analystwho requires more information on recentdevelopments.

For the future, the reduction in cost of LC-MSsystems will increase their accessibility and, incombination with GC-MS, will greatly improve theefficiency and accuracy with which the analysis ofantidegradants, cure systems, plasticisers and otheradditives can be carried out. The combination ofthese two instruments will enable the full spectrumof polarity and molecular weight to be covered andenable a quantum leap in capability to be achievableby all analytical laboratories. Experiments which foryears have had to be carried out by TLC because ofthe limitations of conventional HPLC instrumentswill now be carried out by LC-MS.

The specific analysis techniques SIMS, XPS andLIMA are becoming increasing routine and, as aresult, cost effective for consultants to use incharacterisation and failure diagnosis work andtherefore an expansion of their use is guaranteed.

In the thermal analysis field, a number ofdevelopments have occurred in recent years, withmodulated temperature forms of TGA, DSC andTMA being brought out by manufacturers.Modulating the temperature enables these techniquesto deliver better, more informative data on samples.Another development within the thermal analysisgroup is the micro-thermal analysis (micro-TA)instrument. This technique combines thetopographical mapping capabilities of a scanningprobe microscope with the ability to performlocalised thermal analysis (DTA and TMA) on amicron scale. The instrument is also capable of beingconnected to a GC-MS via a heated interface for thechemical identification of specific features.

It is clear that, even with the development of newand more advanced techniques, the analysis of plasticcompounds and products will continue to present thepolymer analyst with complex and difficultchallenges.


39

Additional References

a.1 Surface Characterisation of AdvancedPolymers, Eds., L. Sabbatini and P.G.Zambonin, Wiley-VCH, 1993.

a.2 G. Lawson and J. Sidwell, Plastics and RubberInternational, 1983, 8, 6, 15.

a.3 J.L. Koenig, Spectroscopy of Polymers,Elsevier, 1999.

a.4 T.R Crompton, Manual of Plastics Analysis,Plenum, 1998.

a.5 T.R. Crompton, Practical Polymer Analysis,Plenum Press, 1993.

a.6 Polymer Spectroscopy, Ed., A.H. Fawcett,Wiley, 1996.

a.7 J. Haslam, H.A. Willis and D.C.M. Squirrell,Identification and Analysis of Plastics, 2nd

Edition, Butterworth, 1972.

a.8 P.J. Wyatt, Analytica Chimica Acta, 1992,272, 1.

a.9 D.O. Hummel, Atlas of Polymer and PlasticsAnalysis, Volume 2, Carl Hanser Verlag, 1984.

a.10 H.B.S Conacher and B.D. Page, Journal ofChromatographic Science, 1979, 17, 188.

a.11 P. Tittareli, T. Zerlia, A. Colli and G. Ferrari,Analytical Chemistry, 1983, 55, 220.

a.12 F. Lafferty and D.B. Stauffer, Wiley/NBSRegistry of Mass Spectral Data, John Wiley &Sons, 1989.

a.13 J. Udris, Analyst, 1971, 96, 130.

a.14 A. Groagova and M.A. Pribyl, AnalyticalChemistry, 1968, 234, 423.

a.15 F. Belpaire, Revue Belge des MatieresPlastiques, 1965, 6, 201.

a.16 D. Simpson and B.R. Currell, Analyst, 1971,96, 515.

a.17 L.N. Mal’kova, A.I. Kalanin and E.M.Derepletchikova, Zhurnal AnaliticheskoiKhimii, 1972, 27, 1924.

a.18 E. Schroeder and K. Thinius, Deutsche FarbenZeitschrift, 1960, 14, 146.

a.19 E. Schroeder and S. Malz, Deutsche FarbenZeitschrift, 1958, 5, 417.

a.20 Practical Surface Analysis, Eds., D. Briggs andM.P. Seah, John Wiley and Sons, 1988.

a.21 Handbook of X-Ray PhotoelectronSpectroscopy, Ed., G.E. Muilenberg, PerkinElmer Corporation, Eden Prarie, MN, 1979(update 1992-95).

a.22 D. Brigg, A. Brown and J.C. Vickerman, ALibrary of Standard Static SIMS Spectra,Wiley, 1989.


40


41

Appendix 1

Solubility Parameters of Plastics, Plasticisers and Typical Solvents

scitsalpfosretemarapytilibuloS

epyTcitsalP retemaraPytilibuloS

EFTP 2.6

EFTCP 2.7

enelyhteyloP 0.8

enelyporpyloP 0.8

yloP t etalyrcahtemlytub- 3.8

yloP n etalyrcahtemlyxeh- 6.8

yloP n etalyrcahtemlytub- 7.8

etalyrcalytubyloP 8.8

etalyrcahtemlyhteyloP 0.9

enerytsyloP 2.9

etalyrcahtemlyhtemyloP 2.9

CVP 5.9

etanobracylopAlonehpsiB 5.9

edirolhcenedilynivyloP 2.21-8.9

esolulleclyhtE 3.01-5.8

etartin-idesolulleC 55.01

TEP 7.01

sremyloplatecA 1.11

etateca-idesolulleC 53.11

6,6nolyN 6.31

lyhtemyloP α etalyrcaonayc- 1.41

elirtinolyrcayloP 1.41

sresicitsalpfosretemarapytilibuloS

resicitsalP retemaraPytilibuloS

sliociniffaraP 5.7

sliocitamorA 0.8

etapidalytcoiD 7.8

etacabeslytcoiD 7.8

etalahthplycediD 8.8

etacabeslytubiD 9.8

etalahthplytcoiD 9.8

etalahthplyhteyxotub-2iD 3.9

etalahthplytubiD 4.9

etahpsohplynehpirT 8.9

etahpsohplylotirT 8.9

etahpsohplylyxirT 9.9

rehtelyznebiD 0.01

etalahthplyhtemiD 5.01


42

stnevlosfosretemarapytilibuloS

tnevloS retemaraPytilibuloS

enatnep-oeN 3.6

n enaxeH- 6.6

rehtelyhteiD 4.7

enoteklyporposi-iD 0.8

enaxehocyC 2.8

ces etatecalymA- 3.8

edirolhcartetnobraC 6.8

enidirepiP 7.8

enelyX 8.8

rehtelyhtemiD 8.8

eneuloT 9.8

enaporporolhciD-2,1 0.9

FHT 1.9

etatecalyhtE 1.9

enezneB 2.9

mroforolhC 3.9

)KEM(enoteklyhtelyhteM 3.9

enelyhteorolhcirT 3.9

enelyhteorolhcarteT 4.9

enahteorolhcirT 6.9

)MCD(enahtemorolhciD 7.9

enonaxeholcyC 7.9

edirolhcidenelyhtE 8.9

N,N edimatecalyhteiD- 9.9

enotecA 9.9

o enezneborolhciD- 0.01

ediflusidnobraC 0.01

N,N edimamroflyhteiD- 6.01

n lonatuB- 4.11

lonaxehocyC 4.11

elirtinotecA 9.11

N,N edimamroflyhtemiD- 1.21

dicacitecA 6.21

lonahtE 7.21

edixofluslyhtemiD 9.21

dicacimroF 5.31

lonahteM 5.41

lonehP 5.41

locylgenelyhtE 6.41

lorecylG 5.61

retaW 4.32


43

Appendix 2

Specific Gravities of Plastics and Compound Ingredients

sremylopfoseitivargcificepS

remyloP ytivarGcificepS

enelyhteylopytisnedwoL 29.0

enelyhteylopytisnedhgiH 69.0

enelyporpyloP 09.0

edirolhclynivyloP 14.1

EFTP 2.2

EFTCP 1.2

ediroulfenedilynivyloP 5.1

edirolhcenedilynivyloP 7.1

enerytsyloplatsyrC 50.1

enerytsyloptcapmimuideM 50.1

enerytsyloptcapmihgihyreV 20.1

NAS 60.1

SBAtcapmimuideM 70.1-40.1

SBAtcapmihgiH 40.1-10.1

SBM 01.1-70.1

etalahthperetenelytubyloP 13.1

etalahthperetenelyhteyloP 73.1

nisercilonehpesopruplareneG 53.1

nisercilonehp-enimaleM 6.1-5.1

edyhedlamrof-aerU 6.1-5.1

enoflusyloP 42.1

etanobracyloP 2.1

edixoenelynehpyloP 60.1

remylopomohlatecA 34.1

remylopoclatecA 14.1

edimiyloP 24.1

6,4nolyN 81.1

6,6nolyN 41.1

6nolyN 31.1

01,6nolyN 90.1

21,6nolyN 70.1

11nolyN 40.1

21nolyN 20.1


44

stneidergnignidnuopmoccitsalpfoseitivargcificepS

tneidergnI ytivarGcificepS

etacilismuinimulA 01.2

edixoirtynomitnA 04.5

nemutiB 40.1

etaflusmuiraB 03.4

etacilismuiclaC 01.2

kcalbnobraC 08.1

xawabuanraC 99.0

yalcanihcdeniclaC 05.2

)niloak(yalcanihC 06.2

erbifnottoC 50.1

locylgenelyhteiD 21.1

etihparG 40.2

edixonorI 1.5-5.4

nilonaL 80.1

)emil(edixomuiclaC 91.2

egrahtiL 03.9

edixomuisengaM 06.3

etanobracmuisengaM 12.2

aciM 08.2

liolareniM 19.0

dicacielO 09.0

lioniffaraP 08.0

xawniffaraP 09.0

nisoR 70.1

aciliS 59.1

dicaciraetS 58.0

rufluS 50.2

)etacilismuisengam(claT 08.2

)esatana(edixoidmuinatiT 09.3

)elitur(edixoidmuinatiT 02.4

etanobracmuiclaC 56.2

edixocniZ 55.5

etaraetscniZ 01.1


45

Abbreviations and Acronyms

AAS atomic absorption spectroscopy

ABS acrylonitrile-butadiene-styrene

amu atomic mass units

APCI atmospheric pressure chemical ionisation

API atmospheric pressure ionisation

ATR attenuated total reflectance

BS British standard

DCM dichloromethane

DMTA dynamic mechanical thermal analysis

DOP dioctyl phthalate

DSC differential scanning calorimetry

Edax energy dispersive analysis

EI electron ionisation

ELS evaporative light scattering

EPA Environmental Protection Agency (US)

ESC environmental stress cracking

ESI electrospray ionisation

EVA ethylene-vinyl acetate copolymer

FID flame ionisation detector

FT Fourier transform

FTIR Fourier transform infrared spectroscopy

GC gas chromatography

GC-MS gas chromatography-mass spectrometry

GPC gel permeation chromatography

HDPE high density polyethylene

HIPS high impact polystyrene

HPLC high performance liquid chromatography

ICP inductively coupled plasma

IR infrared spectroscopy

ISO International Standards Organisation

KE kinetic energy

LALLS low angle laser light scattering

LAMMS laser microprobe mass spectroscopy

LC-MS liquid chromatography-mass spectroscopy

LDPE low density polyethylene

LIMA laser induced mass analysis

LLDPE linear low density polyethylene

MALLS multi-angle laser light scattering

MBS methylmethacrylate-butadiene-styrene


46

MEK methyl ethyl ketone

micro-TA micro-thermal analysis

Mn number average molecular weight

MSD mass selective detector

Mw weight average molecular weight

Mz Z average molecular weight

NIH National Institute of Health (US)

NIST National Institute of Standards and Technology (US)

NMR nuclear magnetic resonance

NPD nitrogen/phosphorus detector

OVA organic vapour analyser

PE polyethylene

PET polyethylene terephthalate

PMMA polymethylmethacrylate

PP polypropylene

PTFE polytetrafluoroethylene

PVC polyvinyl chloride

Rf Rf value is defined as ‘the distance from the start line on the plate to the analyte spot afterdevelopment, divided by the distance from the start line to the solvent front’ and is reasonablyconstant for a given TLC plate type and developing solvent

RI refractive index

SAN styrene-acrylonitrile copolymer

SEM scanning electron microscope

SFC supercritical-fluid chromatography

SIMS secondary ion mass spectrometry

SML specific migration limits

TAC triallyl cyanurate

TAIC triallyl isocyanurate

TEM transmission electron microscopy

Tg glass transition temperature

TGA thermogravimetric analysis

THF tetrahydrofuran

TLC thin layer chromatography

Tm melting temperature

TMA thermomechanical analysis

UV ultraviolet

VA vinyl acetate

Vis visible light

XPS X-ray photoelectron spectroscopy

XRD X-ray diffraction

XRF X-ray fluorescence

References and Abstracts

© Copyright 2002 Rapra Technology Limited 47

Abstracts from the Polymer Library Database

Item 1Polymer Testing

21, No.5, 2002, p.591-5

SPECTROSCOPIC BEHAVIOUR OF POLYVINYLALCOHOL FILMS WITH DIFFERENTMOLECULAR WEIGHTSAbd El-Kader K M; Orabi A S

Suez Canal,University

Details are given of the preparation of PVAL films by a

casting technique. Optical absorption and transmission

measurements were performed. The identification of

molecular structures and assignments of energy bands

were also studied using FTIR and NMR. Correlations

between refractive index and molecular weight were

investigated. 17 refs.

EGYPT

Accession no.856878

Item 2International Journal of Polymeric Materials

51, No.4, 2002, p.315-23

EFFECTS OF CURING TEMPERATURE ONPOLY(ETHYLENE TEREPHTHALATE)Al-Raheil I A

Mu’tah,University

The effect of cure temperature over the range from 280

to 350C on PETP was investigated and changes in polymer

structure analysed by various techniques, including DSC,

TGA, scanning electron microscopy and hot-stage

microscopy. Changes in the crystallisation behaviour of

PETP at the different cure temperatures and the

morphology of the PETP spherulites are discussed and

melting data of the melt crystallised PETP at 215C are

presented. 16 refs.

JORDAN

Accession no.856733

Item 3Journal of Applied Polymer Science

84, No.8, 23rd May 2002, p.1524-32

KINETIC STUDY OF HINDERED AMINE LIGHTSTABILIZER UNDER NATURAL WEATHERINGCONDITIONSKaci M; Hebal G; Benhamida A; Boukerrou A;

Djidjelli H; Sadoun T

Bejaia,University

The photografting kinetics of a hindered amine light

stabiliser (HALS) containing a polymerisable double bond

in low density polyethylene (LDPE) films was studied

under natural weathering conditions. The HALS (PBH-

3, chemical structure shown) was added to the polymer

at a concentration of 0.3 wt.%. The photografting kinetics

were determined by spectroscopic measurement of the

absorption band area of the stabiliser around 308 nm in

the UV spectra and 1605 cm -1 in the FTIR spectra,

corresponding to benzylidene malonate and benzylidene

malonic groups respectively. Parallel measurements on

the free PBH-3 content after chloroform extraction of the

photostabiliser from the polymer matrix by UV and gas

chromatography showed that in natural weathering

grafting took place in the LDPE film after very short

exposure times of 127 and 168 hours as indicated by UV

and FTIR respectively. The curves for the photografting

and the free HALS kinetics were similar. The

photografting mechanism was thought to involve a quick

photoreaction between the methylene double bond of the

stabiliser and the polymer macroalkyl radicals, with

consequent formation of polymer-bonded aminyl

stabiliser derivatives. 24 refs.

ALGERIA

Accession no.853710

Item 4Polymer Bulletin

48, No.1, March 2002, p.43-51

PYROLYSIS OF GAMMA-IRRADIATEDBISPHENOL-A POLYCARBONATENavarro-Gonzalez R; Coll P; Aliev R

CNRS; Mexico,Universidad Nacional Autonoma

This work shows the application of quantitative pyrolysis-

gas chromatography coupled with infrared spectroscopy

and electron impact mass spectrometry in the study of

radiation-induced scission of bisphenol-A polycarbonate

(PC). PC under vacuum was gamma-irradiated using a

60Co source in the dose range from 0.125 to 1.0 MGy.

This was followed by flash pyrolysis under an inert

atmosphere observed by GC-FTIR-MS. Pyrolysis of the

irradiated PC gave different products depending on the

dose. Yields of carbon dioxide and methane decreased

with dose whereas those of phenol and 4-methylphenol

increased. The yields of benzene and toluene were

unaffected by irradiation. Analysis of the products in this

study helped to infer two main pathways for the radiation-

induced scission of PC that involve carbonate bond

rupture or aliphatic-aromatic bond rupture. 30 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;

MEXICO; WESTERN EUROPE

Accession no.853698

Item 5Journal of Polymers and the Environment

8, No.4, Oct. 2000, p.167-74

SENSITIVE ELECTROCHEMICAL IMPEDANCESPECTROSCOPY METHOD FOR DETECTIONOF POLYIMIDE DEGRADATION BY


48 © Copyright 2002 Rapra Technology Limited

MICROORGANISMSGu J-G; Cheng S-P; Liu J; Gu J-D

Shenyang,Agricultural University; Nanjing,University;

Beijing,University of Aeronautics & Astronautics;

Hong Kong,University

An electrochemical impedance spectroscopy method was

evaluated for monitoring the microbial degradation of

polyimides for electronic packaging. A mixed culture of

fungi isolated from degraded polyimides was used as the

microbial inoculum and scanning electron microscopy

was employed to examine fungi growing on the surface

of the inoculated polyimides. The data from the

microscopic analysis was utilised to further support the

relationship between changes in the impedance spectra

and microbial degradation of the polyimide. 30 refs.

CHINA; HONG KONG

Accession no.853552

Item 6PVC 2002: Towards a Sustainable Future. Proceedings

of a conference held Brighton, 23rd-25th April 2002.

London, IOM Communications Ltd., 2002. Paper 14,

p.157-65, 21cm, 012

PLATE-OUT IN PVC EXTRUSIONGilbert M; Varshney N; Van Soom K; Schiller M

Loughborough,University; Honeywell; Chemson

(Institute of Materials)

The results are reported of a study of plate-out in PVC

extrusion carried out using several analytical techniques,

including DSC, SEM-EDX, FTIR spectroscopy and laser

ionisation mass spectrometry. A special die and calibrator

unit developed to investigate plate-out are illustrated and

the reproducibility of the method evaluated. The effects

of water content and anti-plate-out additives, such as

alumina and silica, on plate-out are discussed and

mechanisms explaining the formation of plate-out are

proposed. 11 refs.

AUSTRIA; BELGIUM; EUROPEAN COMMUNITY; EUROPEAN

UNION; UK; WESTERN EUROPE

Accession no.852750

Item 7PVC 2002: Towards a Sustainable Future. Proceedings

of a conference held Brighton, 23rd-25th April 2002.

London, IOM Communications Ltd., 2002. Paper 9,

p.116-23, 21cm, 012

DETERMINING THE LEVEL OF GELATION BYODSC ON PVC WINDOW PROFILESKlingenfuss H; Zahn A

Sueddeutsches Kunststoff-Zentrum

(Institute of Materials)

The degree of gelation of PVC window profiles and of

weld beads was investigated using oscillating differential

calorimetry (ODSC). Tests carried out on a PVC dry blend

revealed that this analytical technique was capable of

determining the degree of gelation of very small samples

and permitted the determination of gelation at every point

of the profile and weld without the need for calibration

samples. 7 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;

UK; WESTERN EUROPE

Accession no.852745

Item 8Polymer International

51, No.5, May 2002, p.379-85

STUDIES OF CURE KINETICS OFPOLYISOIMIDE BY DIFFERENTIAL SCANNINGCALORIMETRY IN THE SOLID STATEKim Y J; Son G I; Kim J-H

Sung Kyun Kwan,University

Detailed kinetic studies of the thermal imidisation of

polyisoimide by DSC are described. Both isothermal and

dynamic methods were used to obtain kinetic parameters

and a phenomenological rate equation for estimating the

degree of imidisation as a function of time. 15 refs.

KOREA

Accession no.851649

Item 9Journal of Adhesion

76, No.1, 2001, p.55-74

EVALUATING CURE OF A PMDI-WOODBONDLINE USING SPECTROSCOPIC,CALORIMETRIC AND MECHANICALMETHODSHarper D P; Wolcott M P; Rials T G

Washington State,University; US,Dept.of

Agriculture,Forest Service

The cure of polymeric diphenylmethane diiso-

cyanate(pMDI)/wood bondline in a controlled saturated

steam environment was monitored using micro-dielectric

analysis(micro-DEA). Saturated steam environments were

produced between 110 and 140C. The degree of cure

calculated from micro-DEA was a basis for further

spectroscopic, calorimetric and mechanical evaluation.

Interpretation of calorimetric and spectroscopic analysis

revealed a high consumption of isocyanate early in cure.

Mechanical strength, however, as revealed by lap shear

tests, did not develop until late in cure. Low lap shear

strengths and a plateau in conversion rates were detected

for samples pressed at 110 and 120C. Several components

of the analysis suggested that low temperature cure could

result in crystal formation, leading to diffusion controlled

cure. 24 refs.

USA

Accession no.851472

Item 10Journal of Advanced Materials

34, No.2, April 2002, p.33-7



DEGREE OF CURE, HEAT OF REACTION ANDVISCOSITY OF 8552 AND 977-3 HM EPOXYRESINSNg S J; Boswell R; Claus S J; Arnold F; Vizzini A

US,Naval Air Warfare Center; Maryland,University

The heat of cure, degree of cure and viscosity of two epoxy

resins (Hexcel 8552 and Cytec Fiberite 977-3 HM) were

investigated using a modulated differential scanning

calorimeter and a rheometric digital analyser.

Mathematical models were developed to correlate the rate

of the degree of cure and the viscosity with the degree of

cure and used to predict the kinetic behaviour of the epoxy

resins, which was then compared with that of Hercules

3501-6. A comparison was also made of cure models

developed based on neat and prepreg forms of the

viscosity data. 6 refs.

USA

Accession no.850900

Item 11Polymers & Polymer Composites

10, No.3, 2002, p.237-48

CURE BEHAVIOUR AND STRUCTURE OFDICYANATE-EPOXY NOVOLAC BLENDSGuo B; Fu W; Jia D; Qiu Q; Wang L

South China,University of Technology

The objectives of this work are to investigate the cure

behaviour and structure of bisphenol A dicyanate-novolac

epoxy blends. The cure characteristics were investigated

by gel time determination and dynamic DSC. To disclose

the structural differences between cured cyanate-novolac

epoxy blends and more traditional cyanate-diglycidyl

ether systems, FTIR investigations were performed on

the two kinds of blends, and in situ FTIR was used to

examine the Bauer mechanism. The effects of epoxy

concentration in the blend on the cure kinetics was

investigated using two blends with different molar ratios,

and in situ FTIR. 33 refs.

CHINA

Accession no.850546

Item 12Macromolecular Chemistry & Physics

203, No.4, 15th March 2002, p.653-62

MISCIBILITY AND CRYSTALLIZATIONBEHAVIOUR OF POLYETHYLENETEREPHTHALATE/POLYVINYLIDENEFLUORIDE BLENDSRahman M H; Nandi A K

Indian Association for the Cultivation of Science

The miscibility of PETP and PVDF was studied. The Tg,

melting point, the crystallisation temperature and the

crystallinity values of the blends of different

compositions, prepared at different conditions were

measured. The polymer-polymer interaction parameter

was measured from equilibrium melting point depression

data. 50 refs.

INDIA

Accession no.850061

Item 13Chichester, John Wiley & Sons, 1999, pp.xiv,409.

23cm. 911

MICROSTRUCTURAL CHARACTERISATIONOF MATERIALSBrandon D; Kaplan W D

Haifa,Technion Institute

This unreferenced book describes the technical and

theoretical aspects of a wide range of techniques for studying

the microstructure of materials, including X-ray and electron

diffraction; optical microscopy, including polarised optical

microscopy and interference microscopy; transmission and

scanning electron microscopy; X-ray microanalysis; electron

energy loss spectroscopy; and surface analysis by

photoelectron spectroscopy, Auger electron spectroscopy,

and secondary ion mass spectrometry. The techniques are

described from sample preparation through information

acquisition to interpretation of results. A final chapter

describes the derivation of quantitative structural data from

the results of these techniques. Examples used in the

book mainly involve highly ordered materials such as

metals and inorganic crystalline materials, but many of

the techniques used are applicable to polymers. Problems

for the reader are included.

ISRAEL

Accession no.849739

Item 14Polimeros: Ciencia e Tecnologia

11, No.4, Oct./Dec.2001, p.213-21

Portuguese

NEAR-INFRARED SPECTRA OFPOLYSTYRENE, POLY(METHYLMETHACRYLATE) AND POLYCARBONATEDe Araujo S C; Kawano Y

Sao Paulo,Instituto de Quimica

The near-infrared (NIR) spectra of amorphous polymers

PS, PMMA and polycarbonate (PC) are studied. The

tentative assignment of the overtone and combination

frequencies is made using the curve fitting calculations and

the local mode theory. Anharmonicity correction and

mechanical frequency are determined from a Birge-Sponer

plot. A tentative assignment of stretch overtone frequency

of CH2 and CH functional groups of PS; CH3 and CO

functional groups of PMMA; and CH, CH3 and CO

functional groups of PC is made. An anharmonicity

correction of 57 and 58 cm-1 is obtained for CH2 and CH

stretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretch

modes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3

and CO stretch modes of PC, respectively. 21 refs.

BRAZIL

Accession no.849333




35, No.7, 26th March 2002, p.2667-75

THERMAL PROPERTIES OF CROSS-LINKEDPOLYISOPROPYLACRYLAMIDE,POLYMETHACRYLIC ACID, THEIR RANDOMCOPOLYMERS, AND SEQUENTIALINTERPENETRATING POLYMER NETWORKSDiez-Pena E; Quijada-Garrido I; Frutos P; Barrales-

Rienda J M

CSIC

The thermal properties of polyisopropyl acrylamide,

polymethacrylic acid, isopropyl acrylamide-methacrylic

acid copolymers and their blends were investigated by

DSC and TGA. The state of the water was studied on the

basis of DSC traces of swollen samples. The Tg of the

same series of materials was also measured. 64 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;

WESTERN EUROPE

Accession no.849122

Item 16Applied Spectroscopy

56, No.2, Feb.2002, p.187-91

RAMAN MICROSCOPY AND MAPPING AS APROBE FOR PHOTODEGRADATION INSURFACE RELIEF GRATINGS RECORDED ONLAYER-BY-LAYER FILMS OF CONGO RED/POLYELECTROLYTEConstantino C J L; Aroco R F; He J A; Zucolotto Z; Li

L; Olveira O N; Kumar J; Tripathy S K

Windsor,University; Lowell,Massachusetts University

Raman microscopy, mapping and surface-enhanced

Raman scattering techniques are applied to investigate

the degradation of Congo Red (CR) in a surface relief

grating (SRG) recorded on electrostatically assembled

layer-by-layer film of CR alternated with polydimethyl

diallylammonium chloride (PDAC). Photoinduced

degradation is suggested by a decrease in the Raman bands

assigned to CR with a concomitant increase in the

background signal. More degradation is observed in the

valleys of the SRG, which correspond to the most

illuminated areas. In a line mapping across the SRG, the

Raman intensity of CR bands follows the modulation of

the grating, which indicates that photodegradation of CR

contributes at least partially to the SRG formation.

Surface-enhanced resonance Raman scattering (SERRS)

indicates that the phenyl ring groups are located at the

film surface. Mapping of the Raman signal over many

periods of SRG shows that, within the limits of detection,

the chromophores appear to be oriented in much the same

way throughout the film. They have no preferred

orientation in the peaks and valleys of the SRG after the

recording process is completed. 23 refs.

CANADA; USA

Accession no.848921

Item 17Injection Molding

10, No.1, Jan. 2002, p.40-4

THE MATERIALS ANALYST: PART 50. THECASE OF THE DISAPPEARING CONTAMINANTSepe M

Dickten & Masch Mfg.

A report is presented on the diagnosis of the failure of a

component made from a 33% glass-reinforced nylon 66

on the assembly line with the aid of DSC, thermal

gravimetric analysis, which was utilised to determine filler

content and type, X-ray fluorescence and IR spectroscopy.

The analytical procedures employed indicated that failure

of the component could be attributed to the presence of

chlorine probably arising from contamination of the

process by PVC.

USA

Accession no.848744

Item 18Journal of Polymer Science: Polymer Physics Edition

40, No.5, 1st March 2002, p.434-53

FREE VOLUME, GLASS TRANSITION, ANDDEGREE OF BRANCHING IN METALLOCENE-BASED PROPYLENE/ALPHA-OLEFINCOPOLYMERS: POSITRON LIFETIME,DENSITY, AND DIFFERENTIAL SCANNINGCALORIMETRIC STUDIESDlubek G; Bamford D; Rodriguez-Gonzalez A;

Bornemann S; Stejny J; Schade B; Alam M A; Arnold M

Bristol,University; ITA Institut fuer Innovative

Technologien GmbH; Martin-Luther-Universitat Halle

Results of the above studies are presented and are

discussed with particular reference to Tg and degree of

branching, local free volume and degree of branching,

local free volume and Tg, specific volume and degree of

branching, and number density of holes and degree of

branching. 56 refs.


UK; WESTERN EUROPE

Accession no.848572

Item 19Polymer Preprints. Volume 42. Number 2. Fall 2001.

Proceedings of a conference held Chicago, Il., 7th-11th

April 2002.

Washington, D.C., ACS,Div.of Polymer Chemistry,

2001, p.13-4

POSITRON ANNIHILATION SPECTROSCOPYAS A NOVEL SURFACE PROBE OF POLYMERSJean Y C; Zhang R; Mallon P; Chen H; Huang C-M; Li

Y; Zhang J; Huang Y Y; Sandreczki T C; Wu Y

Missouri-Kansas City,University

(ACS,Div.of Polymer Chemistry)

Positron annihilation spectroscopy (PAS) is a special non-

destructive evaluation (NDE) technique for materials



characterisation, which uses the positron (anti-electron).

Positron-electron annihilation gamma-rays reveal useful

information about the electronic and defect properties of

materials under study. The unique repulsive force between

the positron and the ion cores of materials makes the

positron ideal for probing defects at the atomic and

molecular levels. In recent years, PAS was developed as a

useful tool to probe the microscopic properties of polymeric

materials. One of the great successes in this line of research

is the direct determination of polymer free volume and hole

properties at an atomic scale (0.2-2 nm). Most existing PAS

studies emphasise the bulk of polymers in measuring

positron annihilation lifetime. Recently, another method

of positron annihilation radiation, Doppler broadening of

energy spectra, coupled with a slow positron beam, has

been developed to examine the defect profile near the

surface. The results of experiments on the photodegradation

of polymer-based coatings induced by 313 nm UV

irradiation as studied by slow positron annihilation

spectroscopy are reported and correlated with gloss

measurements. The sub-nanometer defect S parameter is

found to decrease with exposure time. Current results

suggest that the slow positron technique is a sensitive tool

for detecting degradation of polymers in a time much earlier

than for any existing testing methods. It is particularly

sensitive to the surface defect properties. Applications of

PAS to systems of polymers and fillers appear to be

interesting to investigate in the near future. 6 refs.

USA

Accession no.847946

Item 20Adhesives & Sealants Industry

9, No.1, Feb. 2002, p.38-40

ENHANCED DSC INSTRUMENTATIONIMPROVES DESIGN ANDCHARACTERIZATION OF ADHESIVESCassel R B

TA Instruments

The use of differential scanning calorimetry (DSC) for the

characterisation and development of adhesive products is

discussed. The Q Series DSC with Advanced Tzero

Technology from TA Instruments is described, with

reference to the advantages it affords as a new and enhanced

tool for improved design and characterisation of adhesives.

The development incorporates a new measurement

principle with an additional sensor that together provide

compensation for intrinsic instrument distortion of the DSC

signal. With distortion virtually eliminated, it is possible

to measure specific-heat capacity directly in a single scan,

and to achieve greater sensitivity and accuracy. Analysis

time is also reduced, especially for modulated temperature

differential scanning calorimetry. It’s use in curing analysis

of a two-part epoxy, and of pressure-sensitive adhesives is

demonstrated. 3 refs.

USA

Accession no.847415


35, No.5, 26th Feb. 2002, p.1797-804

LIQUID CHROMATOGRAPHY OF SYNTHETICPOLYMERS UNDER CRITICAL CONDITIONS.THE CASE OF SINGLE ELUENTS AND THEROLE OF THETA CONDITIONSMacko T; Hunkeler D; Berek D

Swiss Federal Institute of Technology; Slovak

Academy of Sciences

PMMA, polybutyl methacrylates and polystyrenes in

various solvents were investigated with bare silica gel

and silica C18 bonded phases. The effect of variations in

eluent nature on polymer retention is discussed. Critical

conditions were identified in some single eluents which

are thermodynamically poor solvents for the polymers.

37 refs.

SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERN

EUROPE

Accession no.847047


35, No.5, 26th Feb. 2002, p.1677-84

LOW-TEMPERATURE CRYSTALLIZATION OFETHYLENE-RAN-PROPYLENE COPOLYMERS.CONFORMATIONAL REARRANGEMENT OFSEQUENCES DURING THE FORMATION OFTHE AGGREGATESBracco S; Comotti A; Simionutti R; Camurati I;

Sozzani P

Milan,University; Basell Spa

Low-temperature crystallisation of ethylene-propylene

copolymers was followed by DSC and solid-state NMR.

The trans conformation fraction identifying the aggregates

was detected for all temperatures independent of thermal

history. 41 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;

WESTERN EUROPE

Accession no.847031

Item 23Macromolecular Materials and Engineering

286, No.7, 27th July 2001, p421-8

THERMOGRAVIMETRY OF THERMOPLASTICPOLYIMIDE POWDERS UNDER FOURDIFFERENT ATMOSPHERESXin-Gui Li; Mei-Rong Huang; He Bai; Yu-Liang Yang

Tongji,University; Tianjin Customs Central Laboratory;

Fudan,University

The high resolution thermogravimetry technique uses a

variable heating rate response to changes in the weight

loss rate to both reduce test times and improve definition.

The thermal degradation of a thermoplastic polyimide

polymer in nitrogen, helium, argon and air was analysed

using both conventional and high resolution



thermogravimetric analysis techniques. It was concluded

that the thermal degradation results varied with both

atmosphere and test technique with the high resolution

technique providing more precise data in the inert

atmosphere tests but less resolution in air.

Thermogravimetric analysis data for a number of

polyimide polymers is tabulated. The thermoplastic

polyimide polymer evaluated was more thermally stable

than many other polyimides. Complete details of the test

techniques are given with full discussion of the results.

40 refs.

CHINA

Accession no.846773


83, No.12, 2002, p.2522-7

CRYSTALLIZATION AND CROSSLINKING OFPOLYAMIDE-1010 UNDER ELEVATEDPRESSUREJun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu;

Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui Su

Changchun,Institute of Applied Chemistry;

Jilin,University

This study looked at the structural changes to polyamide-

1010 (PA1010) when it was treated at 250 degC for 30

min at a pressure of 0.7-2.5 GPa. Crystals grew when the

pressure was below 1.0 GPa or above 1.2 GPa.

Crosslinking occurred in the pressure range 1.0-1.2 GPa.

DSC and wide angle x-ray diffraction showed that PA1010

lost its crystallisation ability after treatment at pressures

of 1.0-1.2 GPa. Crystallised PA1010 had a greater thermal

stability than crosslinked PA1010 at 400 degC. 20 refs.

CHINA

Accession no.846587

Item 25Kautchuk und Gummi Kunststoffe

55, No.1-2, 2002, p.9-14

German

ANALYSIS OF TECHNICAL POLYMER BLENDSWITH COUPLING OF LIQUIDCHROMATOGRAPHY WITH FTIRSPECTROSCOPYPasch H; Rode K; Kloninger C; Esser E

Deutsches Kunststoff-Institut

The coupling of liquid chromatography with FTIR

spectroscopy provides a new and interesting method for

the detailed analysis of complex polymer systems. The

application of this hyphenated technique to the analysis

of polymer blends shows that it is possible to identify the

different blend components by their spectral

characteristics. Components of different chemical

compositions are determined selectively and their

chemical structure is analysed through well-resolved

FTIR spectra. For structure elucidation, all facilities of

state-of-the-art FTIR spectroscopy can be used. From the

chromatographic and spectroscopic data, contour

diagrams are generated that present the molecular

heterogeneity of the sample in the coordinates molar mass

and chemical composition. 17 refs.


WESTERN EUROPE

Accession no.846265

Item 26Polymer

43,No.6,2002,p.1835-47

THERMAL DEGRADATION OF PET ANDANALOGOUS POLYESTERS MEASURED BYTHERMAL ANALYSIS-FOURIER TRANSFORMINFRARED SPECTROSCOPYHolland B J; Hay J N

Birmingham,University

The thermal degradation of two commercial PET samples

and two laboratory prepared polyesters, poly(ethylene

isophthalate) and poly(diethylene glycol terephthalate),

was studied using thermogravimetry and thermal analysis-

FTIR. The commercial PET samples were copolymerised

with diethylene glycol and isophthalic acid groups in

different proportions, and their thermal stabilities were

found to differ. Through a study of the thermal degradation

of poly(diethylene glycol terephthalate) and poly(ethylene

isophthalate), it was found that diethylene glycol and

isophthalate units promoted thermal degradation through

increased chain flexibility and more favourable bond

angles, respectively. The thermal degradation of all the

polyesters tested led to the formation of non-volatile

residue. IR spectroscopic analysis indicated that the

residue consisted almost exclusively of interconnected

aromatic rings. 21 refs.

EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;

WESTERN EUROPE; WESTERN EUROPE-GENERAL

Accession no.846155

Item 27Progress in Organic Coatings

43, No.4, Dec.2001, p.226-32

SIMPLE RAMAN TECHNIQUE TO MEASURETHE DEGREE OF CURE IN UV CURABLECOATINGSNichols M E; Seubert C M; Weber W H; Gerlock J L

Ford Research Laboratory

The curing of four UV-curable clearcoats was studied by

confocal Raman microscopy. The disappearance of the

C:C line near 1636/cm provided the signature for the

curing of the samples, but quantification of the degree of

cure by standard peak fitting and baseline subtraction

methods did not work well because of sample

fluorescence, baseline shifts and overlapping peaks. A

smoothed second-derivative processing approach

overcame all of these difficulties and provided a simple,



rapid and objective quantification procedure. Steep cure

gradients through the thickness of the clearcoat, due to

screening of the bottom of the clearcoat by both the UVA

and photoinitiator, were observed. Cure gradients at the

top of the clearcoat due to oxygen inhibition were also

observed. The most complete cure throughout the film

thickness was obtained with a mixture of standard and

red-shifted photoinitiators. 9 refs.

USA

Accession no.846135

Item 28Polymer

43, No.5, 2002, p.1587-97

FULL COPOLYMER CHARACTERIZATION BYSEC-NMR COMBINED WITH SEC-MALDIMontaudo M S

CNR

Random copolymers with units of methyl methacrylate,

butyl acrylate, styrene and maleic anhydride were studied

by fractionating the copolymer by size exclusion

chromatography(SEC), collecting 30 to 40 fractions and

then recording both the NMR and MALDI spectra of the

fractions. In a successive step, bivariate distribution of

chain sizes and composition maps were derived from

knowledge of the molar mass, weight and composition

of the copolymer fractions. The compositional distribution

was obtained by summation of the sections of the bivariate

distribution which belonged to a narrow compositional

range. A model for SEC fractionation of copolymers was

developed which allowed prediction of the composition

and D(x) of the SEC fraction, D(x) being the ratio between

the number-average and the weight-average molar mass,

with x being the fraction number. Off-line SEC-MALDI

measurements were performed in order to measure D(x)

experimentally for the random copolymers. 31 refs.


WESTERN EUROPE

Accession no.846119


21, No.2, 2002, p.155-61

BISPHENOL A-BASED POLYCARBONATES:CHARACTERIZATION OF COMMERCIALSAMPLESDelpech M C; Coutinho F M B; Habibe M E S

Rio de Janeiro,Universidade Federal; Rio de

Janeiro,Universidade Estadual; Polialden Petroquimica SA

Samples of bisphenol A polycarbonate were characterised

by DSC, TGA, FTIR spectroscopy, size exclusion

chromatography(SEC), vapour pressure osmometry

(VPO) and viscometry. The samples exhibited the same

FTIR spectrum profile and almost the same values of Tg

and initial temp. of degradation. Slight differences were,

however, observed in differential TGA curves, which

could be due to the presence of additives. The number-

average molec.wts. of the samples, as received and

purified, were determined by VPO in two different

solvents, trichloromethane and THF. Viscometric average

molec.wts. were obtained in trichloromethane at 25C. Five

different equations were used to calculate intrinsic

viscosities and viscometric constant values. Relative

molec.wts. and polydispersities were determined by SEC,

in THF at 35C and in trichlorobenzene at 135C. It was

confirmed that the results obtained in the latter solvent

were in better agreement with those obtained by the other

techniques. 25 refs.

BRAZIL

Accession no.845967

Item 30Plastics Engineering

58, No.2, Feb. 2002, p.40/55

PLASTICS ANALYSIS - THE ENGINEERSRESOURCE FOR TROUBLESHOOTINGPRODUCT AND PROCESS PROBLEMS ANDFOR COMPETITIVE ANALYSISEzrin M

Connecticut,University

Methods for competitive analysis, troubleshooting process

and product problems, plastics analysis, analysis of failed

products and analysis of polymeric formulations are

discussed. Procedures covered include FTIR spectroscopy,

Raman spectroscopy, NMR spectroscopy, surface analysis

by spectroscopy, gas chromatography/mass spectrometry,

atomic force microscopy and techniques for analysing

unidentified formulations. 47 refs.

USA

Accession no.845139

Item 31Journal of Applied Medical Polymers

5, No.2, Autumn 2001, p.77-9

NOVEL TECHNIQUE FOR THE DETECTION OFA HINDERED AMINE LIGHT STABILIZER,BASED ON SILICON TECHNOLOGYNarayan S; Lee R E; Hallberg D; Malatesta V

Great Lakes Chemical Corp.; Great Lakes Chemical

Italia

Details are given of the development of a novel method

to detect the presence of a hindered amine light stabiliser

in PP, based on silicon technology. The method consisted

of extracting the stabiliser from the PP matrix followed

by detection and quantification using proton NMR. 3 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA;

WESTERN EUROPE

Accession no.844622

Item 32Adhasion Kleben & Dichten

45, No.12, 2001, p.34-8

German



NON-DESTRUCTIVE NUCLEAR MAGNETICRESONANCE CONTACT TECHNIQUE -EXAMPLES AND POSSIBILITIESHartwig A; Wolter B

Fraunhofer-Institut fuer Ang.Materialforschung;

Bundesministerium fuer Wirtschaft; DECHEMA

On page 25 of the November 2001 issue of Adhaesion,

Kleben & Dichten, the nuclear magnetic resonance

contact technique was introduced as a new sort of method

for non-destructive characterisation of polymers. This

article uses examples from the area of epoxy resins and

thick-layer bondings to give an impression of typical,

potential applications for this new non-destructive testing

method. 2 refs.


WESTERN EUROPE

Accession no.844288


55, No.12, Dec.2001, p.1729-32

FORENSIC ANALYSIS OF SINGLE FIBRES BYRAMAN SPECTROSCOPYMiller J V; Bartick E G

Washington G.,University; US,FBI

Microscopical analysis by FT-IR spectroscopy has been

the preferred method for obtaining additional information

on the polymeric composition of a fibre. It allows

unequivocal determination of the generic class and

frequently permits sub-classification. FT-IR analysis

cannot be conducted while the fibre is mounted due to

the strong absorption of IR radiation by glass. The fibre

must be removed from the slide and rinsed to clean off

the mounting medium before preparing the fibre. This

increases sample preparation time and the chance for

sample loss. Glass produces little response to Raman

spectroscopy. Therefore, Raman analysis of fibres can be

conducted while the fibre remains mounted on a glass

slide under coverslips. The theoretical beam width of the

laser is 0.8 mu m; thus, Raman will potentially permit

measurement of microfibres used in some fabrics in the

current market. The samples do not need to be thinned or

flattened, as with IR, because the photons are scattered

from the surface and not transmitted through the sample.

The current literature contains limited reports and citations

on the use of Raman microprobe spectroscopy for forensic

analysis of fibres. It has previously been shown that it is

possible to scan fibres while they are taped onto a glass

slide. By the same sample preparation method, it has been

demonstrated that it is possible to differentiate between

several generic and sub-generic classes of fibres. It is

illustrated that it is possible to scan through a glass

coverslip and mounting medium to obtain polymeric

identification of non-dyed fibres. 14 refs.

USA

Accession no.843701


83, No.5, 31st Jan.2002, p.956-66

SAFETY ASSESSMENT OF POLYMERICADDITIVES FOR FOOD PACKAGING:HYDROLYSIS OF POLYMERIC PLASTICISERSBY DIGESTIVE FLUIDSHamdani M; Thil L; Gans G; Feigenbaum A E

Institut National de la Recherche Agronomique; BASF AG

The safety of polymeric plasticisers capable of migrating

into food was assessed by an in vitro study of the hydrolysis

of poly(1,2-propylene adipate) (PPA) by digestive fluid

liquids. Freshly prepared simulated intestinal fluid solutions

produced a high degree of hydrolysis. As indicated by high

performance size exclusion chromatography, the bulk

plasticiser disappeared completely, and low molecular

weight oligomers were produced within 4 hours. Gas-phase

chromatography indicated no significant conversion to free

monomers after hydrolysis, and NMR tests showed that

the cleavage selectivity occurred selectively at primary ester

linkages. Silica gel fractionation of the hydrolysate gave

six oligomeric fractions, which were recovered and

analysed. Proton NMR was used to evaluate the absolute

molecular weight of the plasticisers and the hydrolysis

products. Under simulated gastric and saliva conditions the

degree of hydrolysis was less than 2%. 3 refs.


GERMANY; WESTERN EUROPE

Accession no.842741


81, No.7, 15th Aug.2001, p.1588-94

CHARACTERIZATION OF BRANCHEDPOLYMERS BY SIZE EXCLUSIONCHROMATOGRAPHY COUPLED WITHMULTIANGLE LIGHT SCATTERINGDETECTOR. I. SIZE EXCLUSIONCHROMATOGRAPHY ELUTION BEHAVIOR OFBRANCHED POLYMERSPodzimek S; Vlcek T; Johann C

Wyatt Technology Corp.; Pardubice,University; Wyatt

Technology Deutschland GmbH

The elution behaviour of randomly branched PS and star-

branched poly(benzyl methacrylate) with different levels

of branching was studied by size exclusion

chromatography (SEC) coupled with a multiangle light

scattering detector. The highly branched polymers showed

abnormal SEC elution behaviour. After normal elution at

small elution volumes, the molar mass and root mean

square radius of the eluting molecules increased with

increasing elution volume. Reasons for this were explored

and discussed. SEC separation was compared with

separation by thermal field flow fractionation. 8 refs.

CZECH REPUBLIC; EUROPEAN COMMUNITY; EUROPEAN

UNION; GERMANY; USA; WESTERN EUROPE

Accession no.842695



Item 36Revista de Plasticos Modernos

81, No.538, April 2001, p.461-6

Spanish

APPLICATION OF INFRARED SPECTROSCOPYAND THERMAL ANALYSIS IN MONITORINGTHE CURE OF THERMOSETTING RESINSUSED IN THE AIRCRAFT INDUSTRYSanchez-Blazquez A

CASA

The amine cure of Hexcel 8552 epoxy resin, for use as

the matrix in carbon fibre-reinforced composites for

application in aircraft construction, was monitored by

near-infrared spectroscopy. This technique was validated

by comparison of the results with those obtained by

modulated DSC. 18 refs.

HEXCEL COMPOSITESEUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;

WESTERN EUROPE

Accession no.842573

Item 37Progress in Colloid & Polymer Science

Vol.117, 2001, p.167-71

SURFACE CHARACTERISATION OFPOLYLACTIDE/POLYGLYCOLIDECOPOLYMERSKiss E; Lam C N C; Due T M; Vargha-Butler E I

Budapest,Eotvos Lorand University;

Toronto,University; Biophy Research

The wettability and the surface composition of

biodegradable polymers used as drug delivery particles

are determined and compared. Films of polylactic acid,

polyglycolic acid and their copolymers with four different

lactide, glycolide ratios of 85/15, 75/25, 65/35 and 50;

50 are formed by solvent-casting on polar (silicone wafer

glass and silica) substrates. Advancing and receding water

contact angles are measured goniometrically and also by

using the automated axisymmetric drop shape analysis

method. Both the advancing and the receding water

contact angles of the copolymers are higher than expected

from the values obtained for the two homopolymers

considering the increasing glycolide content of the

copolymers. Surface analysis of the polyester films is

performed by X-ray photoelectron spectroscopy at various

take-off angles to get information on the depth distribution

of the components. Surface enrichment of the nonpolar

(lactide) component in the outermost layer of the

copolymer films is detected. The wettability behaviour is

in accordance with the surface composition, results

suggesting a surface activity effect resulting in the

orientation of the nonpolar segments of the copolymer

chains towards the surface of the film and hence producing

more hydrophobic character for the copolymer films than

should be due to their bulk composition. 20 refs.

Accession no.842190

Item 38Synthetic Metals

124, No.2-3, 22nd Oct.2001, p.407-14

STUDY OF THE SURFACE POTENTIAL ANDPHOTOVOLTAGE OF CONDUCTINGPOLYMERS USING ELECTRIC FORCEMICROSCOPYBarisci J N; Stella R; Spinks G M; Wallace G G

Wollongong,University

The effect of the polymer composition, preparation

method and nature of the substrate on the surface potential

(SP) of conducting polymer films is investigated. Both

the average value and the distribution of SP across the

polymer surface are influenced by these factors.

Polythiophenes, potentially useful for solar energy

conversion, are used to examine the generation of light-

induced changes in SP. Results suggest the possibility of

determining the local variations of the surface

photovoltage and the photovoltaic properties of polymer

films intended for use in photovoltaic devices. 16 refs.

AUSTRALIA

Accession no.842093

Item 39Polymer Degradation and Stability

75, No.1, 2002, p.185-91

STUDY ON METHANOLYTICDEPOLYMERIZATION OF PET WITHSUPERCRITICAL METHANOL FORCHEMICAL RECYCLINGYong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu;

Yongwang Li

Chinese Academy of Sciences

Polyethylene terephthalate (PET) was subjected to

methanolytic depolymerisation with supercritical

methanol in a stirred stainless steel autoclave at

temperatures of 523-543 deg.C, pressure 8.5-14.0 MPa,

and a 3-8 methanol to PET weight ratio. The solid products

obtained, consisting mainly of dimethyl terephthalate and

small amounts of methyl-(2-hydroxyethyl) terephthalate,

bis(hydroxyethyl) terephthalate, dimers, and oligomers,

were analysed by high performance liquid

chromatography (HPLC), and the liquid products, mainly

ethylene glycol and methanol were analysed by gas

chromatography (GC). The temperature, weight ratio of

methanol to PET, and the reaction time had a very marked

effect on dimethyl terephthalate yield and the degree of

PET depolymerisation, but the effect of pressure was

insignificant above the methanol critical point. The

optimum PET depolymerisation conditions were:

temperature 533-543 K, pressure 9.0-11.0 MPa, and a

methanol to PET weight ratio of 6-8. The

depolymerisation of several PET wastes from the Chinese

market was studied under the optimum conditions. 28 refs.

CHINA

Accession no.841527




75, No.1, 2002, p.153-9

THE EFFECT OF ULTRAVIOLET STABILISERSON THE PHOTODEGRADATION OFPOLY(ETHYLENE TEREPHTHALATE)Fechine G J M; Rabello M S; Souto-Maior R M

Pernambuco,Federal University; Paraiba,Universidad

Federal

The weathering behaviour of polyethylene terephthalate

(PET) samples obtained by bi-axial tension in the

laboratory over a period of up to about 1100 hours was

studied. The mechanical properties of films obtained from

the samples having different types of UV stabilisers, e.g.

a triazine ultraviolet absorber (Tinivin 1577), carbon

black, or a TiO2/BaSO4 mixture, were tested, and the

films were examined by UV-VIS spectroscopy, titration,

size exclusion chromatography, and FTIR. The results

showed that the unstabilised films were easily degraded,

resulting in considerable deterioration in mechanical

properties and a molecular weight decrease. The triazine

was the most effective stabiliser. 38 refs.

BRAZIL

Accession no.841524


75,No.1, 2002, p.123-9

INITIAL STEPS AND EMBRITTLEMENT INTHE THERMAL OXIDATION OF STABILISEDPOLYPROPYLENE FILMSFayolle B; Audouin L; Verdu J

Ecole Nationale Superieure des Arts et Metiers

Physicochemical and mechanical characterisation

methods were used to study the oxidation of 100 micron

stabilised polypropylene films at 130 deg.C in air.

Stabiliser consumption (UV spectrophotometry) and

molecular weight decrease (steric exclusion

chromatography) could be observed during the induction

period, when no carbonyl build-up could be detected by

IR spectroscopy. These structural modifications had an

effect on the fracture properties, as indicated by the

essential work of fracture (EWF) method, whereas the

ultimate tensile elongation showed no significant changes.

The results show that the EWF method is useful for

characterising the degradation induced embrittlement of

initially ductile polymers. The experimental data reported

suggest that the problem of the spatial heterogeneity of

the oxidation process requires further discussion. 21 refs.


WESTERN EUROPE

Accession no.841521

Item 42Biomaterials

23, No.6, March 2002, p.1439-46

EFFECTS OF THE STERILISATION METHODON THE WEAR OF UHMWPE ACETABULARCUPS TESTED IN A HIP JOINT SIMULATORAffatato S; Bordini B; Fagnano C; Taddei P; Tinti A;

Toni A

Bologna,Istituti Ortopedici Rizzoli; Bologna,Universita

Details are given of the effects of sterilisation methods

on the wear and changes in physical properties of ultra-

high molecular weight PE acetabular cups. The

crystallinity of the cups was evaluated by micro-Raman

spectroscopy as a function of the inner surface position.

The partial least square calibration was used to correlate

the Raman spectra with the crystallinity of the polymer

measured by DSC. 52 refs.


WESTERN EUROPE

Accession no.840964

Item 43Polymer Preprints. Volume 41. Number 2. Conference

proceedings.

Washington, D.C., 20th-24th Aug.2000, p.1792-3

CHARACTERISATION OF PLANT FIBRES BYINFRA-RED SPECTROSCOPYGarside P; Wyeth P

Southampton,University


The application of IR spectroscopy with respect to the

characterisation of cellulosic (plant) fibres is

demonstrated. The ability to characterise fibres is of

importance to textile conservators, as this information aids

in the determination of the age and origin of the artefact

from which they are taken, and may influence the choice

of treatment. The fibres under examination are taken

largely from the bast group (flax, hemp, jute and ramie);

in addition, sisal and cotton are compared. FT-IR

microspectroscopy and ATR techniques are employed. To

complement the conventional use of these methods, the

inherent polarisation effects of the equipment are

exploited to record polarised IR spectra. Jute, sisal and

cotton are readily differentiated, but flax, hemp and ramie

prove more difficult to distinguish. Peak ratio techniques

are applied in the latter case. 2 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; UK;

WESTERN EUROPE

Accession no.840045

Item 44Journal of Coatings Technology

73, No.923, Dec. 2001, p.43-50

ON THE USE OF THE ATOMIC FORCEMICROSCOPE TO MONITOR PHYSICALDEGRADATION OF POLYMERIC COATINGSURFACESVanLandingham M R; Nguyen T; Byrd W E; Martin J W

US,National Inst.of Standards & Technology



Changes in the surface properties of a model thermosetting

acrylic melamine polymeric coating system similar to

systems widely used as automotive clearcoats were

followed using atomic force microscopy (AFM). The

samples were exposed to a range of relative humidities,

different temperatures and various UV wavelengths and

a full factorial experimental design was utilised. A

mechanism for the formation of pits in the surface of the

coatings, as observed by AFM, was developed and the

relationship between the chemical and physical

degradation of the coatings discussed. 21 refs.

USA

Accession no.839365

Item 45Polymer Plastics Technology and Engineering

40, No.5, 2001, p.767-81

STABILISATION OF FREE RADICALS INFILLED OLIGOESTER ACRYLATESKadossov E B; Kovarski A L; Kasparov V V;

Zapadinski B I; Tikhonov A P

Russia,Academy of Science; Mendeleev University of

Chemical Technology

The results are reported of a study of the formation and

decay of free radicals during the photocrosslinking of an

oligocarbonate methacrylate filled with two types of silica

differing in particle size or hydroxyapatite using ESR

spectroscopy. The data are correlated with those obtained

for molecular mobility using a spin probe and the kinetics

of radical accumulation during photocrosslinking are

discussed along with the kinetics of termination of

radicals. 17 refs.

RUSSIA

Accession no.839176


81, No.537, March 2001, p.345-52

Spanish

ANALYSIS OF SYNTHETIC POLYMERS BYCAPILLARY ELECTROPHORESISSimo C; Barbas C; Cifuentes A

Instituto de Fermentaciones Industriales; San Pablo-

CEU,Universidad

The principles of the various modes of capillary

electrophoresis are examined, and applications of these

techniques in the molecular weight characterisation of

polymers are discussed. 40 refs.


WESTERN EUROPE

Accession no.839085


55, No.11, Nov. 2001, p.1514-22

RAMAN SPECTROSCOPY DETERMINATIONOF THE THERMOPLASTIC CONTENT WITHINEPOXY RESIN-COPOLYETHERSULFONEBLENDSvan Overbeke E; Devaux J; Legras R; Carter J T;

McGrail P T; Carlier V

Louvain,Universite Catholique; ICI

Details are given of the possibility of using Raman

spectroscopy to determine the local thermoplastic content

within an epoxy resin/copolyethersulphone blend. The

required calibration of the Raman data is presented. The

applicability of the calibrations to blends containing

chlorine-ended copolyethersulphone is discussed. Results

obtained with small or large Raman confocal holes were

also compared. 40 refs.

BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;

UK; WESTERN EUROPE

Accession no.838755


74, No.2, 2001, p.321-6

XPS CHARACTERIZATION OF FRIEDEL-CRAFTS CROSS-LINKED POLYSTYRENEJianqi Wang; Jianxin Du; Hongyang Yao; Wilkie C A

Beijing,Institute of Technology; Marquette,University

The combination of a difunctional alkylating agent, either

hydroxymethylbenzyl chloride or alpha,alpha’-dichloroxylene, with PS or high-impact PS together with

a Friedel-Crafts catalyst, 2-ethylhexyldiphenylphosphate,

and an amine for reaction with hydrogen chloride was

studied by X-ray photoelectron spectroscopy. The results

confirmed the theories proposed from previous

investigations using TGA, i.e. crosslinking of the polymer

occurred as the temp. was raised and the alcohol-

containing alkylating agent gave a greater amount of

crosslinking than did the dichloro compound. 13 refs.

CHINA; USA

Accession no.838285


202, No.16, 7th Nov. 2001, p.3228-33

CHARACTERIZATION OF THECROSSLINKING KINETICS OF A THINPOLYMERIC LAYER BY REAL-TIMEDIELECTRIC RELAXATION SPECTROSCOPYSchonhals A; Fritz A; Pfeiffer K

Berlin,University; Micro Resist Technology GmbH

The crosslinking kinetics of a thin polymeric layer on a

prepolymer of a phthalic acid diallyl ester was studied by

real-time dielectric spectroscopy. Activation energies were

estimated for the reaction using the temperature

dependence of the time constant. The change of the

relaxation rate of the dynamic Tg with the reaction time

was obtained from dielectric loss data. 20 refs.




WESTERN EUROPE

Accession no.838158

Item 50LCGC Europe

14, No.12, Suppl., Dec.2001, p.8/21

CONSIDERATIONS ON COLUMN SELECTIONAND OPERATING CONDITIONS FOR LC-MSSandra P; Vanhoenacker G; Lynen F; Li L; Schelfaut M

Kortrijk,Research Institute for Chromatography;

Ghent,University

Mass spectrometry is slowly, but surely becoming the

detection system of choice for liquid chromatography

analysis in many areas. An overview is presented of

column and mobile phase selection for LC-MS. Relatively

simple guidelines are advanced to successfully optimise

LC-MS for several applications. This article discusses the

fundamentals of LC related to MS hyphenation, adapting

LC to LC-MS methods, normal-phase liquid

chromatography, supercritical fluid chromatography,

reversed-phase liquid chromatography, size exclusion

chromatography, ion-exchange chromatography, affinity

chromatography and capillary electrophoresis. 25 refs.


WESTERN EUROPE

Accession no.837996

Item 51Polymer

42, No.20, 2001, p.8461-7

STATES OF WATER IN DIFFERENTHYDROPHILIC POLYMERS - DSC AND FTIRSTUDIESPing Z H; Nguyen Q T; Chen S M; Zhou J Q; Ding Y D

Fudan,University; Rouen,University

Differential scanning calorimetry and Fourier transform

infrared spectroscopy techniques were used to study the

structure of water molecules in polyvinyl alcohol and

polyethylene grafted acrylate hydrophilic polymers.

Varying amounts of water were added to test samples and

the samples conditioned to the sorption equilibrium state

in sealed containers for 24 hours prior to evaluation. It was

concluded that below a threshold water content, depending

on the polymers physical and chemical structure, water

molecules absorbed in hydrophilic polymer cannot form

ice crystals in the polymer matrix. Above this threshold

content, the water crystallises but below zero. It was also

demonstrated that the absorbed water in hydrophilic

polymers develops differing hydrogen bonds in the first

and second hydration layers. It was concluded that the

potential influence of these intermolecular interactions

should therefore be taken into account whenever a polymer

is used with a solvent. 25 refs.

CHINA; EUROPEAN COMMUNITY; EUROPEAN UNION;

FRANCE; WESTERN EUROPE

Accession no.837027

Item 52Polymer

42, No.20, 2001, p.8425-34

PHYSICAL AND MECHANICAL PROPERTIESOF POLYETHYLENE FOR PIPES IN RELATIONTO MOLECULAR ARCHITECTURE. PART I.MICROSTRUCTURE AND CRYSTALLISATIONKINETICSHubert L; David L; Seguela R; Vigier G; Degoulet C;

Germain Y

Institute Nationale des Sciences Appliquees; Atofina

Five high density polyethylene bimodal copolymers with

varying molecular architectures designed for pipe

applications were tested to evaluate the relationships

between structure properties contributing towards

improved end use properties. Crystallisation kinetics were

studied in relation to molecular architecture using

chromatography, density columns, differential scanning

calorimetry, X-ray scattering, rising temperature elution

fractionation and infrared spectroscopy. From the test

results, it was concluded that the normal correlation

between kinetics, molecular structure and molecular

topology found with unimodal copolymers does not apply

with bimodal copolymers as the crystal surface free energy

was sensitive to topological changes resulting from

architectural molecular changes. Complete details of the

experimental procedures and test results are given with

extensive discussion of the background theory and results.

60 refs.


FRANCE; WESTERN EUROPE

Accession no.837023

Item 53LCGC Europe

14, No.9, Sept. 2001, p.564/9

INVESTIGATION OF A NOVEL SOL-GELDERIVED STATIONARY PHASE FOR GASCHROMATOGRAPHYCervini R; Day G; Hibberd A; Sharp G; Froud A

SGE International Pty Ltd.; SGE Europe Ltd.

The effectiveness of using a novel, sol-gel material

incorporating PEG or wax as a capillary column stationary

phase is described. Chromatograms demonstrating

inertness, partitioning capability and robustness for a

range of applications are presented. 10 refs.

AUSTRALIA; EUROPEAN COMMUNITY; EUROPEAN UNION;

UK; WESTERN EUROPE

Accession no.836916

Item 54Polymer Engineering and Science

41, No.10, Oct.2001, p.1714-30

TEMPERATURE MODULATED DSC STUDIESOF MELTING AND RECRYSTALLIZATION INPOLY(OXY-1,4-PHENYLENEOXY-1,4-



PHENYLENECARBONYL-1,4-PHENYLENE)(PEEK)Kampert W G; Sauer B B

DuPont Central Research & Development

The thermal and crystal morphological properties of

amorphous and melt-crystallised PEEK were investigated.

Two different molec.wts. were studied by temp.-

modulated DSC(TMDSC) over a broad range of annealing

times and temps. The lower molec.wt. PEEK under all

crystallisation conditions was found to exhibit secondary

crystal melting in the low endotherm region, followed by

melting of primary crystals superimposed with a large

recrystallisation contribution. Primary crystal melting

broadly overlapped with melting of the recrystallised

species and contributed to the broad highest endotherm.

Recrystallisation contributions and the interpretation of

TMDSC were partially confirmed by independent rapid

heating rate m.p. determinations and variable heating rate

DSC. The higher molec.wt. PEEK showed many

similarities but generally had smaller levels of

reorganisation above the annealing temp. under most

higher temp. crystallisation conditions. TMDSC provided

good resolution of recrystallisation and related events

compared with standard DSC. The broad and substantial

exothermic recrystallisation in amorphous samples was

also examined, showing that recrystallisation continued

through the final melting region. 42 refs.

USA

Accession no.836355

Item 55Macromolecular Symposia

Vol.174, Aug.2001, p.413-34

STRATEGIES IN TWO-DIMENSIONAL LIQUIDCHROMATOGRAPHIC SEPARATION OFCOMPLEX POLYMER SYSTEMSBerek D

Slovak,Academy of Sciences

The separation of complex polymer systems by two-

dimensional liquid chromatography is discussed. Methods

are reviewed in which the effect of polymer molec.wt. on

polymer retention is suppressed. The resulting ‘one

parameter separation systems’ can be on-line or off-line

connected to another separation system such as size

exclusion chromatography in order to provide more detailed

characterisation of complex polymers. Selected procedures

for the re-concentration of diluted polymer solutions are

also considered. These could be used for increasing the

concentration of sample(s) leaving the first dimension

separation column. Some arrangements for controlled

sample re-introduction into the second dimension

separation column are outlined. 48 refs. (World Polymer

Congress, IUPAC MACRO 2000, 38th Macromolecular

IUPAC Symposium, Warsaw, Poland, July 2000)

SLOVAK REPUBLIC; SLOVAKIA

Accession no.836231


81, No.536, Feb.2001, p.244-8

Spanish

PERMEABILITY OF METHANOL, TOLUENE,FUELS AND OXYGENATED FUELS IN ANETHYLENE-VINYL ALCOHOL COPOLYMERUSED AS A BARRIER COMPONENT TO GASES,AROMAS AND HYDROCARBONSLagaron J M; Powell A K

Jaume I,Universitat; BP Chemicals Ltd.

Measurements were made of the permeation rates of

methanol, toluene, a 50/50 toluene/isooctane fuel (fuel

C) and fuel C with 10% ethanol or 15% methanol through

EVOH films. Large scale methanol and water induced

plasticisation was suggested by large solvent uptakes and

confirmed by the observation of considerable decreases

in Tg. The permeability of fuel C increased significantly

when methanol was present, while the high barrier

properties of EVOH to hydrocarbons was maintained for

fuel C containing ethanol. 9 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;

WESTERN EUROPE

Accession no.835449


81, No.536, Feb.2001, p.236-43

Spanish

ETHYLENE-VINYL ALCOHOL COPOLYMERSAND THEIR APPLICATIONS IN FOODPACKAGINGCerrada M L

Instituto de Ciencia y Tecnologia de Polimeros

The gas barrier properties of ethylene-vinyl alcohol

copolymers are examined as a function of ethylene and

vinyl alcohol content, and their use in combination with

other plastics in films, bottles and other containers for

food packaging is discussed. Results are presented of a

study of the crystal structure of three copolymers having

different compositions. 11 refs.


WESTERN EUROPE

Accession no.835448


proceedings.


MAPPING CHEMICALLY HETEROGENEOUSPOLYMER SYSTEM USING CHEMICALMODIFICATION AND ATOMIC FORCEMICROSCOPYRaghavan D; Gu X; VanLandingham M; Nguyen T

Washington,Howard University; US,National Inst.of

Standards & Technology




Interactions between a film and its external environment

are strongly influenced by the surface chemistry and

morphology of the film. Extensive research has been

conducted to provide in-depth microstructural information

of thin polymer films using analytical techniques such as

small-angle X-ray scattering, X-ray photoelectron

spectroscopy, neutron scattering and secondary ion-mass

spec trometry. However, these techniques lack the lateral

resolution to detect and map the heterogeneity in polymer

films. With the advent of atomic force microscopy (AFM),

it is possible to provide direct spatial mapping of surface

topography and surface heterogeneity at nanometer

resolution. A combination of tapping mode and force

mode AFM techniques has been effective in mapping

mechanically heterogeneous regions in multi-component

polymer systems. Recent developments in chemically

functionalised AFM tips have allowed mapping of

chemically heterogeneous lithographically patterned

surfaces by AFM at the molecular scale. This technique

is known as chemical force microscopy. However,

mapping chemical heterogeneity in a polymer system by

chemical force microscopy pose difficulties because of

chain length variation and irregular packing of chains at

the probe surface. The objective is to chemically degrade

one component of a model blend and then identify the

degraded component by AFM. A model blend consisting

of polyethylene acrylate (PEA) and PS is selected due to

the difference in the hydrolysis characteristics of PEA

and PS. Acid is selected as the aggressive chemical

medium so as to accelerate the hydrolysis of one

component in the model blend film. 9 refs.

USA

Accession no.835296


proceedings.


OVERVIEW OF STATE-OF-THE-ART SPM OFCRYSTALLINE POLYMERSMiles M J; Hobbs J K; McMaster T J; Baker A A;

James P J; Blakely S T; Aissaoui M-N

Bristol,University


Scanning probe microscopy is a family of a dozen or more

microscopies essentially based on the concept and

technology of the founding member, scanning tunnelling

microscopy. The most appropriate and widely-used of

these microscopies in the study of polymer systems is

atomic force microscopy (AFM), which in many of its

modes of operation is suitable for imaging relatively soft

solids such as polymers and biological materials. In the

simplest AFM modes of operation (contact and ‘tapping’),

topographic images representing the surface of the

polymer specimen can be obtained. At the lamellar crystal

level, such images have generally confirmed morphology

and crystalline structures deduced from transmission

electron microscopy (TEM) or X-ray studies. However,

the resolution of the AFM can go beyond that easily

achievable with TEM imaging of polymers. At higher

resolution, AFM has, in some cases, revealed unpredicted

surface structures. 26 refs.


WESTERN EUROPE

Accession no.835289

Item 60Polymer

43, No.1, 2002, p.159-70

QUANTIFYING SHORT CHAIN BRANCHINGMICROSTRUCTURES IN ETHYLENE 1-OLEFINCOPOLYMERS USING SIZE EXCLUSIONCHROMATOGRAPHY AND FOURIERTRANSFORM INFRARED SPECTROSCOPY(SEC-FTIR)Deslauriers P J; Rohlfing D C; Hsieh E T

Chevron Phillips Chemical Co.

Ethylene-1-olefin copolymers are used to demonstrate an

SEC-FTIR method for the analysis of short chain

branching distribution (SCBD) across the molecular

weight distribution (MWD). The chromatograms were

obtained using the root mean square absorbance in the

3000-2700 cm power -1 spectral range (with FTIR serving

as a concentration detector). The spectra from individual

time sections of the chromatogram were then analysed

for comonomer branch levels using a chemometric

method, and the error in the reported SCB content of each

section was estimated. By using the appropriate training

sets, chemometric models for giving SCB versus

chemometric models were constructed for obtaining SCB

versus MWD profiles of enough accuracy for detecting

trends resulting from catalysis and process changes in low-

and high-density polyethylene samples. The model was

used for accurate quantification of branching levels in

polyolefins within plus or minus 0.5/1000 total carbons

(i.e. about 0.1 mol percentage) in samples having

relatively low SCB levels, i.e. less than 10 SCB/total

carbons and mixed branch types. 20 refs.

USA

Accession no.835164


82, No.7, 14th Nov.2001, p.1677-90

SURFACE MODIFICATION OF LOW DENSITYPOLYETHYLENE (LDPE) FILM ANDIMPROVEMENT OF ADHESION BETWEENEVAPORATED COPPER METAL FILM ANDLDPEJu-Shik Kong; Dong-Jin Lee; Han-Do Kim

Pusan,National University

The effects of chromic acid treatment for periods of time

between 1 and 60 minutes and oxygen plasma treatment



for periods of time between 30 and 90 seconds on the

surface of low density polyethylene films were examined

by attenuated total reflectance fourier transform infrared

spectroscopy, electron spectroscopy for chemical analysis

(ESCA), scanning electron microscopy and water contact

angle. The effect of chromic acid treatment on the tensile

strength of the samples was evaluated and tensile strength

reduced with increasing treatment time. Adhesion of

copper film to the treated surface was evaluated by a

scratch test. It was found that both surface roughness and

number of polar groups on the surface increased with

increasing treatment times of both chromic acid and

oxygen plasma, resulting in lowered water contact angle.

Blackening of a film sample occurred after 30 minutes

treatment in chromic acid. Adhesion of copper film

initially increased with increasing treatment times, but

optimum adhesion properties consistent with tensile

strength retention were established with 30 minutes

chromic acid treatment followed by 30 seconds oxygen

plasma treatment. 14 refs.

KOREA

Accession no.834851

Item 62Advanced Materials & Processes

159, No.10, Oct.2001, p.66-7

SURFACE ENGINEERING TECHNOLOGIESSudarshan T S

Materials Modification Inc.

The 15th International Conference on Surface

Modification Technologies will be held in November in

Indianapolis. This article presents a few paper abstracts

and lists the titles of the sessions. Papers include: structure

and properties of HVOF sprayed amorphous polymer

matrix nanocomposite coatings; field experience with

advanced soft-metal surfaces on carbon steel bolting

materials used in gall-prone gasketed joints that operate

at elevated temperatures; characterisation of industrial

coatings with atomic force microscopy; characterising

aluminium pretreatments for structural adhesive bonding;

the Air Force manufacturing technology laser peening

initiative; and iron aluminide based coating deposited by

high energy density processes.

USA

Accession no.834668


82, No.6, 7th Nov.2001, p.1382-90

PROPERTIES AND MORPHOLOGY OFPOLY(ETHYLENE TEREPHTHALATE) ANDHIGH-DENSITY POLYETHYLENE BLENDGuerrero C; Lozano T; Gonzalez V; Arroyo E

Nuevo Leon,Universidad Autonoma

Blends of polyethylene terephthalate (PET) and high

density polyethylene (HDPE), widely used in the soft

drinks industry, were studied with and without a

compatibiliser. The compatibilising agent was a surlyn

copolymer of ethylene and methacrylic acid partially

neutralized with zinc, the olefinic segment of which is

compatible with HDPE, whereas the carboxylic acid

groups form hydrogen bonds with the PET carbonyl

groups. Infrared spectroscopy, differential scanning

calorimetry, scanning electron microscopy, and the

mechanical properties were used to assess the

effectiveness of the compatibiliser. 29 refs.

MEXICO

Accession no.832040


73, No.3, 2001, p.467-70

CORRELATION BETWEEN THERMALPROPERTIES AND CONFORMATIONALCHANGES IN POLY(ETHYLENETEREPHTHALATE)/POLY(ETHER IMIDE)BLENDSRuvolo-Filho A; de Fatima Barros A

Sao Carlos,Universidade Federal

Virgin and recycled polyethylene terephthalate (PET) was

blended with polyether-imide (PEI) in proportions

between 0 and 50 percent PEI content and samples were

examined by differential scanning calorimetry and Fourier

transform infrared spectroscopy. All blends were

completely miscible, as indicated by a single glass

transition temperature which is dependent on blend

composition. Crystallisation rates of PET were retarded

strongly at 20 percent PEI content and above, but degree

of crystallinity was easily determined from a linear

correlation between a structural parameter measured

spectroscopically and enthalpy of fusion. Trans conformer

activation energy measurement confirmed the effects of

PEI content on crystallisation of PET. 9 refs.

BRAZIL

Accession no.831829


73, No.3, 2001, p.463-6

EFFECT OF INTERFACE MODIFICATION ONTHE PHOTO-STABILITY OF PIGMENTEDPOLYETHYLENE FILMSAnna P; Bertalan G; Marosi G; Ravadits I; Maatoug M

A

Budapest,University of Technology & Economics

Examination of the ageing characteristics of high density

polyethylene films containing phthalocyanine green and

titanium white and other pigments with those of lightly

stabilised polymer film without pigments was carried out

using tensile analysis, differential scanning calorimetry

and ultraviolet spectroscopy. The early failure of the

phthalocyanine pigmented sample, and subsequent UV



spectroscopic examination showed that the cause was

adsorption of stabilisers onto the pigment surface.

Reactive surfactant coating of pigments was shown to

considerably extend the film stability by reducing their

adsorbency. 9 refs.

EASTERN EUROPE; HUNGARY

Accession no.831828


73, No.3, 2001, p.387-92

MECHANISM OF PHOTOSTABILIZATION OFPERFLUOROPOLYETHER COATINGS BYHINDERED AMINE STABILISERSLuda M P; Camino G; Laurenti E; Novelli S;

Temtchenko T; Turri S

Torino,Universita; Centro Ricerche Ausimont

The mechanism of operation of hindered amine stabilisers

(HAS) against photodegradation in perfluoro polyethers

incorporated into a coating material of polyurethane has

been studied by infrared spectroscopy, gas

chromatography-mass spectrometry and electron spin

resonance spectroscopy. Under curing conditions

normally utilised for coil coating (280 degrees Centigrade

for 1 minute in air), the HAS was found to increase the

number of urea bridges in the polyurethane network, and

reduce the amount of unreacted isocyanate, giving a

structure which is more resistant to photooxidation.

Byproducts of the high temperature cure process, caused

by partial transformation of the HAS into -NH derivatives

act as antioxidants. The unreacted HAS was found to

slowly evaporate from the test film, but whilst present

acted as a radical scavenger. 8 refs.


WESTERN EUROPE

Accession no.831816

Item 67Plast’ 21

No.101, April 2001, p.77-9

Spanish

INFRARED THERMOGRAPHY: THE COLOURSOF HEATASCAMM

The use of IR thermography in the study of injection

moulds and injection moulded plastics parts is discussed,

and details are given of research and development projects

being undertaken by ASCAMM of Spain using this

technique.


WESTERN EUROPE

Accession no.831329

Item 68Polymers for Advanced Technologies

12, No.9, Sept, 2001, p.515-23

HIGH RESOLUTION SOLID-STATE CARBON 13NMR STUDY OF AS-CURED AND IRRADIATEDEPOXY RESINSNgono-Ravache Y; Foray M-F; Bardet M

Grenoble,University

Details are given of the effects of strong ionising

radiations on the physico-chemical modifications of

epoxy resins. The sensitivity of the epoxy resins to

radiation was determined using carbon 13 NMR. 20 refs.


WESTERN EUROPE

Accession no.831124


55, No.8, Aug. 2001, p.984-91

RAMAN AND INFRAREDMICROSPECTROSCOPIC MAPPING OFPLASMA-TREATED AND GRAFTED POLYMERSURFACESKeen I; Rintoul L; Fredericks P M

Queensland,University of Technology

A section of the surface of a predominantly PP substrate

containing a small amount of PE copolymer and a small

amount of blended EPM was characterised before and

after plasma treatment and after graft copolymerisation

with PS by means of Raman and ATR/IR mapping. The

maps constructed indicated variations in crystallinityacross the surface, the distribution of EPM and the

distribution of hydroxy groups introduced onto the surface

by plasma treatment. 24 refs.

AUSTRALIA

Accession no.830453

Item 70POLYMER PROCESSING ENGINEERING. 01.

Proceedings of a conference held June 2001.

London, IOM Communications Ltd., 2001, Paper 5,

p.46-58, 012

AT-PROCESS RAMAN SPECTROMETRY OFPOLYMER MELTSDhamdhere M; Li J; Deshpande B; Patil P; Hansen M G

Tennessee,University

(Institute of Materials; Interdisciplinary Research

Centre)

In-line monitoring of EVA extrusion was carried out using

in-line fibre optic Raman spectroscopy. Vinyl acetate

content in the random copolymer and melt indices of

various grades of the EVA were determined and vinyl

acetate content in the samples correlated using linear least

squares and PLS analysis. Hierarchical Cluster analysis was

employed as a pattern recognition technique to follow the

natural clustering tendencies of the EVA samples. 10 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA;

WESTERN EUROPE

Accession no.830358




20, No.7, 2001, p.729-40

DIRECT SOLID SAMPLING METHODS FORGAS CHROMATOGRAPHIC ANALYSIS OFPOLYMER/ADDITIVE FORMULATIONSBart J C J

Messina,University

The present ‘state of the art’ in direct solid sampling

methods for gas chromatographic analysis of additives

encapsulated in polymers is reviewed. Techniques

considered are static and dynamic headspace methods,

thermal desorption and solid phase microextraction.

Applications for each method are discussed. 54 refs.


WESTERN EUROPE

Accession no.830211

Item 72Antec 2001.Conference proceedings.

Dallas, Texas, 6th-10th May, 2001, paper 620

DETERMINATION OF CONDENSABLEVOLATILES DURING POLYMER PROCESSINGUSING AN ANALYTICAL EXTRUDERBuzanowski W C; Gunderson J; Froelicher S

Dow Chemical Co.

(SPE)

A method of collecting and analysing the volatiles created

during extrusion is described, in which the extruder is part

of the analytical instrumentation. A non-vented 19 mm (3/

4 in) single screw extruder was fitted with a right angle 3.2

mm single strand die, which in turn carried a glass tube

with a bulb near the die exit to allow for polymer swell,

and a side arm for attachment of the sampling system. The

polymer extruded into the glass tube, the less volatile

materials condensing in the tube, and the more volatile

materials being withdrawn by the side arm and trapped in

a set of three impingers containing an appropriate chilled

trapping solution. The volatiles from the glass tube were

removed by rinsing and analysed by Fourier transform

infrared spectroscopy and gas chromatography-mass

spectrometry. The trapping solutions were analysed directly.

The equipment was used to determine the influence of

extrusion time on volatile emissions from polycarbonate,

the influence of melt temperature on volatile loss from a

polycarbonate/styrene-acrylonitrile copolymer blend, and

the influence of additives on volatile loss from a glass-

filled polymer. 6 refs.

USA

Accession no.830052


81, No.8, 22nd August 2001, p.1902-13

DYNAMIC MECHANICAL ANALYSIS STUDYOF THE CURING OF PHENOL-

FORMALDEHYDE NOVOLAC RESINSMarkovic S; Dunjic B; Zlatanic A; Djonlagic J

Belgrade,University

Using dynamic mechanical analysis the curing reactions

of typical phenol-formaldehyde novolac resins were

followed. The evolution of various rheological parameters

was recorded for samples of the resins on cloth. A third-

order phenomenological equation described the curing

reaction. The influences of the structure, composition and

physical treatment on the curing kinetics were evaluated.

20 refs.

EASTERN EUROPE; YUGOSLAVIA

Accession no.829458


81, No.11, 12th Sept.2001, p.2779-85

RIGID AMORPHOUS PHASE AND LOWTEMPERATURE MELTING ENDOTHERM OFPOLY(ETHYLENE TEREPHTHALATE)STUDIED BY MODULATED DIFFERENTIALSCANNING CALORIMETRYSong M

Loughborough,University

Three similar samples of polyethylene terephthalate (PET)

prepared by isothermal cold crystallisation in the

differential scanning calorimetry (DSC) cell (PET1), meltcrystallisation at a steady cooling rate and annealing for

various times in the DSC cell (PET2), and quenching from

300 degrees centigrade to -20 degrees over a period of 5

minutes (PET3) were used to study the glass transition

effects in the rigid amorphous phase and the low

temperature melting endotherm using modulated DSC.

As annealing time increased in PET2 the increment of

heat capacity (IHC) at annealing temperature increased

and the IHC at the glass transition temperature decreased.

It was deduced that the low temperature melting

endotherm originated with transitions in the rigid

amorphous fraction, and it was noted that the glasslike

transition of this fraction occurred between glass transition

and melting temperatures. 23 refs.


WESTERN EUROPE

Accession no.829381


81, No.10, 6th Sept.2001, p.2387-98

COMPARISON OF THERMAL DEGRADATIONCHARACTERISTICS OF POLY(ARYLENESULFONE)S USING THERMOGRAVIMETRICANALYSIS/MASS SPECTROMETRYLi-Hsiang Perng

Ta Hwa,Institute of Technology

Thermogravimetric analysis with gas chromatography and

mass spectrometry were used in the analysis of the thermal



degradation of polyether sulphone (PES) and

polysulphone (PSF). Evolution of sulphur dioxide and

phenol from random chain scission in a one stage

pyrolysis was observed in both cases with apparent initial

thermal stability of the PES being lower than PSF, but

fire retardation of PES was better due to reduction of the

sulphone group by hydrogen radicals. More pyrolysis

products were identified from the PSF than from the PES.

Thermal stability of ether and sulphone groups appeared

similar in PES but in PSF the sulphone groups proved

the more stable. A simple kinetic model was developed

which showed good agreement between theoretical and

experimental pyrolysis curves for both polymers. 20 refs.

TAIWAN

Accession no.829337


81, No.12, 19th Sept.2001, p.3064-8

TEMPERATURE AND ATMOSPHEREINFLUENCES ON SMOKE COMPOSITIONDURING THERMAL DEGRADATION OFPOLY(ETHYLENE TEREPHTHALATE)Malgorzata Dzieciol; Jerzy Trzeszczynski

Szczecin,Technical University

The less volatile compounds formed during the thermal

degradation of polyethylene terephthalate (PET) under

different conditions at 200-700 deg.C in nitrogen and air

atmospheres were studied. The compounds were trapped

on a glass fibre filter and analysed by capillary gas

chromatography using a mass spectrometer (GC-MS), and

high performance liquid chromatography. The results

were tabulated, and plots were drawn of the degradation

temperatures in nitrogen and air atmospheres versus the

weight changes of terephthalic acid and monovinyl

terephthalate evolved from PET. The effects of the

atmosphere and temperature on smoke emission and

composition during PET thermal degradation were

considered. 28 refs.

EASTERN EUROPE; POLAND

Accession no.826911


34, No.15, 17th July 2001, p.5224-8

STUDIES OF MISCIBILITY BEHAVIOUR ANDHYDROGEN BONDING IN BLENDS OFPOLYVINYLPHENOL ANDPOLYVINYLPYRROLIDONEKuo S W; Chang F C

Taiwan,National Chiao Tung University

Blends of polyvinyl phenol with polyvinyl pyrrolidone

were prepared by solution casting from DMF solutions.

DSC, FTIR, and NMR were used to investigate the

hydrogen bonding and miscibility of the blend. The Tg

of the blend was determined. 22 refs.

CHINA

Accession no.825682

Item 78Journal of Thermal Analysis and Calorimetry

64, No.2, 2001, p.549-55

CRYSTALLIZATION AND MELTING OFPOLYCARBONATE STUDIED BYTEMPERATURE-MODULATED DSC (TMDSC)Schick C; Wurm A; Merzlyakov M; Minakov A;

Marand H

Rostock,University; Moscow,General Physics Institute;

Virginia,Polytechnic Institute & State University

TMDSC measurements conducted at reasonably high

frequencies for bisphenol-A polycarbonate(PC, Lexan)

allowed for the determination of base-line heat capacity.

Vitrification and devitrification of the rigid amorphous

fraction(RAF) could be directly observed. 0.01 Hz

appeared to be a reasonably high frequency for PC. The

RAF of PC was established during isothermal

crystallisation. Devitrification of the RAF seemed to be

related to the lowest endotherm. For PC, the melting of

small crystals between the lamellae was expected to yield

the lowest endotherm. 27 refs.

GENERAL ELECTRIC CO.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;

RUSSIA; USA; WESTERN EUROPE

Accession no.825045

Item 79Shawbury, Rapra Technology Ltd., 2001, p.iv, 174,

25cm, 91T

EASY IDENTIFICATION OF PLASTICS ANDRUBBERSVERLAYE G A L; ROEGES N P G; DE MOOR MO

KaHo Sint-Lieven

This book presents an identification scheme developed

over the last thirty years for thermoplastics, common

thermosets, a few copolymers and elastomers. The

techniques used are based on simple tests such as the

behaviour of polymers in liquids and in a flame. The book

also covers Infrared spectroscopy. Main headings are:

Simple tests (melting, solubility, burning characteristics,

odour recognition, dripping, flotation, halogen test,

nitrogen- and sulphur-test); Recording an IR spectrum;

Identification flow charts; Thermoplastics; Cellulose and

starch; Thermosets; Elastomers. (15 Refs)


UK; WESTERN EUROPE

Accession no.824868

Item 80UTECH 2000. Proceedings of a conference held The

Hague, Netherlands, 28th-30th March 2000.

London, 2000, Other Rigid Foam Developments

Session, Paper 1, pp.4, 012



LONG-TERM ENERGY EFFICIENCY OF PU-INSULATION FOR REFRIGERATIONSeifert H; Biedermann A

Elastogran GmbH

(Crain Communications Ltd.; European Isocyanate

Producers’ Association)

The ageing behaviour of rigid PU foams was investigated

using gas chromatographic quantitative evaluation of the

cell gas composition in the foams. The change in thermal

conductivity of the foams during ageing was also

examined as was the dimensional stability of the foams

under diffusion open conditions and the results obtained

correlated with the K x A-values from refrigerator cabinets

via the change in cell gas composition. The data obtained

revealed that the ageing process of appliances could be

simulated in a tenth of the time by measuring diffusion

opened PU foams. 2 refs.


NETHERLANDS; WESTERN EUROPE

Accession no.824859

Item 81International Polymer Science and Technology

28, No.5, 2001, p.T/79-80

STUDY OF POLYMER-FILLER INTERACTIONBY INVERSE GAS CHROMATOGRAPHYGukasyan S Z

The surface modification of fillers with polymeric

substances is discussed with reference to improvement

of the properties of filled polymers. When the fillers are

modified with polymers, the boundary layer contains not

only the matrix filler, but also the modifying polymer,

and when the modifying polymer interacts with the surface

filler, the properties of both the mineral component and

the modifier are altered. One characteristic which reflects

the result of polymer-filler interaction is the glass

transition temperature of the modifier. To determine this

parameter for a very low content of polymer, the method

of inverse gas chromatography was used using the

modified filler as the stationery phase. The study

investigated the use of travertine and tuff, the surfaces of

which were modified with latices of a copolymer of

styrene and methacrylic acid. 3 refs. (Article translated

from Plasticheskie Massy, No.8, 2000, p.36)

RUSSIA

Accession no.824324

Item 82Molecular Crystals & Liquid Crystals

Vol.353, 2000, p.95-108

COMPOSITES MADE FROMLIGNOCELLULOSICS AND THERMOSETPOLYMERSAramguren M I; Marcovich N E; Reboredo M M

INTEMA

Preparation and testing of composites from a styrene/

unsaturated polyester thermoset matrix and wood flours

from different wood species was carried out. Studies were

carried out on Pine (Pino Eliottis), eucaliptus (Eucaliptus

Saligna) and marmelero (Ruprechia Laviflora), a

softwood and two semi-hard woods, respectively. The

particles were used untreated and chemically modified

with maleic anhydride. For the characterisation of

untreated and treated flours, thermogravimetric analysis

and analytical techniques were utilised. Dispersion of the

fibrous particles, in addition to maximum fibre

concentration (accompanied by complete wetting of the

wood fibres) was dependent on the treatment and on the

wood species utilised. Bending and compression tests

suggested some improvement in the performance of the

composites, if the wood flour was previously esterified.

Changes in the fracture surfaces due to maleic anhydride

treatment of the fibres were observed using scanning

electron microscopy. 12 refs.

ARGENTINA

Accession no.824162


73, No.2, 2001, p.251-7

THERMAL CHARACTERISTICS OF ADDITION-CURED PHENOLIC RESINSReghunadhan C P; Bindu R L; Ninan K N

Vikram Sarabhai Space Centre

The thermal cure characteristics, kinetics of thermal

degradation and pyrolysis of four different addition cured

phenolic resins were investigated using various

techniques, including DSC, DMA, FTIR spectroscopy,

TGA and X-ray diffraction. Resins investigated were

propargyl ether resins and phenyl azo-, phenyl ethynyl-

and maleimide-functional resins. A comparison of the data

obtained for all the phenolic resins was made as a function

of molecular structure. 12 refs.

INDIA

Accession no.824043

Item 84UTECH 2000. Proceedings of a conference held The

Hague, Netherlands, 28th-30th March 2000.

London, 2000, Innovations: Flexible Foam

Developments Session, Paper 5, pp.4, 012

VOC DETECTION IN POLYURETHANEFLEXIBLE FOAMSOcchiello E; Tavan M; Pannocchia P; Fava F

EniChem

(Crain Communications Ltd.; European Isocyanate

Producers’ Association)

The detection of volatile organic compounds in polyols

and PU foams using SPME, gas chromatography and gas

chromatography-mass spectroscopy is demonstrated.



Accession no.823982




73, No.1, 2001, p.163-7

THERMAL, PHYSICAL AND CHEMICALSTABILITY OF POROUS POLYSTYRENE-TYPEBEADS WITH DIFFERENT DEGREES OFCROSSLINKINGYanhong Li; Yunge Fan; Jianbiao Ma

Nankai,University

The thermal decomposition of porous polystyrene beads

with differing crosslinking degrees using divinyl benzene

were evaluated using thermogravimetry and differential

scanning calorimetry techniques. The test results showed

that the thermal stability of the beads increased with higher

degrees of crosslinking. DSC analysis revealed that the

glass transition temperatures gradually increased with

crosslinking levels up to 30% crosslinking by weight, but

above this level beads were thermally stable as the glass

transition temperature was replaced by an exothermic

peak. Complete details of the testing procedures and

results are given 15 refs.

CHINA

Accession no.823950


73, No.1, 2001, p.69-74

EXAMINATION OF A LOW DENSITYPOLYETHYLENE (LDPE) FILM AFTER 15YEARS OF SERVICE AS AN AIR AND WATERBARRIERMoller K; Gervert T; Holmstrom A

Sweden,National Testing & Research Institute

Comparisons between accelerated ageing tests and tests

on polymeric materials aged in actual service conditions

to identify possible degradation mechanisms appear to

be the only reliable method of predicting long term service

lifetimes. A low density polyethylene film used as an air

and water barrier for 15 years in an exterior wall

construction was characterised using tensile testing,

spectroscopy and chromatography techniques. Although

the mechanical properties of the film were unaffected by

ageing, its antioxidant stabilisers were severely degraded.

Full details of the ageing conditions, test methods and

results are given. 16 refs.

EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERN

EUROPE

Accession no.823940


73, No.1, 2001, p.47-67

VACUUM PYROLYSIS OF COMMINGLEDPLASTICS CONTAINING PVC. PART II.PRODUCT ANALYSISMiranda R; Pakdel H; Roy C; Vasile C

Quebec,Universite Laval; Pyrovac Institute Inc.; Petru

Poni,Institute of Macromolecular Chemistry

Vacuum pyrolysis was performed on HDPE, LDPE, PP,

PS and PVC materials individually, and also on a mixed

plastics sample containing the five polymers. The main

gaseous and liquid products, including chlorinated

hydrocarbons, were identified by chromatography, and

the yields and pyrolysis products were compared for the

individual and mixed runs. The results suggested that the

pyrolysis yields of the plastics mixtures were similar to

those calculated from the pyrolysis of the individual

polymers. However, the chlorine content was lower than

expected indicating limited interaction during pyrolysis.

Full details of the experimental procedures are given

including a detailed tabulation of all the pyrolysis

products. 54 refs.

CANADA; EASTERN EUROPE; RUMANIA

Accession no.823939


73, No.1, 2001, p.15-22

THERMO-OXIDATIVE STABILITY OF PPWASTE FILMS STUDIED BY IMAGINGCHEMILUMINESCENCE

The spread of oxidation in artificially recycled PP

materials, with and without stabilisation, was monitoredusing imaging chemiluminescence techniques. The results

were compared with estimates made using Fourier

transform infrared spectroscopy and differential scanning

calorimetry techniques. It was concluded that although

the conventional techniques gave residual lifetimes of five

cycles, imaging chemiluminescence showed that a

significant reduction in oxidative stability had occurred

after only two cycles. Full details of the imaging

chemiluminescence technique used are given with

detailed results. 12 refs.

Accession no.823934

Item 89DEVELOPMENTS IN POLYMER ANALYSIS AND

CHARACTERISATION Proceedings of a conference

held Shawbury, UK, 10th May 1999.

Shawbury, 1999, Paper 4, p.1-15, 012

CHEMICAL CHARACTERISATION OFPOLYURETHANESForrest M J


(Rapra Technology Ltd.)

Polyurethane chemistry is briefly outlined, additives

generally used in polyurethanes are indicated and the

analytical techniques used to characterise the structure,

composition and properties of PUs and PU-based products

are discussed in a comprehensive manner. Techniques

covered include spectroscopic, chromatographic techniques

and miscellaneous techniques, such as wet chemistry



techniques. Sections are included dealing with the

characterisation of polymer structure and starting materials,

molecular weight determinations, characterisation of

additives and cure reaction studies. 14 refs.


WESTERN EUROPE

Accession no.822952


Vol. 169, May 2001, p.45-55

CHARACTERIZATION OF THEINTERACTIONS IN POLYMER/SILICASYSTEMS BY INVERSE GASCHROMATOGRAPHYVoelkel A; Milczewsk K; Jeczalik J

Poznan,University of Technology

The inverse gas chromatography technique, (IGC) is

presented as a method of characterisation of the

interactions in polymer-modified silica systems. The

authors propose to express the magnitude of modified

filler/polymer interactions by means of the Flory-Huggins

parameter. Polyether-urethane/modified silica systems

containing different amounts of filler were investigated,

and information relating to the physicochemical properties

of oligomer and modified silicas were presented by means

of the solubility factor to describe the properties of the

polymer layer, and the Flory-Huggins parameter which

describes the polymer-solute or mixture polymer/silica-

solute interactions. These parameters are obtained from

inverse gas chromatography experiments. The influence

of the IGC experiment temperature, the content of

modified silica, and the nature of test solute on the

evaluated parameters are presented and discussed. 7 refs.


Accession no.822644


80, No.8, 23rd May 2001, p.1305-11

EFFECT OF RECYCLED POLYPROPYLENE ONPOLYPROPYLENE/HIGH DENSITYPOLYETHYLENE BLENDSBonelli C M C; Martins A F; Mano E B; Beatty C I

Rio de Janeiro,Universidade Federal;

Florida,University

A study was made of the effects of addition of recycled

polypropylene on the incompatible blends of virgin

polypropylene with high-density polyethylene. The

characteristics of the recycled polypropylene were

determined by spectrographic and thermal analysis means.

The mechanical properties of the blends were determined.

The 50/50 blend of the two virgin polymers benefited most

from the addition of the recycled polypropylene. 9 refs.

BRAZIL; USA

Accession no.821546


72, No.1, 2001, p.175-86

CHEMICAL AND MORPHOLOGICALMODIFICATIONS OF IRRADIATED LINEARLOW DENSITY POLYETHYLENE (LLDPE)Guadagno L; Naddeo C; Vittoria V; Camino G;

Cagnani C

Salerno,University; Turin,University; Montell Italia

SpA

Spherilene technology produced films of linear low

density polyethylene which were exposed to UV

irradiation to simulate accelerated weathering.

Comparison was made with a set of films annealed at

60C and no irradiation. The resulting chemical structures

were examined using FTIR. The findings were that the

degradation is dominated by the formation of carbonyl

and vinyl species. 22 refs.


WESTERN EUROPE

Accession no.820850


72, No.1, 2001, p.31-45

FACTORS AFFECTING THE ADSORPTION OFSTABILISERS ON TO CARBON BLACK (FLOWMICRO-CALORIMETRY STUDIES). IV.SECONDARY ANTIOXIDANTSPena J M; Allen N S; Edge M; Liauw C M; Valange B

Manchester,Metropolitan University; Cabot Corp.

Using flow micro-calorimetry, X-ray photoelectron

spectroscopy and Fourier transform infra-red

spectroscopy techniques the surface activity of different

types of carbon black with secondary antioxidants (aryl

phosphites and phosphonites) have been examined. Both

in the overall adsorption activity and the levels of probe

adsorption significant differences were observed. Two

factors were reported which were found to influence the

behaviour of phosphite stabilisers. 29 refs.


UK; WESTERN EUROPE

Accession no.820835


50, No.6, June 2001, p.635-42

DEGRADATION OF HIGH BARRIERETHYLENE-VINYL ALCOHOL COPOLYMERUNDER MILD THERMAL-OXIDATIVECONDITIONS STUDIED BY THERMALANALYSIS AND INFRARED SPECTROSCOPYLagaron J M; Gimenez E; Suara J J

Jaume I,Universitat

The thermooxidative degradation of a solution cast

ethylene-vinyl alcohol copolymer (containing 32



mol.percent ethylene) used in barrier applications was

studied at three temperatures immediately above the

melting point using thermogravimetric analysis, DSC and

FTIR spectroscopy. The weight loss measured by

thermogravimetric analysis was fast at short times and

slowed down progressively. The weight loss of about 3.6

percent measured by thermogravimetric analysis resulted

from chemical alterations in the polymer. DSC showed

small changes in crystallinity, melting point and glass

transition and broadening of the melting endotherms in

samples exposed to the more severe thermooxidative

treatments. FTIR showed a transformation of the vinyl

alcohol hydroxyl groups into carbonyl groups and the

creation of double bonds. Changes in degradation kinetics,

and possibly mechanisms, were thought to occur with

increasing time. FTIR measurements indicated that

transformation of the hydroxyl groups led to a weakening

of the overall hydrogen bonding strength in the degraded

samples so a reduction in the intermolecular cohesion,

and hence the barrier properties of the copolymer, could

be anticipated. 19 refs.


WESTERN EUROPE

Accession no.819207

Item 95Polymer Science Series B

43, Nos. 3-4,March/April 2001, p.105-8

TRANSFORMATIONS OF ANTIMONY-HALOGEN- AND NITROGEN-PHOSPHORUS-BASED FLAME RETARDANTS INPOLYOLEFINS AND THEIR PERFORMANCEBogdanova V V

Belorussian,State University

Degradation products from both antimony-halogen based

and nitrogen-phosphorus based flame retardants were

studied using X-ray diffraction and atomic emission

analysis. Evidence of the retardation mechanisms in use

against combustion was obtained for each system and in

each case emission of volatile combustion inhibitors at

the degradation temperature of the polymer matrix was

the critical factor. 11 refs

BELARUS; BELORUSSIA

Accession no.818458

Item 96Polimery

45, Nos.11-12, 2000, p.51-8

Polish

PYROLYSIS GAS CHROMATOGRAPHY ANDNEW POSSIBILITIES OF ITS USE IN THEANALYSIS OF POLYMERSHetper J

Major conditions are formulated to ensure that pyrolysis

gas chromatography yields reliable and repeatable results,

particularly when non-volatile substances such as

polymers are analysed. The author’s own modification

of PGC is presented, involving the use of a pyrolysis

attachment with the mobile reaction zone. Resulting data

are compared with those obtained by conventional

pyrolysis gas chromatography. 34 refs.

Accession no.816530

Item 97New York, John Wiley & Sons, Inc., 1999, pp.xv,752

CHEMICAL SEPARATIONS- PRINCIPLES,TECHNIQUES, AND EXPERIMENTSMELOAN, C E

KANSAS STATE UNIVERSITY

This combination laboratory manual and reference source

provides a working knowledge of an array of separation

methods. In forty-two chapters, it explores all major

categories of separation. With an emphasis upon everyday

practice rather that theory, this book explains the

principles and parameters of these methods and provides

59 specific experiments to demonstrate proper procedures.

These experiments feature step-by-step protocols for each

separation scheme, precise instructions on setting up the

apparatus, and checklists for essential chemicals and

supplies. Main Headings include Separations involving

phase changes; Separations involving extraction;

Separations involving chromatography; Separations

involving ion exchange resins; Separations involving

electric fields; Separations involving flotation;

Separations involving membranes; Separations involving

miscellaneous techniques.

USA

Accession no.816497


46, No.2-3, April 2001, p.191-6

MISCIBILITY OF POLYETHERIMIDE ANDPOLYBUTYLENE NAPHTHALATE BLENDSLin C H; Wang C S

Taiwan,Kung Shan Institute of Technology;

Taiwan,National Cheng Kung University

DSC, optical microscopy, and SEM were performed to

characterise the miscibility of a blend of polybutylene

naphthalate and polyetherimide. Data were compared with

theoretical predictions. 6 refs.

CHINA

Accession no.816205

Item 99Journal of the National Institute of Materials and

Chemical Research

8, No.4, 2000, p.149-59

Japanese

POSITRONIUM FORMATION AND DIFFUSIONIN POLYMERS



Hirata K; Kobayashi Y

High-energy positrons injected into condensed matter

quickly lose their energy, become thermalised and

annihilate with one of the electrons of the medium into

gamma rays. In polymers, some of the positrons form a

hydrogen-like bound state between a positron and an

electron prior to the annihilation. This bound state is called

positronium (Ps). Ps is formed by recombination of a

positron and one of the electrons released from the

molecules in terminal positron spur. Positron-electron

recombination in the positron spur competes with other

reactions, so that the Ps formation probability depends

on various factors. The influence of additives, polar

groups and external field on Ps formation in polymers is

discussed. A possibility of using Ps as a radiation chemical

probe for polymers is described. Ps formed as a result of

positron-electron recombination interacts with a

subnanometer-size free volume hole, and diffuses over a

certain distance before annihilation. The diffusion

coefficient of Ps is determined using a chemical reaction

between Ps and an additive, and its diffusion length in

amorphous polymers is estimated to be ca.1 nm. This

result is of fundamental importance to apply Ps as a probe

for studying free volume in polymers. 68 refs.

JAPAN

Accession no.815833


80, No.11, 13th June 2001, p.2120-2

SOLID-STATE NMR AND XPS STUDIES OF PVA/SUGARCANE COMPOSITESTavares M I B; Stael G C; Gorelova M M; de Menezes

S M C

Rio de Janeiro,Cidade Universitaria

Bagasse, taken directly from the sugarcane mills, was

dried, cut to lengths of 5 mm, and blended with

poly(ethylene-co-vinyl acetate) in proportions up to 60

wt%. The composites were characterised by solid-state

nuclear magnetic resonance spectroscopy and X-ray

photoelectron spectroscopy. A homogeneous copolymer

covering on the surface of the fibres was achieved, the

samples exhibiting homogeneity at the molecular level.

The best physical interaction between the fibres and the

matrix was achieved with the sample containing 60 wt%

fibre. 10 refs.

BRAZIL

Accession no.814366


39, No.3, 1st Feb.2001, p.337-41

PHYSICAL AGING OF POLYCARBONATEINVESTIGATED BY DYNAMICVISCOELASTICITYApaki O; Horie M; Masuda T

Kyoto,University

Dynamic viscosity measurements were used to determine

the physical ageing at 110C of polycarbonate using

samples quenched from the molten state. The test results

showed that there was a memory effect in the

polycarbonate of the quenching processes, but as

equilibrium is reached then the memory becomes lost.

Evidence is shown that the structure of the polymeric

chain in the glassy state relaxes over larger segment scale

lengths because the scale of the movable segments is

related to temperature. 29 refs.

JAPAN

Accession no.814126

Item 102Polymer

42, No.13, 2001, p.5523-9

SEC-FTIR CHARACTERIZATION OF SEMI-CRYSTALLINE HDPE AND PPVerdumen-Noel L; Baldo L; Bremmers S

DSM Research

A pressure transducer in combination with the size

exclusion chromatography-FTIR technique was used to

characterise semi-crystalline materials such as HDPE and

random PP copolymers. The comonomer content (butene

for HDPE and ethylene for PP) decreased with increasing

molar mass. For two HDPE samples produced by the dualreactor process, this decrease occurred stepwise with a

constant comonomer amount on either side of the step.

For all the HDPE samples, the amount of end

unsaturations decreased with molar mass. The

concentration of side and trans unsaturations was too low

to be determined. 8 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION;


Accession no.813974


286, No.3, 30th March 2001, p.161-7

MATRIX-ASSISTED LASER DESORPTION/IONIZATION MASS SPECTROMETRY OFSYNTHETIC POLYMERS, 5A. ANALYSIS OFPOLY(PROPYLENE OXIDE)S BY COUPLEDLIQUID CHROMATOGRAPHY AT THECRITICAL POINT OF ADSORPTION ANDMALDI-TOF MASS SPECTROMETRYKeil C; Esser E; Pasch H

Darmstadt,Deutsches Kunststoff-Institut

Poly(propylene oxide)s were analysed efficiently by

coupled liquid chromatography and MALDI-TOF mass

spectrometry. The techniques were coupled via a robotic

interface where the matrix was coaxially added to the

eluate and spotted dropwise onto the MALDI target. Size

exclusion chromatography and liquid chromatography at

critical conditions of adsorption coupled to MALDI-TOF



gave useful structural information on oligomer masses

and chemical composition; The technique showed the

presence of diols and monools in addition to the triols in

poly(propylene oxide) triols. The oligomer distributions

of all functionality fractions were determined. 23 refs.


WESTERN EUROPE

Accession no.813967

Item 104Polimery

45, No.10, 2000, p.701-6

Polish

OXIDATION AND DESORPTION OF OXYGENFROM THE UPPER LAYER OF ACTIVATEDPOLYPROPYLENE FILMZenkiewicz M

Photoelectron spectroscopy was used to study oxidation

of biaxially oriented polypropylene film. X-rays and

ultrahigh vacuum associated with the method of study

were found to promote oxygen desorption from the upper

layer. 6 refs. Articles from this journal can be requested

for translation by subscribers to the Rapra produced

International Polymer Science and Technology.

Accession no.813667


34, No.8, 10th April 2001, p.2667-72

SELF-FOCUSING IN GRADIENT LIQUIDADSORPTION CHROMATOGRAPHY OFPOLYMERSDegoulet C; Perrinaud R; Ajdari A; Prost J; Benoit H;

Bourrel M

TotalFinaElf; Atofina; Elf Atochem North America

Inc.; ESPCI; Institut Curie; Institut Charles Sadron

The separation process occurring during liquid

chromatography of polymers in a gradient of composition

of the eluent was examined. The main feature was that,

after a transient regime, the concentration profile tended

to move as a front, i.e. without diffusive spreading in time.

This results in relatively sharp peaks and the observation

that long columns were useless. A simple analytical model

was proposed for this self-focussing process that allowed

optimal conditions of operation to be determined. This

analysis was supported by experimental tests. 13 refs.


USA; WESTERN EUROPE

Accession no.813456


34, No.8, 10th April 2001, p.2395-7

NONDESTRUCTIVE MEASUREMENT OF AGLASS TRANSITION TEMPERATURE AT SPIN-CAST SEMICRYSTALLINE POLYMER SURFACES

Hyun J; Aspnes D E; Cuomo J J

North Carolina,State University

A non-destructive technique for characterisation of the

surface Tg in PETP is described which involves analysis

of the variation of the ellipsometrically measured

refractive index with temp., using the spectral dependence

of the penetration depth of light to discriminate between

surface and bulk transitions. The surface Tg is shown to

be lower than that of the bulk for spin-cast semicrystalline

PETP films because of density variation and Tg is found

to be lowered further by plasma processing. 18 refs.

USA

Accession no.813421


Vol.165, March 2001, p.91-8

RECENT DEVELOPMENTS IN POLYOLEFINCHARACTERISATIONPasch H


A brief review is presented on techniques for the analysis

of polyolefins and additives in polyolefins. Techniques

considered include high-temperature GPC combined with

FTIR spectroscopy for the analysis of chemical

composition as a function of molar mass, crystallisation

fractionation for the analysis of short-chain branching inLLDPE and of polyolefin blends and pyrolysis-gas

chromatography-mass spectrometry for the determination

of additives, such as antioxidants, in polyolefins. 13 refs.

(3rd Annual UNESCO School & IUPAC Conference on

Macromolecules and Materials Science, Stellenbosch,

South Africa, 2000)


WESTERN EUROPE

Accession no.813085

Item 108Vinyltec 2000. Conference proceedings.

Philadelphia, Pa., 11th-12th Oct.2000, p.198-202

USE OF ADVANCED ANALYTICAL METHODSTO ENHANCE THE PERFORMANCE OF VINYLMATERIALSIsner J D; Eiden R W

Polymer Diagnostics Inc.

(SPE,Vinyl Div.; SPE,Philadelphia Section)

Analytical laboratories are asked to perform a variety of

test methods in order to solve problems relating to the

performance or otherwise of vinyl materials, and whilst

there are many individual problems that need to be solved,

they can be categorised, it is argued, by a relatively small

number of questions. Five of these questions are

addressed, and ways in which a laboratory may answer

them are discussed. Suggestions are made for techniques

that may be used for each question, and examples of

problems are given. Recent advances in analytical



techniques can be used to address topics such as lifetime

prediction and failure analysis. Questions related to

identification, commercialisation, competitiveness, failure

and performance.

USA

Accession no.811310

Item 109Journal of Materials Science Letters

20, No.3, 1st Feb.2001, p.257-8

COMMENTS ON A NEW RAMAN PEAK IN AHIGH-DENSITY POLYETHYLENERodriguez A B; Young R J

Navarra,Universidad Publica; Manchester,University;

UMIST

Raman spectroscopy yields information about the

molecular structure of materials based on the observation

of scattered light spectra, and has been used extensively

in the investigations of polymer structure and

composition: chemical structure and interactions,

morphology, crystalline and amorphous structure,

processing effects and orientation, etc. As an analytical

technique, however, it is not free from artefacts, i.e.

apparent experimental results that are not actually real

but are due to the experimental methods or conditions.

One factor that may be responsible for the presence of

artefacts in Raman spectroscopy is external background

light. There are numerous potential sources of external

background light that lead to sharp spectral peaks. If they

are not excluded from the collection optics of the Raman

instrument, they can lead to noise, or artefacts,

superimposed on the Raman spectrum from the sample.

This background light can come from either the sample

or from the environment around the sample. A study of

the latter is reported. 14 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;

WESTERN EUROPE

Accession no.811165


80, No.7, 16th May 2001, p.1071-84

PHASE BEHAVIOUR AND MOLECULARMOBILITY IN POLYURETHANE/STYRENE-ACRYLONITRILE BLENDSVatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis P

Kozani,Technological Education Institute;

Athens,University; Athens,Kapodistrian University

The molecular mobility and microphase separation in

blends of crosslinked polyurethane (PUR) and styrene-

acrylonitrile (SAN) copolymer were investigated. The

PUR and SAN copolymer were prepared by reactive

blending with polymer polyols. DSC, thermally

stimulated depolarisation currents (TSDC) techniques,

dielectric relaxation spectroscopy (DRS) and dynamic

mechanical thermal analysis over a wide range of

temperatures and frequencies were used in the

investigation. Results by each technique indicated that

the degree of microphase separation of PUR into hard-

segment (HS) microdomains and soft-segment (SS)

microphase increases on addition of SAN. The various

techniques used were initially compared with each other.

Results showed that for the dynamic glass transition of

the PUR SS microphase the characteristic time scales at

the same temperature are similar for DSC, TSDC and

DMTA and shorter for DRS. The PUR/SAN blends are

classified as fragile systems. 40 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;

WESTERN EUROPE

Accession no.810314

Item 111Macromolecular Rapid Communications

22, No.2, 8th Feb.2001, p.51-67

EVANESCENT WAVE LIGHT SCATTERING.FUSION OF THE EVANESCENT WAVE ANDLIGHT SCATTERING TECHNIQUES TO THESTUDY OF COLLOIDS AND POLYMERS NEARTHE INTERFACEMatsuoka H

Kyoto,University

The evanescent wave light scattering technique, which is

produced by a fusion of the evanescent wave technique

and light scattering technique, is a very powerful an useful

tool for investigation of colloidal particles and polymers

near the surface and interfaces. Two kinds of evanescent

wave light scattering apparatuses are developed. One is

the evanescent wave dynamic light scattering (EVDLS)

technique and the other is the evanescent wave light

scattering microscope (EVLSM). By EVDLS, the diffusion

behaviour of a colloidal particle near the interface can be

extracted quantitatively as a function of the distance from

the interface. The diffusion coefficient is smaller than those

for particles in bulk, reflecting electrostatic and

hydrodynamic interactions. By EVLSM, the interaction

potential profile between a colloidal particle and the surface

in dispersion can be directly evaluated. EVLSM will play

an import role in colloidal interaction studies, especially at

a low ionic strength. It is also shown that a particle dynamics

study is possible by the EVLSM technique. A new field

will be developed in colloid science and polymer science

by application of the evanescent wave light scattering

technique, i.e. fusion of the evanescent light and a scattering


JAPAN

Accession no.809623


79, No.6, 7th Feb.2001, p.1101-12

ULTRASONICATION AND MICROWAVEASSISTED EXTRACTION OF DEGRADATIONPRODUCTS FROM DEGRADABLE



POLYOLEFIN BLENDS AGED IN SOILContat-Rodrigo L; Haider N; Ribes-Greus A; Karlsson

S

Stockholm,Royal Institute of Technology;

Valencia,Polytechnical University

Degradation in soil of samples of a polyolefin blend

treated with two different biodegradable additives (a

starch/iron mixture and a commercial product (Mater-Bi

AF05H)) was studied using two non-conventional

extraction techniques. The period studied was from 0 to

21 months, and extracted products were analysed by gas

chromatography mass spectroscopy. Molecular weight

changes were monitored using high-temperature size

exclusion chromatography. Extraction techniques were

ultrasonication and microwave assisted extraction (MAE).

Reproducibility of ultrasonification was found better with

improved extraction of carboxylic acids and other

products than MAE methods, but both were found faster

than conventional (soxhlet) extraction techniques. Tables

indicate the relative amounts of different extraction

products and molecular weight changes in the polymer

blend found over the 21-month period for both

biodegradable additive types. 17 refs


SCANDINAVIA; SPAIN; SWEDEN; WESTERN EUROPE

Accession no.808785


10, No.4, Oct./Dec.2000, p.202-8

Portuguese

ETHYLENE COPOLYMERS ANALYSIS BYFRACTIONATION TECHNIQUESEscher F F N; Silva L P; Galland G B; Benetti A

Rio Grande do Sul,Universidade Federal; Ipiranga

Petroquimica SA

Ethylene-butene copolymers were fractionated according

to molecular size by direct extraction by different solvents

and at different temperatures. Samples were also

fractionated by differences in crystallinity using DSC.

Fractions were characterised using carbon 13 NMR, FTIR,

GPC and DSC. 9 refs.

BRAZIL

Accession no.808128

Item 114Journal of Polymer Science: Polymer Chemistry

Edition

39, No.5, 1st March 2001, p.630-9

NEW SEGMENTED POLYESTER-URETHANESFROM RENEWABLE RESOURCESLiu Y; Lindblad M S; Ranucci E; Albertsson A-C

Sweden,Royal Institute of Technology

The physical and mechanical properties of aliphatic

polyesters from propanediol and succinic acid were

improved by their combination with aromatic urethane

segments capable of establishing strong intermolecular

hydrogen bonds. Characterisation was carried out using

proton NMR, size exclusion chromatography, DSC, and

dynamic mechanical analysis. The influence of the ratio

of hard and soft segments on degree of crystallinity, Tg,

melting point, tensile strength, elongation and Young’s

modulus was examined. 24 refs.


EUROPE

Accession no.808057


80, No.1, 4th April 2001, p.1-9

CROSSLINKING AND ITS EFFECTS ONPOLYANILINE FILMSTan H H; Neoh K G; Liu F T; Kocherginsky N; Kang E T

Singapore,National University

Polyaniline base films with varying degrees of

crosslinking were cast from methylpyrrolidone solutions

at different processing temperatures. The effects of

crosslinking on solubility, morphology, tensile strength,

doping characteristics and transport of ions across the

films were investigated. Characterisation was undertaken

using UV visible spectroscopy, atomic force microscopy,

and elemental analysis. 18 refs.

SINGAPORE

Accession no.807643


Vol.162, Dec.2000, p.227-33

STUDY OF POLYMER COMPLEXES BYEXCLUSION CHROMATOGRAPHY COUPLEDWITH LIGHT SCATTERING IN COMBINATIONWITH FLUORESCENCE SPECTROSCOPYMrkvickova L; Pokorna V; Pecka J

Czech Republic,Academy of Sciences

PMMA stereocomplexes prepared at different

concentration in dilute tetrahydrofuran solutions are studied

by size exclusion chromatography coupled with refractive

and light scattering detectors in combination with

fluorescence spectroscopy. A considerable increase in

segment density due to complexation compared with free

PMMA chain is only slightly affected by the polymer

concentration in solution where stereocomplexes are

formed. At polymer concentrations up to 3 x 10-3 g cm-3,

an increase in non-uniformity of polymer complex

molecular weight and size and a shift to higher values of

both are observed. In semidilute solutions stereocomplexes

virtually do not become heavier and larger. 6 refs.

CZECH REPUBLIC

Accession no.806260

Item 117Polymer

42, No.8, 2001, p.3859-66



STRUCTURE FORMATION DURING THEISOTHERMAL CRYSTALLISATION OFORIENTED AMORPHOUS POLY(ETHYLENETEREPHTHALATE) FILMSRadhakrishnan J; Kaito A

Japan,National Institute of Materials & Chemical

Research

A study was made of structure formation during the

isothermal crystallisation of oriented, amorphous PETP

film from the glassy state using in situ FTIR spectroscopy,

in situ wide-angle X-ray diffraction and small angle X-

ray scattering. The PETP films were prepared by rolling

melt quenched films to a draw ratio of 2 and an evaluation

made of the changes in the conformation and orientation

order of the PETP chains during crystallisation along with

the development of crystalline structure. Structure

organisation before and during isothermal crystallisation

is discussed and a comparison made of the crystallisation

behaviour of oriented with that of isotropic PETP. 27 refs.

JAPAN

Accession no.806185


Orlando, Fl., 7th-11th May, 2000, paper 678

USE OF CONTACT-ATOMIC FORCEMICROSCOPY IN PLASTIC MATERIALSURFACESReyes E; Guerrero C

Nuevo Leon,Universidad Autonoma

(SPE)

Using thin films of isotactic polypropylene, poly(ethylene

terephthalate) and polystyrene, the range of atomic force

microscopy contact forces and the scanning frequencies

required to obtain sharp and clear 3-D images of polymer

surfaces was determined, by systematically varying these

parameters, starting with typical values used for rigid

surfaces. The optimum values were determined to be a

contact force of 88-150 nN, and a scanning frequency of

1.0-1.5 Hz. 12 refs.

MEXICO

Accession no.805686


79, No.3, 18th Jan.2001, p.473-8

PYROLYSIS GAS CHROMATOGRAPHICANALYSIS OF POLYACRYLONITRILEMinagawa M; Onuma H; Ogita T; Uchida H

Yamagata,University

In the pyrolytic gas chromatographic analysis (PGCA) of

acrylonitrile polymer under an inert atmosphere at 500-900

deg.C, lower nitriles, including methyl cyanide, HCN, and

acrylonitrile were the main degradation products, but lower

hydrocarbons, e.g. methane and ethylene, resulting from

secondary decomposition, were also detected. Thermo-

analytical data, including data on the relation between

retention time and nitrile polarity, and the limiting yield on

pyrolysis as a function of temperature were obtained. On

the basis of these results, specific applications of PGCA and

the usefulness of this method for studying the thermal

degradation of acrylonitrile polymer are indicated. 20 refs.

JAPAN

Accession no.804442

Item 120West Conshohocken, Pa., 2000, pp.3. NALOAN

ASTM D 3465-. TEST METHOD FOR PURITY OFMONOMERIC PLASTICISERS BY GASCHROMATOGRAPHYAmerican Society for Testing & Materials

ASTM D 3465-

Version 2000. Photocopies and loans of this document

are not available from Rapra.

USA

Accession no.801052

Item 121Polymer News

25, No.10, Oct.2000, p.359-60

ANALYSIS OF AIRCRAFT COATING BYSECONDARY ION MASS SPECTROSCOPYUsmani A M; Donley M

UDC; Wright-Patterson Air Force Base

An analysis was made of a flat aircraft coating using

secondary ion mass spectroscopy, which revealed that the

coating was a polyurethane C type based on isophorone

diisocyanate, diethylene glycol and adipic acid. X-ray

photoelectron spectroscopy was employed to determine

pigments and extenders. 10 refs.

USA

Accession no.800157



THERMODYNAMIC AND KINETIC ANALYSISOF SEMICRYSTALLINE RECYCLATES BY DSCCassel R B; Li L

Perkin-Elmer Inc.

(SPE)

Developments in differential scanning calorimetry (DSC)

for the characterisation of semicrystalline thermoplastics,

including mixed recyclates are discussed. The techniques

include stepwise DSC for the accurate determination of

specific heat capacity, rapid determination of crystallinity

using the Gray-Mathot total enthalpy technique, and

analysis of crystallisation kinetics. The techniques show

the influence of impurities on the glass transition

temperature, crystallinity and crystallisation. 6 refs.

USA

Accession no.799956





NOVEL TECHNIQUE FOR THE DETECTION OFA HINDERED AMINE LIGHT STABILIZER(HALS), BASED ON SILICON TECHNOLOGYNarayan S; Lee R E; Hallberg D; Malatesta V

Great Lakes Chemical Corp.; Great Lakes Chemical

Italia

(SPE)

A technique for the determination of HALS in

polypropylene was developed. The HALS, based on a

polysiloxane backbone with tetramethyl piperidine side

chains, was melt blended with the polypropylene which

was then spun into fibres. The chopped fibres were

dissolved in toluene, the polymer precipitated using

methanol, and the filtrate dried. A solution of the filtrate

was then prepared and analysed by proton nuclear

magnetic resonance spectroscopy. The peak at 0.1 ppm

was attributed to the methyl group on the silicon atom of

the HALS, and was used for quantitative purposes.

Polypropylene pellets were also prepared containing a

lower concentration of HALS, which was subsequently

subjected to direct extraction to prevent the loss which

may occur during polymer reprecipitation. 3 refs.

USA

Accession no.799954



ANALYTICAL METHODOLOGIES EMPLOYEDIN A COMPREHENSIVE FDA FOOD CONTACTCOMPLIANCE INVESTIGATION: ANALYSISFOR RESIDUAL MONOMERS, RESINOLIGOMERS, ADDITIVES AND MODIFIERS INSEVERAL FOOD SIMULATING SOLVENTSEberhard J S; McCort-Tipton M M

Covance Laboratories

(SPE)

The FDA considers that materials which come into contact

with food, such as processing machinery and packaging,

to be indirect food additives, and the potential migration

of materials into the food requires determination. Ethanol/

water solutions and food oils are commonly used as food

simulating solvents when determining migration. The

subsequent determination of the migrating species (which

may include residual monomers, oligomers, additives and

modifiers) may be by liquid and gas chromatography, and

mass spectroscopy.

USA

Accession no.799953

Item 125Polymer

42, No.4, 2001, p.1449-59

PHASE SEPARATION IN MISCIBLE POLYMERBLENDS AS DETECTED BY MODULATEDTEMPERATURE DIFFERENTIAL SCANNINGCALORIMETRYDreezen G; Groeninckx G; Swier S; Van Mele B

Leuven,Catholic University; Brussels,Free University

The phase separation of two partially miscible polymer

blends was studied using modulated temp.

DSC(MTDSC). The lower critical solution temp.

demixing behaviour of PEO blended with polyether

sulphone(PES) and with poly(3,4'-diphenylene ether

isophthaloyl amide), as determined by cloud point temps.

with optical microscopy, was in good agreement with

results obtained from non-isothermal MTDSC

measurements. The non-isothermal MTDSC apparent

heat capacity evolution was time-dependent. It was

influenced by the endothermic demixing enthalpy and,

in the case of PEO/PES blends, by the vitrification of a

high-Tg phase formed. Quasi-isothermal MTDSC

measurements contained information on the kinetics of

demixing and remixing, emphasising the added value

of MTDSC to follow in situ the diffusion-controlled

phase separation processes of partially miscible polymer

blends. 32 refs.


WESTERN EUROPE

Accession no.798922


Vol.283, Nov.2000 p.153-62

CHARACTERIZATION OF FLAME-SPRAYEDPEEK COATINGS BY FTIR-ATR, DSC ANDACOUSTIC MICROSCOPYSimonin L; Liao H

CREST; Belfort-Montbeliard,Universite de

Technologie

Poly (aryl ether ether ketone) (PEEK) was utilised as a

name-sprayed coating because of its good mechanical

properties, low friction coefficient and high thermal

stability. Fine polymeric powders were warmed up in

oxyacetylene flame and sprayed onto a previously heated

aluminium substrate. Investigation of the degree of

crystallinity of PEEK coatings was carried out using

differential scanning calorimetry (DSC), according to

the rate of cooling after the spraying process. Structural

modifications were revealed by FTIR-ATR, attributed

to interactions between the flame and the polymeric

powders. Ultrasonic methods were developed, especially

acoustic microscopy, to study the variations of

mechanical properties at the surface and the defects

inside the material. In general terms, flame-sprayed

coatings contain a large amount of porosity. Particularly

suited to the observation of large defects (exceeding 50

microns) inside the polymeric materials is low-frequency

microechography, a non-destructive technique. 19 refs.

Accession no.798668



Item 127Polymer Preprints, Volume 40, Number 2, August

1999, Conference proceedings.

New Orleans, La., August 1999, p.1043-4

MALDI/TOF/MS STUDY OF HOMOPOLYMERSAND AMPHIPHILIC DIBLOCK COPOLYMERSBASED ON SULPHONATED POLYSTYRENEYang A; Nonidez W K; Mays J W

Birmingham,University of Alabama


Matrix-assisted laser desorption ionisation time of flight

mass spectroscopy (MALDI/TOF/MS) provides a new

way to probe polymers; it can provide information on

molecular weight, molecular weight distribution, mass

of end groups and mass of repeating units. Further

information, such as reactivity ratios, individual block

chain length and its distribution, etc., can be obtained

based on mass information. Polystyrene sulphonic acid

and its sodium salt form have been successfully

characterised by MALDI/TOF/MS, but no MALDI/TOF/

MS study of diblock copolymers containing a polystyrene

sulphonic acid block appears to be evident. The results

of such a study of amphiphilic diblock copolymers,

NaPSS-b-PtBS, and their precursors, PSb-PtBS, are

reported. Number-average and weight-average molecular

weights (Mn and Mw), polydispersity indices and extents

of sulphonation are obtained. 13 refs.

USA

Accession no.798428


71, No.1, 2001, p.123-34

QUALITY-DETERMINATION OF RECYCLEDPLASTIC PACKAGING WASTE BYIDENTIFICATION OF CONTAMINANTS BY GC-MS AFTER MICROWAVE ASSISTEDEXTRACTION (MAE)Camacho W; Karlsson S

Sweden,Royal Institute of Technology

The resulted are reported of an investigation into the

quality of recycled HDPE and PP separated from mixed

municipal solid waste carried out using gas

chromatography-mass spectrometry. The development of

a simple and rapid microwave assisted extraction method

for the systematic analysis of low molec.wt. compounds,

such as decomposition products and additives, in

polymers is also reported and successfully applied to the

analysis of contaminants in the above recycled plastics.

15 refs.


EUROPE

Accession no.796627


70, No.2, Nov.2000, p.269-75

RAMAN SPECTRAL MAPPING OFPHOTOOXIDISED POLYPROPYLENEBlakey I; George G A

Queensland,University of Technology

The photooxidation of unstabilised, isotactic PP was

investigated using Raman spectral mapping in

combination with SEM/energy dispersive X-ray analysis,

which permitted the determination of Ziegler-Natta

catalyst residue distribution throughout the PP. It was

found that oxidation was heterogeneous at a microscopic

scale and that a high local concentration of catalyst

residues resulted in the stabilisation of the polymer in the

immediate vicinity and the formation of mobile reactive

species, which initiated oxidation at sites away from the

catalyst. 30 refs.

AUSTRALIA

Accession no.795269


33, No.19, 19th Sept.2000, p.7088-92

SOLUTION CARBON-13 NMRCHARACTERIZATION OF NYLON 66:QUANTITATION OF CIS AMINECONFORMERS, ACID AND AMINE GROUPS,AND CYCLIC UNIMERSSouthern Mississippi,University

Edited by: Davis R D; Steadman S J; Jatterr W L;

Mathias L J

Using a mixed 2,2,2-trifluoroethanol/deuteriochloroform

solvent system, well-resolved solution carbon-13 NMR

spectra of nylon-66 samples were obtained which showed

several low intensity peaks which were not seen in more

acidic solvents. The low intensity peaks were correlated

with the methylene carbons near cis amide conformers,

acid and amine end groups and within cyclic oligomers.

The quantitative contents of these components for a

typical nylon-66 sample were 1.1 mol% cis amide

conformers, 1.0 mol% acid end groups and 0.5 mol%

amine end groups. From end group concentrations, the

number-average molecular weight of the nylon-66 was

calculated to be 30 177 g/mol. The chemical shift values

of methylene carbons in the end groups and in cyclic

oligomers was pH sensitive and thus depended on the

relative concentrations of acid and amine groups in each

sample. 12 refs.

USA

Accession no.794402


40, No.11, Nov.2000, p.2442-55

EVALUATION OF THREE METHODS FOR THEMEASUREMENT OF CRYSTALLINITY OF PETRESINS, PREFORMS, AND BOTTLESBashir Z; Al-Aloush I; Al-Raqibah I; Ibrahim M



SABIC R & D

The crystallinity of PETP resins, preforms and bottles was

investigated using DSC, modulated DSC and density

measurements. The PETP employed was a bottle-grade

PETP copolymer containing 1.5% isophthalic acid. The

accuracy, precision and validity of the techniques

employed were evaluated and problems encountered in

interpreting the results assessed. 47 refs.

SAUDI ARABIA

Accession no.793608

Item 132Kautchuk und Gummi Kunststoffe

53, No.10, Oct.2000, p.574/81

German

DIRECT ANALYSIS OF ADDITIVES INPOLYMERIC MATERIALS BY PYROLYSIS-GASCHROMATOGRAPHY-MASS SPECTROMETRYMeyer-Dulheuer T; Pasch H; Geissler M


This article describes the direct analysis of additives by

pyrolysis-gas chromatography-mass spectrometry. Using

this method it is possible to identify additives quickly

and reliably without separation of the polymer matrix. A

small specimen of the sample is pyrolysed, i.e. degraded

under inert gas atmosphere. The pyrolysis products are

separated by gas chromatography and ionised in the massspectrometer by electron-impact ionisation. By comparing

the results with library data it is possible to identify

unknown additives unambiguously and with high

accuracy. 10 refs.


WESTERN EUROPE

Accession no.792613


61, No.2, 2000, p.589-96

CALORIMETRIC ANALYSIS OF AN ISOTACTICPOLYPROPYLENE GAMMA-IRRADIATED INVACUUMSpadaro G; Valenza A

Palermo,University

The molecular modifications induced in an isotactic PP

gamma-irradiated in vacuum under a complete set of

experimental conditions are studied by means of calorimetric

analysis. The influence of the irradiation parameters, the total

absorbed dose, D, and the dose rate, I, has previously been

analysed and a simple kinetic model based on the rates of

the main reactions occurring during irradiation, i.e. beta-

scission, addition to double bonds and termination, was also

discussed. It is shown how thermal analysis confirms the

model forecasts and in particular the existence of the

‘inversion conditions’: below them the main effect is

molecular degradation, while above them the main effects

are chain-branching and crosslinking. 12 refs.


WESTERN EUROPE

Accession no.792350

Item 134ICAC 99. Conference proceedings.

Bristol, UK, 23rd-24th Sept.1999, p.133-43

IDENTIFICATION OF KEY CURE STAGES INLIQUID MOULDING PROCESSES BYPARALLEL PLATE DIELECTRIC ANALYSISMcIlhagger A T; Matthews S T; Brown D; Hill B

Ulster,University

(IOM Communications Ltd.; Ulster,University;

IMechE)

The aerospace industry has recognised the major benefits

associated with fibre reinforced composite materials. The

more popular techniques available for composite

production are the traditional wet lay-up or autoclave and

resin transfer moulding (RTM). Efforts to further reduce

processing time and improve part quality have focused

on improved process control. To date this has been based

on off-line techniques. The need for on-line cure

monitoring is widely recognised and this will require the

development of suitable in-mould sensors. The

Engineering Composites Research Centre (ECKE) has

investigated and concentrated on the specific problems

encountered in the aerospace industry. Of the available

cure monitoring methods, parallel plate dielectric analysis

(DEA) appears to offer the greatest potential for

determining the through-thickness cure state of the resin

during cure. A laboratory dielectric instrument is utilised

to simulate RTM and autoclave cure cycles for composite

structures containing non-conductive and conductive

fibres and for different resin systems used in the aerospace

industry. Key resin cure stages are identified by an

appropriate dielectric signal and correlated with data from

other thermal and mechanical techniques. Insulated

parallel plate dielectric sensors are being developed for

use in the laboratory instrument with the potential for

incorporation into composite production tooling. 26 refs.


WESTERN EUROPE

Accession no.790059

Item 135Polymer Journal (Japan)

32, No.7, 2000, p.610-5

INFRARED SPECTROSCOPIC ANDMODULATED DIFFERENTIAL SCANNINGCALORIMETRY STUDY OF PHYSICAL AGINGIN BISPHENOL A POLYCARBONATEJin Lu; Yong Wang; Deyan Shen

Academia Sinica

FTIR spectroscopy was used to study the conformational

changes in quenched bisphenol A polycarbonate films

during physical ageing. The conformation changed

gradually from the high energy trans-cis conformation to



the low energy trans-trans conformation on sub-glass

transition temperature annealing. In-situ FTIR studies on

the conformational changes of films quenched from the

rubbery and sub-glass transition temperature annealed for

different times were carried out while increasing the

temperature through the glass transition region. The

results indicated that incremental changes in the

population of trans-cis conformers in the quenched sample

were gradual, whereas rather abrupt changes occurred in

the sub-glass transition temperature annealed samples.

The energy absorbed during the abrupt conformational

change represented only part of the endothermic peak

observed by modulated DSC. The authors concluded that

some new cohesional entanglements may be formed

during physical ageing. 28 refs.

CHINA

Accession no.789734


32, No.7, 2000, p.560-6

CALORIMETRIC AND INFRAREDSPECTROSCOPIC ANALYSIS OF MULTIPLEMELTING ENDOTHERMS OFPOLY(ETHYLENE TEREPHTHALATE)Yong Wang; Jin Liu; Deyan Shen


The multiple melting behaviour of PETP was studied

using DSC, FTIR spectroscopy and temperature

modulated DSC by examining PETP samples subjected

to special schemes of crystallisation and annealing

treatment at different temperatures. On one-step and two-

step annealing, a series of multiple endothermic minor

peaks was observed, resulting from the melting of

imperfect crystals during crystallisation. Both dual

morphology and melting-recrystallisation-remelting

mechanisms were probably responsible for the observed

multiple melting behaviour which was dependent on the

thermal history of the PETP samples. 34 refs.

CHINA

Accession no.789727

Item 137Analytical Chemistry

72, No.19, 1st Oct.2000, p.4550-4

GPC SEPARATION OF POLYMER SAMPLESFOR MALDI ANALYSISHanton S D; Liu X M

Air Products & Chemicals Inc.; Lab Connections Inc.

MALDI mass spectrometry was combined with GPC

analysis for broad polydispersity polymers with the use

of liquid chromatography interface. Results for PMMA

were compared with a blend of five narrow PMMA

standards that mimic the broad dispersed material. 24 refs.

USA

Accession no.789529

Item 138Polymers Paint Colour Journal

190, No.4432, Sept.2000, p.25-6

WATCHING PAINT DRYMiddleton J

The development of nuclear magnetic resonance imaging,

a technique previously only used in medicine, to provide

various information, including the drying rate, position

of water and curing in waterborne coatings, is discussed.

The principles of magnetic resonance imaging are outlined

and work conducted at Surrey University in conjunction

with Resonance Instruments to design equipment for

coatings analysis is described.

SURREY,UNIVERSITY; RESONANCE

INSTRUMENTSEUROPEAN COMMUNITY; EUROPEAN UNION; UK;

WESTERN EUROPE

Accession no.789465


78, No.5, 31st Oct.2000 p.1009-16

CRYSTALLIZATION OF LOW-DENSITYPOLYETHYLENE- AND LINEAR LOW-DENSITYPOLYETHYLENE-RICH BLENDSDrummond K M; Hopewell J L; Shanks R A

RMIT University

Using differential scanning calorimetry (DSC) the

crystallisation of a series of low-density polyethylene

(LDPE)- and linear low-density polyethylene (LLDPE)-

rich blends was examined. After continuous slow cooling

DSC analysis showed a broadening of the LLDPE melt

peak and subsequent increase in the area of a second

lower-temperature peak with increasing concentration of

LDPE. Melt endotherms following stepwise

crystallisation (thermal fractionation) detailed the effect

of the addition of LDPE to LLDPE, showing a nonlinear

broadening in the melting distribution of lamellae, across

the temperature range 80-140 degrees Celsius, with

increasing concentration of LDPE. A rise in the population

of crystallites melting in the region between 110 and 120

degrees Celsius, a region was observed where as a pure

component LDPE does not melt. A decrease in the

crystallite population over the temperature range where

LDPE exhibits its primary melting peaks (90-110 degrees

Celsius) was noted, indicating that a proportion of the

lamellae in this temperature range (attributed to either

LDPE or LLDPE) were shifted to a higher melt

temperature. 30 refs.

Accession no.789066


49, No.9, Sept.2000, p.1007-13

USING SPECTROSCOPY WITHCHEMOMETRICS TO MEASURE POLYMER



MOLAR MASSShenton M J; Herman H; Stevens G C

Surrey,University

The ability to determine the molar mass of a polymer is

of fundamental importance to describe polymer molecular

characteristics. Conventional methods for measuring

molar mass include viscometry, osmometry, light

scattering and analytical gel permeation chromatography.

Although high quality data can be obtained by these

methods, the results can be significantly affected by

sample preparation, and they are often time consuming

and unsuitable for real-time on-line processing. The

potential of determining polymer molar mass using optical

spectroscopy combined with chemometric analysis is

demonstrated. This is technically attractive because

optical spectroscopy is routinely used to collect process

data on-line and some refineries routinely monitor and

control blending using near-infrared spectroscopy. A

comparable development to monitor polymer molar

masses on-line from systems already being used to

measure density and melt index, would be of potential

value to many sectors of the polymer production and

processing industry. Chemometrics is a multivariate

methodology that allows the information from entire

spectra to be used; it can be considered as a maximal

compression technique. Extracted ‘factors’ can then be

regressed against property data by using a well-

characterised set of ‘training’ samples to produce

predictive regression models. It is shown that simple

spectroscopic methods, such as the Raman technique

discussed, when coupled with chemometrics, are capable

of providing molar mass and distribution information.

This is illustrated with reference to polydimethylsiloxanes

in the liquid phase. 18 refs.


WESTERN EUROPE

Accession no.787562

Item 141Composite Interfaces

7, No.2, 2000, p.81-92

INVESTIGATING INTERPHASEDEVELOPMENT IN WOOD-POLYMERCOMPOSITES BY INVERSE GASCHROMATOGRAPHYRials T G; Simonsen J

USDA; Oregon,State University

The influence of secondary interactions on the

development of interfacial structure in composites of

wood and amorphous thermoplastic polymers is not well

understood. Inverse gas chromatography is used to

investigate the effect of different polymers on the surface

energy of partially or fully coated white pine wood meal.

In this way, the development of the interphase is

monitored as a function of polymer depth on the wood

surface. The polymers are selected to provide a range of

functional groups and include PS, PMMA, PVC,

polymethacrylic acid and polymethacrylonitrile. The

overall variation of the dispersive component of the

surface energy and the ratio of acceptor to donor

coefficients appear to group themselves into two

categories based upon the polarity of the polymer’s

functional groups. In addition, the high loadings required

for stabilisation of the less polar polymers suggest that a

relatively large volume of the matrix phase isaffected by

the wood filler. 20 refs.

USA

Accession no.786897

Item 142Polymer Science Series B

42, Nos.5-6, May-June 2000, p.169-74

IR SPECTROSCOPY STUDY OF POLYMERPOROSITYPakhomov P M; Kruglova E V; Khizhnyak S D

Tver,State University

IR spectroscopic method is developed for evaluating the

porosity (concentration and size of pores) in polymers.

PE and PAN films of various porosity are prepared from

the solutions in liquid and solid paraffins. The

concentration and maximum pore size in the bulk and in

a surface layer of the samples are determined by IR

spectroscopy in the transmission and reflection modes,

respectively. The results obtained are in agreement with

the data of optical and atomic force microscopy. 12 refs.

RUSSIA

Accession no.786845

Item 143Iranian Polymer Journal

9, No.2, April 2000, p.117-24

STUDY OF CRYSTALLINITY OF HIGH-DENSITY POLYETHYLENE BY INVERSE GASCHROMATOGRAPHYGhaemy M; Hadjmohammadi M R; Tabaraki R

Mazandaran,University

The crystallinity of HDPE (Poliran-HD0035 and Irapol-

5620) was investigated using inverse gas chromatography.

The effects of flow rate of carrier gas and sample size on

peak retention volume and of the amount of injection on

retention volume were evaluated. Retention diagrams and

degrees of crystallinity of the HDPEs were determined

and compared with those of LDPE. 15 refs.

IRAN

Accession no.786383


77, No.7, 15th Aug.2000, p.1419-31

CURE MODELING AND MONITORING OFEPOXY/AMINE RESIN SYSTEMS. 1. CUREKINETICS MODELING



Karkanas P I; Partridge I K

Cranfield,University

An investigation using differential scanning calorimetry

was carried out under both isothermal and dynamic curing

conditions to determine the cure kinetics of four epoxy/

amine resins. Various cure kinetic models were used to

compare them with the results of the DSC results. Good

fits were found, in good agreement with the experimental

results for the resin systems. 22 refs.


WESTERN EUROPE

Accession no.786048

Item 145International Polymer Science and Technology

27, No.6, 2000, p.T/7-T/9. (Translation of Muanyag es

Gumi, No.3, 2000, p.89)

APPLICATION OF STATE-OF-THE-ARTMETHODS IN ADHESION TECHNOLOGY. 1Vabrik R; Czajlik I; Bertoti I; Keresztes Z; Ille A;

Rusnak I; Vig A; Kalman E

The use is demonstrated of microscopic analysis

techniques for the investigation of adhesive failure. PVC

sheet was bonded to glass using a M35R hybrid UV

curable adhesive based on epoxy resin. Atomic force

microscopy and X-ray induction photoelectron

spectroscopy were used for the chemical characterisation

of of failure surfaces. 11 refs.


Accession no.785593


78, No.1, 3rd Oct. 2000, p.166-72

EFFECT OF POLY(VINYL CHLORIDE)/CHLORINATED POLYETHYLENE BLENDCOMPOSITION ON THERMAL STABILITYKlaric I; Vrandecic N S; Roje U

Split,University

The miscibility of PVC and chlorinated PE and the effect

of the blend composition on the heat stability of the PVC

were investigated using several techniques, including

TGA and DSC. The apparent activation energy of PVC

dehydrochlorination in the blends was calculated and

experimental TGA curves compared with those predicted

using the additivity rule. It was found that the blends were

heterogeneous and that addition of chlorinated PE in a

specific temperature range resulted in an improvement

in the heat stability of the PVC. 22 refs.

CROATIA

Accession no.784861

Item 147Polymer

41, No.22, Oct.2000, p.8161-5

APPLICATION OF MODULATED-TEMPERATURE DIFFERENTIAL SCANNINGCALORIMETRY TO THE STUDY OFCRYSTALLISATION KINETICS IN POLY(E-CAPROLACTONE)-POLY(STYRENE-COACRYLONITRILE) BLENDSSong M; Hourston D J

Loughborough,University

In order to evaluate the application of modulated-

temperature differential scanning calorimetry (M-TDSC)

to the study of the crystallisation kinetics of semi-

crystalline polymers, isothermal crystallisation kinetics

in poly(e-caprolactone)-SAN blends are investigated. The

temperature dependence of d ln G/dT (G =crystal growth

rate), determined by M-TDSC agrees approximately with

previous experimental data and theoretical values. These

were obtained from direct measurements of spherulite

growth rate by optical microscopy. Here, theoretical and

M-TDSC experimental results show that the d ln G/dT

versus temperature plots are not sensitive to the non-

crystalline component in the poly(e-caprolactone)-SAN

blends. 15 refs.


WESTERN EUROPE

Accession no.784242

Item 148Polymer

41, No.22, Oct.2000, p.8151-4

PORE DIMENSION OF WATER TREES IN PE:NMR STUDIESJudeinstein P; Carmo Lanca M; Marat-Mendes J; Rault J

Paris-Sud,Universite; Portugal,Universidade Nova de

Lisboa

In PE films aged under electric field the crystallisation of

water (and melting of ice) is studied by quadrupolar NMR,

this technique allows determination of water concentration

as low as 10 -4. It is shown that the pore dimensions of

the tracks forming the water trees of the order of 2.5 nm

are independent of the ageing time. The mobility of water

in these water trees and in porous glass, of similar pore

dimensions, are compared. 17 refs.


PORTUGAL; WESTERN EUROPE

Accession no.784240


77, No.10, 6th Sept.2000, p.2178-8

CURE MODELLING AND MONITORING OFEPOXY/AMINE RESIN SYSTEMS. II.NETWORK FORMATION ANDCHEMOVISCOSITY MODELLINGKarkanas P I; Partridge I K

Cranfield,University

The glass transition temperature (Tg) advancement and

the chemoviscosity development under isothermal



conditions are investigated for four epoxy/amine systems,

including commercial RTM6 and F934 resins. Differential

scanning calorimetry is the thermoanalytical technique

used to determine the Tg advancement, and rheometry

for determination of the chemoviscosity profiles of these

resin systems. The complex cure kinetics are correlated

to the Tg advancement via a one-to-one relationship using

Di Benedetto’s formula. It is revealed that the three-

dimensional network formation follows a single activated

mechanism independent of whether the cure kinetics

follow a single or several activation mechanisms. The

viscosity profiles show the typical characteristics of

epoxy/amine cure. A modified version of the Williams-

Landel-Ferry equation (WLF) is adequate to model the

viscosity profiles of all the resin systems, in the

temperature range 130 to 170 deg.C, with a very good

degree of accuracy. The parameters of the WLF equation

are found to vary in a systematic manner with cure

temperature. Further correlation between Tg and viscosity

shows that gelation, defined as the point where viscosity

reaches 10 4 Pas, occurs at a unique Tg value for each

resin system, which is independent of the cure conditions.

16 refs.


WESTERN EUROPE

Accession no.784172

Item 150Fire & Materials

24, No.2, March/April 2000, p.101-12

SMOKE GAS ANALYSIS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY -SUMMARY OF THE SAFIR PROJECT RESULTSHakkarainen T; Mikkola E; Laperre J; Gensous F;

Fardell P; Le Tallec Y; Bajocchi C; Paul K; Simonson

M; Deleu C; Metcalfe E

VTT Building Technology; Centexbel; Elf Atochem

SA; UK,Building Research Establishment; CEMATE;

LSF SUD srl; Rapra Technology Ltd.; Sweden,National

Testing & Research Institute; Ghent,University;

Greenwich,University

The determination of toxic components from fire gases

is difficult because the environment is hot, reactions are

often temperature dependent, and a lot of soot may be

produced. Due to the different properties of the gas

components, a different time-consuming procedure for

each species has traditionally been used. The use of FTIR

(Fourier transform infrared) spectrometers as a continuous

monitoring technique overcomes many of the problems

in smoke gas analyses. FTIR offers an opportunity to set

up a calibration and prediction method for each gas

showing a characteristic spectral band in the infrared

region of the spectrum. The objective of the SAFIR project

was to further develop the FTIR gas analysis of smoke

gases to be an applicable and reliable method for the

determination of toxic components in combustion gases

related to fire test conditions. The optimum probe design,

filter parameters and the most suitable sampling lines in

terms of flow rate, diameter, construction material and

operating temperature have been specified. In the large

scale, special concern was given to the probe design and

the effects of the probe location as well as practical

considerations of the sampling line length. Quantitative

calibration and prediction methods have been constructed

for different components present in smoke gases.

Recommendations on how to deal with interferents, non-

linearities and outliers have been provided and a

verification method for the spectrometer for unexpected

variations and for the different models have been

described. FTIR measurement procedures in different fire

test scenarios are studied using the recommendations of

this project for measurement techniques and analysis and

an interlaboratory trial of the FTIR technique in smoke

gas analysis is carried out to define the repeatability and

reproducibility of the method in connection with a small

scale fire test method, the cone calorimeter. 9 refs.


FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK;

WESTERN EUROPE

Accession no.784096

Item 151Polymer

41, No.23, Nov.2000, p.8241-5

USE OF RAMAN SPECTROSCOPY TO STUDYTHE REACTION BETWEEN AN AMINE-TERMINATED THERMOPLASTIC AND EPOXYRESINSvan Overbeke E; Carlier V; Devaux J; Carter J T;

McGrail P T; Legras R

Louvain,Universite Catholique; ICI Plc

Reactive thermoplastics are often used as toughening

modifiers for epoxy resins. Raman spectroscopy was used

to follow the reaction of aromatic amines with epoxide

monomers through the evolution of an amine-substituted

aromatic vibration. A double shift of this peak was correlated

with the formation of secondary and tertiary amines. Band

assignment was confirmed by the study of model

compounds. Using this method, qualitative observation of

the reaction between an amine-terminated copolyether-

sulphone thermoplastic and epoxide was performed.

Unfortunately, in the blend studied containing the curing

agent, a band appearing upon curing overlapped with the

band characterising the end group reaction. 17 refs.


UK; WESTERN EUROPE

Accession no.783075


68, No.3, 2000, p.437-43

SEMI-QUANTITATIVE ANALYSIS OFTHERMAL DEGRADATION INPOLYPHENYLENE ETHER



Kinoshita M; Nemoto T; Souda T; Takeda K

Koito Mfg.Co.Ltd.; Shibaura,Institute of Technology

The use of simple computer simulation and analysis of

the thermal degradation products of differently thermally

aged samples of melt processed polyphenylene ether film

gave information on possible degradation routes for this

polymer. An increase in dimeric products was noted with

increased thermal ageing, but not in monomeric products.

To explain the distribution of scission products found

experimentally, the simple computer model was arranged

to simulate cleavage rates of methylene bridge, ether and

sidechain links. Although results were not totally

conclusive, it was noted that both ether bridge and side

chain cleavage rates were similar, and approximately nine

times lower than cleavage rates of the methylene bridge.

It is suggested that quantitative results determined will

give detailed information on flame retardance due to the

understanding of rates of volatile product generation at

the polymer surface. 28 refs.

JAPAN

Accession no.782776


68, No.3, 2000, p.321-6

COMPARATIVE ANALYSIS OF THE PHOTO-OXIDATION OF POLYSTYRENE ANDPOLY(ALPHA-METHYLSTYRENE)Mailhot B; Jarroux N; Gardette J-L

Ensemble Universitaire des Cezeaux

Fourier transform infrared spectroscopy (FTIR) and mass

spectroscopy were used to study the photo-oxidation of

both poly(alpha-methylstyrene) (PMS) and polystyrene

(PS) films which had been irradiated at different

temperatures and with different radiation sources under

an oxygen atmosphere. The oxidised films were treated

with ammonia or sulphur tetrafluoride and photolysis

carried out under vacuum. Photoproducts from both

polymers were broadly similar, but aromatic ketone

concentration was higher from the PMS and a new ketone

was also identified from this source. Routes for formation

of identified photoproducts are proposed. 13 refs.


WESTERN EUROPE

Accession no.782763

Item 154ACS, Polymeric Materials Science & Engineering Fall

Meeting 1999. Volume 81. Conference proceedings.

New Orleans, La., 22nd-26th Aug.1999, p.242-3

ANALYSIS OF THE NANOPHASE STRUCTUREOF SEMICRYSTALLINE POLYMERS WITHATOMIC FORCE MICROSCOPY (AFM),MICROCALORIMETRY (MC) ANDTEMPERATURE-MODULATEDCALORIMETRY (TMC)

Wunderlich B

Tennessee,University; Oak Ridge National Laboratory

(ACS,Div.of Polymeric Materials Science & Engng.)

Semicrystalline, polymeric materials consist usually of

metastable aggregates of strongly coupled microphases or

nanophases with their constituent, micrometre-long, flexible

molecules traversing multiple phase domains. Some 40 years

ago it was established that well-formed crystals are often

lamellar with a thickness of only about 10 nm. Between these

lamellae one can find the remaining amorphous phase with

even smaller dimensions. Less perfect crystallisation can

decrease the crystal dimensions to as little as 1-2 nm in all

dimensions. An operational definition of the microphase is

its having at least one dimension smaller than a micrometre,

while nanophases are approached when the small dimension

approaches 10 nm. Characteristic of the microphases is the

need to consider the surface properties for their description,

i.e. the melting temperature depends on the surface free

energy. Nanophases, in turn, show an interaction between

opposing surfaces, i.e. they may show no bulk properties. If

the dimensions decrease below 1 nm, the macroscopic phase

description has reached its limit. Many macromolecules can,

however consist of alternating sequences of nanometer-

length chain segments that are immiscible, so that in all their

phase structures there is a strong tendency of nanophase

separation. It is shown that special tools must be developed

to probe the nanophase structures and properties of polymers.

Some new information available by using three rather new

techniques their combinations are described. 10 refs.

USA

Accession no.780666




CRYSTALLISATION AND MELTING OFPOLYMER CRYSTALS REVEALED BY T-M DSCToda A; Oda T; Tomita C; Hikosaka M; Arita T;

Saruyama Y

Hiroshima,University; Kyoto,Institute of Technology


Temperature-modulated differential scanning calorimetry

(T-MDSC) applies a thermal modulation in temperature

to a conventional DSC run and determines a dynamic heat

capacity from the relationship between the modulation

components of temperature and of heat flow. Primary

application of this technique has been the measurement

of specific heat capacity and the examination of the

anomaly in a relaxation process such as alpha process

related to the glass transition. An application to the first-

order phase transitions of crystallisation and melting of

polymer crystals has recently been suggested. The method

and typical results are described. 13 refs.

JAPAN

Accession no.780663






FILM FORMATION IN POLYMER LATEXBLENDS: MICROSPECTROSCOPIC 3D STUDIESZhao Y; Urban M W

North Dakota State University


A series of previous studies on latex films indicates that

mobility of low molecular weight species in particular

surfactant molecules, may be affected by latex glass

transition temperature, and subsequently, by free volume

of a polymer matrix, surface tension at the film/air and

film/substrate interfaces, compatibility and coalescence

times, to name just a few. It appears that there are other

factors that not only influence distribution of individual

components including distribution of surfactants, but also

may significantly affect film formation. In an effort to

enhance understanding of these multi-phase latex blends

and their coalescence, a series of experiments on latexes

containing PS and poly-n-butyl acrylate (p-nBA) blends

is presented. An attempt is made to identify factors

affecting film formation of PS/p-nBA latex blends using

multi-dimensional vibrational spectroscopic methods, and

these findings are compared with respective copolymers.

The effects of SDOSS exudation by latex composition,

particle and annealing temperatures are also addressed in

terms of phase separation and dynamics of

macromolecular segments. 21 refs.

USA

Accession no.780632




FAILURE STUDIES OF ADHESION BY UVREFLECTION AND FLUORESCENCETECHNIQUESKim N-J; Jeong C N; Sung C S P; Sung N-H

Connecticut,University; Tufts University


Various techniques such as optical and electron microscopy,

IR-ATR ESCA and SIMS have been used for failure mode

analysis in polymeric adhesive joints. However, these

techniques are not amenable for in situ, non-destructive

examination of the failure surfaces as failure occurs. In

order to develop in situ techniques, UV reflection and

fluorescence methods are evaluated, as they can be applied

via optical fibres to the actual failure surface. Failure

surfaces of two types of adhesive joints are examined by

UV reflection and fluorescence, complemented by FT-IR

ATR studies. The first joint studied is PU on epoxy-coated

steel. The second is PETP/PE/PETP. 8 refs.

USA

Accession no.780560


72, No.11, 1st June 2000, p.2490-8

CHARACTERISATION OF POLYETHER ANDPOLYESTER POLYURETHANE SOFT BLOCKSUSING MALDI MASS SPECTROMETRYMehl J T; Murgasova R; Dong X; Hercules D M;

Nefzger H

Vanderbilt University; Bayer Corp.

Selective degradation reactions combined with MALDI

analysis were applied for molecular weight determination

of polyether and polyester polyurethane soft blocks. Size

exclusion chromatography was combined with MALDI to

provide accurate molecular weight determination. 44 refs.

USA

Accession no.778970


Vol.152, March 2000, p.267-78

ANALYSIS OF COMPLEX POLYMERS BYMALDI-TOF MASS SPECTROMETRYPasch H; Ghahary R

German Plastics Institute

The results are reported of an analysis of the functionality,

molar mass and chemical composition of complex

polymers, using MALDI-TOF mass spectrometry and acombination of MALDI-TOF mass spectrometry and

liquid chromatography. Polymers investigated included

polyamide-12, bisphenol A polycarbonate, methoxylated

melamine-formaldehyde resin, carboxy-terminated PS

and PMMA. 33 refs.


WESTERN EUROPE

Accession no.778702

Item 160Journal of Injection Molding Technology

4, No.2, June 2000, p.84-91

ANALYSIS OF STYRENE PLASTIC RESIDUESON INJECTION MOULDING TOOLSMakinen M; Astola J; Poutanen J; Alen R; Paakkonen E

Tampere,University of Technology;

Jyvaskyla,University

The contaminating substances formed during the injection

moulding of ABS and PS parts were removed from the

mould surface. The residues were characterised using

FTIR, gas chromatography, pyrolysis gas

chromatography, elemental analysis, detection reaction

test of bromine, and different dissolving tests. The

chemical composition of the contamination was clarified

and suitable solvents for dissolving these products were

selected. 6 refs.

EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN

EUROPE

Accession no.776471



Item 161Polymer

41, No.15, 2000, p.5949-55

UNDERSTANDING VITRIFICATION DURINGCURE OF EPOXY RESINS USING DYNAMICSCANNING CALORIMETRY ANDRHEOLOGICAL TECHNIQUESLange J; Altmann N; Kelly C T; Halley P J

Queensland,University

The gelation and vitrification transitions during cure of

an epoxy resin-amine system were examined using

rheological, modulated DSC and FTIR techniques. The

results of DMA showed that gelation was observed before

vitrification at all temps. where it could be rheologically

defined. By comparing different rheological criteria for

vitrification, it was seen that the vitrification transition

was a gradual process that extended over a large part of

cure at all temps. where it occurred. Results from

modulated DSC measurements showed that the

calorimetric vitrification times were longer than the

vitrification times obtained from rheological

measurements at cure temps. above 100C, but that at lower

temps. calorimetric vitrification occurred before, or at the

same time as, rheological vitrification. Theoretical

gelation times, estimated from FTIR conversion data,

were found to be consistently shorter than the observed

gelation times. Theoretical vitrification times agreed well

with the observed times. The magnitude of the vitrification

transition, expressed either as amount of change in heat

capacity or as maximum value of loss tangent, was found

to decrease approximately linearly with increasing cure

temp. 34 refs.

AUSTRALIA

Accession no.776348


33, No.8, 18th April 2000, p.3180-3

COMPLETE ASSIGNMENT OF PROTON ANDCARBON 13 NMR SPECTRA OFPOLYVINYLCARBAZOLEKarali A; Froudakis G E; Dais P; Heatley F

Crete,University; Manchester,University

Details are given of the assignment of the proton and

carbon 13 spectra of polyvinylcarbazole by using a

number of modern gradient two-dimensional NMR

experiments. The relationship between the assignments

and the conformational and dynamic properties of the

polymer is discussed. 13 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; UK;

WESTERN EUROPE

Accession no.776167


59, Nos.1-2, 2000, p.409-24

CHARACTERISATION OF POLYURETHANECOATINGS USING THERMOANALYTICALTECHNIQUESGinic-Markovic M; Choudhury N R; Matisons J G;

Williams D R G

South Australia,University; Adelaide,University

A two-pack PU coating was analysed using

thermoanalytical techniques. The curing reaction was

monitored using pressure differential calorimetry,

rheometry and dynamic mechanical analysis. The

decomposition behaviour was examined using TGA. 13

refs.

AUSTRALIA

Accession no.776090


8, No.6, June 2000, p.42/50

MATERIALS ANALYST: PART 33 -DETERMINING COMPOSITIONSepe M


This article focuses on the problems associated with

identifying a polymer. There are three major techniques

that are particularly helpful in identifying the type of

polymer used in a compound. These are DSC, TGA and

IR spectroscopy. Each of these techniques has itsstrengths, and in determining the composition of the

polymer, the task is to highlight properties and behaviour

that are distinctive.

USA

Accession no.775805

Item 165Polymer

41, No.11, 2000, p.4361-5

RAPID MICROWAVE INDUCEDDEPOLYMERISATION OF POLYAMIDE 6Klun U; Krzan A

Ljubljana,National Institute of Chemistry

Polyamide 6 depolymerisation was performed using

microwaves as the energy source for the acid catalysed

hydrolysis, with phosphoric acid as the catalyst. The

product mixture was analysed by chromatographic and

spectroscopic methods. 19 refs.

SLOVENIA

Accession no.774158

Item 166Polymer

41, No.11, 2000, p.4039-46

MATRIX-ASSISTED LASER DESORPTION/IONISATION MASS SPECTROMETRY OFSYNTHETIC POLYMERS. IV. COUPLING OFSIZE EXCLUSION CHROMATOGRAPHY AND



MALDI-TOF USING A SPRAY-DEPOSITIONINTERFACEEsser E; Keil C; Braun D; Montag P; Pasch H

Darmstadt,Deutsches Kunststoff-Institut

Size exclusion chromatography and MALDI-TOF mass

spectrometry was coupled via a robotic interface. For

polydisperse synthetic polymers a continuous track of

matter was deposited onto the matrix surface. Spectra

were taken from different positions of the polymer track.

Data are presented for PS, PMMA and butyl methacrylate-

methyl methacrylate copolymers. 20 refs.


WESTERN EUROPE

Accession no.774127

Item 167Muanyag es Gumi

37, No.3, 2000, p.89-91

Hungarian

APPLICATION OF STATE-OF-THE-ARTMETHODS IN ADHESION TECHNOLOGY. I.Vabrik R; Czajlik I; Bertoti I; Keresztes Zs; Ille A;

Rusznak I; Vig A; Kalman E

Atomic force microscopy (AFM) and X-ray photoelectron

spectroscopy (XPS) were used to study the nature of the

failure interface and the failure mechanism in a PVC film/

adhesive/glass system. The failure mode was found to be

mostly interfacial, occurring at the glass/adhesive interface,

and also partially cohesive, located in the adhesive layer

very close to the interface. The results are discussed in

relation to the chemical nature of the interface and the

failure mechanism. 11 refs. Articles from this journal can

be requested for translation by subscribers to the Rapra

produced International Polymer Science and Technology.

Accession no.773793


78, No.521, Nov.1999, p.541-6

Spanish

STRUCTURAL CHARACTERISATION OFMULTILAYER POLYMERIC MATERIALS BYMICRORAMAN SPECTROSCOPYSanz R; Martin B; Merino J C; Pastor J M

Valladolid,Universidad

Results are presented of a study in which confocal

microRaman spectroscopy was used to determine the

structure of the individual polymers present in a series of

multilayer food packaging films. 8 refs.

AMCOR FLEXIBLES ESPANA SAEUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;

WESTERN EUROPE

Accession no.773260

Item 169Iranian Journal of Polymer Science & Technology

12, No.2, Summer 1999, p.1-8

Persian

KINETIC STUDY OF THE AUTO-OXIDATIONOF POLYURETHANESemsarzadeh M A; Salehi H

Tarbiat Modarres University

Gel permeation chromatography was used to study the

kinetics of the auto-oxidation of polyurethane. The

stationary state rate and the induction time were

determined at various temperatures. FTIR and H NMR

were used to determine the alcohol, acetate and formate

compounds in the auto-oxidation products.

IRAN

Accession no.773140

Item 170Journal of Macromolecular Science B

B39, No.2, 2000, p.279-96

TIME-RESOLVED FTIR STUDY OFCRYSTALLISATION BEHAVIOUR OF MELT-CRYSTALLISED POLYPHENYLENE SULPHIDEYu J; Asai S; Sumita M

Tokyo,Institute of Technology; China,Textile

University

The crystallisation behaviour of polyphenylene sulphide

was studied using time-resolved FTIR spectroscopy and

the results obtained correlated with DSC measurements.

The 1073 cm/1 amorphous band was selected for the time-resolved measurements. The procedure provided details

on the microstructure of the PPS, including heterogeneity

of the amorphous phase above and below Tg. A method

is proposed for calculating the rigid, amorphous fraction

in terms of the increase in the slope of the absorbance

variation with temperature at the glass transition. 43 refs.

CHINA; JAPAN

Accession no.772147


76, No.6, 9th May 2000, p.938-46

OPTIMIZATION OF EXPERIMENTALPARAMETERS FOR THE QUANTIFICATION OFPOLYMER ADDITIVES USING SFE/HPLCThilen M; Shishoo R

Swedish Institute for Fibre & Polymer Research

A study was conducted with the aim of extracting the

antioxidants Irganox 1010 and Irgafos 168 from a PP

matrix by using the supercritical fluid extraction(SFE)

technique and by subsequent analysis using high-

performance liquid chromatography(HPLC). The

experimental parameters of temp., pressure and modifiers

were varied to find the best extraction conditions. The

optimum temp. and pressure for extraction of these

polymer additives were found to be 120 and 384 bar, with

methanol as the modifier. The quantitative extractions

were significantly faster than those reported previously

in the literature. The results showed that the SFE/HPLC



technique used in these experiments was a reliable and

environmentally-friendly alternative to the commonly-

used liquid extraction and analytical methods. 22 refs.


EUROPE

Accession no.770687


Vol.148, Dec.1999, p.463-81

CHARACTERIZATION OF ACRYLIC DENTALPOLYMERSVera-Graziano R; Martinez-Richa A; Palacios-Alquisira

J; Barcelo-Santana F; Castano-Meneses V

Mexico,Universidad Nacional Autonoma;

Guanajuato,Universidad

The chemical composition, dimensions and the molecular

parameters of four dental acrylic polymer materials and

two polyacrylic acids of different molec.wt. used as model

compounds were studied by NMR and IR spectroscopies,

GPC, intrinsic viscosity and light scattering

measurements. Two of the dental polymers were shown

to be mainly polyacrylic acid, while one showed the peak

pattern for an acrylic acid/methyl acrylate copolymer of

about 2:1 composition and one was an oligomer derived

from 2-hydroxyethyl methacrylate. The steric hindrance

parameter, molecular stiffness and second virial

coefficient were calculated using different thermodynamic

models. The Flory-Fox-Shafgagen and the Stockmayer-

Fixman models fitted the experimental data reasonably

well and could be use to describe the molecular parameters

of the acrylic polymers. 18 refs. (7th International

Conference on Polymer Characterization (POLYCHAR-

7), Denton, Texas, USA, Jan.1999)

MEXICO

Accession no.770356

Item 173Flame Retardants 2000. Conference proceedings.

London, 8th-9th Feb.2000, p.185-92

PRACTICE OF FTIR ANALYSIS FOR FIREGASES (SAFIR)Mikkola E

VTT Building Technology

(BPF; Interscience Communications Ltd.; APME;

European Flame Retardant Assn.; Fire Retardant

Chemicals Assn.)

The use of FTIR (Fourier transform infrared)

spectrometers as a continuous monitoring technique

overcomes many of the problems associated in analyses

of hot fire gases. FTIR offers an opportunity to set up a

calibration and prediction method for each gas showing

a characteristic spectral band in the infrared region of the

spectrum. A European project, SAFIR, aims to further

develop the FTIR gas analysis of smoke gases to be an

applicable and reliable method for the determination of

toxic components in combustion gases related to fire test

conditions. Within this project, optimal working

conditions including sampling, calibration and analysis

for FTIR fire gas method are defined and verified under

a variety of fire test scenarios. The FTIR method are

shown to be a repeatable and reproducible method for

the determination of the most important toxic gas

components of real fires. Moreover, the findings of this

project concerning sampling techniques are most relevant

for other methods used for defining fire gases. 5 refs.

EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERN

EUROPE

Accession no.768669

Item 174Surface Coatings International

83, No.3, March 2000, p.111-8

DETERMINATION OF VOC EMISSIONS FROMLATEX PAINTS DURING AND AFTERAPPLICATION; METHODS, PERFORMANCEAND PRECISIONZeh H

Wacker Polymer Systems GmbH

VOC emissions from indoor latex paints during and after

application is determined by four different test methods:

a chamber method in which an emission chamber is

combined with gas chromatography, two practical

methods in which VOC emitted in a room is measured

either by the determination of the total organic carbon or

by infrared spectroscopy, and an ‘in-can-individual-VOC

method’ which determines the VOC of a liquid paint by

the quantitative analysis of each volatile component. VOC

emission data gathered by these methods are compared

with calculations from a dynamic computer model

describing the time-dependence of the VOC emission in

the room atmosphere. This comparison indicates that the

‘in-can-individual-VOC method’ with computer

calculation allows variations in the size of the room, the

application rate, VOC content of the paint and the rate of

air change, without the necessity of additional

experiments, and therefor, offers an approach with a

reduction in costs. 10 refs.


WESTERN EUROPE

Accession no.768107


72, No.902, March 2000, p.53-61

ACID ETCH OF AUTOMOTIVE CLEARCOATS.II. COMPARISON OF DEGRADATIONCHEMISTRY IN LABORATORY AND FIELDTESTINGSchmitz P J; Holubka J W; Xu L-F

Ford Motor Co.

X-ray photoelectron spectroscopy was used to determine

whether exposure conditions used in the laboratory

gravimetric etch testing of acrylic melamine clearcoats



simulated field degradation pathways. The surface

chemistry of the field exposed panels was examined and

the results compared with those for laboratory treated

powders having identical technologies. Consistency in the

formation of a melamine salt and ammonium sulphate

upon field exposure and laboratory acid treatment

indicated that the laboratory treatment conditions

simulated the field exposure conditions. 7 refs.

USA

Accession no.767768

Item 176Journal of Adhesion Science and Technology

14, No.5, 2000, p.745-64

XPS ANALYSIS OF THE COVERAGE ANDCOMPOSITION OF COATINGS ON GLASSFIBRESThomason J L; Dwight D W

Owens-Corning Science & Technology Center

The use of X-ray photoelectron spectroscopy as a method

for characterising different sizings on glass fibres was

evaluated. A model, based on a patchy sizing overlay

hypothesis, was developed to aid in the reduction of data

obtained from the X-ray photoelectron spectroscopic

analysis. It is shown that the spectroscopic results, when

combined with the weight fraction of the sizing, provide

a quantitative value for the coverage of the fibre surface

by the sizing. 25 refs.

USA

Accession no.767755


25, No.2, Feb.2000, p.56-8

POLYMER ANALYSIS ANDCHARACTERISATIONGarbassi F

EniChem SpA

Analytical techniques, such as mass spectroscopy, atomic

absorption spectroscopy and atomic emission

spectroscopy, for the detection of trace elements, mainly

metal trace elements, in polymers, used particularly in

food, are briefly considered. The disadvantages and

suitability of such techniques are summarised. 10 refs.


WESTERN EUROPE

Accession no.766702

Item 178Adhesion ’99. Conference Proceedings.

Cambridge, UK, 15th-17th Sept.1999, p.369-73

INTERPHASE CHEMISTRY OF CARBON FIBRECOMPOSITE MATERIALSPrickett A C; Vickers P E; Smith P A; Watts J F

Surrey,University

(IOM Communications Ltd.)

The fibre-matrix interface in carbon fibre-reinforced

epoxy resin composites was studied by time of flight

secondary ion mass spectrometry (ToF-SIMS) using novel

preparation techniques. The initial adsorption between

uncured resin or amine curing agent and the fibre was

investigated by the use of adsorption isotherms obtained

by the analysis of fibre surfaces following immersion in

liquid solutions of the resin. The intact interphase of a

composite could be examined by ToF-SIMS following

mode I or mode II failure within the spectrometer by the

use of carefully designed in-situ fracture stages. 11 refs.


WESTERN EUROPE

Accession no.765326

Item 179Adhesion ’99. Conference Proceedings.

Cambridge, UK, 15th-17th Sept.1999, p.347-50

MICRO THERMAL ANALYSIS ATINTERPHASESHassler R; zur Muhlen E

Dresden,Institut fuer Polymerforschung; TA

Instruments GmbH

(IOM Communications Ltd.)

Details are given of a thermal analysis technique, referred

to as micro thermal analysis, which combines the high

resolution positioning of scanning probe microscopy with

some of the quantitative analysis capabilities of conventional

thermal analysis. The application of this technique in

characterising the thermal properties of interfaces in

aluminium/epoxy resin adhesive joints and in glass fibre-

reinforced epoxy resin composites is described. 7 refs.


UK; WESTERN EUROPE

Accession no.765322


33, No.1, 11th Jan.2000, p.120-4

BRANCHING AND CROSSLINKING INRADIATION-MODIFIED PTFE. A SOLID-STATENMR INVESTIGATIONFuchs B; Scheler U

Dresden,Institute of Polymer Research

High-resolution fluorine 19 NMR was used to investigate

the structural changes resulting from PTFE electron

irradiation under vacuum. A quantitative analysis of the

data was used to establish the density of side groups and

branches. 20 refs.


WESTERN EUROPE

Accession no.764731

Item 181Color and Appearance Retec 1999. Conference

proceedings.



Nashville, Tn., 27th-29th Sept.1999, p. 178-87

USING MICROSCOPY AS A PROBLEMSOLVING TOOL IN PLASTICSCompton C

Sun Chemical Corp.

(SPE,Color & Appearance Div.)

Microscopy is a valuable tool for pigment evaluation and

problem solving in plastics and other applications. The

organic pigments used in plastic applications are typically

sub-micron in size. Pigment performance is greatly affected

by how well the pigment particles are incorporated in the

polymer medium. Various microscopic evaluation

techniques that can be used to investigate dispersion quality,

strength development and thermal stability are reviewed.

In addition, various microscopic techniques for identifying

contaminants are discussed. 7 refs.

USA

Accession no.764247

Item 182Composites Part A: Applied Science and

Manufacturing

31A, No.2, 2000, p.165-71

FAILURE PHENOMENA IN TWO-DIMENSIONAL MULTI-FIBREMICROCOMPOSITES. PART IV: A RAMANSPECTRASCOPIC STUDY ON THE INFLUENCEOF THE MATRIX YIELD STRESS ON STRESSCONCENTRATIONSvan den Heuval P W J; Peijs T; Young R J

Eindhoven,University of Technology; UMIST; Queen

Mary & Westfield College

Raman spectroscopy is used to study the influence of shear

yield stress of the matrix on stress situations in carbon

fibre/epoxy resin composites containing a planar fibre

array. A mixture of two curing agents, with different

functionality and molecular weights, are used to cure the

epoxy resin in order to obtain a matrix with varying cross-

linked density. The carbon fibres are surface treated to

give good fibre-matrix adhesion. Three matrix systems

are investigated in the study, each with a different yield

stress. The mechanical properties of each material are

measured under tension and shear conditions. 35 refs.


NETHERLANDS; UK; WESTERN EUROPE

Accession no.763633

Item 183Journal of Macromolecular Science A

A36, No.11, 1999, p.1751-8

POLYPROPYLENE PIPES FOR DRINKINGWATER SUPPLYHametner C

Austrian Plastics Institute

The migration of phenolic antioxidants (which are

typically used for the stabilisation of PP pipes) into

drinking water in contact with PP pipes was studied.

Austrian, German and International Standard methods

were used for water at 23C and 60C. The low molecular

degradation product 2,4-di-tert-butylphenol, rather than

the high molecular antioxidants, was detected in the

aqueous extracts. In warm water extracts, the

concentration of phenols, the total organic carbon content

and the effect on odour and flavour were considerably

higher than in cold. Alkaline water extracted higher

amounts of phenols but acidic drinking water showed no

effect. Thermal loading of PP during the extrusion process

significantly increased the extractable phenols, total

organic carbon content and flavour number/threshold

odour. 7 refs.

AUSTRIA; EUROPEAN UNION; WESTERN EUROPE

Accession no.763574

Item 184West Conshohocken, PA, 1999, pp.6. NALOAN.

ASTM D 2124-. METHOD FOR ANALYSIS OFCOMPONENTS IN POLY (VINYL CHLORIDE)COMPOUNDS USING AN INFRAREDSPECTROPHOTOMETRIC TECHNIQUEAmerican Society for Testing & Materials

ASTM D 2124-

Version 99. Photocopies and loans of this document are

not available from Rapra.

USA

Accession no.760789


72, No.900, Jan.2000, p.69-74

ANALYSIS OF EXEMPT PAINT SOLVENTS BYGAS CHROMATOGRAPHY USING SOLID-PHASE MICROEXTRACTIONBodrian R R

California,Polytechnic University

Acetone, methyl acetate and parachlorobenzotrifluoride

have been exempted as VOC solvents by the EPA. In

measuring coating VOC content, separate methods for

determining exempt solvents are required. One such

method utilises solid-phase microextraction to sample the

headspace of solvent-based coatings to which the

surrogates acetone-d6, methyl acetate-d3 and/or

metachlorbenzotrifluoride have been added. The sampled

exempt coating solvents are thermally desorbed and

analysed using gas chromatography with flame ionisation

or mass spectral detection. This paper presents the results

obtained for acetone and toluene in a large number of

aerosol paints. Additionally, the results from a round-robin

study for acetone, methyl acetate and

parachlorobenzotrifluoride in commercial solvent-based

coatings are reported. 17 refs.

USA

Accession no.760572




57, No.3, 1999, p.847-51

IDENTIFICATION OF POLYETHYLENE BYDIFFERENTIAL SCANNING CALORIMETRYTsukame T; Kutsuzawa M; Sekine H; Saitoh H;

Shibasaki T

Saitama,Criminal Investigation Laboratory;

Saitama,University

A forensic sample consisting of melt-recrystallised

polymers recovered from the scene of a fire in a factory

is identified by differential scanning calorimetry. The

factory commonly used two kinds of film sheets, A and

B, made by different manufacturers. It is necessary to

decide whether the forensic sample related to material A

or B. The forensic sample and reference samples of

materials A and B are subjected to IR spectroscopy and

pyrolysis gas chromatograph mass spectrometry

measurements, which reveal their PE nature. The thermal

behaviour of the samples is examined by differential

scanning calorimetry (DSC) and they are found to be

blends of two kinds of PEs, LDPE and LLDPE. The

samples can be identified and distinguished from each

other via the DSC measurements. 6 refs.

JAPAN

Accession no.760331


58, No.1, 1999, p.13-8

THERMAL CHARACTERISATION OFPOLYURETHANE ACRYLATE RESINSLedru J; Saiter J M; Grenet J; Yuossef B; Burel F;

Bunel C

Rouen,University; Rouen,Institut National des Sciences

Appliquees

Polyurethane acrylate resins cured by two different

methods, thermally and photochemically, are investigated

by means of differential scanning calorimetry and

thermally stimulated depolarisation currents. Even if both

curing methods lead to the same material from a chemical

point of view, important differences exist between the

thermocured resin and the photocured resin in terms of

molecular relaxation behaviour. 8 refs.


WESTERN EUROPE

Accession no.760327


53, No.11, Nov.1999, p.1412-8

IN-LINE NEAR-INFRARED MONITORING OFPOLYMER PROCESSING. I. PROCESS/MONITOR INTERFACE DEVELOPMENTReshadat R; Desa S; Joseph S; Mehra M; Stoev N;

Balke S T

Toronto,University

Near-infrared inline monitoring of polymer processing

means using an optical fibre-assisted spectrometer to

obtain spectra of the polymer melt flowing through

commonly used processing equipment (an extruder).

Conditions in the extruder are typically 200 deg.C and

20 MPa. The design of interfaces between the

spectrometer and the molten polymer is shown. Three

designs are shown, each permitting monitoring at a

different location in the process: a melt-at-die interface,

a melt-in-barrel interface and a strand interface. These

designs are for monitoring just before the extruder exit,

in the main barrel of the extruder and after the product

exits from the extruder as a strand, respectively. All these

interfaces protect the inserted optical fibre probe from

the harsh environment within the extruder while

permitting easy replacement or a probe without

interrupting the process. This latter characteristic is very

important because it permits easy probe repair as well as

the use of other types of probes (for monitoring colour or

particles, for example) to be used during a run. Examples

of near-infrared spectra obtained with each of the

interfaces used with an immiscible blend of PE and PP

are shown. Large differences in the spectra demonstrate

that the design of the interface will affect multivariate

analysis directed at composition prediction. Subsequent

papers are directed at using the melt-at-die interface for

composition prediction and accounting for nonlinear

relationships between absorbance and concentration. 6

refs.

CANADA

Accession no.760231


53, No.11, Nov.1999, p.1403-11

THERMAL VOLATILISATION ANALYSIS: AVERSATILE PLATFORM FORSPECTROSCOPIC INVESTIGATION OFPOLYMER DEGRADATION PROCESSESGuo X; Huang B; Dyakonov T; Chen Y; Padron L;

Vickstrom T; Kuhn J; Hodkiewicz J; Stevenson W T K

Wichita,State University; Harrick Scientific Co.;

Oklahoma State University; Koch Industries Inc.; ATI

Instruments

Thermal volatilisation analysis (TVA) and sub-ambient

thermal volatilisation analysis (SATVA) techniques are

described. In addition to rate profiling of the volatile

product flux of thermal degradation under high-vacuum

conditions through measurement of pressure in the

vacuum line as a function of sample temperature, the TVA

technique is shown to afford a convenient method for an

on the basis of volatility under high-vacuum conditions,

of product fractions of thermal degradation for subsequent

spectroscopic analysis. The capacity and flexibility of

TVA as a platform for these analyses are illustrated in a

case study format by degrading poly(bisphenol A, 2-



hydroxy propylether). The overall degradation process is

quantified, and most significant pathways of thermolysis

are identified through subsequent spectroscopic analysis

of products of decomposition. The design and construction

of a modified vacuum-tight long-path gas IR cell, as an

interface allowing for the application of Fourier transform

infrared spectroscopy (FT-IR) for the online analysis of

volatile products of polymer degradation, is described.

Proof of concept and application of this new analytical

technique, subsequently referred to as TVA/FT-IR, is

illustrated through the examination of appropriate aspects

of the thermal degradation of PMMA polymers. 49 refs.

USA

Accession no.760230


71, No.21, 1st Nov.1999, p.4793-9

GEL PERMEATION CHROMATOGRAPHYCOUPLED TO FOURIER TRANSFORM MASSSPECTROMETRY FOR POLYMERCHARACTERIZATIONAaserud D J; Prokai L; Simonsick W J

Florida,University

On-line coupling of GPC to Fourier transform(FT) mass

spectrometry(MS) using a modified commercial

electrospray ionisation(ESI) interface was studied.

Selected oligomer profiles for the sodiated oligomer ions

of a narrow molec.wt. PMMA were generated and used

for obtaining a calibration curve. Using the MS-generated

calibration curve and the refractive index response for

quantification, an accurate MWD was calculated and

shown to be in good agreement with the value specified

by the supplier. GPC/ESI/FT-MS also allowed for an

unequivocal end group determination and characterisation

of a secondary distribution due to the formation of cyclic

reaction products. A glycidyl methacrylate/butyl

methacrylate copolymer with a broad MWD was

analysed, fractionation and high resolving power being

required for adequate characterisation. MWD data showed

the advantages of coupling high-resolution MS and GPC

to overcome the difficulty of analysing polydisperse

polymers with MS alone. 34 refs.

USA

Accession no.759794

Item 191Polymer

40, No.26, 1999, p.7341-50

SURFACE STRUCTURE OF KEVLAR FIBRESTUDIED BY ATOMIC FORCE MICROSCOPYAND INVERSE GAS CHROMATOGRAPHYRebouillat S; Peng J C M; Donnet J-B

Du Pont de Nemours International SA; Haute-

Alsace,Universite

Kevlar fibre surface structure is primarily and directly

observed in the filament configuration by the tapping

mode atomic force microscopy (AFM). The

microfibrils feature is observed with an average width

of 500 nm, composed of various types of periodical

units of an average size 50 nm in a pleating appearance.

At the less crystalline spot on the Kevlar fibre surface,

the periodical organisations exhibit the skin core-like

differentiation. In contrast, at the highly crystalline

spot, the periodicity is more uniformly arranged by a

rectangular network manner. Inverse gas

chromatography (IGC) is used as a tool to investigate

the surface structure heterogeneity by calculating the

surface energy of different types of probes adsorbed

on the Kevlar fibre surface. The energy sites

distribution plot of n-hexylamine adsorption at finite

dilution exhibits a two-adsorbing-peaks curve. At the

higher energy site, a possible hydrogen bonding

interaction is proposed between n-hexylamine and

oxygen-containing groups formed at the less crystalline

surface. According to the AFM and IGC results, a

Kevlar fibre surface organisations model at the

nanometer scale is proposed. 19 refs.


SWITZERLAND; WESTERN EUROPE

Accession no.758987


200, No.10, Oct.1999, p.2345-55

THERMAL DEGRADATION MECHANISMS OFPOLYETHERIMIDE INVESTIGATED BYDIRECT PYROLYSIS MASS SPECTROMETRYCarroccio S; Puglisi C; Montaudo G

Istituto per la Chimica e la Tecnol.dei Mat.Pol.;

Catania,University

The thermal degradation of poly(2,2'-bis(3,4-

dicarboxyphenoxy)phenylpropane-2-phenylenediimide)

was investigated by TGA and direct pyrolysis mass

spectrometry and the pyrolysis of this polyimide

compared with that of an aromatic polyamide (NOMEX).

The structure of preformed oligomers from the purified

polyetherimide and the structure of high temperature

pyrolysis products obtained at 620C were examined and

the thermal degradation pathways involved in the

degradation elucidated. 32 refs.


WESTERN EUROPE

Accession no.757742


200, No.10, Oct.1999, p.2205-7

COLLECTION OF SOLID-STATE CARBON-13CP/MAS NMR SPECTRA OF COMMONPOLYMERSWilhelm M; Neidhoefer M; Spiegel S; Spiess H W

Max-Planck-Institut fuer Polymerforschung; Wiley-

VCH Verlag GmbH



A collection of high resolution solid-state Carbon-13

NMR spectra of a wide range of polymers is presented. It

is useful for reference purposes in case of unknown or

partly unknown samples, such as polymer blends, block

copolymers or polymeric latices. 16 refs.


WESTERN EUROPE

Accession no.757725


66, No.1, 1999, p.107-25

VACUUM PYROLYSIS OF PVC. II: PRODUCTANALYSISMiranda R; Pakdel H; Roy C; Darmstadt H; Vasile C

Quebec,Universite Laval; Institut Pyrovac Inc.; Petru

Poni,Institute of Macromolecular Chemistry

Vacuum pyrolysis of pure PVC was carried out at various

temperatures between 220 and 520C and under a total

pressure of 2 kPa. The main gaseous and liquid pyrolysis

products obtained during the different stages of thermal

degradation were identified and quantified by

chromatographic methods. Global mass balance and

chlorine mass balance were determined and different

methods of capturing hydrogen chloride under vacuum

conditions were tested. The elemental composition,

surface properties and calorific value of the solid residue

were determined. 43 refs.

CANADA; EASTERN EUROPE; RUMANIA

Accession no.757340

Item 195Polymer Recycling

4, No.1, 1999, p.13-25

COMPOSITIONAL ANALYSIS ANDFEASIBILITY STUDY OF RECYCLED HDPEFOR DIRECT FOOD CONTACT APPLICATIONSSalafranca J; Cacho J; Nerin C

Zaragoza,University

Five HDPE samples, consisting of a virgin HDPE for

food-contact applications, three samples of this polymer

taken after each of the three sequential recycling cycles

and a real post-consumer sample were analysed. Two

different extraction methods were applied: a combination

of maceration and sonication; and the total dissolution of

the polymer. In order to evaluate both the feasibility of

using these polymers in food-contact applications and the

evolution of HDPE composition through the recycling

process, samples were analysed by both qualitative and

quantitative GC-MS. Furthermore, GC-FID was applied

to the determination of alpha-alkenes, the most

representative compounds as indicators of polymer matrix

degradation. Finally, antioxidants were analysed by

reversed phase HPLC. 34 refs.


WESTERN EUROPE

Accession no.756660


48, No.10, Oct.1999, p.1042-5

EFFECTS OF UV RADIATION ON SEVERALHIGH-PERFORMANCE POLYIMIDECOMPOSITESKiefer R L; Herring K; Wylie B J; Orwoll R A;

Thibeault S A

Williamsburg,College of William & Mary; NASA

Langley Research Center

Three carbon fibre-reinforced polyimides were exposed

to UV radiation at 177C, at three different intensities for

three different times, so that the product of intensity and

time was a constant. Intensities of 1, 2 and 3 suns, where

one sun is the power in space at one earth-sun distance,

were used, for a time periods of 500, 250 and 167 h. The

samples were characterised by X-ray photoelectron

spectroscopy (XPS), thermogravimetric analysis,

thermomechanical analysis and dynamic mechanical

analysis. Measurement of bulk properties showed no

difference between samples exposed to heat and UV

radiation, and control samples. Surface analysis by XPS

showed an apparent decrease in carbonyl concentration

on the surface of some exposed samples. This was

correlated to surface contamination by a silicone-

containing material. 3 refs.

USA

Accession no.756185

Item 197Composites Part A: Applied Science and

Manufacturing

30A, No.12, 1999, p.1401-13

USE OF XPS FOR CHARACTERISATION OFGLASS FIBRE COATINGSThomason J L; Dwight D W


X-ray photoelectron spectroscopy was applied to a study

of commercial and experimental glass fibres using three

different instruments. A protocol for plotting ratios of

appropriate atom concentrations was developed and the

plots used to estimate the surface coverage of the coating

on the glass fibres and provide data on the chemical

composition of the coating. The relationships between

the spectroscopic data and coated glass fibre parameters

are demonstrated using an overlay model and data from

the three instruments are compared. 22 refs.

USA

Accession no.755993


71, No.20, 15th Oct.1999, p.4776-80

COMPOSITION AND MICROSTRUCTUREDETERMINATION OF A LATEX SYSTEM BYPYROLYSIS GAS CHROMATOGRAPHY



Frank Cheng-Yu Wang

Dow Chemical Co.

The composition and microstructure of polymers in a

latex system were studied by pyrolysis gas

chromatography. The composition and microstructure

of a polymer in the emulsion phase were identified by

direct pyrolysis of the latex system, followed by

comparing the trimer peak pattern with appropriate

microstructure standards. The polymer in the aqueous

phase was pre-pyrolysis derivatised with

tetrabutylammonium hydroxide to convert the acid to

its butyl ester. Similar procedures were then used to

explore the composition and microstructure of the

polymer in the aqueous phase. Polymers analysed

included SCX-2660 (probably a styrene-methyl

methacrylate-butyl acrylate terpolymer), styrene-butyl

acrylate copolymer and styrene-alpha-methylstyrene-

butyl acrylate terpolymer. 17 refs.

JOHNSON S.C.,& SON INC.USA

Accession no.755899

Item 199Oxford, Butterworth-Heinemann Ltd., 1999,

pp.xxvii,920. 24cms. 12/1/00. 011

PLASTICS MATERIALS. 7TH EDN.Brydson J A

The latest edition, now the seventh, of this reputable text

book, provides an overview of the scientific, technological

and economic aspects of currently available plastics and

related materials, and also focuses on new materials -

many based on metallocene catalyst technology.

Developments with condensation polymers, including

several new polyester-type materials of interest for bottle

blowing and/or degradable plastics, are also covered. This

edition also attempts to explain the basis of metallocene

polymerisation. The commercial importance of the

materials discussed is also noted.

Accession no.755818


74, No.10, 5th Dec.1999, p.2432-8

CHARACTERIZATION OF BISPHENOL A-BASED EPOXY RESINS BY HPLC, GPC, GPC-MALLS, VPO, VISCOMETRY, AND END GROUPANALYSIS: ON THE IDENTIFICATION OF 2,3-DIHYDROXYPROPYL-CONTAININGCOMPOUNDS, DETERMINATION OF MOLARMASS DISTRIBUTION, AND BRANCHINGPodzimek S; Kastanek A

SYNPO

Results of the above characterisation are presented and

discussed with particular reference to determination of

alpha-glycol-containing compounds, determination of

molar mass and molar mass distribution, determination

of branching and determination of refractive index

increment. 19 refs.

CZECH REPUBLIC

Accession no.755647

Item 201Journal of Vinyl and Additive Technology

5, No.3, Sept.1999, p.148-58

NMR SPECTRA OF LEAD STABILISERSGrossman R F

Halstab Corp.

High resolution proton and 13C NMR spectra of lead-

based heat stabilisers and their reaction products, obtained

using the magic angle spinning technique, support

structural assignments inferred from IR spectra. These

demonstrate that lead stabilisers are unique compounds,

rather than the double salts of lead oxide found in

textbooks. 8 refs.

USA

Accession no.755491

Item 202Polymers for Advanced Technologies

10, No.4, April 1999, p.237-43

CHARACTERISATION OF THE SURFACE OFBULK-MOULDED COMPOUNDSVallat M F; Schultz J; Mauzac C; Jacquin M

Institut de Chimie des Surfaces et Interfaces; PSA

Etudes et Recherches Centre Technique de Belchamp

The surface characterisation of bulk moulding compound

(BMC) automotive parts using complementary techniques

of surface analysis, i.e. SEM, X-ray photoelectron

spectroscopy, time of flight secondary ion mass

spectroscopy, glow discharge spectroscopy and contact

angle is described. Similarities and differences between

BMC surfaces and sheet moulding compound (SMC)

surfaces are pointed out. Particular emphasis is placed on

mould release agents (polymeric and stearate) on the surface

which can influence future bonding behaviour. 14 refs.


WESTERN EUROPE

Accession no.754736


200, No.9, 1999, p.2074-9

INVESTIGATION OF MOLECULARDIMENSIONS OF POLYSTYRENE AS AFUNCTION OF SOLVENT COMPOSITION:APPLICATION TO LIQUIDCHROMATOGRAPHY AT THE EXCLUSION-ADSORPTION TRANSITION POINTBaran K; Laugier S; Cramail H

ENSCPB

Liquid chromatography was used to study PS standards at

the exclusion-adsorption transition point using silica



adsorbents having differing porosities in various eluents. The

behaviour of model PS chains in solvent mixtures

corresponding to the critical adsorption conditions was

evaluated using viscometry and light scattering. It was found

that critical adsorption conditions could be achieved if the

polymer chains entered the pores of the stationary phase and

that the characteristics of the elution mode could be defined

with the aid of the polarity index of the eluent. 20 refs.


WESTERN EUROPE

Accession no.752269


Vol.141, 1999, p.95-101

RECENT ADVANCES IN THE ANALYSIS OFPOLYMERS AND COPOLYMERS BY MASSSPECTROMETRYMontaudo M S

Istituto per la Chimica e la Tecnol.dei Mat.Pol.

Progress which has been made in the use of MALDI mass

spectroscopy to provide reliable molec.wt. and MWD

values is reported. Molec.wt. averages and MWD of

polydisperse samples (PMMA, siloxanes, polyesters and

copolyesters) were obtained by off-line coupling of SEC

equipment with the MALDI mass spectrometer. SEC

traces of the samples were recorded, selected fractions

were analysed by MALDI-TOF and the average

molec.wts. of the fractions were determined from the mass

spectrum. A method for analysing unknown copolymers,

which involves the use of Markoffian statistics, is also

presented. 26 refs.


WESTERN EUROPE

Accession no.752091

Item 205Polimery

44, No.4, 1999, p.246-54

Polish

USE OF PHOTOELECTRON SPECTROSCOPYIN STUDIES OF THE DEPTH PROFILE OFPOLYPROPYLENE FILMZenkiewicz M; Golebiewski J

Metalchem Plastics Processing Institute

The physical fundamentals of photoelectron spectroscopy

are reviewed and the range of applications is given. Three

PP films were examined and the depth of oxidation was

found to be in the nanometer range. The oxidation level

of the external layer increases as the specific energy of

corona discharges is increased. 27 refs. Articles from this

journal can be requested for translation by subscribers to

the Rapra produced International Polymer Science and

Technology.


Accession no.747688

Item 206LCGC International

12, No.9, Sept.1999, p.577/87

LC-MS ANALYSIS OF POLYMER ADDITIVESBY EL AND API: IDENTIFICATION ANDQUANTIFICATIONYu K; Block E; Balogh M

Waters Corp.

Mass spectrometry can be the ideal detector for liquid

chromatography because it offers both universality and the

required selectivity for complex analytical problems. The

two most popular types of interface for the benchtop single

quadrupole LC-mass spectrometer are the particle beam

interface and the atmospheric pressure ionisation interface.

The particle beam interface is used to generate electron

ionisation spectra and the API interface is used to generate

either electrospray or atmospheric pressure chemical

ionisation. This comprehensive article supplies a detailed

analysis of a study in which organic extractable from

polypropylene was used as the model analyte to

demonstrate how the information obtained separately from

EI and API can be complementary. Seven compounds were

separated and detected by both MS detectors. 35 refs.

USA

Accession no.747567

Item 207Macplas International

No.10, Aug.1999, p.64-70

DIFFERENTIAL SCANNING COLORIMETRYAND INFRARED SPECTROSCOPY INPOLYMER ANALYSISPanarotto A; Bertucci M

Cesap

Differential scanning calorimetry is one of the most

commonly used methods for characterising the thermal

properties of polymers. This method, particularly if

complemented by IR spectroscopic analysis, also allows

the nature of the materials under test to be determined.

The principles involved in DSC and IR spectroscopy are

discussed.


WESTERN EUROPE

Accession no.745360

Item 208Polimery Tworzywa Wielkoczasteczkowe

44, No.3, 1999, p.218-21

Polish

DETERMINATION OF MIGRATION OFDIMETHYL TEREPHTHALATE ANDDIMETHYL ISOPHTHALATE FROM PLASTICSStareczek T; Kaminska G; Ermel J; Kortylewska

Edited by: Gliwice,Institute of Plastics & Paint Industry

A gas chromatographic method is described for

determining dimethyl terephthalate and dimethyl



isophthalate in food simulants. The method consists in

extracting DMT and DMIP from the food simulants with

chloroform and analysing of the compounds by GC with

the use of calibration curves and diethyl terephthalate as

an internal standard. 3 refs. Articles from this journal can

be requested for translation by subscribers to the Rapra

produced International Polymer Science and Technology.


Accession no.745025


73, No.2, 11th July 1999, p.221-6

EVALUATION OF EVA-PVAC BLENDBEHAVIOUR BY 1-D AND 2-D SOLID-STATENMRDe Souza C M G; Pacheco C R; Tavares M I B

Rio de Janeiro,Universidade Federal; PETROBRAS

Ethylene-co-vinyl acetate and poly(vinyl acetate) blends

were prepared in different proportions by melting in a

HAAKE Rheomix mixer. The blends were prepared at a

fixed temperature, rotation rate, and processing time.

High-resolution solid state NMR was used to characterise

the blends with respect to structure-mobility-compatibility

using magic angle spinning with cross-polarisation and

high power hydrogen decoupling and measurements of

the proton spin-lattice relaxation time in the rotating

frame. Miscibility between polymer chains was also

studied by two-dimensional hydrogen ion/carbon-13 shift

correlation (HETCOR). 21 refs.

BRAZIL

Accession no.743489


32, No.11, 1st June 1999, p.3671-3

LIQUID ADSORPTION CHROMATOGRAPHYOF COPOLYMERS: MOLAR MASS(IN)DEPENDENT RETENTIONBerek D

Slovak Academy of Sciences

Liquid adsorption chromatography with a continuous

solvent gradient elution was shown by several previous

authors to be capable of separating random and graft

copolymers according to their chemical composition, with

their molar masses not playing an important role. A

tentative explanation of this finding is presented. It is

assumed that the copolymer species travel along the

column with a velocity which exactly corresponds to that

of the eluent composition, exhibiting a displacing power

just necessary to prevent a fast progress of the

macromolecules due to their exclusion. Under specific

conditions, retention of macromolecules at this adsorption

promoting ‘barrier’ depends almost exclusively on the

copolymer composition and not on its molar mass. This

hypothesis is based on the mechanism of the recently-

proposed and tested liquid chromatographic elution of

homopolymers under limiting conditions of desorption

and takes into account the simultaneous effect of

adsorption and exclusion of macromolecules onto/from

the column packing. 17 refs.


Accession no.743327

Item 211Polymer Recycling

3, No.4, 1997/1998, p.263-7

PROCEDURES FOR THE COMPOSITIONALANALYSIS OF REINFORCED POLYESTERRECYCLATEBream C E; Hornsby P R

Brunel University

In order to consider effective strategies for the recovery

and reuse of plastics recyclates, a quantitative method is

described for the characterisation of polyester-based

moulding compounds. Analytical procedures are

described for the quantification of fibre, filler and fire

retardant contents in polyester moulding compounds

containing calcium carbonate filler, glass fibre

reinforcement, and aluminium hydroxide flame retardant.

3 refs.


WESTERN EUROPE

Accession no.742796

Item 212High Performance Plastics

Aug.1999, p.10

IDENTIFICATION OF PLASTICS IN WASTE

A review is presented of the methods used in the

identification of plastics waste prior to recycling

operations, which was published in International Polymer

Science and Technology, and translated from a Polish

source. Rapid spectroscopic methods are indicated, and

their use in packaging and automotive recycling are

discussed.


Accession no.742675


37, No.13, 1st July 1999, p.1485-94

GLASS TRANSITION AND MISCIBILITY INBLENDS OF TWO SEMI-CRYSTALLINEPOLYMERS: POLYARYL ETHER KETONE ANDPOLYETHER ETHER KETONEWoo E M; Tseng Y C

Taiwan,National Cheng Kung University

A study was made of the miscibility in the amorphous

region of melt mixed blends composed of a novel polyaryl

ether ketone (PK99) and PEEK using various methods,



including optical microscopy, DSC, SEM, FTIR

spectroscopy and wide-angle X-ray diffraction. Samples

were physically aged in order to resolve any possible

overlapping Tg’s but only one single Tg was detected over

the entire composition range. No evidence for

isomorphism was found and the crystal forms of the

respective polymers remained distinct and unchanged by

miscibility in the amorphous region. 14 refs.

TAIWAN

Accession no.742306


53, No.6, June 1999, p.672-81

POST-CONSUMER PLASTIC IDENTIFICATIONUSING RAMAN SPECTROSCOPYAllen V; Kalivas J H; Rodriguez R G

Idaho,State University

The suitability of Raman spectroscopy, when used with

K-nearest neighbours, library searching or cyclic subspace

regression, for computerised classification of post-

consumer plastics was evaluated. Plastics investigated

were PETP, PP, PS, PVC, HDPE AND LDPE.

Modifications were made to the original cyclic subspace

regression algorithm for modelling multiple sample

properties and the adapted algorithm employed to directly

compare the mechanisms of principal component

regression and the PLS2 form of partial least-squares. It

was found that Raman spectroscopy could be used to

identify both HDPE and LDPE. 33 refs.

USA

Accession no.741260


53, No.5, May 1999, p.557-64

COMPARISON OF NEAR-INFRARED ANDRAMAN SPECTROSCOPY FOR THEDETERMINATION OF CHEMICAL ANDPHYSICAL PROPERTIES OF NAPHTHAMin-Sik Ku; Hoeil Chung

SK Corp.

Near-infrared and FTIR Raman spectroscopy were

compared and evaluated for the quantitative analysis of

naphtha using partial least-squares regression. 19 refs.

SOUTH KOREA

Accession no.740339


53, No.5, May 1999, p.551-6

FOURIER TRANSFORM RAMAN SPECTRA OFLINEAR LOW-DENSITY POLYETHYLENE ANDPREDICTION OF THEIR DENSITY BYMULTIVARIATE DATA ANALYSIS

Sano K; Shimoyama M; Ohgane M; Higashiyama H;

Watari M; Tomo M; Ninomiya T; Ozaki Y

Kwansei-Gakuin,University; Hyogo,Prefectural Police

Headquarters; Yokogawa Electric Co.

FTIR spectra were measured for pellets of sixteen kinds

of LLDPE with short branches and one kind of PE without

any branch to explore the effects of the branches on the

physical properties and the Raman spectrum. Partial least

squares analysis regression was applied to the Raman

spectra after multiplicative scatter correction to propose

a calibration model that predicts the density of LLDPE.

38 refs.

JAPAN

Accession no.740338


71, No.893, June 1999, p.53-60

INVERSE GAS CHROMATOGRAPHY, SURFACEPROPERTIES, AND INTERACTIONS AMONGCOMPONENTS OF PAINT FORMULATIONSZiani A; Xu R; Schreiber H P; Kobayashi T

Ecole Polytechnique de Montreal; Nippon Paint Co.

Inverse gas chromatography analysis at very high dilution

and at finite concentrations of probe injection was carried

out on a series of polymers and pigments used in paint

formulations. Values of dispersion surface energies, andof acid-base interaction parameters were obtained for the

materials, and pair interaction parameters were calculated

from the results. The dispersion stability of each pigment/

polymer combination was measured and correlated with

the acid-base interaction parameters of the materials, and

is shown to justify the availability of fundamental

thermodynamic interaction data to optimise performance

aspects of protective coatings. 23 refs.

CANADA; JAPAN

Accession no.739845


71, No.10. 15th May 1999, p.2037-45

ANALYSIS OF POLYMERIC FLAMERETARDANTS IN ENGINEERINGTHERMOPLASTICS BY PYROLYSIS GASCHROMATOGRAPHY WITH AN ATOMICEMISSION DETECTORWang F C Y

Dow Chemical Co.

Halogen-containing polymeric flame retardants in

engineering thermoplastics were analysed by pyrolysis

gas chromatography(Py-GC) with an atomic emission

detector(AED) and a mass selective detector(MSD). The

AED was very effective in monitoring halogen-containing

pyrolysates after Py-GC. The type of polymeric flame

retardant used in thermoplastics could be identified by

peak pattern recognition through an AED halogen element



trace. A set of thermoplastic resins containing different

brominated polymeric flame retardants was studied. After

generation of the pyrogram by Py-GC/AED, those

pyrolysates produced from polymeric flame retardants

were identified by MSD analysis of a complex total ion

chromatogram generated by the thermoplastic resins. The

results demonstrated the effectiveness of the AED in the

tasks of specific element monitoring and component

pattern recognition. The advantages and disadvantages

of using the AED are also discussed. 11 refs.

USA

Accession no.738049

Item 219ACS, Polymeric Materials Science and Engineering.

Vol.76. Conference proceedings.

San Francisco, Ca., Spring 1997, p.128-9. 012

ATOMIC FORCE MICROSCOPY STUDY OFINTRAOCULAR LENS IMPLANTS -TOPOGRAPHY AND SURFACE PROPERTIESKowalewski T; Ravi V N

Washington,University; St.Louis,Veterans Affairs

Medical Center


Cataracts are one of the most common causes of

worldwide blindness. They are presently corrected by

surgery in which the natural cataractous lens is replaced

by a synthetic intraocular lens. Successful visual

rehabilitation is not only a function of patients’ health

and the surgical technique, but it also depends on the

optical, mechanical and bioperformance of the intraocular

lens. Visual deterioration after surgery has been attributed

to cellular debris deposited on the lens surface and

capsular opacification resulting from inflammation.

Although the exact sequence of events that take place

when an implant is exposed to the ocular environment in

vivo is not known, protein adsorption, complement

activation and cellular adhesion have been implicated and

believed to be influenced by the surface properties of the

implants. The surface characteristics (surface topography

and viscoelasticity) of intraocular lenses are investigated

using tapping-mode atomic force microscopy. 9 refs.

USA

Accession no.737604

Item 220Polymer

40, No.17, 1999, p.4763-7

MODULATED DIFFERENTIAL SCANNINGCALORIMETRY: 14. EFFECT OF MOLECULARINTERACTIONS ON GLASS TRANSITIONBEHAVIOUR AND INCREMENT OF HEATCAPACITY IN MISCIBLE POLYMER BLENDSSong M; Hourston D J; Pollock H M; Hammiche A

Loughborough,University; Lancaster,University

Modulated differential scanning calorimetry was used

to study miscible polymer blends. The blends studied

were poly(vinyl acetate)/poly(methyl acrylate),

poly(phenylene oxide)/PS and two poly(styrene-co-

acrylonitrile)/PMMA blends, the last two containing

different acrylonitrile contents. Specific molecular

interactions determined whether the glass transition

temperature and the increment of heat capacity versus

composition showed positive or negative deviations

from linearity for the blend systems. In the non-

interacting system (poly(vinyl acetate)/poly(methyl

acrylate)), the glass transition temperature and increment

of heat capacity showed linear behaviour with

composition. Thermodynamic theories for the observed

results were discussed. 17 refs.


WESTERN EUROPE

Accession no.737361

Item 221LCGC International

12, No.7, July 1999, p.432/6

QUANTITATIVE ANALYSIS OFPOLY(METHYLMETHACRYLATE) IN DRUGSBY CURIE-POINT PYROLYSIS GASCHROMATOGRAPHYMuguruma S; Uchino S; Oguri N; Kiji J

Japan Analytical Industry Co.Ltd.; Tottori,University

Curie-point pyrolysis gas chromatography was used for

the quantitative analysis of residual synthetic adsorbent

crosslinked PMMA used in drug purification. Levels of

PMMA adsorbent below 0.15% in drug substances were

successfully measured quantitatively by Py-GC using

characteristic peaks that reflect the structure of the

adsorbent, demonstrating that this analytical technique

can be used to monitor compliance with the limit of 0.1%

organic impurity in drug substances stipulated by ICH

guidelines. 12 refs.

JAPAN

Accession no.736647


72, No.7, 16th May 1999, p.913-25

HIGH-PERFORMANCE LIQUIDCHROMATOGRAPHY-MASS SPECTROMETRYOF EPOXY RESINSFuchslueger U; Rissler K; Stephan H; Grether H J;

Grasserbauer M

Ciba Specialty Chemicals Inc.; Vienna,Technical

University

The application of liquid chromatography coupled to

mass spectrometry for the analysis of epoxy resins was

shown in two examples. Electrospray (ESI) and

atmospheric pressure chemical ionisation (APCI) were

compared with respect to the ionisation of diglycidyl

ether of bisphenol A (DGEBA)-based epoxy resins. By-

products in a typical modified solid DGEBA-based



epoxy resin and in a new weatherable crosslinker for

powder coating applications were characterised and

discussed. 26 refs.

AUSTRIA; SWITZERLAND; WESTERN EUROPE

Accession no.734831


13, No.5, 1999, p.629-45

ADHESION CHARACTERISATION OFPROTECTIVE ORGANIC COATINGS BYELECTROCHEMICAL IMPEDANCESPECTROSCOPYDeflorian F; Fedrizzi L

Trento,University

This review describes in detail the influences on adhesion

of different pretreatments or organic coatings, considering

aluminium, galvanised steel, and stainless steel substrates,

and it was shown that the information obtained using an

electrochemical approach can be used for adhesion

evaluation, with particular attention to monitoring of

adhesion in an aqueous environment, which is the most

detrimental for protective organic coatings. 40 refs.


WESTERN EUROPE

Accession no.733531


200, No.5, May 1999, p.1134-42

POSSIBILITIES AND LIMITS OF PHOTONCORRELATION SPECTROSCOPY INDETERMINING POLYMER MOLECULARWEIGHT DISTRIBUTIONSFaraone A; Magazu S; Maisano G; Villari V; Maschio G

Messina,University

The effect of concentration and polydispersity on the

collective diffusion coefficient(Dc) evaluated using

photon correlation spectroscopy was investigated on

PMMA in acetone solutions. The concentration

dependence of the Dc followed a linear regression law,

the slope being fairly independent of polydispersity,

molec.wt. and temp. The diffusion coefficient at infinite

dilution obeyed a given scaling law. The inversion of the

scattered intensity autocorrelation data by the

regularisation method CONTIN permitted the evaluation

of the MWD function of the polymeric samples. Although

this algorithm gave valuable information on average

amounts or on the widths of the distribution, it had limited

resolution power. A comparison with the results obtained

by size exclusion chromatography was therefore carried

out for a set of samples having monomodal and bimodal

distribution functions. 22 refs.


WESTERN EUROPE

Accession no.733222

Item 225Coloring Technology for Plastics.

New York, N.Y., Plastics Design Library, 1999, p.197-

207. 52

MEASURING STABILISERS IN PIGMENTEDPLASTICS WITH NEAR-INFRAREDSPECTROSCOPYSolera P; Nirsberger M; Castillo N

Ciba Specialty Chemicals Corp.

Edited by: Harris R M

Near-infrared (NIR) spectroscopy has become a

commonplace analytical tool in the plastics industry. NIR

techniques have made quantification of many organic

components in polymer processing easy and quick. The

work presented outlines the methodology for using NIR

to measure stabiliser levels in colour concentrates and

natural polymer formulations. Advantages and limitations

are considered as well as particle size and product form.

4 refs.

USA

Accession no.732217

Item 226Coloring Technology for Plastics.

New York, N.Y., Plastics Design Library, 1999, p.191-

5. 52

PRACTICAL ANALYSIS TECHNIQUES OFPOLYMER FILLERS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY(FTIR)Coles B J; Hall C J

Hauser Inc.

Edited by: Harris R M

The identification of polymers by FTIR is often

complicated by the presence of fillers. However, for kaolin

clay, FTIR analysis should be able to identify the filler

and predict its concentration using a standard curve. The

resulting percentage is more reliable than a simple ash,

which may change the chemical composition of the filler.

2 refs.

USA

Accession no.732216

Item 227Pitture e Vernici

75, No.5, March 1999, p.7-8

English; Italian

E.I.S. EVALUATION OF ATTACHED AND FREEPOLYMER FILMSCastela A S; Simoes A M P

Evaluation of the volume fraction of water in organic

coatings in immersion is often made by electrochemical

impedance spectroscopy, EIS, and based upon the

evolution of the coating capacitance. Among the several

models and equations proposed for this determination,

the most frequently used is the Brasher equation. Most



frequently these determinations are made with applied

coatings, although studies can be found in the literature

using free films. The behaviour of a commercial coating

- PVC plastisol - is studied, both applied on a metallic

substrate and as a free film.


WESTERN EUROPE

Accession no.731759


55, No.2, 1999, p.559-63

TG/FT-IR STUDIED OF POLY(VINYLCHLORIDE) BLENDSPielichowski K

Krakow,Technical University

Thermogravimetry coupled with FTIR was used to

investigate the stabilising action of 3-(2,4-

dibromophenylazo)-9-(2,3-epoxypropane)carbazole on

the degradation of PVC. This secondary stabiliser

increased the initial temperature of hydrogen chloride

evolution (the main process responsible for PVC

decomposition), thereby allowing its application for novel

PVC systems with enhanced thermal stability. 10 refs.


Accession no.731454


71, No.9, 1st May 1999, p.1809-14

POLYMER ANALYSIS BY LIQUIDCHROMATOGRAPHY/ELECTROSPRAYIONISATION TIME-OF-FLIGHT MASSSPECTROMETRYNielen M W F; Buijtenhuijs F A

Akzo Nobel Central Research

Different liquid chromatography modes in polymer

analysis were successfully interfaced with electrospray

ionisation time-of-flight mass spectrometry in a single

experimental set-up: the mass spectrometry data from size

exclusion chromatography/mass spectrometry of PMMA

were used as absolute calibration points in the size

exclusion chromatography/refractive index

chromatogram, and monomer mass and end groups were

inferred from the isotopically resolved mass spectra. 44

refs.



Accession no.731446

Item 230Polymer Preprints. Volume 40. Number 1. March 1999.

Conference proceedings.

Boston, Ma., March 1999, p.226-7. 012

SURFACE MODIFICATION OF POLYSTYRENESTUDIED BY IR-VISIBLE SUM FREQUENCY

GENERATION SPECTROSCOPYZhang D; Dougal S; Yeganeh M S

Exxon Research & Engineering Co.


The effects of UV light and oxygen plasma on PS surfaces

is investigated using SFG spectroscopy. The observed

spectral changes provide strong support for the

photooxidation of the aromatic ring at the PS surface, as

observed by the dramatic decrease in the aromatic C-H

vibration during photo irradiation and plasma treatment.

It is also found that the kinetics of the photooxidation of

the PS surface, monitored by SFG, is much faster than

similar process observed by other techniques, such as

FTIR or SIMS. 13 refs.

USA

Accession no.730043

Item 231Polymer Composites

20, No.2, April 1999, p.314-20

CHARACTERISATION OF MIXED FIBRENYLON COMPOSITES INCORPORATINGCOMPOSITE SCRAPLicea-Claverie A; Carrillo F J U; Alvarez-Castillo A;

Castano V M

Tijuana,Instituto Tecnologico; Zacatepec,Instituto

Tecnologico; UNAM

Recycling of engineering thermoplastics and their

composites is discussed. A study on nylon-6,6 based

composites with mixed glass fibre and carbon fibre

reinforcement, including nylon composite scrap in their

formulation, were reported. Several formulations were

prepared by injection moulding and were characterised

by stress-strain measurements, impact testing,

simultaneous DTA and TGA, density measurements and

SEM. Mechanical and thermal properties of the resulting

composites are presented, discussed, and compared with

a virgin standard composite. 26 refs.

MEXICO

Accession no.729302


71, No.7, 1st April 1999, p.1316-22

CHARACTERIZATION OF NATURAL RESINSHELLAC BY REACTIVE PYROLYSIS-GASCHROMATOGRAPHY IN THE PRESENCE OFORGANIC ALKALIWang L; Ishida Y; Ohtami H; Tsuge S; Nakayama T

Nagoya,University; Gifu Shellac Manufacturing

Co.Ltd.

A method for determining the chemical composition of

natural resin shellac was developed based on reactive

pyrolysis-gas chromatography(Py-GC) in the presence of

an organic alkali, tetramethylammonium

hydroxide(TMAH). Py-GC using 25% TMAH aqueous



solution permitted the highly sensitive determination of

terpenic acids, aleuritic acid, several minor fatty acids and

the wax components of shellac as their methyl derivatives

on the resulting pyrograms with less than 2.0 % relative

standard deviations without using any cumbersome

pretreatment. The observed average distributions of each

resin acid component determined by reactive Py-GC for

shellac samples from India and Thailand showed that the

average ratios among terpenic acids, aleuritic acid and the

other fatty acids were about 53:24:14 for Indian shellac

and 51:35:14 for Thailand shellac, respectively, suggesting

a slightly significant difference. Clearer discrimination of

the shellac samples from the two different countries was,

however, achievable by applying principal component

analysis for the mole percent distributions of all the acidic

components determined by reactive Py-GC. 24 refs.

INDIA; JAPAN; THAILAND

Accession no.727139

Item 233ACS Polymeric Materials Science and Engineering.

Fall Meeting 1997. Volume 77. Conference

proceedings.

Washington, D.C., 1997, p.594-5 .012

EFFECT OF SECOND DIMENSION SAMPLINGRATE AND PARTICLE SIZE ON RESOLUTIONAND RUN TIME IN TWO DIMENSIONALLIQUID CHROMATOGRAPHY FOR THEANALYSIS OF POLYMERSMurphy R E; Schure M R; Foley J P

Rohm & Haas Co.; Villanova,University


The optimisation of a two dimensional high performance

liquid chromatography (HPLC) (reverse phase liquid

chromatography/gel permeation chromatography (GPC))

system for the analysis of low molecular weight polymers

is described. A test mixture of polyethylene glycols and a

commercial surfactant was used. The analysis time of the

second dimension, GPC, was varied by using different

columns. The columns had different particle sizes and

lengths, and the two dimensional resolution was compared

by varying the run time in the second dimension.

Following the optimisation, it was possible to complete a

two dimensional analysis in the time normally taken for

a normal gradient HPLC run. It was established that

conventional columns could be run with higher flow rates

without a significant loss of resolution. The combination

of shorter and smaller particle GPC columns resulted in

lower sampling periods at lower flow rates than

conventional columns. The highest sampling rate into the

second dimension gave the best resolution. 7 refs.

USA

Accession no.726180

Item 234Shawbury, Rapra Technology Ltd., 1997, pp.315.

220.00. 30cms. 9922

RAPRA COLLECTION OF INFRARED SPECTRAOF RUBBERS, PLASTICS ANDTHERMOPLASTIC ELASTOMERS. SECONDEDITIONSidwell J A

This book provides a set of transmission and pyrolysate

spectra of a comprehensive range of technically important

rubber and plastics materials including copolymers and

blends which are in current use. Materials are indexed

under both polymer and trade name.

Accession no.725345

Item 235Polymer

40, No.12, 1999, p.3479-85

INVERSE GAS CHROMATOGRAPHICCHARACTERIZATION OF POLY(ETHYLENEOXIDE)Al-Saigh Z Y

Columbus,State University

The inverse gas chromatography method was used to

obtain the thermodynamic properties and the surface

energy of a semicrystalline polymer, PEO. PEO was used

as a stationary phase in the chromatographic column and

16 solutes with a different chemical nature were used as

eluents. Alkanes showed endothermic interaction

parameters and the molar heat of mixing in a temp. range

of 70-130C. Acetates and alcohols showed better

interactions with the PEO layer and butanol was found to

be the best solvent for PEO among all solutes used. The

variation in molec.wt. of PEO above 400 g/mol showed

no apparent effect on the interaction coefficients. The

dispersive contribution of the surface energy of PEO was

measured as a function of temp., which ranged from 8.00

and 13.00 mJ/sq m, indicating a poor surface energy of

PEO. 43 refs.

USA

Accession no.721885

Item 236Journal of Adhesion

68, Nos.1-2, 1998, p.117-42

QUANTIFICATION OF COATING ADHESIONUSING LASER INDUCED DECOHESIONSPECTROSCOPYMeth J S; Sanderson D; Mutchler C; Bennison S J

DuPont Co.

A new technique, laser induced decohesion spectroscopy,

is presented, which is capable of measuring the practical

work of adhesion between a transparent polymer coating

or substrate. A laser pulse directed onto the sample creates

a blister at the transparent/opaque interface. The blister’s

internal pressure depends on the laser pulse energy, and

at a critical pressure the sample fractures, creating an

annular debond similar to that obtained in the standard

blister test. By measuring physical variables such as the



curvature of the blister, and its radius and thickness, it is

possible to deduce the practical work of adhesion. 19 refs.

USA

Accession no.721348


13, No.3, 1999, p.379-91

DETERMINATION OF THE ADHESIONPROPERTIES OF AN ALKYD PIGMENTEDCOATING BY ELECTROCHEMICALIMPEDANCE SPECTROSCOPYGonzalez J E G; Rosca J C M

Gran Canaria,University

Impedance measurements were performed in different

frequency ranges at open circuit potential for an alkyd

coating with titanium dioxide as a mineral pigment in

3% sodium chloride. The most probable impedance

equivalent circuit method was considered for data

analysis. The interpretation of the impedance spectra

permitted the determination of water permeation, the

formation of blisters, swelling of the coating, and the loss

of adhesion. 17 refs.


WESTERN EUROPE

Accession no.721335

Item 238ACS Polymeric Materials Science and Engineering.Fall

Meeting 1997.Volume 77.Conference proceedings.

Washington, D.C., 1997, p.48-9 012

QUANTITATION IN THE ANALYSIS OFOLIGOMERS BY HPLC WITH ELSDTrathnigg B; Kollroser M; Maier B; Berek D; Janco M

Graz,Karl-Franzens-Universitat; Slovak Academy of

Sciences


The influence of the operating parameters used when

operating evaporative light scattering detectors in

conjunction with high performance liquid

chromatography for the characterisation of oligomers was

investigated, using polyether samples. It was concluded

that the instrument was useful because it provided gradient

elution, however, very careful calibration was required

to obtain reliable quantitative data. 16 refs.

AUSTRIA; WESTERN EUROPE

Accession no.720839



Washington, D.C., 1997, p.46-7 012

APPLICATION OF SEC AND HPLC TO THECHARACTERIZATION OF POLYMERS,OLIGOMERS, AND SMALL MOLECULES USEDIN COATINGS AND INKS

Kuo C; Grieser M D; Robinson D

Henkel Corp.


Applications are given of the use of size exclusion

chromatography and high performance liquid

chromatography for the characterisation of coatings

systems which either use water as the major solvent or

utilise low molecular weight polymers, oligomers, and

reactive additives which are then reacted to produce high

molecular weight and crosslinked films. 6 refs.

USA

Accession no.720838



Washington, D.C., 1997, p.35-6 012

LIQUID CHROMATOGRAPHY OFMACROMOLECULES UNDER LIMITINGCONDITIONS OF SOLUBILITY: FIRSTEXPERIMENTAL OBSERVATIONSBartkowiak A; Hunkeler D; Murgasova R; Berek D

Szczecin,Technical University; Swiss Federal Institute

of Technology; Slovak Academy of Sciences


Liquid chromatography at the critical adsorption point

(LC LCS) was investigated. The solubility ofmacromolecules, the sensitivity of LC LCS to such

variables as the injection volume, concentration injected,

mobile phase flow rate and mixing between the injection

zone, were investigated, using polymethyl methacrylate

(PMMA) and polyacrylamide standards. It is proposed

that using tetrahydrofuran and n-hexane as eluents for

PMMA, at the LC LCS, limited polymer insolubility or

even local precipitation is combined with the size

exclusion of macromolecules. 12 refs.

EASTERN EUROPE; POLAND; SLOVAK REPUBLIC;

SLOVAKIA; SWITZERLAND; WESTERN EUROPE

Accession no.720833



Washington, D.C., 1997, p.31-2 012

LIQUID CHROMATOGRAPHY OFMACROMOLECULES AT THE CRITICALADSORPTION POINT: PROBLEMS ANDPITFALLSBerek D; Janco M



The role of column packing pore size in liquid

chromatography at the critical adsorption point was

investigating using three silica gels and a series of

polymethyl methacrylates (PMMA), using toluene,

tetrahydrofuran (THF) or their mixtures as eluents.



Toluene strongly promotes adsorption of PMMAs on the

silica surface, whereas THF suppresses adsorption. It was

established that the pore size of the column packings

played an important role in liquid chromatography at the

critical adsorption point. The column with the smallest

pores largely determined the behaviour of the whole set.

The feasibility of using silica gel as column packings for

liquid chromatography at the critical adsorption point is

questioned. 14 refs.


Accession no.720831



Washington, D.C., 1997, p.22-3 012

2D-LC OF FUNCTIONAL POLYETHERSTrathnigg B; Kollroser M; Parth M

Graz,Karl-Franzens-Universitat


A combination of liquid chromatography under critical

conditions using coupled density and RI detection in one

dimension, and gradient high performance liquid

chromatography in the second dimension, was used in

the two-dimensional chromatographic analysis of the

oligomers present in fatty alcohol ethoxylates. Full

resolution was achieved. 6 refs.


Accession no.720827



Washington, D.C., 1997, p.20-1 012

MOLECULAR CHARACTERIZATION OFCOMPLEX POLYMERS BY COUPLED LIQUIDCHROMATOGRAPHIC PROCEDURESBerek D



Size exclusion chromatography alone cannot characterise

the constituents of complex polymer systems. Separation

selectivity and characterisation of complex systems may

be enhanced with liquid chromatographic (LC) methods

utilising combinations of different separation

mechanisms. These are termed coupled LC procedures.

The applications of a variety of coupled LC procedures

are discussed. 16 refs.


Accession no.720826

Item 244ACS Polymeric Materials Science & Engineering,

Spring Meeting 1998. Volume 78. Conference

proceedings.

Dallas, Tx., Spring 1998, p.102-3. 012

COUPLED PROGRAMMED PYROPROBE-MASSSPECTROMETRY ANDTHERMOGRAVIMETRIC-MASSSPECTROMETRYCarraher C E; Molloy H M; Louda J W; Baker E

Florida,Atlantic University; Florida,Center for

Environmental Studies; Midwest Research Institute


In 1977, a thermogravimetric analysis unit was

successfully coupled with a mass spectrophotometer, TG-

MS. More recently, a coupled programmed pyroprobe-

mass spectrophotometry system, also utilising IR

spectroscopy, was employed as a means of describing

degradation sequences as a function of temperature. The

application of these tools as a means to define polymer

structure and degradation products is described. 9 refs.

USA

Accession no.719193

Item 245ACS Polymeric Materials Science & Engineering,

Spring Meeting 1998. Volume 78. Conference

proceedings.

Dallas, Tx., Spring 1998, p.219-20. 012

SECONDARY TRANSITIONS IN POLYMERSPROBED BY DIFFERENTIAL SCANNINGCALORIMETRYBertolucci P R H; Harmon J P

South Florida,University


The use of differential scanning calorimetry to identify

secondary transitions in thermoplastics is studied. The

temperature and breadth of the secondary transition are

related to the those of the alpha transition in a variety of

methacrylate, acrylate and styrene polymers, as well as

polycarbonate. The effect of thermal history and the

position and sharpness of these endothermic transitions

is discussed. Some comparisons are made between this

technique and results obtained via dielectric analysis and

dynamic mechanical analysis obtained in the laboratory.

7 refs.

USA

Accession no.718740


200, No.2, Feb.1999, p.413-21

THERMAL PROPERTIES ANDCRYSTALLISATION BEHAVIOUR OFPOLYHYDROXYBUTYRIC ACID IN BLENDSWITH CHITIN AND CHITOSANIkejima T; Yagi K; Inoue Y

Tokyo,Institute of Technology

Films of blends of polyhydroxybutyric acid with chitin

and chitosan were prepared as completely biodegradable



polyester-polysaccharide composites. Crystallisation was

examined using DSC. Data are given from FTIR and

carbon 13 NMR. 31 refs.

JAPAN

Accession no.716972

Item 247Journal of Biomedical Materials Research (Applied

Biomaterials)

48, No.1, 1999, p.5-8

EXTRACTABLE FREE MONOMERS FROMSELF-CURED DENTAL SEALANTS RESULTINGFROM DISPENSING ERRORSVaubert V M; Moon P C; Love B J

Virginia,Polytechnic Institute

HPLC experiments were performed on a series of self-

curing polybisglycidyl methacrylate dental sealants that

were deliberately mismixed. The amount of extractable

sealant under conditions of nonideal processing was

measured. 13 refs.

USA

Accession no.716163

Item 248Macromolecular Rapid Communications

20, No.2, Feb. 1999, p.95-7

CURING OF MONOMER COMPOSITES. II. USEOF NMR TO MONITOR REAL TIME CURINGDYNAMICSMartin S J; McBrierty V J; Dowling J; Douglass D C

Dublin,Trinity College; Bausch & Lomb Inc.

Details are given of a method for monitoring the real-

time curing dynamics of composite monomers, exploiting

site specific information provided by high resolution

NMR. Data using polyvinylpyrrolidone, polyhydroxy-

ethyl methacrylate and polybutylhydroxycyclohexyl

methacrylate are compared with results from a computer

simulation based on a multicomponent kinetic model.

7 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;

WESTERN EUROPE

Accession no.716161


13, No.1, 1999, p.19-34

RHEO-PHOTOACOUSTIC (RPA) FTIRSPECTROSCOPIC STUDIES OF THEADHESION OF THERMOSETS TOPOLYOLEFINSPennington B D; Urban M W


Rheophotoacoustic FTIR analysis and previously

developed theory were utilised in an attempt to correlate

the molecular level interactions in polymer bilayer

systems under elongational interactions in polymer bilayer

systems under elongational deformations and changes in

potential energy, leading to determination of the work of

adhesion. This research expands the scope of previous

findings and provides a relationship between the C-H

stretching vibrational energy changes for acrylic/PE,

epoxy/PE, acrylic/PP, and epoxy/PP bilayer systems and

the interfacial forces responsible for adhesion. 39 refs.

USA

Accession no.715972


71, No.2, 15th Jan.1999, p.468-75

IDENTIFICATION AND DETERMINATION OFCROSSLINKERS IN CROSSLINKEDPOLYVINYLPYRROLIDONE(PVP) BYPYROLYSIS-GAS CHROMATOGRAPHY(GC)/MASS SPECTROMETRY(MS)Cheng T M H; Malawer E G

International Specialty Products

Pyrolysis-GC and pyrolysis-GC/MS were used to identify

and quantify specific nitrogen-containing crosslinker

compounds incorporated into the structures of crosslinked

PVP polymers which appeared to be identical by FTIR

spectroscopy. The pyrolyser regenerated and volatilised

specific crosslinkers which could be distinguished from

other pyrolysate compounds by either peak retention time

or mass spectral release. Individual compounds studied

included 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'-

ethylidenebis(1-vinyl-2-pyrrolidone) and N,N’-

divinylimidazolidone. In general, the level of specific

crosslinkers in various commercial products ranged from

1.8 to 2.5% w/w. The effect of pyrolysis temp. on this

level varied with the crosslinkers studied. The crosslinker

content obtained by this technique correlated with the

swell volume data for a specific series of crosslinked PVP

samples made with a single crosslinker and having similar

particle size distributions. The pyrolysis methodology

could not distinguish the level of crosslinker which was

incorporated as a pendant functionality from that portion

which was incorporated through both vinyl groups. 26

refs.

USA

Accession no.715578


17, No.8, Dec.1998, p.533-41

NMR STUDY OF COMMERCIALPOLYETHYLENE-CO-VINYL ACETATEde Souza C M G; Tavares M I B

Rio de Janeiro,Cidade Universitaria

Two EVA materials with distinct vinyl acetate ratios are

studied by nuclear magnetic resonance using solution and

solid techniques. These studies are made in order to obtain a



relation between the structure-properties-mobility and this

response can be utilised in order to have precise information

for new applications as well as better understanding of the

material behaviour. The results show that these polymers

present characteristic mobilities as a function of vinyl acetate

in the copolymer. Thus, as the quantity of vinyl acetate

increases the dyads and tryads distribution and the molecular

mobility in the copolymer change, as a consequence of the

different commercial applications. 13 refs.

BRAZIL

Accession no.714141


54, No.2, 1998, p.565-76

METHOD FOR ANALYSIS OF THE MEASUREDCURVES OF TEMPERATURE-MODULATEDDIFFERENTIAL SCANNINGCALORIMETRY(TMDSC) INVESTIGATION INTHE MELTING REGION OF POLYMERSSchawe J E K; Bergmann E; Winter W

Ulm,University; IFA GmbH

The measured signal of the TMDSC was examined for the

case of polymer melting. Fourier transform analysis was

used to evaluate the data, the resulting information being

the amplitude and the phase shift of the first harmonic of

the periodic heat flow component. It was shown that this

procedure was not sufficient for quantitative discussions if

deviations from the symmetric curve shape occurred in the

measured heat flow curves. For polymer melting, it was

shown that asymmetric curves would be measured if the

experimental temp. amplitude was too large. 15 refs.


WESTERN EUROPE

Accession no.713454


54, No.2, 1998, p.477-99

APPLICABILITY OF TEMPERATURE-MODULATED DIFFERENTIAL SCANNINGCALORIMETRY(TMDSC) TO POLYMERICSYSTEMS. GENERAL THEORETICALDESCRIPTION BASED ON THE FULL HEATCAPACITY FORMULATIONScherrenberg R; Mathot V; Steeman P

DSM Research

An overview is presented of the different aspects of

TMDSC, using a general theoretical description based

on the full heat capacity formulation. It is demonstrated

that processes studied with the aid of TMDSC can be

simply classified into three distinct regimes, depending

on the time scale and the susceptibility of the process to

the temp. modulation. 47 refs.



Accession no.713453

Item 254Muanyag es Gumi

34, No.12, 1997, p.A12-4

Hungarian

ASSESSMENT OF THE THERMAL HISTORY OFEXTRUDED UPVCMarossy K

BorsodChem Rt.

The paper deals with the investigation by differential

scanning calorimetry of extruded rigid PVC formulations.

The DSC traces of processed UPVC depend on the

thermal history of the melt. The DSC tests can be used to

estimate extrusion conditions e.g. of failed products. 16

refs. Articles from this journal can be requested for

translation by subscribers to the Rapra produced

International Polymer Science and Technology.


Accession no.713264

Item 255Surface Coatings International

82, No.1, Jan.1999, p.26-30

USE OF ELECTROCHEMICAL IMPEDANCESPECTROSCOPY FOR THE DETERMINATIONOF THE PROTECTIVE PROPERTIES OFSOLVENT- AND WATER-BASED PAINTSYSTEMSAl-Hashem A; Carew J A; Hasan A

Kuwait,Institute for Scientific Research

In this work, electrochemical impedance spectroscopy

was used to evaluate the corrosion protection properties

of the solvent-based coatings and water-based coating

systems currently being proposed for use in the industrial

installations in the Arabian Gulf region. Evaluation of

corrosion damage levels for three coating systems after

90 day immersion in 0.5M NaCl was performed using

the EIS and visual observations. 22 refs.

KUWAIT

Accession no.713236

Item 256Journal of Materials Science

33, No.19, 1st Oct.1998, p.4721-5

RAMAN SPECTRA OF HIGH MODULUSPOLYETHYLENE FIBRES BY RAMANMICROSCOPYLu S; Russell A E; Hendra P J

Southampton,University

Raman microscopy was used to analyse a series of high

modulus PE fibres, relating the Raman scattering

anisotropy to the mechanical performance of the

filaments. Measurements of the band intensity ratio of

the fibres were made and related to their Young’s modulus.

This relationship is useful in morphological studies of

PE fibres. 10 refs.




WESTERN EUROPE

Accession no.711133


52, No.12, Dec.1998, p.1498-504

MEASUREMENT OF ORIENTATION ANDCRYSTALLINITY IN UNIAXIALLY DRAWNPOLY(ETHYLENE TEREPHTHALATE) USINGPOLARISED CONFOCAL RAMANMICROSCOPYEverall N J

ICI Wilton Research Centre

Polarised confocal Raman microscopy was used to

measure molecular orientation in uniaxially drawn PETP

films, prepared with draw ratios from 1 to 3.5. The

orientation of both polarised Raman microscopy and

polarised attenuated total reflection IR spectroscopy.

Crystallinity profiles were measured through the thickness

of the film samples and compared with the orientation

gradients existing in the films. This procedure was to

determine whether the intuitive assumption that

orientation and crystallinity would be positively correlated

actually holds true on the microscopic scale for these

samples. 18 refs.


WESTERN EUROPE

Accession no.711041

Item 258Plasticheskie Massy (USSR)

No.3, 1997, p.30-3

Russian

BREAKDOWN OF AMMONIUM SALTS WITHREFERENCE TO THEIR INTRODUCTION INTOWOOD-BASED COMPOSITESVigdorovich A I; Efremov V N

The possibility was studied of using ammonium salts as

plasticisers for wood-based composites, and the

breakdown of the ammonium salts during heating was

studied by differential thermal gravimetry. 15 refs. Articles

from this journal can be requested for translation by

subscribers to the Rapra produced International Polymer

Science and Technology.

RUSSIA

Accession no.710456


38, No.11, Nov.1998, p.1873-81

PHYSICAL AND RELAXATION PROPERTIESOF FLAME-SPRAYED ETHYLENE-METHACRYLIC ACID COPOLYMERBrogan J A; Berndt C C; Simon G P; Hewitt D

Stony Brook,University; Monash,University

Details are given of the range of physical and chemical

properties of flame-sprayed ethylene-methacrylic acid

copolymer following different processing conditions.

Coatings were produced at a range of specific

temperatures by varying the propane flow rate and gun

traverse rate. Coatings were scanned using dielectric

relaxation spectroscopy. 24 refs.

AUSTRALIA; USA

Accession no.709520


30, No.10, 1998, p.771-4

CRYSTALLITE SIZES AND LATTICEDISTORTIONS OF GEL-SPUN ULTRA-HIGHMOLECULAR WEIGHT POLYETHYLENEFIBRESXiao-Ping Hu; You-Lo Hsieh

California,University

A detailed method is reported for deriving the lattice

distortions and crystallite sizes of UHMWPE fibres using

a full wide angle X-ray diffraction patterns. The

instrumental broadening and the background scattering

is represented by a binomial. A discussion is included

about the diffraction trace, peak assignments, and unit

cell dimensions. 26 refs.

USA

Accession no.709342

Item 261Chinese Journal of Polymer Science

16, No.4, 1998, p.332-8

DETECTION OF TG BY MODULATEDDIFFERENTIAL SCANNING CALORIMETRYRui Song; Jing Chen; Jingui Gao; Xin Lin; Qingrong Fan


The glass transition of PETP samples which were

subjected to solvent induced crystallisation (SINC) was

investigated by modulated differential scanning

calorimetry (MDSC) and density measurements. The

differential heat capacity signal from MDSC was used to

monitor the SINC process. 16 refs.

CHINA

Accession no.709335


71, No.1, 3rd Jan.1999, p.1-6

MICROWAVE PLASMA REACTIONS OFIMIDAZOLE ON POLY(VINYL CHLORIDE)SURFACES: A SPECTROSCOPIC STUDYSchmitt B R; Heung Kim; Urban M W


A closed-system microwave plasma reactor was used to react

imidazole molecules to PVC surfaces. Newly created



surfaces were analysed using ATR FTIR spectroscopy.

Surface reactions on PVC were heavily dependent on a prior

thermal history of the PVC substrate. A mechanism for the

PVC-imidazole reactions was also presented. The PVC was

useful as an implant for biomedical applications. 10 refs.

USA

Accession no.709309


52, No.11, Nov.1998, p.1483-7

SAMPLING CONSIDERATIONS FOR FT-RAMAN SPECTROSCOPY OF POLYMERS ANDSOLUTIONSBarrerra B A; Sommer A J

Miami,University

Details are given of the determination of apparent

absorption coefficients and optimal sample thickness of

PE, PETP, cellulose, and cyclohexane by FT-Raman

analysis. A relationship was developed that permits the

optimal sample thickness for FT-Raman measurements

to be determined by measuring the absorbance spectrum

of a sample whose thickness is known. Results are

discussed in the context of scattering theory, sampling

considerations, and spectral artifacts. 9 refs.

USA

Accession no.709038


71, No.3, 18th Jan.1998, p.371-5

PROPYLENE OLIGOMERS: EXTRACTIONMETHODS AND CHARACTERISATION BYFTIR, HPLC, AND SECEl Mansouri H; Yagoubi N; Scholler D; Feigenbaum A;

Ferrier D

INRA

Details are given of the isolation of propylene oligomers

from polymer matrix by dissolution precipitation and

Soxhlet methods. Characterisation was undertaken by

FTIR, UV spectroscopy, HPLC, and GPC. Data were used

to explain their behaviour toward packaged food products

in PP packaging. 18 refs.


WESTERN EUROPE

Accession no.708984

Item 265European Polymer Journal

34, No.12, Dec.1998, p.1817-28

CURING OF POLYMER COMPOSITES. I. NMRCHARACTERIZATION OF COMPONENTMONOMERSMartin S J; O’Brien J E; Dowling J; McBrierty V J

Dublin,Trinity College; Bausch & Lomb Inc.

The use of NMR to probe the in-situ curing of monomer

mixtures commonly encountered in the manufacture of

contact lenses was studied. Spectral lines were identified

which monitored curing with time of individual

components in the monomer mix. This information can

aid in gaining an understanding of the overall curing

dynamics and provide important guidance in establishing

suitable protocols in the manufacturing process. As a

precursor to this goal, several commonly-used component

materials were characterised by high resolution proton

and carbon-13 NMR spectroscopies. The efficacy of the

overall procedure is demonstrated. 20 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;

WESTERN EUROPE

Accession no.706520


8, No.1, Jan./March 1998, p.46-53

Portuguese

THERMAL STABILITY OF POLYETHYLENETEREPHTHALATE PACKAGING:DETERMINATION OF OLIGOMERSFreire M T de A; Reyes F G R; Castle L

Campinas,Universidade Estadual; UK,Min.of

Agriculture,Fisheries & Food

PETP food packaging materials were subjected to

different heating conditions (50 minutes at 120-230C),

and oligomers were identified by HPLC coupled with

mass spectrometry and used as a parameter for evaluating

the thermal stability of PETP. Small changes in oligomer

distribution were observed only for samples heated at

230C, suggesting that PETP was thermally stable under

the heating conditions employed. The results also

suggested the suitability of PETP as a food packaging

material for use in conventional and microwave ovens,

and for secondary recycling under controlled conditions.

28 refs.

BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;

WESTERN EUROPE

Accession no.706082


52, No.2, 1998, p.261-74

THERMAL ANALYSIS OF SOMEENVIRONMENTALLY DEGRADABLEPOLYMERSDay M; Cooney J D; Shaw K; Watts J

Canada,National Research Council

The thermal characteristics of a series of degradable

polymers for use in commercial composting facilities was

investigated using TGA and DSC. Phase changes

associated with some of the polymers investigated may

cause problems in the interpretation of data from

composting degradation studies. Several biodegradable



polymers were observed to have melt transitions at

temperatures similar to those found in a composting

environment. 19 refs.

CANADA

Accession no.705674


70, No.12, 19th Dec.1998, p.2457-61

NUCLEAR MAGNETIC RESONANCE STUDYOF COMMERCIAL POLY(VINYL ACETATE)De Souza C M G; Tavares M I B

Rio de Janeiro,Universidade Federal

The commercial poly(vinyl acetate) bulk was studied by

NMR at solution and solid state to understand the

behaviour of this polymer to obtain information on

structure, sample molecular mobility, and heterogeneity.

To analyse the behaviour of this polymer, NMR

techniques were chosen, such as carbon-13 solution,

magic angle spinning, cross-polarisation/magic angle

spinning, proton spin-relaxation time in the rotating frame

parameter and dipolar dephasing experiment. 13 refs.

BRAZIL

Accession no.705529


52, No.1, 1998, p.145-55

German

THERMOANALYTICAL CHARACTERISINGUV-CURED POLYMER FILMSHosselbarth B; Friese K; Geyer W

Institut fuer Oberflaechenmodifizierung eV; Leipzig-

Halle Ltd.; Umweltforschungzentrum

Thermooxidative and thermomechanical stabilities of

radiation-cured acrylates and epoxides were examined by

TGA, DMA and DSC. The polymeric trifunctional

acrylates PETIA, TMPTA and THEIC displayed the

highest temperatures of onset of degradation. The high

crosslinking density of the films resulted in an almost

temperature-independent complex E-modulus, as

measured by DMA. With increasing degree of

ethoxylation or propoxylation of the monomers, decreases

in thermal stability and strength were found. For

difunctional polymeric acrylates and epoxides, the TG

temperature was measured. The average degree of curing

of UV-cured epoxy films could be determined from the

temperature of the maximum in the loss modulus. 13 refs.


WESTERN EUROPE

Accession no.705282


52, No.1, 1998, p.131-43

German

DETERMINATION OF VINYL ACETATECONTENT IN EVA COPOLYMERS. FACILITIESAND LIMITS OF APPLICATIONS OF MASSSPECTROMETRY ANALYSIS METHODSHaussler L; Pompe G; Albrecht V; Voigt D

Dresden,Institut fuer Polymerforschung

Ethylene-vinyl acetate copolymers were investigated by

simultaneous thermal analysis and pyrolysis gas

chromatography. Both devices were coupled to a mass

spectrometer. Calibration with polyvinyl acetate led to

sufficient accuracy in relation to the vinyl acetate content,

because of the linear calibration plot. Quantitative

determination of vinyl acetate was carried out at both 500

and 700 C. The calibration plot was linear provided that

the mass of vinyl acetate did not exceed a critical value.

18 refs.


WESTERN EUROPE

Accession no.705281

Item 271Composites Science & Technology

58, No.10, 1998, p.1641-7

CHEMICAL ANALYSIS OF A FIELD-FAILEDCOMPOSITE SUSPENSION INSULATORChughtai A R; Smith D M; Kumosa M S

Denver,University

The type of corrosive environment responsible for brittlefracture of suspension composite insulators was

established. A series of FTIR experiments was performed

to identify chemical functionalities formed during the

degradation process of composite insulators affected by

brittle fracture. It was shown that the brittle fracture

process was caused by the formation of nitric acid either

outside or inside an insulator leading to stress corrosion

cracking of the glass/polymer composite rod material.

Nitrate was detected on the composite fracture surfaces

inside a 115 kV suspension composite insulator which

failed in service by brittle fracture. 17 refs.

USA

Accession no.705241

Item 272International Journal of Adhesion & Adhesives

18, No.5, 1998, p.319-31

LOW RESOLUTION PULSED NMR ANDULTRASOUND STUDY TO MONITOR THECURE OF AN EPOXY RESIN ADHESIVECocker R P; Chadwick D L; Dare D J; Challis R E

Keele,University; Manchester,Metropolitan University

The cure of an epichlorohydrin-bisphenol A resin and

curing agent containing a primary diamine and an amido-

polyamine was studied using two complementary

techniques, low resolution pulsed NMR spectroscopy and

measurement of pulsed broad bandwidth ultrasound

propagation velocity and absorption changes. The two



techniques independently gave a similar picture of the

cure process, predicting cure events at the same times.

The results obtained indicated that the cure followed

distinct phases, i.e. an initial liquid stage where short

polymer chains were formed, followed by a second stage

where longer molecules developed, a third stage where

crosslinking between chains occurred and the adhesive

began to solidify, and a final stage when solidification

was completed. 19 refs.


WESTERN EUROPE

Accession no.704884


62, No. 1, Oct. 1998, p.41-8

MECHANISMS OF THERMAL DEGRADATIONOF A POLYESTER FLAME-RETARDED WITHANTIMONY OXIDE/BROMINATEDPOLYCARBONATE STUDIED BYTEMPERATURE-PROGRAMMED ANALYTICALPYROLYSISSato H; Kondo K; Tsuge S; Ohtani H; Sato N

Nagoya,University; Toray Research Center Inc.

Thermal degradation of a flame-retarded PBTP consisting

of PBTP and a synergistic flame-retardant system based

on brominated polycarbonate (copolycarbonate

containing units from bisphenol A and tetrabrominated

bisphenol A plus tribromophenoxy end groups) and

antimony trioxide was studied by means of various

temperature-programmed analytical pyrolysis techniques

such as temperature-programmed pyrolysis-mass

spectrometry, temperature-programmed pyrolysis-atomic

emission detection and temperature-programmed

pyrolysis-gas chromatography. During the degradation of

the flame-retarded PBTP, brominated phenols were first

observed to evolve at temperatures slightly lower than

those for the flammable product evolution from the

substrate polymer PBTP, followed by the evolution of

hydrogen bromide over the whole range of degradation

temperatures for the substrate polymer. These degradation

processes were closely related to the synergistic effects

of antimony trioxide on the decomposition of brominated

polycarbonate in the flame-retardant system to promote

the thermal degradation of brominated polycarbonate at

lower temperatures than those for pure brominated

polycarbonate. Furthermore, the evolution of the flame

poisoning antimony tribromide formed through the

reaction between brominated polycarbonate and antimony

trioxide could also be monitored directly by temperature-

programmed pyrolysis techniques. On the basis of the

data obtained by these temperature-programmed pyrolysis

techniques, the thermal degradation of the flame-retarded

PBTP and synergistic flame-retarding mechanisms are

discussed. 10 refs.

JAPAN

Accession no.704607


74, No.495, Sept.1997, p.255-61

Spanish

FTIR SPECTROPHOTOMETRY FOR THEDETECTION OF MICROSTRUCTURALCHANGES IN A POLYPROPYLENE/POLYETHYLENE COPOLYMER CAUSED BYARTIFICIAL AGEINGRomeu J; Pages P; Carrasco F

Cataluna,Universidad Politecnica; Girona,Universidad

A study was made of microstructural changes occurring

in blue and red samples of an ethylene-propylene

copolymer exposed to artificial ageing in a Xenotest

chamber for up to 5000 hours. The effects of ageing

were quantified by Fourier transform IR

spectrophotometry. By calculating the reduced

absorption in selected spectral bands, it was possible

to detect oxidation and chain scission reactions and

variations in isotacticity which differed in the

differently coloured specimens. 8 refs.


WESTERN EUROPE

Accession no.702522


70, No.7, 14th Nov.1998, p.1307-10

MULTIDIMENSIONAL SPECTROMETRY ANDMAPPINGFateley W G; Deverse R A; Hammaker R M

Kansas State University

A new inexpensive approach is described for mapping

molecular structure in polymeric materials which includes

the combination of interferometers and Hadamard

transform techniques to perform multidimensional

spectometry and mapping. 17 refs.

USA

Accession no.702159

Item 276Journal of Materials Science.Materials in Medicine

9, No.9, Sept.1998, p.529-33

INVESTIGATION OF GLASS-IONOMERCEMENTS USING DIFFERENTIAL SCANNINGCALORIMETRYKhalil S K H; Atkins E D T

Bristol,University

Six commercial glass-ionomer cements commonly used

for various dental applications were investigated using

DSC. Heat flow behaviour and heat capacity of the

cements were measured during isothermal (at 37 C) setting

reactions. All materials underwent an exothermic setting

process, but with different enthalpies of reactions and

different heat capacities; there were no remaining endo-

or exothermic reactions after the setting of the cement.



All materials examined were effective thermal insulators.

18 refs.


WESTERN EUROPE

Accession no.702142


33, No.14, 15th July 1998, p.3511-7

MOLECULAR ORGANISATION INSTRUCTURAL PVDFGlennon D; Cox P A; Nevell R T; Nevell T G; Smith J

R; Tsibouklis J; Ewen R J

Portsmouth,University; West of England,University

Poly(vinylidene fluoride) containing 10% dibutyl sebacate

plasticiser, as used in the construction of flexible oil and

gas pipelines, was exposed to raised temperatures for

prolonged periods of time, to acid etching and to various

tensile deformation regimes. The effects of these

treatments on crystallinity and surface properties of this

material were examined in the light of analytical data

obtained by FTIR, DSC, X-ray diffraction, X-ray

photoelectron spectroscopy, goniometry and a variety of

microscopy techniques. 36 refs.


WESTERN EUROPE

Accession no.701984

Item 278Food Additives and Contaminants

15, No.3, 1st April 1998, p.346-54

PARTS-PER-TRILLION DETERMINATION OFSTYRENE IN YOGHURT BY PURGE-AND-TRAPGAS CHROMATOGRAPHY WITH MASSSPECTROMETRY DETECTIONNerin C; Rubio C; Cacho J; Salafranca J

Zaragoza,University

Headspace sampling methods prior to capillary gas

chromatography are widely used for the determination

of volatile compounds present in very different types of

samples. An automated and rapid system for

determination of volatiles from yoghurt was developed.

Thirty-five volatile organic compounds(VOCs) were

identified in PS cups used for yoghurt packaging and 42

VOCs from yoghurt samples. Quantitative analysis of

styrene in several samples from the Spanish retail market

was carried out. 16 refs.


WESTERN EUROPE

Accession no.700270


70, No.6, 7th Nov.1998, p.1201-7

PHOTODEGRADATION OF TEFLON AF1600DURING XPS ANALYSIS

Popovici D; Sacher E; Meunier M

Montreal,Ecole Polytechnique

Teflon, type AF1600, which contains perfluorinated

dioxole rings, was found to suffer significant degradation

when exposed to X-rays whilst undergoing investigation

by X-ray photoelectron spectroscopy. The degradation

mechanism was significantly different to that of

fluoropolymers which contain only carbon and fluorine.

It was established that oxygen was at least as twice as

susceptible as fluorine, and that the amounts of oxygen

loss were equal to those of fluorine. Oxygen could be

degraded by the breaking of only one bond, the oxygen

then forming a free radical. The free radicals produced

by scission of carbon-carbon bonds participated in

reactions leading to degradation and crosslinking. 9 refs.

CANADA

Accession no.700200


47, No.1, Sept.1998, p.72-5

TEMPERATURE-MODULATED DIFFERENTIALSCANNING CALORIMETRY. II.DETERMINATION OF ACTIVATION ENERGIESZhong Jiang; Hutchinson J M; Imrie C T

Aberdeen,University

Alternating differential scanning calorimetry (ADSC), acommercial development of temperature-modulated

differential scanning calorimetry, was used to determine the

activation energy associated with the relaxation processes

in polycarbonate in the region of the glass transition. In this

procedure the frequency of the temperature modulation is

varied over a range of approximately one decade, and the

mid-point of the step change in the complex heat capacity is

evaluated. In these experiments, two different amplitudes

of temperature modulation were employed. The results were

in agreement with each other, and in good agreement with

published values. Ripples seen on the Fourier-transformed

signals are attributed to the mode of the data analysis, and

not to noise on the data. 7 refs.


WESTERN EUROPE

Accession no.700165

Item 281Materials World

6, No.10, Oct.1998, p.617-9

THROWING LIGHT ON FIBRES ANDCOMPOSITESYoung B

Manchester,University

The use is discussed of Raman spectroscopy to monitor

the stresses and strains on individual fibres in composite

materials. New instrumentation has caused rapid growth

in the use of Raman spectroscopy for materials

characterisation, including the introduction of charged-



coupled device cameras which offer significant

improvements in sensitivity and very low noise, and also

holographic notch filters which are used to remove the laser

line and allow single monochromators to be used. Both

these developments are incorporated in the Raman imaging

microscope developed by Renishaw in collaboration with

Leeds University Physics Department. Its use is described

with reference to aramid fibre reinforced PP. 5 refs.

RENISHAW PLCEUROPEAN COMMUNITY; EUROPEAN UNION; UK;

WESTERN EUROPE

Accession no.699334

Item 282Farbe und Lack

104, No.10, 1998, p.93/8

German

MODULATED DIFFERENTIAL SCANNINGCALORIMETRYHaessler R

Dresden,Institut fuer Polymerforschung

The use of modulated DSC for improved interpretation

of product characteristics under thermal effects was

investigated. Tgs, for example, which are masked by post-

curing or enthalpy relaxation, could be detected in a single

measurement and compared. The separation of complex

transitions in multicomponent systems into individual

parts such as melts, transition temps. and relaxations was

shown to be feasible. The potential for use of modulated

DSC in the field of epoxy resins was demonstrated using

examples of the determination of Tg near the regions of

enthalpy relaxation, melt and post-curing. 7 refs.


WESTERN EUROPE

Accession no.699054

Item 283Structure and properties of Oriented Polymers. Second

Edition.

London, Chapman & Hall, 1997, p.234-68. 9

NUCLEAR MAGNETIC RESONANCESpeiss H W

Max-Planck-Institut fuer Polymerforschung

Edited by: Ward I M

(Leeds,University)

The basics of solid state NMR are outlined and the site-

selective information available from multi-dimensional

NMR spectra about molecular order and dynamics in

oriented polymers is illustrated with specific experimental

examples. 55 refs.


WESTERN EUROPE

Accession no.697739

Item 284Structure and properties of Oriented Polymers. Second

Edition.

London, Chapman & Hall, 1997, p.181-233. 9

INFRARED DICHROISM, POLARISEDFLUORESCENCE AND RAMANSPECTROSCOPYBower D I

Leeds,University

Edited by: Ward I M

(Leeds,University)

The three spectroscopic techniques for studying

molecular orientation in polymers described in detail

use polarised electromagnetic radiation. The principles

of the techniques are outlined, relevant theory and

experimental details described, and a selection of results

presented. 79 refs.


WESTERN EUROPE

Accession no.697738

Item 285Polymer

39, No.20, 1998, p.4973-6

EFFECTS OF SUBSTRATE INTERACTIONS INTHE LIQUID CHROMATOGRAPHY OFPOLYMERSKosmas M K; Bokaris E P; Georgaka E G

Ioannina,University

The elution behaviour of PMMA samples was studied

through two liquid chromatographic columns, one

containing a substrate of silica covered with trimethylsilyl

groups and the other a substrate of pure silica. Both

substrates had the same pore size and the solvent was the

same for both columns. The results were discussed and

they showed that the polymer-surface interactions

changed when the nature of the substrate was changed.

14 refs.


WESTERN EUROPE

Accession no.696588


15, No.1, 1st Jan.1998, p.93-9

SYSTEMATIC STUDY ON THE STABILITY OFSELECTED POLYMER ANTIOXIDANTS IN EUOFFICIAL AQUEOUS AND ALTERNATIVEFOOD SIMULANTS USING HPLCDemertzis P G; Franz R

Fraunhofer Institute for Food Technol. & Packag.

Details are given of the stability of five commercial

antioxidants in food simulants and in an alternative fat

simulant. Analysis was performed using a rapid HPLC

method with UV detection. 23 refs.


WESTERN EUROPE

Accession no.695963



Item 287Colloid & Polymer Science

276, No.7, July 1998, p.565-9

DESCRIPTION OF THE GLASS TRANSITIONMEASURED BY TEMPERATURE MODULATEDDIFFERENTIAL SCANNING CALORIMETRYSchawe J E K

Ulm,University

The temp. modulated DSC (TMDSC) technique could be

used for heat capacity spectroscopy in the low frequency

range. The measured property was the complex heat

capacity. The frequency-dependent relaxation transition

measured by TMDSC occurred in the temp. range of the

thermal Tg. The non-equilibrium of the glassy state thus

influenced the TMDSC curves. Experimental evidence

was the dependence of the shape of the heat capacity curve

on the thermal history. A theoretical description of the

influence of the non-equilibrium state on the spectroscopic

curves, based on the Tool-Narayanaswamy-Moynihan

model, is presented. 23 refs.


WESTERN EUROPE

Accession no.695591

Item 288Composites Plastiques Renforces Fibres de Verre

Textile

No.21, May/June 1997, p.48-54

French

DURABILITY OF COMPOSITES: HOW TOACHIEVE RELIABLE ACCELERATED AGEINGSiampiringue N; Gaumet S; Lemaire J

Centre National d’Evaluation de Photoprotection

The use of accelerated ageing tests and

spectrophotometric techniques in studying the

photooxidative degradation of unsaturated polyester resins

and glass fibre-reinforced composites is examined.

Results of accelerated and natural ageing tests are

compared, and criteria to be taken into account in

achieving accelerated test results representative of reality

are discussed. 5 refs.


WESTERN EUROPE

Accession no.695308


7, No.3, July/Sept.1997, p.19-23

Portuguese

FAILURE ANALYSIS OF MATERIALS BYADVANCED MICROSCOPIC TECHNIQUESChinaglia C R; Correa C A

Sao Carlos,Universidade Federal

Failure analysis techniques allowing the determination

of the chemical composition of a sample and its correlation

with the observed fracture mode are examined. Topics

discussed include the use of SEM in studying fracture in

mineral filled thermoplastics, secondary electron imaging

in obtaining information on sample topography,

backscattered electron imaging in studying filler

dispersion in polymer matrices, and energy dispersive X-

ray spectroscopy in determining the chemical composition

of the fillers or contaminants responsible for fracture

initiation. 5 refs.

BRAZIL

Accession no.695299

Item 290Journal of Polymer Science : Polymer Physics Edition

36, No.12, 15th Sept.1998, p.2165-75

DESCRIPTION OF THERMAL RELAXATION OFPOLYSTYRENE CLOSE TO THE THERMALGLASS TRANSITIONSchawe J E K

Ulm,University

Using spectroscopic methods at relatively high frequency,

the alpha-relaxation was measured in the thermodynamic

equilibrium. In the caloric case this phenomenon is called

thermal relaxation transition. Using a conventional

differential scanning calorimeter, the transition of the

equilibrium (the melt) into a nonequilibrium (the glassy

state) was measured. This effect is called thermal glass

transition. Temperature-modulated DSC curves in the

glass transition region were described using the Tool-

Narayanaswamy-Moynihan model. 54 refs.


WESTERN EUROPE

Accession no.694872


36, No.12, 15th Sept.1998, p.2103-9

RAPID DETERMINATION OF COMONOMERCONTENT, CRYSTALLINITY, AND LONGSPACING BY MULTIPLE-PULSE PROTON NMRIN ETHYLENE-VINYL ALCOHOLCOPOLYMERSPerez E; Cerrada M L; Vanderhart D L

Instituto de Ciencia y Tecnologia de Polimeros;

US,National Institute of Standards & Technology

Capitalising on the superior sensitivity of proton NMR,

relatively rapid estimates of three parameters, namely,

comonomer content, crystallinity, and long spacing, were

determined for three ethylene-vinyl alcohol copolymers

using solid state proton NMR measurements. Multiple-pulse

techniques were utilised (a) in conjunction with magic angle

spinning for measuring comonomer content, (b) in

conjunction with a relaxation time measurement for

determining crystallinity, and (c) in conjunction with a

relaxation time-based spin diffusion measurement for

determining the long spacing. These three parameters,

extracted from data collected in a total spectrometer time of



about 20 min., and were compared with similar parameters

obtained using more conventional DSC, small angle X-ray

scattering (including synchrotron), and solution-state NMR

measurements, with good agreement. 23 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA;

WESTERN EUROPE

Accession no.694867

Item 292Smart Materials & Structures

7, No.4, Aug. 1998, p.557-68

IN SITU CURE MONITORING USING OPTICALFIBRE SENSORS. A COMPARATIVE STUDYPowell G R; Crosby P A; Waters D N; France C M;

Spooncer R C; Fernando G F

Brunel University; Cranfield,University

A comparative study is presented for different types of

optical fibre sensor developed to monitor the cure of an

epoxy resin system. The sensors were based on

transmission spectroscopy, evanescent wave spectroscopy

and refractive index monitoring. 19 refs.


WESTERN EUROPE

Accession no.694840

Item 293Polymer Testing ’97. Day 3: Chemical Analysis.

Conference proceedings.

Shawbury, 7th-11th April 1997, Paper 4. 9T

RAMAN SPECTROSCOPY OF POLYMERSWilliams K P J; Wilcock I C

Renishaw plc

(Rapra Technology Ltd.; Plastics & Rubber Weekly;

European Plastics News)

Raman spectroscopy is now coming of age as a routine

analytical method. Advances in Raman technology have

meant that robust, user-friendly equipment can be

manufactured at a reasonable cost. These advances are

described, together with applications of Raman imaging

microscope systems to polymer analysis. 11 refs.


WESTERN EUROPE

Accession no.694712

Item 294International Polymer Processing

13, No.2, July 1998, p.142-8

PEROXIDE INDUCED CROSSLINKING ANDDEGRADATION OF POLYAMIDEYu Q; Zhu S

McMaster University

Peroxide-induced crosslinking and degradation of nylon

12 were investigated using ESR. Various reaction

mechanisms are proposed. 20 refs.

CANADA

Accession no.694268


199, No.8, 1998, p.1623-9

THERMAL STABILITY ANDCRYSTALLISATION KINETICS OF PEEKChen J-Y; Chen M; Chao S-C

Taiwan,National Sun Yat-Sen University

TGA, dynamic rheological analysis and polarised light

microscopy were used to assess thermal stability of PEEK.

Emphasis is given to the effect of melting temperature on

thermal stability. 23 refs.

CHINA

Accession no.694246


6, No.8, Aug. 1998, p.56/9

MATERIALS ANALYST: PART 13.PERFORMANCE PROBLEMS: WHEN THEPELLETS DON’T MATCH THE PARTSSepe M


The use of differential scanning calorimetry and

thermogravimetric analysis as analytical tools in part

failure determination is applied. Problems are examined

in part performance of moulded 30% glass-reinforced,

low-viscosity PEI and a second part moulded from PPS

with proprietary additives to improve wear resistance. The

importance of checking the composition of the basic

material is stressed.

USA

Accession no.693205


69, No.11, 12th Sept.1998, p.2175-85

IR SPECTROSCOPY AS A QUANTITATIVE ANDPREDICTIVE ANALYSIS METHOD OFPHENOL-FORMALDEHYDE RESOL RESINSHolopainen T; Alvila L; Rainio J; Pakkanen T T

Joensuu,University; Dynoresin Oy

A set of resin samples was characterised by IR and carbon-

13 NMR spectroscopy. The suitability of IR spectroscopy

for the quantitative analysis of resins was evaluated by

statistical methods using the NMR reference data as

calibration. The values of interesting properties, e.g. the

amount of free phenol and the formaldehyde-to-phenol

molar ratio, of the resins being similar to the calibration

resins were predicted from the IR spectra. The predicted

results were compared with those observed by carbon-13

NMR spectroscopy. 15 refs.

FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.692990


33, No.13, 1st July 1998, p.3245-9



XPS MONITORING OF THE REMOVAL OF ANAGED POLYMER COATING FROM A METALSUBSTRATE BY TEA-CARBON DIOXIDELASER ABLATIONCottam C A; Emmony D C; Cuesta A; Bradley R H

Loughborough,University; Aberdeen,Robert Gordon

University

X-ray photoelectron spectrometry was used to observe

the changes in surface chemistry during the removal of

paint from a zinc coated steel substrate using TEA-carbon

dioxide laser ablation. Laser ablation at both plasma and

sub-plasma fluences were investigated and their relative

merits discussed. The laser was shown to be effective in

paint removal and was not impaired by ageing in the paint.

32 refs.


WESTERN EUROPE

Accession no.692055


70, No.15, 1st Aug.1998, p.3298-303

IMPROVEMENTS IN POLYMERCHARACTERIZATION BY SIZE-EXCLUSIONCHROMATOGRAPHY AND LIQUIDCHROMATOGRAPHY AT THE CRITICALCONDITION BY USING ENHANCED-FLUIDITYLIQUID MOBILE PHASES WITH PACKEDCAPILLARY COLUMNSHao Yun; Olesik S V; Marti E H

Ohio,State University; Ashland Chemical Co.

The use of the above combination of techniques is

described and results obtained for samples of PS, PMMA,

styrene-methyl acrylate copolymers and functionalised

PS are presented and discussed. 32 refs.

USA

Accession no.691471

Item 300Polymer

39, No.22, 1998, p.5293-300

QUANTITATIVE CARBON-13 SOLID-STATENMR AND FT-RAMAN SPECTROSCOPY INNOVOLAC RESINSOttenbourgs B; Adriaensens P; Carleer R; Vanderzande

D; Gelan J

Limburg,University

A qualitative and quantitative study of the curing behaviour

of a high-ortho novolac resin with paraformaldehyde under

different conditions was conducted. The degree of cure as

a function of the formaldehyde/phenol ratio, the degree of

conversion and the final structure after curing were

determined on the basis of a quantitative carbon-13 solid

state NMR with cross-polarisation and magic angle

spinning. The spin-lattice relaxation time was measured

as a probe to follow the evolution of cure. Fourier

transform-Raman spectroscopy was proposed as a

qualitative tool to follow the degree of crosslinking in this

high-ortho novolac. 54 refs.


WESTERN EUROPE

Accession no.689414

Item 301Antec ’98. Volume II. Conference proceedings.

Atlanta, Ga., 26th-30th April 1998, p.1415-7. 012

IN SITU SPECTROSCOPY OF CO2-INDUCEDPLASTICISATION OF GLASSY POLYMERSKazarian S G; Brantley N H; Eckert C A

Georgia,Institute of Technology

(SPE)

In situ spectroscopy is used to study the plasticisation of

glassy polymers by high-pressure and supercritical CO2.

The methodology for in situ spectroscopic analysis of the

interactions between CO2 and polymers is described. The

changes in IR spectra of CO2 incorporated into various

polymers indicate a specific interaction between CO2 and

polymer functional groups. Increased polymer segmental

mobility is also observed, indicative of the plasticisation

phenomenon. Implications of these discovered molecular

interactions are discussed. 25 refs.

USA

Accession no.687565



QUANTITATIVE ANALYSIS OF CHEMICALBLOWING AGENTS BY DSCPrasad A; Shanker M

Millennium Petrochemicals Inc.

(SPE)

It is shown that differential scanning calorimetery (DSC)

can be used to determine quantitatively the level and

composition of chemical blowing agents such as

azodicarbonamide (azo) in commercial formulations.

DSC can also be used to obtain the onset of decomposition

temperature and the rate of decomposition of azo in the

presence of group II and group IV metal salt activators.

DSC has the potential to detect the level of undecomposed

blowing agents present in processed foam products and

to qualitatively determine the degree of dispersion of the

blowing agent and the activators in commercial

formulations. Advantages of DSC over the currently used

EGA technique are ease of operation, shorter analysis time

and detection of azo concentrations as low as 1%. 12 refs.

USA

Accession no.687551





APPLICATION OF GC/MS INTHERMOPLASTICS PROBLEM SOLVINGShaker D C; Kim H C

LNP Engineering Plastics

(SPE)

The use of GC/MS (gas chromatography/mass spectrometry)

in the thermoplastics problem solving area is outlined. GC/

MS is a hyphenated technique; i.e. it combines the two

techniques, chromatography and spectroscopy. In this

procedure, a material is introduced into the GC, components

are separated and sent to the MS where they are ionised, and

the resulting particles are separated by mass. The applications

of GC/MS to solving complex problems are discussed

through positive identification of base resins, contamination,

odours and solvents.

USA

Accession no.687499



TEMPERATURE GRADIENT INTERACTIONCHROMATOGRAPHY OF POLYMERSChang T; Lee W; Lee H C; Mays J W; Harville S;

Frater D J

Pohang,University of Science & Technology;

Alabama,University at Birmingham

(SPE)

Temperature gradient interaction chromatography (TGIC)

is a conventional reversed phase BPLC technique, but the

column temperature is varied during elution. A very fine

and reproducible control of interaction between polymer

chains and the stationary phase can be achieved by changing

the column temperature. Under a suitable temperature

programming, this method provides a far superior resolution

to conventional size exclusion chromatography. In addition,

elution in TGIC is more sensitive to molecular weight alone.

Thus it provides an excellent route to separating branched

polymer molecules of similar hydrodynamic volume but

differing molecular weight. 8 refs.

KOREA; USA

Accession no.687496



MODULATED DIFFERENTIAL SCANNINGCALORIMETRY TO STUDY REACTINGPOLYMER SYSTEMSVan Mele B; Van Assche G; Van Hemelrijck A

Brussels,Free University

(SPE)

Modulated (temperature) differential scanning calorimetry

(MTDSC or MDSC) is used to simultaneously study the

evolution of heat flow and heat capacity for the isothermal

and non-isothermal reactions of polymer systems. An

epoxy-anhydride thermosetting system is used as an

example. Vitrification and devitrification steps are

observed. The heat flow phase during isothermal and

nonisothermal cure is always small, but its evolution

contains information on relaxation phenomena, vitrification

and devitrification, in the course of the chemical reaction.

Modelling of the (heat flow related) chemical kinetics and

the (heat capacity related) mobility restrictions contributes

to a better understanding of the reaction mechanism and

reaction kinetics up to a high degree of chemical

conversion. The use of MTDSC as a tool for a quantitative

construction of the vitrification curve in Temperature-Time-

Transformation and Continuous-Heating-Transformation

diagrams is illustrated. 20 refs.


WESTERN EUROPE

Accession no.687483



PRACTICAL ANALYSIS TECHNIQUES OFPOLYMER FILLERS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY(FTIR)Coles B J; Hall C J

Hauser Inc.

(SPE)

The identification of polymers by FTIR is often

complicated by the presence of fillers. However for kaolin

clay, an FTIR analysis should be able to identify the filler

and predict its concentration using a standard curve. The

resulting percentage is more reliable than a simple ash,

which may change the chemical composition of the filler.

2 refs.

USA

Accession no.687418


38, No.6, June 1998, p.922-5

IDENTIFICATION OF OFF-FLAVOURCOMPOUNDS IN HDPE WITH DIFFERENTAMOUNTS OF ABSCENTSVillberg K; Veijanen A; Gustafsson I

Jyvaskyla,University; Borealis AB

Details are given of the addition of zeolite to HDPE

drinking water pipes in an attempt to eliminate odours

and to remove odour-causing compounds. The system

used for analysis of volatile organic compounds was a

gas chromatographic/mass spectrometric sniffing system.

Purge and trap techniques were used to introduce the

volatile, off-flavour components into the gas

chromatograph. 16 refs.

FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.686400



Item 308Polymer

39, No.19, 1998, p.4665-73

SURFACE GLASS TRANSITION BEHAVIOUROF AMORPHOUS POLYMER FILM BYSCANNING FORCE MICROSCOPY ANDSURFACE SPECTROSCOPYKakiyama T; Tanaka K; Takahara A

Kyushu,University

The surface molecular motion of amorphous polymeric

solids was measured by lateral force microscopy, scanning

viscoelasticity microscopy, and differential X-ray

photoelectron spectroscopy. Data are given for PS and

styrene-methyl methacrylate copolymers. 35 refs.

JAPAN

Accession no.686392


73, No.487, Jan.1997, p.26-31

Spanish

TEMPERATURE MODULATED DIFFERENTIALSCANNING CALORIMETRY: A STEP FORWARDIN STUDYING THE THERMAL PROPERTIESOF POLYMERSPerena J M

Instituto de Ciencia y Tecnologia de Polimeros

The principles of temperature modulated DSC are

described, and a number of examples are presented of its

application to studies of the thermal properties of plastics.

Some limitations of the technique are also examined. 6

refs.


WESTERN EUROPE

Accession no.686251


70, No.13, 1st July 1998, p.456A-61A

CHARACTERISING SYNTHETIC POLYMERSBY MALDI MSKuang Jen Wu; Odom R W

Evans C.,& Associates

An review is given of the use of matrix-assisted laser

desorption/ionisation time-of flight (MALDI TOF) mass

spectroscopy to determine MWDs and structures of

synthetic organic polymers, including the ion desorption

mechanism, synthetic polymer analysis, molecular weight

analysis, and its use in calibration of GPC profiles. 30

refs.

USA

Accession no.686157


15, No.2, 1998, p.217-28

EFFECTS OF PACKAGING AND STORAGECONDITIONS ON VOLATILE COMPOUNDS INGAS-PACKED POULTRY MEATEilamo M; Kinnunen A; Latva-Kala K; Ahvenainen R

VTT Biotechnology & Food Research;

Finland,Technical Research Centre

Volatile compounds released by raw chicken legs packed

in modified atmosphere packages were determined to

develop a spoilage indicator for monitoring the shelf life

of raw chicken. The effects of four packaging factors

(headspace volume, oxygen transmission rate of the

package, residual oxygen and carbon dioxide

concentration) and three storage factors (temperature,

illumination and storage time) on the amounts of volatile

compounds in the headspace of gas packages containing

two chicken legs were studied. Statistical experimental

design was applied and a linear screening design

comprising 18 experiments (fractional factorial) was

utilised. Volatile compounds in package headspace were

determined by gas chromatography/mass spectrometry.

The results were compared with the results of sensory

evaluation and microbial determinations. 8 refs.

FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.686119

Item 312International Journal of Adhesion & Adhesives

18, No.3, 1998, p.193-8

USE OF XPS AND TOF-SIMS TO INVESTIGATEADHESION FAILURE OF A CATIONICRADIATION CURED COATING ONGALVANISED STEELLeadley S R; Watts J F; Rodriguez A; Lowe C

Surrey,University; Becker Industrial Coatings

Details are given of coating delamination in a hot, humid

environment for a cationic radiation cured coating of

cycloaliphatic epoxy resin. X-ray photoelectron

spectroscopy and time-of-flight mass spectroscopy of the

delaminated surface showed that the phosphorus

hexafluoride anion of the photoinitiator segregates to the

interface. The durability of the coating was improved by

reformulation with a reduced concentration of

photoinitiator. 7 refs.


WESTERN EUROPE

Accession no.684932

Item 313Antec ’98. Volume I. Conference proceedings.


METHODS FOR THE MEASUREMENT OFCRYSTALLINITY OF PREFORMS ANDBOTTLES MADE FROM PETPBashir Z; Al-Alouish I; Al-Raqibah I; Ibrahim M

SABIC Corp.



(SPE)

PETP has established itself as a material for making

lightweight, clear and tough bottles. Ideally, a preform

with zero or very low crystallinity (for purposes of clarity)

is sought, while the final bottle should have high

crystallinity (for enhancing gas barrier and mechanical

properties). Monitoring crystallinity is thus important. An

attempt is made to evaluate methods of crystallinity

measurement using density, differential scanning

calorimetry and modulated differential scanning

calorimetry to study the crystallinity of preforms and

bottles. The applicability and appropriateness of each

technique for different PETP sample types, and

interpretation problems are also discussed. 20 refs.

SAUDI ARABIA

Accession no.684627


30, No.5, 1998, p.439-43

DIRECT DETERMINATION OF MOLECULARWEIGHT DISTRIBUTION BY SIZE EXCLUSIONCHROMATOGRAPHY(SEC) WITH 750 MHZPROTON NMR DETECTION (ON-LINE SEC-NMR)Ute K; Niimi R; Hongo S; Hatada K

Osaka,University

The above on-line SEC-NMR technique was used to

analyse MWDs of isotactic PMMAs with Mn ranging

from 3270 to 22,200. The molec.wt. of the polymer in

flowing eluate was determined directly (without a

conventional calibration procedure) from he relative

intensity of NMR signals due to the end group and

repeating units. The MWD determined in this manner was

proved to be accurate by SEC-NMR experiments on

uniform isotactic PMMAs consisting of exactly 23, 40

and 80 repeating units. Investigation was also undertaken

to optimise flow rate and NMR parameters for quantitative

SEC-NMR measurements. The signal-to-noise ratio of

750 MHz SEC-NMR spectra was 9.2 times that obtained

previously with 500 MHz SEC-NMR operated under

similar conditions. 17 refs.

JAPAN

Accession no.684613

Item 315Shawbury, Rapra Technology Ltd., 1996, pp.150.

95.00. 30cms. 9511

ENVIRONMENTAL STRESS CRACKING OFPLASTICSWright D C


This book reviews the factors which influence

environmental stress cracking, and examines the current

state of knowledge regarding specific categories of

plastics. The book is divided into three main sections

focusing on the prediction of ESC and assessment by

testing, factors that influence ESC and data on specific

plastics. Methods for the experimental evaluation of

environmental stress are described. This book is

available for purchase from Publication Sales, Rapra

Technology Ltd.

Accession no.683806


12, No.5, 1998, p.507-21

EFFECT OF CURING TEMPERATURE ON THEADHESION STRENGTH OF POLYAMIDEIMIDE/COPPER JOINTSCho J H; Kong D I; Park C E; Jin M Y

Pohang,University of Science & Technology;

Korea,Research Institute of Chemical Technology

The adhesion strength of polyamideimide/copper joints

was investigated as a function of the curing temperature

and time. The effects of copper oxide formed by thermal

treatment and alkaline treatment on the adhesive strength

of the joints were examined. The locus of failure of the

joints was also studied by SEM and X-ray photoelectron

spectroscopy. 21 refs.

KOREA

Accession no.682955


38, No.4, April 1998, p.566-72

DYNAMIC AND ISOTHERMALTHERMOGRAVIMETRIC ANALYSIS OF APOLYCYANURATE THERMOSETTING SYSTEMZacharia R E; Simon S L

Pittsburgh,University

Isothermal and dynamic thermogravimetric analysis

(TGA) were performed on a polycyanurate thermosetting

material. The effects on thermal stability of the copper

naphthenate catalyst were studied by comparing two

systems with different amounts of catalyst. Tests were

performed isothermally at temperatures ranging from 200-

240C for times up to one week. Dynamic tests were also

performed at rates of 0.1 C/min to 40 C/min at

temperatures ranging from 180 to 600C. Results

demonstrate the difficulties of extrapolating dynamic TGA

data to use conditions to predict long-term thermal

stability. 14 refs.

USA

Accession no.681689


34, No.2, Feb.1998, p.163-70

STUDY OF TALC-ADDITIVE INTERACTIONSBY COMBINED TGA-FTIR SYSTEMBertin D; Boutevin B; Rigal G; Fourty G



Montpellier,Ecole Nationale Superieure de Chimie;

Talcs de Luzenac SA

By using combined TGA/FTIR thermogravimetric

analysis, accurate real time qualitative and quantitative

data can be obtained for thermal decomposition of

polymers. It was used to study interactions between an

additive and a filler (talc), highlighting a degradation

phenomenon of additive by talc, and this phenomenon

depended on the structure and chemical composition of

talc. This procedure also applied to analysis of degradation

of other additives by talc. Thus, polymer formulations

will rapidly be optimised in various areas of filled

polymers. 12 refs.


WESTERN EUROPE

Accession no.681630

Item 319Journal of Polymer Science : Polymer Chemistry

Edition

36, No.9, 15th July 1998, p.1363-71

LIQUID CHROMATOGRAPHY OFMACROMOLECULES AT THE CRITICALADSORPTION POINT. II. ROLE OF COLUMNPACKING: BARE SILICA GELBerek D; Janco M; Meira G R

Slovak,Academy of Sciences; INTEC CONICET

Data are presented manifesting the role of columnpackings from the point of view of both their pore size

and surface chemistry. Bare silica gels that are the most

commonly used LC CAP column packings and model

macromolecules, viz. narrow PMMA, were investigated.

20 refs.

ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA

Accession no.681599

Item 32020th Annual Anniversary Meeting of the Adhesion

Society. Conference proceedings.

Hilton Head Island, S.C., 23rd-26th Feb.1997, p.519-

21. 8(10)

USING XPS TO INVESTIGATE FIBRE/MATRIXCHEMICAL INTERACTIONS AT THEINTERFACE IN CARBON FIBRE REINFORCEDCOMPOSITESWeitzsacker C L; Xie M; Drzal L T

Michigan,State University

Edited by: Drzal L T; Schreiber H P

(US,Adhesion Society)

With composites expanding into areas from aerospace to

recreation, different matrices are being investigated to

tailor composites to specific uses. The degree of adhesion

between the fibre and matrix, influenced by chemical

reactions, mechanical interactions and topography at the

fibre/matrix interface, has been recognised as a critical

factor in determining the performance of fibre-reinforced

composites. The interaction and chemical reaction of

functional groups in the matrix with functional groups at

the fibrer surface contribute to the adhesion. Direct

analysis of the fibre/matrix interface by surface analytical

methods such as X-ray photoelectron spectroscopy is not

trivial due to the thickness of a matrix layer over fibres

and the complexity of the matrix system. Indirect analysis

of the matrix/fibre interface is possible using model

compounds which represent functional groups where

differences in results are indicative of reaction between

fibre and matrix. The matrix functional groups that may

chemically react with the fibre surface can be separated

and investigated individually. Mixtures of model

compounds can be used to investigate functional groups

reactions between the components, and with the fibre

surface. Model compounds based on epoxy, polyimide,

polyphenylene sulphide and vinyl ester matrices are

investigated to characterise the chemical reactions at the

fibre/matrix interface. XPS is used to characterise both

the carbon fibre surfaces and the reacted carbon fibre

surfaces. The model compounds representative of each

of these matrices demonstrate the range of possible

reactions and interactions possible between the fibre and

matrix, ranging from no reaction to distinct chemical

reactions. 4 refs.

USA

Accession no.681439

Item 321Cleanrooms

12, No.5, Suppl. May 1998, p.S13/20

APPLICATION OF FTIR FOR MONITORINGCLEANROOM AIR AND PROCESS EMISSIONSZazzera L; Reagen W

3M Co.

The use of FTIR monitoring methods for HAP, VOC, PFC

and HFC emissions for identification and quantification

in process exhaust and in clean room air, is discussed. A

summary is included of the various protocols, test methods

and references for the use of FTIR spectroscopy to

generate verifiable data. Results of field trials and

laboratory study trials are presented, which demonstrate

its value as a monitoring method in the semiconductor

industry

USA

Accession no.679498


70, No.8, 15th April 1998, p.1563-8

POLYMER ANALYSIS BY MICRO-SCALE SIZE-EXCLUSION CHROMATOGRAPHY(SEC)/MALDI TIME-OF-FLIGHT MASSSPECTROMETRY WITH A ROBOTICINTERFACENielen M W F

Akzo Nobel Central Research



A report is presented on the development of a micro-scale

SEC system in which the MALDI matrix solution is

coaxially added to the column effluent and directly spotted

onto the MALDI targets in a robotic interface. Each spot

corresponds to the 10-s elution window from the micro-

SEC column, thus yielding a narrow polymer distribution

which is amenable to characterisation by MALDI mass

spectroscopy. The performance of the system is

demonstrated by the characterisation of a polybisphenol

A carbonate and a complex dipropoxylated bisphenol A/

adipic acid/isophthalic acid copolyester resin. 29 refs.



Accession no.679150


38, No.2, Feb.1998, p.265-73

DSC STUDIES ON THE CRYSTALLISATIONCHARACTERISTICS OF POLY(ETHYLENETEREPHTHALATE) FOR BLOW MOULDINGAPPLICATIONSDaw-Ming Fann; Huang S K; Jiunn-Yih Lee

Taiwan,National University of Science & Technology

The crystallisation behaviour of blow moulded PETP

bottles, which helps determine the product’s transparency,

was investigated by DSC dynamic cooling experiments

that simulated the cooling that occurs in the injection blow

moulding manufacturing process. DSC measurements

were used to obtain information on related aspects, such

as the ease of crystallisation from glassy and molten states

and crystallinity in the products. An Avrami equation was

used for calculation of the crystallisation kinetic

parameters. 40 refs.

TAIWAN

Accession no.678858

Item 324TAPPI 1997 Polymers, Laminations and Coatings

Conference. Conference Proceedings. Book 1.

Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012

INFLUENCE OF MINERAL FILLERS ON THEPROCESSING OF LLDPE FILMSAnsari D M; Higgs R P

ECC International Ltd.

(TAPPI)

A study was made of the thermal properties and melt

rheology of linear LDPE masterbatches filled with

calcium carbonate, talc and calcined clay. Films were

prepared by extrusion blowing and temperature changes

were monitored along the bubble. Filler distribution within

the films was assessed by optical and electron microscopy.

Rheological properties of the diluted masterbatches were

evaluated over four decades of shear rate. The mineral

fillers increased cooling rates and improved bubble

stability. Coarser calcium carbonate grades gave the

greatest improvement, while fine grades and talc had little

effect. Micrographs revealed the level of interparticle

contact and alignment of anisotropic particles which gave

rise to the observed differences. Filler type and content

did not significantly influence shear rheology at the shear

rates associated with film extrusion. 17 refs.

CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION;

UK; USA; WESTERN EUROPE

Accession no.677503

Item 325TAPPI 1997 Polymers, Laminations and Coatings

Conference. Conference Proceedings. Book 1.

Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012

EFFECT OF TITANIUM DIOXIDE ONEXTRUSION STABILITYMerkley J H

Eastman Chemical Co.

(TAPPI)

Rheological techniques for following the degradation and

changes in molecular weight and MWD of titanium

dioxide-filled polyolefins during extrusion coating are

examined. These include measurements of the crossover

point between loss modulus and storage modulus and the

variation in complex viscosity versus frequency curves

seen in the rotational mechanical spectrometer curves,

variations in viscosity versus shear rate seen in the

capillary extrusion rheometer curves, and shifts in the

DMTA curves.

CANADA; USA

Accession no.677489


Edition

36, No.5, 15th April 1998, p.851-60

PEROXIDE INDUCED CROSSLINKING ANDDEGRADATION OF PVCYu Q; Zhu S; Zhou W

McMaster University

Peroxide induced crosslinking and degradation of PVC

were investigated using an on-line ESR technique. The

reaction variables included temperature, peroxide type and

concentration. The mechanism involved in the reaction

was determined base on the radical information. The gel

content and swelling ratio were also measured. 38 refs.

CANADA

Accession no.674965

Item 327Journal of Materials Science Letters

17, No.6, 15th March 1998, p.511-3

EVIDENCE OF MOLECULAR ORIENTATION INPOLY(3-BUTYLTHIOPHENE) FILMS BYELECTRON SPIN RESONANCEMEASUREMENTS



Pawlicka A; Walmsley L; Faria R M; Nascimento O R

Sao Paulo,University; Paulista,Universidade Estadual

It was demonstrated that ESR could show evidence of

molecular orientation in films of poly(3-butyl thiophene),

making ESR useful to study orientation in conjugated

polymers when it is wished to avoid radiation damage or

for a non-destructive investigation before X-ray

measurements. 11 refs.

BRAZIL

Accession no.674766


30, No.25, 15th Dec.1997, p.7970-6

DSC, FT-IR, AND ENERGY DISPERSIVE X-RAYDIFFRACTION APPLIED TO THE STUDY OFTHE GLASS TRANSITION OF POLY(P-PHENYLENE SULPHIDE)Caminiti R; D’Ilario L; Martinelli A; Piozzi A; Sadun C

Roma,Universita La Sapienza; Roma,Istituto Nazionale

per la Fisica della Materia

The glass transition of PPS was studied by means of DSC,

FTIR spectroscopy and energy dispersive X-ray diffraction.

All of the techniques showed the alpha-transition of the

polymer. The results of the different techniques were

consistent if the onset temperature for the DSC experiments

was taken as representative of the glass transition. The glass

transition temperature was found to vary as a function of

the heating rate. The activation energy of the glass transition

process was calculated by means of a theoretical model.

The results were discussed. 47 refs.


WESTERN EUROPE

Accession no.672088

Item 329Kunststoffe Plast Europe

88, No.2, Feb.1998, p.34-5

WHAT HAS GONE WRONG?Sass A

NRW GmbH

Practical case studies are used to demonstrate how useful

differential scanning microscopy analysis can be for

material testing and damage analysis on plastics and plastic

parts. It measures the physical and chemical properties of

the plastic as a function of temperature. Information gained

by use of the analytical tool is examined, and case studies

relating to fluctuating material quality through the use of

recyclate, and the oxidation of PP water pipes are discussed.


WESTERN EUROPE

Accession no.671875

Item 330Industrial & Engineering Chemistry Research

37, No.3, March 1998, p.1140-53

SHEATH-CORE DIFFERENCES CAUSED BYRAPID THERMOOXIDATION DURING MELTBLOWING OF FIBRESKelley S L; Shambaugh R L

Oklahoma,University

A technique based on intrinsic viscosity measurements

was developed for measuring sheath and core molecular

weights during melt blowing of fibres. A mathematical

model is described which accounts for rapid diffusion and

thermooxidation. Experimental molecular weight

measurements for PP fibres were compared with

theoretical predictions. 29 refs.

USA

Accession no.670584


40, No.2-3, Feb./March 1998, p.227-34

COMPATIBILISATION OF POLYSULPHONE/POLYAMIDE BLENDS BY REACTIVEPOLYSULPHONES. EVIDENCE FORCOPOLYMER FORMATIONWeber M; Heckmann W

BASF AG

Melt blending studies using polysulphone with different

functional groups and polyamide were performed in a batch

type mixer. Blends were investigated by solvent extraction

and TEM. Model experiments revealed the possibility to

compatibilise these blends by reactive blending techniques

using functionalised polysulphones. 14 refs.


WESTERN EUROPE

Accession no.670478


36, No.1, 15th Jan.1998, p.133-41

NEW APPROACH FOR ESTIMATING THERECRYSTALLISATION RATE ANDEQUILIBRIUM MELTING TEMPERATUREHong Gyun Kim; Robertson R E

Michigan,University

A method was described for measuring the heat and rate

of crystallisation following partial melting. The method

uses a specific sequence of temperatures with a differential

scanning calorimeter, and the melting and recrystallisation

processes were confirmed by optical observations. The

method was applied to poly(butylene terephthalate). The

melting temperatures obtained from recrystallisation were

used in the Hoffman-Weeks equation to deduce 236 C as

the equilibrium melting temperature for PBTP. 22 refs.

USA

Accession no.669994

Item 333Composites Science & Technology

57, No.8, Aug.1997, p.975-83



EFFECTS OF SILANE COUPLING AGENTS ONTHE INTERPHASE AND PERFORMANCE OFGLASS-FIBRE REINFORCED POLYMERCOMPOSITESWu H F; Dwight D W; Huff N T


A single filament model of a commercial glass fibre-

reinforcement manufacturing process was used to apply

methacryloxy and amino silanes with one, two and three

silanols to two different glass fibres in a molecular model.

Surface analyses by angular-dependent X-ray

photoelectron spectroscopy, electric-kinetic analysis, and

contact-angle measurements were used to characterise the

surface coatings. The micro-indentation technique was

used to evaluate fibre-matrix interfacial adhesion.

Changes observed in surface chemistry, micromechanics,

and composite properties as functions of silanol type are

correlated. Data includes molecular models of coupling

agent on E-glass surface, chemisorption of coupling agent

into glass surface, isoelectric point values for each

treatment, composite flexural strength, composite TS, and

composite interfacial shear strength before and after 3-

days in boiling water. Matrix was polyester resin (E-701

from Owens Corning). 22 refs. (Presented at 6th Int. Conf.

on Composite Interfaces, Microphenomena in Advanced

Interfaces, Zichron Yaacov, Israel, 5th-8th May 1996).

USA

Accession no.669950


39, No.6, Dec.1997, p.721-7

COMPARISON OF CALIBRATION WITH PPGAND PS STANDARDS IN SIZE EXCLUSIONCHROMATOGRAPHY MEASUREMENTS FORCHARACTERISATION OF OLIGOLACTONEMACROMONOMERSSchoch M; Gopp U; Steurich S; Sandner B

Halle,Martin-Luther-Universitat

The calibration of size exclusion chromatography

measurements for the determination of the molecular

weights of oligolactone macromonomers was carried out

using PPG and PS as standards. Results are compared

with those obtained by end-group analysis with proton

NMR14 refs.


WESTERN EUROPE

Accession no.669429


70, No.1, 1st Jan.1998, p.131-5

USE OF MALDI-TOF TO MEASUREMOLECULAR WEIGHT DISTRIBUTIONS OFPOLYDISPERSE POLYMETHYLMETHACRYLATE

Rashidzadeh H; Baochuan Guo

Cleveland,State University

Using PMMA samples, some of the causes of mass

discrimination encountered in the MALDI-TOF analysis

of polydisperse polymers were investigated. It was found

that detector saturation could be a major instrumental

factor causing mass discrimination. This was due to the

strong signals of matrix-related ions and low-mass

oligomer ions. The matrix effect as another source of mass

discrimination was analysed quantitatively. 34 refs.

USA

Accession no.666829

Item 336Polymer

39, Nos.6-7, 1998, p.1439-43

TEMPERATURE MODULATED DSC STUDY OFPOLYETHYLENE TEREPHTHALATECRYSTALLIZATION. II. APPLICABILITY TONON-ISOTHERMAL PROCESSToda A; Tomita C; Hikosaka M; Saruyama Y

Hiroshima,University; Kyoto,Institute of Technology

The non-isothermal crystallisation of PETP was examined

by temp. modulated DSC(TMDSC). A new analytical

model of TMDSC was applied to the process, taking

account of the response of exothermic heat flow to temp.

modulation in an apparent heat capacity of complex

quantity. By examining the frequency dependence of the

apparent heat capacity, the applicability was successfully

examined for the non-isothermal process. The method was

capable of determining the temp. dependence of crystal

growth rate from TMDSC data analysis. The results were

in good agreement with the dependence determined from

literature values of spherulite growth rate measured by

optical microscopy. 12 refs.

JAPAN

Accession no.666765


29, No.11, 1997, p.910-3

FRACTIONATION OF PEO STAR SAMPLES BYSUPERCRITICAL FLUIDSCansell F; Botella P; Six J-L; Garrabos Y; Tufeu R;

Gnanou Y

CNRS

Details are given of the use of supercritical fluids for the

fractionation of PEO. The fractionation of a binary mixture

of star and linear chains of PEO was studied. 25 refs.


WESTERN EUROPE

Accession no.666545

Item 338Polymer

39, No.2, 1998, p.255-66



INVESTIGATION OF PHYSICAL AGEING INPOLYMETHYLMETHACRYLATE USINGPOSITRON ANNIHILATION, DIELECTRICRELAXATION AND DYNAMIC MECHANICALTHERMAL ANALYSISDavis W J; Pethrick R A

Strathclyde,University

Physical ageing of PMMA was studied using positron

annihilation lifetime spectroscopy (PALS), dielectric

relaxation spectroscopy (DRS) and dynamic mechanical

thermal analysis (DMTA) and the results obtained from

these techniques were compared. A correlation existed

between the free volume as measured by PALS and the

changes which occurred in the DRS and DMTA data. It

was concluded that “thermorheologically simplicity” was

probably an oversimplification for this system and that

physical ageing was associated with a redistribution, not

just a shift, of molecular relaxation processes. The

relaxation distribution changed as the glass transition

temperature was approached. The free volume distribution

probably changed during ageing, but it was not possible

to quantify these changes from the PALS study. 43 refs.


WESTERN EUROPE

Accession no.665913


67, No.3, 18th Jan.1998, p.487-500

SURFACE ENERGY MAPPING OF KEVLARFIBRES BY INVERSE GASCHROMATOGRAPHYRebouillat S; Donnet J B; Guo H; Wang T K

Du Pont (UK) Ltd.; Ecole Nationale Superieure de

Chimie de Mulhouse

The surface energy characteristics of three Kevlar fibres

were systematically studied using two inverse gas

chromatography (IGC) techniques, i.e. at an infinite probe

dilution and at a finite probe concentration, with the latter

allowing a unique mapping of the surface energy levels,

which complements greatly the more traditional

characterisation of the highest energy sites. The standard

thermodynamic parameters, such as the free energy and

the adsorption enthalpy and entropy, as well as the

dispersive and the specific component of the fibre surface

energy, were determined from the retention behaviour at

zero coverage of selected molecules of various polarity.

Using the second IGC approach, i.e. at finite

concentration, the isotherms for the adsorption of n-octane

and n-hexylamine on the three selected Kevlar fibres were

constructed by the one peak method. 29 refs.


WESTERN EUROPE

Accession no.665736


67, No.3, 18th Jan.1998, p.449-53

COMPATIBILITY STUDY OFPOLYCARBONATE-POLYVINYLPYRROLIDONE BLEND USING HIGHRESOLUTION SOLID STATE NUCLEARMAGNETIC RESONANCEda Silva E P; Tavares M I B

Rio de Janeiro,Universidade Estadual do Norte

Fluminense; Rio de Janeiro,Universidade Federal

The combining NMR techniques in the solid state permit

the evaluation of the polymeric systems homogeneity. In

polycarbonate-polyvinyl pyrrolidone blends, the response

of proton spin-lattice relaxation time in the rotating frame

was the determinant to obtain information on the transition

when the quantity of polyvinyl pyrrolidone is close to 40

wt% and a better organisation of amorphous phase was

detected. 13 refs.

BRAZIL

Accession no.665732


51, No.12, Dec.1997, p.1823-5

INVESTIGATION OF CHEMICALINTERACTIONS AT THE STEEL/POLYMERINTERFACE BY FT-IR DIFFUSEREFLECTANCE SPECTROSCOPYBistac S; Vallat M F; Schultz J

Institut de Chimie des Surfaces et Interfaces

Interactions between a steel surface and an ethylene-vinyl

acetate copolymer grafted with maleic anhydride were

investigated by FTIR diffuse reflectance spectroscopy.

The failed surfaces obtained after a mechanical separation

of the polymer/steel assemblies were analysed. A two-

step mechanism was proposed: the opening of the

anhydride cycle by a hydrolysis reaction, leading to the

formation of a carboxylic diacid, followed by the reaction

of the acid with some oxidised metallic elements present

at the metal surface. This study underlines the contribution

of FTIR reflectance techniques to the understanding of

adhesion mechanisms. 7 refs.


WESTERN EUROPE

Accession no.665698


51, No.12, Dec.1997, p.1784-90

DEPTH PROFILING STUDY OF EFFECT OFANNEALING TEMPERATURE ON POLYMER/POLYMER INTERFACES IN LAMINATESUSING CONFOCAL RAMANMICROSPECTROSCOPYHajatdoost S; Olsthoorn M; Yarwood J

Sheffield,Hallam University; Utrecht,University

The effect of annealing temperature on molecular

interactions at the interface of polymer laminates was



reported. Depth profiling was carried out using confocal

Raman microspectroscopy to study polyacrylonitrile/

polyvinyl alcohol and polyacrylonitrile/polyacrylic acid

laminates. The laminates were annealed at 65, 75 and 90C.

It was demonstrated that the degree of hydrogen bonding

interaction between the nitrile and alcohol groups near

the interfacial region changes between laminates annealed

at different temperatures. For comparison, Raman

mapping of a polyacrylonitrile-polyvinyl alcohol blend

was used to study the interactions between the polymers

in this (disordered) system. 29 refs.


NETHERLANDS; UK; WESTERN EUROPE

Accession no.665697


51, No.11, Nov.1997, p.1741-4

CHARACTERISATION OF DENTURE ACRYLICRESIN SURFACES MODIFIED BY GLOWDISCHARGESSuzer S; Ozden N; Akaltan F; Akovali G

Bilkent,University; Ankara,University; Middle

East,Technical University

Resin samples prepared by compression moulding using

a PMMA denture base material were exposed to radio

frequency glow discharges to improve the wettability of

the material. FTIR reflectance, X-ray photoelectron

spectroscopy and contact angle measurements were used

to characterise the changes introduced by the glow

discharge plasma. 18 refs.

TURKEY

Accession no.665695


51, No.11, Nov.1997, p.1736-40

GENERALISED TWO-DIMENSIONAL FOURIERTRANSFORM INFRARED PHOTOACOUSTICSPECTRAL DEPTH-PROFILING ANALYSISJiang E Y; McCarthy W J; Drapcho D L; Crocombe R

A

Bio-Rad Laboratories Inc.

A new application of generalised two-dimensional

correlation spectroscopy in photoacoustic depth-profiling

analysis. Both rapid-scan and step-scan photoacoustic

spectroscopy (obtained by using the software-based

digital signal processing technique) of multilayer samples

were used to calculate generalised two-dimensional

correlation maps. Advantages of this unambiguous

analysis method in enhancing spectral as well as depth

resolutions, over conventional two-dimensional

correlation and other spectral depth-profiling methods,

were discussed. 31 refs.

USA

Accession no.665694


51, No.11, Nov.1997, p.1668-77

RAPID-SCAN TWO-DIMENSIONAL FT-IR: ANEFFICIENT APPROACH TO DYNAMICINFRARED SPECTROSCOPYSteeman P A M

DSM Research

A new and efficient mode of operation is presented that

involves a continuous rapid-scan FTIR spectrometer, the

measurement technique relying completely on the

utilisation of the digital signal processor for data

acquisition and manipulation. Experimental and

mathematical details were discussed. Application of the

rapid-scan technique was illustrated with some results for

a styrene-acrylonitrile/butadiene copolymer. 17 refs.



Accession no.665692


51, No.11, Nov.1997, p.1593-6

RAMAN IMAGING OF DENTAL ADHESIVEDIFFUSIONWieliczka D M; Kruger M B; Spencer P

Missouri,University

Using micro-Raman spectroscopy, chemical andmorphological information on the dentin/adhesive

interface was collected with minimal sample preparation.

Results provided direct evidence of an adhesive

preparation and demineralisation depth for two adhesive

systems. 17 refs.

USA

Accession no.665691


5, No.12, Dec. 1997, p.44-5

MATERIALS ANALYST: PART 3. LOT-TO-LOTVARIATIONSepe M

Dickten & Masch Mfg.Co.

The use is examined of thermogravimetric analysis as an

analytical tool for the diagnosis of part failure in injection

moulding. The consistent performance of an ethylene

vinyl acetate copolymer was evaluated and the need to

separate the component parts of the material to test for

the amount of vinyl acetate in the compound is discussed

in order to develop a thermal history. Once this history is

established, a customer can institute an incoming QC test

on the material’s composition rather than by adjusting

the process for each new lot and performing product

testing after the parts have been produced.

USA

Accession no.664180




57, No.3, 1997, p.313-24

THERMOANALYTICAL STUDY OF THEEFFECT OF EAA AND STARCH ON THETHERMOOXIDATIVE DEGRADATION OFLDPEBikiaris D; Prinos J; Perrier C; Panayiotou C

Thessaloniki,University

The effect of ethylene-acrylic acid copolymer (EAA) and

plasticised starch (PLST) on the thermooxidative

degradation of LDPE was examined. The course of

oxidation was followed using TGA to monitor the weight

changes during heating and DSC to study the heat changes

taking place during oxidation. Three types of blend were

examined: LDPE-plasticised starch, LDPE-EAA and

LDPE-starch-EAA blends. All blends contained cobalt

stearate as prooxidant. 36 refs.


WESTERN EUROPE

Accession no.664073

Item 349Pitture e Vernici

73, No.17, 1997, p.38-43

English; Italian

RELEASE OF VOLATILE DERIVATIVES FROMINITIATORS IN RADIATION CURINGVisconti M; Cattaneo M; Li Bassi G

Lamberti SpA

Details are given of the development of a technique for

the direct evaluation of volatile organic compounds during

the radiation curing process. This method was used to

evaluate the release of benzaldehyde from commercially

available alpha-hydroxyketones during curing. 8 refs.


WESTERN EUROPE

Accession no.663242

Item 350Iranian Journal of Polymer Science & Technology

10, No.2, Summer 1997, p.35-46

Persian

APPLICATIONS OF HIGH-RESOLUTIONSOLID-STATE CARBON 13 NMRSPECTROSCOPY TO POLYMERSFarahmand F G; Morshedian J

Iran,Polymer Research Centre

A brief review is given of the theory and applications of

carbon 13 NMR to polymer analysis. Mention is made of

conformational analysis, polymer reactions in solid state,

analysis of crosslinked systems, homogeneity of polymeric

blends, analysis of surface species, and variable temperature

carbon 13 NMR solid state spectroscopy. 37 refs.

IRAN

Accession no.663219


69, No.23, 1st Dec.1997. p.4872-7

SAMPLE PRECONCENTRATION USING ION-EXCHANGE POLYMER FILM FOR LASERABLATION SAMPLING INDUCTIVELYCOUPLED PLASMA ATOMIC EMISSIONSPECTROMETRYWing Tat Chan; Yip H H G

Hong Kong,University

An efficient sample pretreatment/introduction technique

for the inductively coupled plasma atomic emission

spectrometry (ICP-AES) using ion exchange for analyte

preconcentration and matrix separation and laser ablation

sampling for sample introduction was developed.

Ammonium pyrrolidone dithiocarbamate-PS films were

coated on glass plates for analyte preconcentration. 32 refs.

HONG KONG

Accession no.662915

Item 352Pigment & Resin Technology

26, No.6, 1997, p.370-7

FTIR SPECTROSCOPY OF LAC RESIN AND ITSDERIVATIVESSarkar P C; Shrivastava A K

Indian Council of Agricultural Research; Ranchi

College

Fourier transform infrared spectroscopy was applied to

the study of lac resin, a complex natural resin of insect

origin, and some of its derivatives. The results obtained

by this method are compared with those from earlier

studies that used classical methods of chemical analysis.

Experiments include the preparation of hard and soft

resins, dewaxed lac, ammoniated lac, lac acetal,

halogenated lac, hydrolysed lac, rebuilt lac (rebulac), and

the preparation of lac metal salts. It is found that FTIR

has several advantages over classical methods, but that

FTIR data requires supplementing by other instrumental

techniques such as FT-Raman spectroscopy and solid state

nuclear magnetic resonance. 21 refs.

INDIA

Accession no.662758

Item 353Journal of Vinyl and Additive Technology

3, No.3, Sept.1997, p.249-55

PRACTICAL GUIDE TO THE IDENTIFICATIONOF MONOMERIC PLASTICIZERS INFLEXIBLE PVC COMPOUNDSKozlowski R R; Gallagher T K

Aristech Chemical

The performance of a flexible PVC compound is often

defined by its plasticiser content and composition and a

simple, accurate and fast method of plasticiser

identification could, therefore, be an effective quality



control and benchmark performance test in new product

development studies. Gas chromatography was shown to

provide the most effective identification method and it

was demonstrated that it could be complemented by IR

spectroscopy, liquid chromatography and physical

observations to confirm identity. 4 refs.

USA

Accession no.661993


30, No.21, 20th Oct.1997, p.6674-6

HIGH-RESOLUTION CALORIMETRY STUDYOF THE ORDER-DISORDER TRANSITION IN ADIBLOCK COPOLYMER MELTVoronov V P; Buleiko V M; Podneks V E; Hamley I W;

Fairclough J P A; Ryan A J; Mai S M; Liao B X; Booth C

Russian Academy of Sciences; Leeds,University;

UMIST; Manchester,University

A new method is reported for locating the order-disorder

transition in a diblock copolymer, namely high-resolution

calorimetry, and the result compared with determinations

by small-angle X-ray spectroscopy and rheology. 13 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; RUSSIA; UK;

WESTERN EUROPE

Accession no.658801

Item 355Polymer Science Series A

39, No.8, Aug.1997, p.953-7

STUDY OF SOLUBLE POLYAMIC ACIDS ANDPOLYESTER IMIDES BY METHODS OFEXCLUSION LIQUID CHROMATOGRAPHYNesterov V V; Kudrysvtsev V V; Svetlichnyi V M;

Gazdina N V; Bel’nikevich N G; Kurenbin O I;

Zhukova T I

St.Petersburg,Institute of Macromol.Compounds

The molecular and conformation characteristics of a series

of polyamic acids and polyester imides, obtained by high-

temp. imidisation of polyamic acids in N-

methylpyrrolidinone or m-cresol, were studied by

viscometry and exclusion liquid chromatography. The

differences in the molec.wts. of the products of polyamic

acid imidisation in N-methylpyrrolidinone and m-cresol

were explained by the different characters of inactivation

of the anhydride groups. 20 refs. (Full translation of

Vys.Soed.A, 39, No.8, 1997, p.1387-91)

RUSSIA

Accession no.658622


30, No.18, 8th Sept.1997, p.5285-9

FURTHER APPLICATION OF A PROCEDUREFOR MOLECULAR WEIGHT ANDMOLECULAR WEIGHT DISTRIBUTION

MEASUREMENT OF POLYDISPERSEPOLYMERS FROM THEIR MATRIX-ASSISTEDLASER DESORPTION/IONISATION TIME-OF-FLIGHT MASS SPECTRAVitalini D; Mineo P; Scamporrino E

Istituto per la Chimica e la Tecnol.dei Mat.Pol.;

Catania,Universita

A recently reported off-line procedure to estimate

molecular weight averages and MWD index, also for

polydisperse polymers, directly from their matrix-assisted

laser desorption/ionisation time-of-flight mass spectra

(MALDI-TOF) was applied to poly(bisphenol A-

carbonate), a poly(ether-sulphone resin) and

poly(dimethylphenylene oxide), all having a wide

polydispersity index. The molecular weight and MWD

obtained values were compared with those determined

by GPC or supplied by makers. A structural

characterisation of these polymers was also performed

by examining their MALDI-TOF mass spectra. 29 refs.


WESTERN EUROPE

Accession no.657168


5, No.10, Oct. 1997, p.60/2

MATERIALS ANALYST: PART 2. BRITTLE PPOSepe M


The use is described of differential scanning spectroscopy

(DSC) as an analytical tool in the diagnosis of part failure.

Degradation of the polymer during processing is

examined, and the example is investigated of a 30% glass

reinforced PPO which showed brittleness and for which

the causes of failure were revealed by means of DSC

analysis.

USA

Accession no.655661


Vol.119, July 1997, p.317-24

CHEMICAL ANALYSIS OF POLYMERS USINGTRANSMISSION ELECTRON MICROSCOPY/ELECTRON ENERGY-LOSS SPECTROSCOPY:THE EXAMPLE OF POLY(ETHYLENETEREPHTHALATE)Varlot K; Martin J M; Quet C; Kihn Y

Lyon,Ecole Centrale; CEMES-LOE

Electron energy-loss spectroscopy analysis of PETP was

performed in the analytical TEM to evaluate the

possibility of chemical analysis of the polymer at sub-

micrometre scale. Due to irradiation damage, it was

necessary to work at the lowest possible electron dose,

and with the specimen cooled to liquid nitrogen

temperature. In the acquired spectra, an identification of



the different chemical bondings in agreement with X-ray

absorption near-edge spectroscopy experiments is

proposed. 14 refs.


WESTERN EUROPE

Accession no.653745


Vol.119, July 1997, p.309-15

CARBON-13, MAGNESIUM-25 AND BORON-11SOLID STATE NMR STUDY OF A FIRERETARDED ETHYLENE-VINYL ACETATECOPOLYMERPecoul N; Bourbigot S; Revel B

Ecole Nationale Superieure de Chimie de Lille; Centre

Commun de Mesures RMN

Flame retardance of ethylene-vinyl acetate copolymer can

be achieved using magnesium hydroxide incorporated in

the polymeric matrix. The adduct of a small amount of

zinc borate as synergistic agent in the formulation

increases the fire-proofing properties. Multinuclei solid-

state NMR appears as a means to characterise materials

before and after combustion. It was shown that

endothermic dehydration, water vapour evolved and

formation of a glassy coating provided the flame

retardancy of interest to the polymer matrix. 12 refs.


WESTERN EUROPE

Accession no.653744


Vol.119, July 1997, p.269-76

QUANTITATIVE ATR-FTIR SPECTROSCOPY ATPOLYMER SURFACES: SORPTION ANDMOLECULAR CONFORMATIONMueller M; Schmitt F J

Dresden,Institute of Polymer Research

Adsorption and diffusion phenomena at or within polymer

systems were investigated by surface sensitive ATR-FTIR

spectroscopy. For a systematic description, a study was

made of (1) the competitive adsorption and desorption

behaviour of proteins on polymer surfaces, (2) swelling

of hydrophilic polymers by water molecules, which can

be accompanied by conformational changes, and (3)

induced orientational changes of hydrophobically

modified polypeptides by apolar solvents. 10 refs.


WESTERN EUROPE

Accession no.653740


Vol.119, July 1997, p.227-34

INELASTIC NEUTRON SCATTERING STUDIES

OF POLYETHYLENE AND N-ALKANESParker S F

Rutherford Appleton Laboratory

High quality inelastic neutron scattering (INS) spectra of

randomly oriented polycrystalline PE, polydeutero-

polyethylene and highly oriented polyethylene are

presented and a number of new features described. 9 refs.


WESTERN EUROPE

Accession no.653736


Vol.119, July 1997, p.157-64

INFRARED ABSORPTION SPECTRA OFPOLYMERS FROM CLASSICAL MOLECULARSIMULATIONSoldera A; Dognon J P

CEA/Le Ripault

A method is proposed to predict the IR spectra of

amorphous polymers. Based on classical molecular

simulation and Kramers-Kronig relations, it allows the

computations of absorption and transmittance spectra of

polymer films in near and middle infra-red domains with

good agreement with experimental data. 22 refs.


WESTERN EUROPE

Accession no.653730


Vol.119, July 1997, p.79-87

CREEP RATE SPECTROSCOPY USING A LASERINTERFEROMETER AS ULTRA-HIGHRESOLUTION TECHNIQUE FOR STUDY OFRELAXATIONSPeschanskaya N N; Yakushev P N; Sinani A B;

Bershtein V A

Russian Academy of Sciences

An original laser interferometry creep rate spectroscopy

(CRS) method was developed and used as the low-

frequency and high-resolution technique for studying

microplasticity and relaxations in different materials

including brittle ones. New possibilities for CRS for

polymers are demonstrated. 13 refs.

RUSSIA

Accession no.653722


Vol.119, July 1997, p.49-63

POTENTIAL OF TWO-DIMENSIONAL NEAR-INFRARED CORRELATION SPECTROSCOPYIN STUDIES OF PRE-MELTING BEHAVIOUR OFNYLON 12



Ozaki Y; Yongliang Liu; Noda I

Kwansei-Gakuin,University; Procter & Gamble Co.

This review paper discusses the potential of generalised

two-dimensional near-infrared correlation spectroscopy

in studies of pre-melting behaviour and hydrogen bonds

of nylon 12. A study on dissociation and hydrogen bonds

of N-methylacetamide is also reviewed as a model

compound study of nylon 12. FTIR spectra were measured

over a temperature range of 30-150C where gradual

weakening of inter- or intramolecular associative

interactions and decrease of local order leading to the

eventual fusion of nylon 12 crystals are observed. 24 refs.

JAPAN; USA

Accession no.653720


Vol.119, July 1997, p.25-48

UNDERSTANDING POLYMERS BYVIBRATIONAL SPECTROSCOPY: SOMERECENT ADVANCES IN THEORY ANDEXPERIMENTMeier R J

DSM Research

A rapid scan version of two-dimensional spectroscopy is

introduced and applied to study the phases of an

acrylonitrile-butadiene-styrene polymer system. Somerecent advances in the application of computational

chemistry to the evaluation of vibrational spectra are

presented. Some specific applications are discussed. 31 refs.



Accession no.653719

Item 366International Journal of Polymer Analysis and

Characterization

3, No.4, 1997, p.369-79

HPLC QUANTIFICATION OF THIOETHERANTIOXIDANTS IN POLYETHYLENE AFTERDISSOLUTION OF POLYMER UNDERPRESSURE IN ALIPHATIC SOLVENTMacko T; Furtner B; Lederer K

Leoben,Montan-Universitat

A new method is described for the quantitative

determination of some sulphur-containing antioxidants in

PE. The polymer matrix is dissolved in hot n-heptane/

isopropyl alcohol, 97/3 v/v at 160 deg.C under elevated

pressure (0.33 MPa) and precipitated by cooling. The

solution is injected directly into a normal-phase silica gel

column flushed with the same solvent as used for the

dissolution of the polymer. This method gives high recovery

of the antioxidants, good repeatability of the analysis and

a low detection limit of 0.011 mg 4,4'-thiobis(3-methyl-6-

tert-butylphenol) (Santonox R) /1 g PE; 0.074 mg

ditetradecyl-beta,beta’-thiodipropionate (Chimox 14) / 1

g PE; and 0.125 mg dioctadecyl-beta,beta’-thiodipropionate

(Irganox PS 802) /1 g PE. 23 refs.


Accession no.653220


Vol.118, June 1997, p.383-8

FREE VOLUME STUDIES IN MISCIBLEPOLYMER BLEND SYSTEMSCampbell J A; Goodwin A A; Ardi M S; Simon G P;

Landry-Coltrain C J T

Monash,University; Eastman Kodak Co.

A brief review is presented of the published literature

relating to the use of positron annihilation lifetime

spectroscopy in studying the effects of miscibility on the

free volume of miscible, amorphous polymer blends.

Studies of a fully miscible polyvinyl phenol/PVAC blend,

a partially miscible polyphenyl methacrylate/

polycarbonate blend and a largely immiscible PS/PVAC

blend are reported. The results indicate that miscible

blends tend to show a negative deviation of free volume

size, and to a lesser degree free volume fraction, on mixing

due to the intimacy of packing of the blend component

macromolecules. The largely immiscible blend shows

positive deviation of free volume size which is ascribed

to additional free volume at the interface. 13 refs.

AUSTRALIA; USA

Accession no.652994


Edition

35, No.12, 15th Sept.1997, p.2431-9

ESR STUDY ON CHEMICAL CROSSLINKINGREACTION MECHANISMS OF PE USING ACHEMICAL AGENT. II. EFFECT OF PHENOLICANTIOXIDANTSYamazaki T; Seguchi T

Hitachi Cable Ltd.; Japan,Atomic Energy Research

Institute

The effect of antioxidant on the reaction mechanism of

chemical crosslinking of PE with dicumyl peroxide at high

temperatures was investigated by ESR. The antioxidant

reacted with the alkyl radicals in PE formed by the thermal

decomposition of dicumyl peroxide above 120C and

disturbed the crosslinking. 10 refs.

JAPAN

Accession no.652659


51, No.8, Aug.1997, p.1176-8

QUANTITATION OF POLYETHYLENE GLYCOLCONCENTRATION USING RAMAN



SPECTROSCOPYMelendez Y; Schrum K F; Ben-Amotz D

Purdue,University; Maryville College

Raman spectroscopy is used to quantitate the amount of

polymer in solution, in particular polyethylene glycol

dissolved in chloroform. For various chain lengths and

polymer weight fraction ranges, it is shown that the ratios

of peak intensifies in the C-H stretching region may be

used to quantitate polymer weight fraction with about 1%

uncertainty. For low polymer weight fraction ranges (0-

10%), the relationship between Raman intensity and

polymer weight fraction is essentially linear, while at

higher ranges (0-50%) the intensity follows a nonlinear

function derived from basic concentration relationships

and indicates a universal scaling with polymer chain

length. 10 refs.

USA

Accession no.652414

Item 370Polymer

38, No.17, 1997, p.4381-5

SEPARATION AND IDENTIFICATION OFETHYLENE-PROPYLENE BLOCKCOPOLYMERJunting Xu; Linxian Feng; Shilin Yang; Yinan Wu;

Yiqing Yang; Xiangming Kong

Zhejiang,University; Shanghai,Research Institute of

Petrochemical Technology

A commercial impact resistant PP alloy was fractionated

using the temperature rising elution fractionation

technique and several ethylene-propylene block

copolymers with different ethylene contents were

obtained. The block structure of the fractions was

identified by combining the fractionation results with

carbon-13 NMR spectroscopy and DSC results. Some

transition segments were found between PE and PP

segments in the block copolymers. With increasing elution

temperature, the number and kind of transition segments

decreased, together with the length and melting

temperature of the PE segment in the block copolymer

fractions. 18 refs.

CHINA

Accession no.651909

Item 371Analyst

122, No.8, Aug.1997, p.777-81

DETERMINATION OF FINISHING OILS INACRYLIC FIBRES BY NEAR-INFRAREDREFLECTANCE SPECTROMETRYBlanco M; Coello J; Fraga J M G; Iturriaga H;

Maspoch S; Pages J

Barcelona,Universidad Autonoma

The potential of near-infrared diffuse reflectance

spectrometry for quality control analyses in the textile

industry is explored with a view to the quantification of

finishing oils in acrylic fibres by partial least-squares

regression, using a rotary cuvette system for recording

spectra. Calibration is performed with a set of samples

that encompasses every source of variability, and the

wavelength region where absorption is mostly due to the

oil is used to construct several models from which that

leading to the minimum relative standard error for a

sample test set is selected. The results provided by various

mathematical treatments used to minimise scattering

resulting from the differential linear density of the samples

reveal no significant differences between prediction

errors. The model is used to quantify levels of finishing

oil in routinely manufactured samples for a period of six

months, during which time two batches show poor

predictions due to a new component appearing in the

product. Modification of the calibration model to account

for this component substantially increases robustness and

allows the accurate quantification of all batches

manufactured after the model is developed. 28 refs.


WESTERN EUROPE

Accession no.651451

Item 372Analyst

122, No.9, Sept.1997, p.101R-15R

ANALYTICAL EXTRACTION OF ADDITIVESFROM POLYMERSVandenberg H J; Clifford A A; Bartle K D; Carroll J;

Newton I; Garden L M; Dean J R; Costley C T

Leeds,University; ICI; Newcastle,University of

Northumbria

Plastics contain many other small molecules as well as

the polymer itself. These include additives to alter the

polymer properties or prolong the life of the polymer,

such as plasticisers, antioxidants and UV light absorbers.

There may also be processing aids, residual monomers,

low molecular weight oligomers and inadvertent

contaminants present. It is important for the manufacturer

and regulators to know the level of these materials in the

polymer to ensure the product is fit for its intended

purpose. Food contact plastics are regulated by maximum

concentrations allowable in the plastic, which applies to

residual monomers and processing aids as well as

additives. There are some methods for determining

concentrations of additives without extraction from the

polymer, such as nuclear magnetic resonance

spectrometry, UV spectrometry and UV desorption-mass

spectrometry. However, in order to determine the levels

in the polymer, it is usually necessary to extract the

compounds quantitatively from the plastic before analysis.

A review is presented of the available extraction



WESTERN EUROPE

Accession no.651430




69, No.16, 15th Aug.1997, p.3304-13

QUANTITATIVE ANALYSIS OF PESTICIDES INPOST-CONSUMER RECYCLED PLASTICSUSING OFF-LINE SUPERCRITICAL FLUIDEXTRACTION(SFE)/GASCHROMATOGRAPHY-ECDNerin C; Batlle R; Cacho J

Zaragoza,University

The SFE of several organochlorine and organophosphorus

pesticides and two metabolites from recycled plastics was

studied. The recycled plastics, used as agricultural soil covers,

were a mixture of LDPE and EVA. The SFE was optimised

and compared with the classical sonication and total

dissolution extraction methods. The plastic was extracted

with supercritical carbon dioxide under different extraction

conditions, depending on the physical matrix characteristics.

Average recoveries of the eleven chemicals studied ranged

from values greater than 90% with an overall relative

standard deviation of 4.3% for plastics films to values lower

than 40% with an overall standard deviation of 7.2% for

plastics pellets. The variables affecting the whole extraction

process and the results obtained in the comparison between

the three extraction methods are discussed. 45 refs.


WESTERN EUROPE

Accession no.650545


33, No.7, July 1997, p.1135-42

FOURIER TRANSFORM INFRAREDSPECTROSCOPY APPLIED TO THE STUDY OFPVC DECOMPOSITIONBeltran M; Marcilla A

Alicante,Universidad

The process of PVC decomposition was studied by FTIR

under dynamic conditions. The IR spectra were directly

obtained from PVC films pyrolysed in-situ in a specially

designed infra red cell. A qualitative description of the

changes observed in the spectra was presented. 35 refs.


WESTERN EUROPE

Accession no.650382


Vol.118, June 1997, p.261-5

HIGH PERFORMANCE LIQUIDCHROMATOGRAPHY CHARACTERIZATIONOF MACROMOLECULESChang T; Lee H C; Lee W

Pohang,University of Science & Technology

A new chromatographic method for polymer molecular

weight characterisation, temperature gradient interaction

chromatography, is described. Fine and reproducible

control of interaction between polymer chains and the

alkyl chain bonded silica packing material can be achieved

by varying the column temperature. The method can be

used to characterise binary polymer mixtures, where one

component is separated by the size exclusion mechanism

and the other is simultaneously separated by the

interaction mechanism in a single isocratic elution. The

application of this technique to the characterisation of PS

and PS/PMMA mixtures is examined. 12 refs.

KOREA

Accession no.649987


30, No.13, 30th June 1997, p.3781-7

CHARACTERISATION OF POLYESTERS BYMATRIX-ASSISTED LASER DESORPTIONIONISATION MASS SPECTROMETRYWilliams J B; Gusev A I; Hercules D M

Pittsburgh,University

A series of aliphatic polyesters, characterised by

asymmetric oligomer distributions, heteroterminated linear

chains, and cyclic oligomers, were studied using MALDI.

Structural characterisation results were compared with

those from fast atom bombardment mass spectrometry,

electrospray ionisation mass spectrometry, NMR and end-

group titration. MALDI molecular weight determination

was contrasted with those from GPC and NMR. 23 refs.

USA

Accession no.649761

Item 377Shawbury, Rapra Technology Ltd., 1997, pp.120. 12

ins. 15/4/97. Rapra Review Rept. No.95, vol.8, No. 11

1997,

THERMAL ANALYSIS OF POLYMERSSepe M P

Dickten & Masch Mfg.Co.

Edited by: Dolbey R


Rapra Review Report No.95

A review is presented of the techniques involved in the

thermal analysis of polymers. Techniques discussed

include differential scanning calorimetry, differential

photocalorimetry, thermogravimetric analysis,

thermomechanical analysis, dynamic mechanical analysis,

dielectric, thermally stimulated current/relaxation map

analysis analysis, and thermal conductivity analysis. 381

refs.


WESTERN EUROPE

Accession no.647258


65, No.3, 18th July 1997, p.595-600



MOLECULAR WEIGHT OF POLYETHYLENEGLYCOLS BY VAPOR PRESSUREOSMOMETRY: AN ALTERNATIVE DATATREATMENTSabadini E; Assano E M; Atvars T D Z

Campinas,Universidade Estadual

The number-average molec.wt. of some polyethylene

glycols was analysed using vapour pressure osmometry.

This technique generally worked with a plot of the

difference in electrical resistance/concentration versus

concentration and the molec.wt. was determined by the

calibration constant obtained from the curve intercept. It

was demonstrated that this method induced a high

dispersion of the data, which could be minimised using a

plot of difference in electrical resistance versus

concentration.. More precise values of molec.wt. could

thus be obtained and the number-average molec.wt. of

several polyethylene glycols could be directly obtained

from the ratio between the curve slopes obtained for a

standard and the polymer sample. 10 refs.

BRAZIL

Accession no.645677

Item 379Speciality Chemicals

17, No.5, June/July 1997, p.165/70

MAKING LIQUID CHROMATOGRAPHY MOREACCESSIBLEKuehler T C; Sellen M; Lavold T; Batt J; Langridge J;

Raso R; Rontree J A

Astra Hassle AB; Micromass AB; Micromass UK Ltd.

Until recently, mass spectrometry was regarded as a highly

sophisticated technique requiring careful use of the

instrument by a sole operator, and demanding meticulous

sample preparation by the chemist. However, moves

towards open-access, chemist-operated systems have been

reported on mass spectrometers equipped with a variety

of ionisation modes. The reliability and robustness of

atmospheric pressure ionisation, the ease and speed of

source tuning, the fact that it is unnecessary to optimise

the source conditions for each sample individually and

the reproducibility of results have made API techniques

the ionisation methods of choice. Details are given. 5 refs.


SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE

Accession no.645281


57, No.2, 1997, p.135-49

THERMAL DEGRADATION KINETICS OFPOLYPROPYLENE. III.THERMOGRAVIMETRIC ANALYSISChan J H; Balke S T

Toronto,University

Thermogravimetric data were obtained for the pyrolysis

of polypropylene, and several previously published

interpretation methods were applied to the data. The wide

temperature range used in this work (45-580C)

encompassed a change in the decomposition mechanism

and this greatly limited the utility of the methods. To

accommodate this mechanism change, the data were

treated as a pseudo-first order reaction. The lower

activation energy occurring at lower degradation

temperatures was attributed to scission of the ‘weak links’

in the polymer. The higher activation energy was similar

to the carbon-carbon dissociation energy and was

associated with random scission throughout the polymer.

47 refs.

CANADA

Accession no.645116


57, No.2, 1997, p.113-25

THERMAL DEGRADATION KINETICS OFPOLYPROPYLENE. I. MOLECULAR WEIGHTDISTRIBUTIONChan J H; Balke S T

Toronto,University

A kinetic model for the thermal degradation of PP was

developed and fitted to MWD data obtained by high

temperature size exclusion chromatography. In a series

of ampoule experiments, reaction temperatures of 275-

315C were examined with reaction times of up to 48 h. A

single-parameter version of the model, containing an

apparent rate constant, was found to provide excellent

fits of all MWDs. Values of the parameter varied with

both temperature and reaction time. 35 refs.

CANADA

Accession no.645114


69, No.13, 1st July 1997, p.2485-95

MASS SPECTROMETRIC INVERSE GASCHROMATOGRAPHY: INVESTIGATION OFPOLYMERIC PHASE TRANSITIONSPanda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun K

S; Parcher J F

Mississippi,University

An improved inverse gas chromatographic method

involving the use of a mass-specific detector for

determination of the Tg of polymeric materials is

described. This new method allows the use of several

probe solutes simultaneously with an automated, closed-

loop injector and stepped temperature programming. The

result is a single continuous chromatogram for each probe

solute over a range of temperatures encompassing the Tg.

Several different methods for the exact determination of

Tg from the chromatogram were investigated. Two new

methods were also proposed for the evaluation of Tg from

either the temperature dependence of the second moments



of the elution peaks for probe solutes or simple inspection

of the variation of elution peak height (width) with

temperature. 51 refs.

USA

Accession no.645093


69, No.12, 15th June 1997, p.15R-28R

COATINGSAnderson D G

Witco Corp.

A review is presented of analytical techniques applicable

to the examination of coatings, raw materials and

substrates since 1995. The most highly referenced areas

were found to be IR spectroscopy, NMR, HPLC, thermal

analysis and gas chromatography. 704 refs.

USA

Accession no.640310


38, No.6, June 1997, p.681-8

SEPARATION OF BLOCK COPOLYMERS FROMPARENT HOMOPOLYMERS BY MEANS OFLIQUID CHROMATOGRAPHY AT THECRITICAL ADSORPTION POINTJanco M; Berek D; Onen A; Fischer C H; Yagci Y;

Schnabel W

Slovak Academy of Sciences; Istanbul,Technical

University; Hahn-Meitner-Institut Berlin GmbH

The principle underlying the above method is described

and results of its application to block copolymers

consisting of methyl methacrylate and tetrahydrofuran

blocks are presented and discussed. The technique is

shown to be suitable for characterisation of block

copolymers with regard to the presence of homopolymer

and multiblock (triblock) fractions. 5 refs.


SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERN

EUROPE

Accession no.640169

Item 385Antec 97. Volume III. Conference proceedings.

Toronto,27th April-2nd May 1997,p.3588-92. 012

FOURIER TRANSFORM INFRARED MICROSPECTROSCOPY MAPPING. APPLICATIONSTO VINYL SIDING INDUSTRYGarcia D; Black J

Elf Atochem North America Inc.

(SPE)

Fourier transform IR (FTIR) spectroscopy is a powerful

analytical technique capable of yielding high quality

information with a spacial resolution as low as 10 microns.

When coupled with an automated mapping stage, it can

offer unique evaluation capabilities. A number of

applications of FTIR spectroscopy mapping to the vinyl

siding industry are described. Examples focus on

determining, in single sample mapping experiments, the

compositional changes associated with capstock to

substrate transition and evaluating the degradation species

and level observed during weathering exposure

throughout the thickness of the siding panel. 4 refs.

USA

Accession no.639927

Item 386Antec 97. Volume II. Conference proceedings.

Toronto, 27th April-2nd May 1997, p.2310-4. 012

QUANTITATIVE ANALYSIS OF LDPE/LLDPEBLEND USING DSC AND FTIR METHODSPrasad A; Mowery D

Quantum Chemical Co.

(SPE)

A blend of LDPE and LLDPE is widely used for blown

film applications. For quality control an accurate and rapid

method is required to identify the type and composition

of alpha-olefin in an LDPE/LLDPE blend. A rapid,

accurate and new test method is developed which utilises

DSC and FTIR techniques. The melting point of LDPE

varies with density and usually is in the range of 106 deg.C

to 112 deg.C for film grade resins. The DSC thermogram

of LLDPE is characterised by a broad range of melting

with a lower melting peak around 106 deg.C to 110 deg.C

and a higher one in the range of 120 deg.C to 124 deg.C.

In the blend with LDPE, the ratio of the two endothermic

peak heights changes. At a given weight percent of LDPE,

this ratio depends on the type of LLDPE. The separate

calibrations for butene-1, hexene-1, and octene-1 LLDPEs

are developed to quantify the blend composition from

DSC thermograms provided the alpha-olefin type is

identified by a rapid method such as FTIR. 17 refs.

USA

Accession no.638387

Item 387Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins.

30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992.

FOOD CONTACT POLYMERIC MATERIALSSidwell J


Edited by: Dolbey R


Rapra Review Report No.61

A review is presented of the current and proposed

European legislation on materials in contact with food,

as well as the latest technological advances. With

reference to legislation, details are given of EC directives

issued, their implementation, FDA regulations, recycling

and waste management legislation. Technical



developments in food contact materials cover barrier

polymers in multilayer packaging films, migration of

species from food contact materials, and methods of

analysis of multilayer food contact materials. 485 refs.


WESTERN EUROPE

Accession no.637749

Item 388Polymer

38, No.12, 1997, p.3035-43

CHARACTERIZATION OF POLYETHYLENETEREPHTHALATE AND POLYETHYLENETEREPHTHALATE BLENDSFox B; Moad G; van Diepen G; Willing I; Cook W D

CSIRO,Div.of Chemicals & Polymers;

Monash,University

A method was developed for direct determination of the

molec.wt. of the PETP component in PETP/ABS blends

by GPC. The technique was used to demonstrate that an

observed deterioration in the mechanical properties, e.g.

Izod impact strength, of PETP/ABS blends on processing

could be correlated with a decrease in the molec.wt. of

the PETP component. Various methods for evaluating the

molec.wt. and the chemical microstructure of PETP were

examined. The use of NMR spectroscopy as a means of

quantitatively identifying end groups and comonomers

that were present at the 1-4% level in commercial PETP

was critically evaluated with reference to the stability of

PETP and PETP end groups in various NMR solvents.

New proton NMR chemical shift assignments for

cyclohexanedimethanol units are presented and the

reactivity of hydroxy end groups in trifluoroacetic acid

mixtures is examined. 34 refs.

AUSTRALIA

Accession no.636573


16, No.2, 1997, p.193-8

NMR CARBON-13 HIGH RESOLUTION STUDYOF POLY(ETHYLENE-CO-VINYL ACETATE)Stael G C; Tavares M I B

CCT/UENF

EVA was analysed by carbon-13 high-resolution using

NMR employing solution and solid state techniques. The

analyses of this copolymer by solution NMR permitted

the copolymer composition to be obtained, and using

solid-state NMR, a study of molecular mobility was

carried out. Both studies were made to correlate the

structure and properties. 9 refs.

BRAZIL

Accession no.634101

Item 390Trends in Polymer Science

5, No.3, March 1997, p.97-102

CHARACTERISATION OF POLYMER BLENDSBY INVERSE GAS CHROMATOGRAPHYAl-Saigh Z Y

Ohio,State University

A brief review is presented of the use of inverse gas

chromatography to characterise polymer blends.

Comparisons between data from inverse gas

chromatography and DSC are discussed. 23 refs.

USA

Accession no.632110


22, No.1, Jan.1997, p.15

POLYMER ANALYSIS ANDCHARACTERISATION. SOLID STATE NMR: ISIT BECOME TRULY POPULAR?Garbassi F

EniChem SpA

A very brief review is presented of specific areas where

solid state NMR can contribute to polymer analysis.

Mention is made of polymer morphology, interactions,

dynamics and polymer reactions. 10 refs.


WESTERN EUROPE

Accession no.632071


69, No.4, 15th Feb.1997, p.618-22

COMPOSITION AND MICROSTRUCTUREANALYSIS OF CHLORINATEDPOLYETHYLENE BY PYROLYSIS GASCHROMATOGRAPHY AND PYROLYSIS GASCHROMATOGRAPHY/MASS SPECTROMETRYCheng-Yu Wang F; Smith P B

Dow Chemical Co.

A pyrolysis gas chromatography method was developed

to determine the composition and microstructure of

chlorinated PE (CPE). The method used specific aromatic

compounds which were formed through

dehydrochlorination of trimers after pyrolysis of CPE

polymers at elevated temperatures. The composition and

microstructure calculation was based on the difference

between the levels of ethylene and vinyl chloride trimers

formed. The composition of CPE polymers used in this

study was corroborated with carbon-13 NMR results and

the manufacturers product specification. 23 refs.

USA

Accession no.629089

Item 393Biomaterials

18, No.5, March 1997, p.415-9



DETECTION OF PEROXY SPECIES IN ULTRA-HIGH MOLECULAR WEIGHTPOLYETHYLENE BY RAMAN SPECTROSCOPYChenery D H

Smith & Nephew Group Research Centre

Samples of gamma-sterilised UHMWPE were examined

using infra-red and Raman spectroscopies. The purpose

of this study was to detect the peroxy intermediates by

the novel use of Raman spectroscopy to confirm that

oxidation proceeded by this mechanism. 16 refs.


WESTERN EUROPE

Accession no.625483

Item 394Polymer

38, No.1, 1997, p.1-7

MODULATED DIFFERENTIAL SCANNINGCALORIMETRY: 6. THERMALCHARACTERISATION OF MULTICOMPONENTPOLYMERS AND INTERFACESHourston D J; Song M; Hammiche A; Pollock H M;

Reading M

Loughborough,University of Technology;

Lancaster,University; ICI Paints

A quantitative thermal method, based on the differential

of heat capacity signal from modulated temperature

differential scanning calorimetry, was described fordetermining the weight fraction of interface and the extent

of phase separation in polymer materials. The interface

was modelled as discrete fractions, each with its own

characteristic increment of heat capacity. The materials

used to demonstrate the range of the method were PS

blended with poly(phenylene oxide) (PPO), pure PS, pure

PPO, a styrene-isoprene-styrene triblock copolymer (SIS),

SIS blended with PPO, PMMA/poly(vinyl acetate) blends

and PVC sandwiched with poly(n-butyl acrylate). Two-

phase and four-phase systems were used. The calculated

results agreed well with experimental results for two- and

four-phase systems. 20 refs.


WESTERN EUROPE

Accession no.621625


69, No.1, 1st Jan.1997, p.66-71

LIQUID CHROMATOGRAPHY AT THECRITICAL CONDITION USING ENHANCED-FLUIDITY LIQUID MOBILE PHASESSouvignet I; Olesik S V

Ohio,State University

The use of enhanced-fluidity liquid mixtures of THF and

carbon dioxide for liquid chromatography at the critical

condition was examined. For PS polymers, the molec.wt.

range that could be analysed at the critical condition was

compared for THF/carbon dioxide and other common liquid

mixtures. As enhanced-fluid liquids were highly

compressible, it was possible to reach the critical condition

by changing the pressure of the THF/carbon dioxide

mixture. Approaching the critical condition by pressure

variation was compared with that possible with temp.

changes. Pressure variation was a more accurate and

reproducible means of reaching the critical condition than

temp. variation. Finally, THF/carbon dioxide mixtures were

used as mobile phases at the critical condition for PS to

characterise styrene-methyl acrylate copolymers. 25 refs.

USA

Accession no.620015

Item 396Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins.

18/7/95. Rapra Review Rept. Vol.7, No.11, 1995,

MOLECULAR WEIGHT CHARACTERISATIONOF SYNTHETIC POLYMERSHolding S R; Meeham E

Rapra Technology Ltd.; Polymer Laboratories Ltd.

Edited by: Dolbey R


Rapra Review Report No. 83

Techniques are examined for the determination of the

molecular weight distribution and molecular weight averages

of synthetic polymers. The use is discussed of gel permeation

chromatography in combination with other techniques such

as light scattering and viscometry to provide information

about the molec.wt. of a polymer and potentially significant

information on the composition of copolymers and blends.

The use of solution viscosity is also examined as a valuable

quality control technique. 411 refs.


WESTERN EUROPE

Accession no.556661


60,No.9,1st May 1988,p.932-7

IDENTIFICATION OF DYES IN SOLIDPOLYMETHYL METHACRYLATE BY MEANSOF LASER DESORPTION FOURIERTRANSFORM ION CYCLOTRON RESONANCEMASS SPECTROMETRYHsu A T;Marshall A G

OHIO STATE,UNIVERSITY

It is demonstrated that the above technique can detect and

identify (by chemical formulae) dyes in solid PMMA

commercial plastics at concentrations at least on order of

magnitude lower (0.1% vs 1-2wt%) than those obtained

by the best currently-available alternative method (ATR

Fourier transform IR spectrometry). Both untreated and

redissolved PMMA can be characterised, in the presence

and absence of up to three dyes in a single sample. 44 refs.

USA

Accession no.357996



Item 398Oxford, Pergamon Press Ltd., 1984, pp.ix,445.

LS.24.50. 9ins. 2copies. 12/7/85. Analytical Chemistry

Vol.8. 91T

ANALYSIS OF PLASTICSCrompton T R

This book covers all aspects of the analysis of plastics by

chemical and physical methods. It is divided into eight

chapters which each deal with a particular polymer or

group of polymers:- polyolefins, polypropylene, higher

alkene polymers, styrene polymers, chlorine-containing

polymers, methacrylates, polybutadienes, polyesters and

polyethers. The techniques discussed include

spectroscopy, chromatography, fractionation,, X-ray

diffraction, autoradiography, DTA, TGA and DSC.

UK

Accession no.280400

Item 399Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687.

12ins. 22/3/82. R.ROOM. 91T

ATLAS OF POLYMER AND PLASTICSANALYSIS. VOL.3....ADDITIVES ANDPROCESSING AIDS: SPECTRA AND METHODSOF IDENTIFICATION. 2ND REV.EDN.Scholl F

The spectroscopic and chromatographic data that arerequired for the identification of plastics additives and

processing aids are presented. Over 1300 IR spectra and

60 UV spectra are included. The functions and

compositions as well as the physical and chemical

methods of identification of the following materials are

discussed: plasticisers, fillers, pigments, antioxidants, UV

stabilisers, optical brighteners, antistatic agents,

biostabilisers, flame retardants, lubricants, accelerators,

hardeners and blowing agents. 608 refs.

Accession no.211056

Item 400Members Rept.49 Shawbury, 1980, pp.12. 12ins.

2copies. 26/6/80. 91T

HIGH PERFORMANCE LIQUIDCHROMATOGRAPHY - ANALYTICALAPPLICATIONS IN THE RUBBER ANDPLASTICS INDUSTRIESSidwell J A

Rubber & Plastics Research Assn.of Gt.Britain

RUBBER & PLASTICS RA.MEMBERS REPT.049

This report details some of the high-performance liquid

chromatography work carried out at RAPRA and reviews

reported in the literature. 11 refs.

RUBBER & PLASTICS RESEARCH ASSN.OF

GT.BRITAIN

Accession no.154074



Subject Index


Subject Index

AABS, 160 164 207 225 345 365 388

398ABSORPTION, 56 226 297 306 374

382ABSORPTION SPECTRA, 274ABSORPTION SPECTROSCOPY,

358 362ACCELERATOR, 399ACCURACY, 131ACETIC ACID, 76 266ACETONE, 185 224 266 311ACETONITRILE, 21 266ACID, 277 288ACOUSTIC MICROSCOPY, 126ACRYLATE, 269ACRYLIC, 199ACRYLIC ACID COPOLYMER,

172 217 348ACRYLIC POLYMER, 33 172 255

299 314 335 371 384 397ACRYLIC-MELAMINE RESIN, 44

175ACRYLONITRILE, 119ACRYLONITRILE COPOLYMER,

57ACRYLONITRILE-STYRENE

COPOLYMER, 72 110 220 345ACTIVATION ENERGIES, 49 75

146 169 280 288 317 328 380381

ADDITIVE, 29 36 71 89 99 107 108112 124 128 132 151 161 171178 181 199 201 206 225 226250 272 288 289 302 306 318324 325 353 366 372 377 387391 397 399

ADHESION, 32 61 62 145 157 167176 202 223 231 236 237 247249 312 316 341 346

ADHESIVE, 9 20 62 167 168 179272 346

ADSORPTION, 46 56 65 93 103178 203 210 221 241 285 319339 360 384

ADSORPTIONCHROMATOGRAPHY, 105 210

AEROPLANE, 36 62 121AFFINITY CHROMATOGRAPHY,

50 97AGEING, 66 80 86 88 112 148 152

274 288 298 309 338 377ALCOHOL, 56 235 288ALCOHOLYSIS, 39

ALKYD RESIN, 237ALPHA TRANSITION, 245 290

328ALUMINIUM, 126 168 179 223 266ALUMINIUM HYDROXIDE, 211ALUMINIUM OXIDE, 6AMINE, 36 48 130 151 161 178 272AMMONIUM PYRROLIDONE

DITHIOCARBAMATE, 351AMMONIUM SALT, 258AMORPHOUS, 14 54 74 78 99 117

141 170 207 213 274 283 340362 367

ANISOTROPY, 13 256 324ANNEALING, 24 54 74 101 135

136 277 308 338 342ANTI-STICK AGENT, 6ANTIMONY, 95ANTIOXIDANT, 65 86 93 107 132

171 183 195 286 288 366 368372 387 399

ANTISTATIC AGENT, 399AQUEOUS, 46 198 223 232ARAMID FIBRE, 281AROMA, 56 57AROMATIC, 48 125 192 278 288

299 392ATMOSPHERIC PRESSURE, 50

206 222ATOMIC ABSORPTION

SPECTROSCOPY, 177ATOMIC EMISSION

SPECTROSCOPY, 95 177 218273 351

ATOMIC FORCE MICROSCOPY,30 38 44 58 59 62 108 115 118142 145 154 167 179 191 219277

ATTENUATED TOTALREFLECTANCESPECTROSCOPY, 43 61 69 126257 262 301 360

AUGER ELECTRONSPECTROSCOPY, 13

AUTOMATION, 46 50 212 278 382AUTOMOTIVE APPLICATION, 44

56 62 67 175 202 212 236 329AUTOOXIDATION, 169

BBACKSCATTERED ELECTRON

IMAGING, 289BAG, 266BAGASSE, 100

BAND STRUCTURE, 262BARIUM SULPHATE, 40BARRIER PROPERTIES, 56 57 86

94 168 387BENZENE, 382BETA RELAXATION, 325BIAXIALLY ORIENTED, 104BIOCOMPATIBLE, 42BIODEGRADABLE, 37 112 267

387BIODETERIORATION, 5 37 112

246 267 387BIOMATERIAL, 42 46 246 262BIOMEDICAL APPLICATION,

262BIREFRINGENCE, 257 284BISPENTAMETHYLPIPERIDYL

SEBACATE, 66BISPHENOL A, 200 222 272 356BISPHENOL A COPOLYMER,

189BISPHENOL A DIGLYCIDYL

ETHER, 178BISPHENOL A EPOXY RESIN,

11BISPHENOL A

POLYCARBONATE, 4 29 78135 159 322 367

BISPHENOL DIGLYCIDYLETHER, 178

BLEND, 11 12 15 25 47 58 60 6364 69 72 77 91 98 107 110 112125 137 139 146 147 151 156186 188 193 209 213 220 228234 246 309 331 340 347 348363 367 375 377 386 388 390391 394

BLOCK COPOLYMER, 127 193274 354 370 384 394

BLOW MOULDING, 313 323BLOWING AGENT, 302 399BLOWN FILM, 324 386BODY ARMOUR, 281BOILING POINT, 120 185 266BONDING, 32 168 202BONDING AGENT, 168 179BONNET, 329BOTTLE, 57 131 212 266 313 323BOUND WATER, 51BOUNDARY LAYER, 81BRANCHING, 18 35 60 102 200

216BRITTLE, 41 62 271 289 357 363BROMINE CONTAINING

COPOLYMER, 273

Subject Index


BUCKET, 67BUILDING APPLICATION, 7 385BULK MOULDING

COMPOUND, 202BUMPER, 67BUTYL ACRYLATE

COPOLYMER, 28 198BUTYL METHACRYLATE

COPOLYMER, 166 190BUTYLENE COPOLYMER, 102

113

CCALCINED CLAY, 324CALCIUM CARBONATE, 65 211

289 324CALCULATION, 8 14 77 98 114

149 162 172 190 227 276 277285 290 310 323 328 330 337344 362 382 390 392 394

CALIBRATION, 6 47 173 190 208216 229 238 270 297 309 310319 334 378 392

CALORIMETRY, 9 61 64 65 74 88133 150 154 186 290 302 305313 354 359

CAPILLARYELECTROPHORESIS, 46 5097

CAPILLARY GASCHROMATOGRAPHY, 76

CAPILLARY RHEOMETRY, 324325

CAR, 56 67CARBON 13, 130 193 209 265

268 297 359 370 389 392CARBON BLACK, 40 93CARBON DIOXIDE, 57 298 301

311 373 395CARBON DISULPHIDE, 311CARBON FIBRE-REINFORCED

PLASTIC, 36 178 182 196 231320

CARBONYL GROUP, 274 288CARBOXYLIC ACID, 288 341CASTING, 94 262 367CELLULAR MATERIAL, 80 84

85 97 302CELLULOSE, 43 82 263CELLULOSE ACETATE, 79CELLULOSE NITRATE, 46 79

185CEMENT, 276CHAIN LENGTH, 272 274CHAIN SCISSION, 274 380CHAR, 194CHEMICAL BONDING, 358

CHEMICAL COMPOSITION, 2572 80 89 103 107 146 159 172197 198 211 213 229 232 289318

CHEMICAL FORCEMICROSCOPY, 58

CHEMICAL IONISATION MASSSPECTROSCOPY, 222

CHEMICAL REAGENT, 53 334CHEMICAL RECYCLING, 39CHEMICAL RESISTANCE, 57

175CHEMICAL STRUCTURE, 1 8 12

16 25 31 47 49 51 53 56 66 6873 77 83 89 93 98 102 103 114130 133 140 152 158 159 164166 168 180 200 222 228 229243 264 268 269 274 275 277283 284 286 291 300 301 308310 317 318 328 331 334 337355 356 364 365 368 370 376382 391

CHEMILUMINESCENCE, 88CHEMOMETRIC ANALYSIS, 140

216CHINA CLAY, 226 306CHITIN, 246CHLORINATED

POLYETHYLENE, 146 392CHLORINE, 17 194 373CHLORODIFLUOROETHANE,

337CHLOROFORM, 3 208 369 382CHROMATOGRAPHIC

ANALYSIS, 66 81 86 89 96 97105 112 119 137 141 152 171191 194 229 235 303 304 366375 382 384

CHROMATOGRAPHY, 3 21 25 2829 30 34 35 39 40 46 50 52 5355 56 60 66 71 72 75 80 81 8486 87 89 96 97 102 103 105107 108 112 113 114 116 119120 124 128 137 141 152 158159 160 166 169 171 172 174183 185 186 190 191 194 195200 203 204 206 208 210 218222 229 233 235 239 240 241242 243 259 264 273 278 285295 299 303 304 307 310 311314 319 322 325 334 349 353355 356 366 372 373 375 376379 381 382 383 384 388 395398 399

CHROMIC ACID, 61CHROMOGEN, 16 288CLAY, 324CLEARCOAT, 27 44 175

CLOUD POINT, 12 98 125COATED FIBRE, 179COATED METAL, 157 227COATING, 19 27 44 62 66 121 126

138 163 168 174 175 185 217222 223 227 236 237 239 255259 266 298 312 325 359 383

COBALT STEARATE, 348COHESION, 94 145 167COLOUR, 274 288COLOURANT, 181COLUMN CHROMATOGRAPHY,

233 375COLUMN PACKING, 50 203 235

241 319 375COMBUSTION, 359COMPATIBILITY, 63 90 209 331

340COMPLEX VISCOSITY, 325COMPOSITE, 10 13 17 36 62 79

81 82 90 100 134 141 176 178179 182 196 197 199 202 211231 234 258 265 271 281 288289 296 318 320 333 339 357377

COMPOSITION, 72 73 100 122123 130 220 241 243 389 392394

COMPUTER AIDED ANALYSIS,46 67 108 173 174 214 309

COMPUTER MODEL, 144 152174 338

COMPUTER SIMULATION, 248367

CONCENTRATION, 55 102 105129 130 183 197 215 224 250262 283 300 311 317 339 353378

CONE CALORIMETER, 150 359CONFOCAL RAMAN

MICROSPECTROSCOPY, 168342

CONFORMATIONALANALYSIS, 360

CONTACT ANGLE, 37 61 202217 277 333 343

CONTACT LENS, 265CONTAINER, 57 266 278CONTAMINATION, 17 128 160

181 289 357COOLING, 57 67 139 309 323 324

358COOLING RATE, 57 126 207 309

323 324COPOLYESTER, 204 322COPOLYETHERSULPHONE, 47COPOLYMER COMPOSITION,

28 57 70 94 198 210 220 370

Subject Index


COPPER, 61 316 317CORONA TREATMENT, 205CORRELATION

SPECTROSCOPY, 344 364CORROSION, 255 271CREEP RATE SPECTROSCOPY,

363CRESOL, 355CRITICAL CONCENTRATION,

241CRITICAL POINT, 103 395CRITICAL SOLUTION

TEMPERATURE, 125CROSS-POLARISATION, 193 209

268 300CROSSLINK, 83 279CROSSLINK DENSITY, 179 269CROSSLINKED, 110 179 221 250CROSSLINKING, 9 10 20 24 27

36 46 48 49 73 85 115 134 161180 187 265 272 279 288 294300 309 326 368 377

CROSSLINKING AGENT, 222288

CRYSTALLINE, 2 59 143 147 283313

CRYSTALLINITY, 2 13 24 42 5457 62 63 64 69 94 102 113 114117 122 126 131 139 143 147168 257 260 274 277 281 291309 313 323 357 364 367 377391

CRYSTALLISATION, 2 9 12 1322 24 26 52 54 57 59 74 78 107117 122 131 136 139 147 148155 170 246 261 295 309 323329 332 336 386

CRYSTALLISATIONTEMPERATURE, 136 309

CRYSTALLITE, 57 139 260CURE TEMPERATURE, 2 48 161CURE TIME, 36 265 309CUREMETER, 134CURING, 8 20 27 36 68 73 83 89

138 144 149 161 163 178 182187 247 248 265 269 272 300305 309 312 316 349 377

CURING AGENT, 36 151 161 178182 222 250 272 288 317

CYCLOHEXANE, 21 263 285

DDATA ANALYSIS, 13 216 237 267

291 319DATA COLLECTION, 291 345DEBONDING, 236DECANE, 382

DEFECT, 67 88 126 289 329DEFORMATION, 41 59 67 249

277 283DEGRADABLE, 37 112 267 387DEGRADATION, 4 16 39 44 58

65 66 80 85 86 87 88 92 94 101112 119 135 148 152 164 175183 189 194 195 213 228 244258 266 267 274 279 288 294298 302 309 311 318 325 326330 338 347 357 374 377 380385

DEGRADATION PRODUCT, 4 1734 75 87 112 128 152 175 183194 274 279 288

DEGRADATIONTEMPERATURE, 194 269 380

DEGREE OF BRANCHING, 18 35DEGREE OF CROSSLINKING, 9

27 300 377DEGREE OF CRYSTALLINITY,

143 313DEGREE OF CURE, 10 36 269DEHYDROCHLORINATION, 146

392DELAMINATION, 255 312DENSITY, 18 52 56 106 131 168

179 216 231 261 289 313 367DENTAL APPLICATION, 172 247

276 343 346DEPOLYMERISATION, 39 165

266DEPTH PROFILING, 205 333 342

344DERIVATIVE

THERMOGRAVIMETRY, 380DESORPTION, 71 93 104 210 310

360DETECTION LIMIT, 56 174 289DIACID, 288 341DIBUTYL PHTHALATE, 76DIBUTYL SEBACATE, 277DICHLOROXYLENE, 48DICHROISM, 284DICUMYL PEROXIDE, 368DICYANATE POLYMER, 11DIELECTRIC ANALYSIS, 9 377DIELECTRIC CONSTANT, 46

237 338DIELECTRIC PROPERTIES, 46

245 338DIELECTRIC RELAXATION

SPECTROSCOPY, 49 110 259338

DIELECTROMETRY, 9DIETHYLENE GLYCOL, 26 121

266DIFFERENTIAL

INTERFERENCEMICROSCOPY, 324

DIFFERENTIALPHOTOCALORIMETRY, 377

DIFFERENTIAL SCANNINGCALORIMETRY, 2 6 7 8 10 1112 15 17 18 20 22 24 29 36 4151 54 56 63 64 65 74 77 78 8385 88 94 95 98 101 110 113 114122 125 126 131 133 134 135136 139 144 146 147 149 154155 161 163 164 170 186 187207 211 213 220 245 246 252253 254 258 261 267 269 276277 280 282 287 290 291 296302 305 309 313 323 324 328329 332 336 348 357 367 370377 382 386 387 390 394 398

DIFFERENTIAL THERMALANALYSIS, 2 6 7 8 10 12 1517 18 20 22 24 29 36 41 54 5663 64 65 74 77 78 83 88 94 9598 101 110 113 114 122 125126 131 133 134 136 139 144146 147 149 154 155 161 163164 170 186 187 207 211 213231 245 246 252 253 254 258267 269 276 277 280 287 290291 296 302 309 313 323 324328 329 332 336 348 357 367370 377 382 386 387 390 398

DIFFUSE REFLECTANCESPECTROSCOPY, 341

DIFFUSION, 9 56 80 99 124 125264 274 346 351 360 372 387394

DIFFUSION COEFFICIENT, 5699 111 224

DIGITAL ANALYSIS, 10DIGLYCIDYL ETHER

BISPHENOL A, 200DIMETHYL FORMAMIDE, 21 77DIMETHYL ISOPHTHALATE,

208DIMETHYL SULPHOXIDE, 342DIMETHYL TEREPHTHALATE,

39 208DIPHENYLMETHANE

DIISOCYANATE, 9DISCOLOURATION, 288DISPERSION, 181 217 289 361DISTILLED WATER, 56DISTORTION, 20 260DISTRIBUTION, 60 102 338DOMESTIC APPLIANCE, 80DOUGH MOULDING

COMPOUND, 211DRAW RATIO, 117 257 283 284

Subject Index


DRINKING WATER, 183 307DUCTILE FAILURE, 289DYE, 16 397DYNAMIC, 71 144 317 323 374DYNAMIC DIFFERENTIAL

SCANNING CALORIMETRY,11

DYNAMIC INFRAREDSPECTROSCOPY, 345

DYNAMIC LIGHTSCATTERING, 111

DYNAMIC MECHANICALANALYSIS, 36 56 73 83 92114 134 161 196 245 269 309377

DYNAMIC MECHANICALTHERMAL ANALYSIS, 325338 367

DYNAMIC PROPERTIES, 179317 325

DYNAMIC SPECTROSCOPY,345

DYNAMIC VISCOELASTICPROPERTIES, 101

EELECTRICAL CONDUCTIVITY,

38ELECTRICAL INSULATOR, 271ELECTRICAL PROPERTIES, 38

46 338 378ELECTROCHEMICAL

IMPEDANCESPECTROSCOPY, 5 223 227237 255

ELECTRODIALYSIS, 97ELECTROKINETIC

CHROMATOGRAPHY, 46ELECTROKINETIC

POTENTIAL, 333ELECTRON DISPERSIVE X-RAY

ANALYSIS, 6ELECTRON ENERGY LOSS

SPECTROSCOPY, 13 358ELECTRON IONISATION MASS

SPECTROMETRY, 206ELECTRON MICROSCOPY, 2 5

13 63 82 108 129 181 289 324ELECTRON SCANNING

MICROSCOPY, 2 5 13 63 82108 129 181

ELECTRON SPECTROSCOPYFOR CHEMICAL ANALYSIS,61

ELECTRON SPIN RESONANCESPECTROSCOPY, 45 66 294326 327 368

ELECTRONIC APPLICATION, 5ELECTROPHORESIS, 46 50 97ELECTROSPRAY IONISATION,

190 222 229 376ELEMENTAL ANALYSIS, 15 115

160 194 351ELUENT, 203 235 375ELUTION, 35 46 203 210 266 285

370 375 382ELUTION CHROMATOGRAPHY,

50ELUTION FRACTIONATION, 52ELUTION VOLUME, 35 285 310

356EMISSION, 56 87 174 321END GROUP, 36 102 130 151 229

274 314END-GROUP ANALYSIS, 190

200 334 376 388ENDOTHERM, 54 56 74 78 94

125 136 139ENDOTHERMIC, 235 245 276

309 329 359ENERGY ABSORPTION, 207ENERGY CONTENT, 357ENERGY DISPERSIVE X-RAY

ANALYSIS, 108 129 289 328ENGINEERING APPLICATION,

309 367ENTHALPY, 36 64 74 125 179 187

276 282 309 339 354 375ENTROPY, 339 375ENVIRONMENTAL SCANNING

ELECTRON MICROSCOPY,324

ENVIRONMENTAL STRESSCRACKING, 315

EPICHLOROHYDRIN, 272EPOXY NOVOLAC RESIN, 11EPOXY RESIN, 10 11 20 32 36 47

62 68 144 145 149 151 157 161178 179 182 199 200 222 249255 269 272 282 292 305 309312 320

EQUIPMENT, 6 46 138 194 197218 309 335 379

ERROR ANALYSIS, 13ETHANOL, 56 311ETHERSULPHONE

COPOLYMER, 47ETHYLENE ACRYLIC ACID

COPOLYMER, 51 348ETHYLENE-BUTYLENE

COPOLYMER, 52ETHYLENE CONTENT, 370 392ETHYLENE COPOLYMER, 22 60

63 102 113 154 209 259 348359 389

ETHYLENE GLYCOL, 39 266ETHYLENE-HEXENE

COPOLYMER, 52ETHYLENE-PROPYLENE

COPOLYMER, 69 274 370ETHYLENE TEREPHTHALATE

COPOLYMER, 131ETHYLENE-VINYL ACETATE

COPOLYMER, 57 70 100 209226 251 270 306 341 347 359373 389

ETHYLENE-VINYL ALCOHOLCOPOLYMER, 56 57 94 291387

ETHYLIDENE VINYLPYRROLIDONE, 250

EVANESCENT WAVESPECTROSCOPY, 111 292

EXCLUSIONCHROMATOGRAPHY, 28 2934 35 40 41 50 52 55 60 97 102103 108 112 114 116 158 166204 210 229 239 240 243 299314 322 334 355 375 381

EXOTHERM, 85 323EXOTHERMIC, 54 276 309 329

336EXTENDER, 121EXTRACTION, 71 97 128 171 185

195 266 331 372 373EXTRACTION

CHROMATOGRAPHY, 97EXTRUSION, 6 7 40 70 72 183

188 195 225 254 266 324 325

FFADING, 288FAILURE, 17 30 36 167 178 182

254 271 289 296 341 347 357FAILURE ANALYSIS, 36 108 145

167 254 289 329FAST ATOM BOMBARDMENT

MASS SPECTROSCOPY, 376FATTY ACID, 232FIBRE, 31 33 43 82 100 178 179

182 231 256 260 330 339 371FIBRE GLASS, 76 176 197FIBRE OPTIC, 36FIBRE-REINFORCED PLASTIC,

36 100 141 178 231 258 281320

FIELD EMISSION SCANNINGTRANSMISSION ELECTRONMICROSCOPY, 289

FIELD-FLOWFRACTIONATION, 35 97

FILLED, 179 318 325

Subject Index


FILLER, 17 43 45 65 81 90 93 184207 211 226 289 306 307 318324 325 399

FILLER CONTENT, 81 90 324FILLER DISTRIBUTION, 289 324FILM, 1 3 16 27 37 38 40 41 49 56

57 61 62 65 86 92 102 104 106115 117 118 135 142 148 156167 168 186 205 246 257 262266 269 288 289 308 324 327349 351 362 373 374 386 387

FINITE ELEMENT ANALYSIS,108

FIRE RETARDANT, 359FLAME IONISATION, 185FLAME RETARDANT, 95 152

211 218 273FLAMMABILITY, 150 173 273

359FLASH CHROMATOGRAPHY,

97FLASH PYROLYSIS, 4FLAVOUR, 183FLEXIBLE, 84 277 283 353FLOATATION, 97FLOW INJECTION ANALYSIS,

50FLOW MICROCALORIMETRY,

93FLOW RATE, 50 143 233 324 372FLUORESCENCE, 17 293FLUORESCENCE

SPECTROSCOPY, 108 116 157FLUOROPOLYMER, 279 387FOAM, 80 84 97 302FOOD-CONTACT

APPLICATION, 124 177 195208 264 286 387

FOOD PACKAGING, 57 124 168195 266 278 311

FORMULATION, 30 108 164 174217 312

FOURIER TRANSFORMINFRARED SPECTROSCOPY,1 3 6 8 11 24 25 26 29 30 34 3640 41 60 63 64 72 77 83 88 9293 94 98 102 107 108 113 117126 135 136 150 153 156 160161 163 165 169 170 173 181189 190 213 215 216 226 228246 249 250 252 259 262 264271 274 275 277 288 300 306309 316 318 321 328 341 343344 345 352 360 364 374 381385 386 397

FRACTION, 35 170 204 394FRACTIONATION, 28 52 97 107

113 337 370 398

FRACTURE, 67 82 98 178 236271 289

FRACTURE MORPHOLOGY, 213 54 61 98 115 191 319 346391 394

FREE ENERGY, 339FREE RADICAL, 45 266FREE VOLUME, 18 56 99 338

367 382FREEZING POINT, 324FREQUENCY, 78 118 179 255 256

287 309 325 336FUEL TANK, 56FUNCTIONAL GROUP, 36 83 274

331FUNGUS, 5FURAN RESIN, 199FURNITURE, 274

GGAMMA-IRRADIATION, 4 99

133 393GAS, 67 80 277 311GAS BARRIER, 56 57 168GAS CHROMATOGRAPHY, 3 4

30 34 39 53 56 66 71 72 75 7680 81 84 87 90 96 107 112 119120 124 128 132 141 143 160174 183 185 186 191 194 195198 208 217 218 221 232 235250 270 273 278 303 307 311339 349 353 373 382 383 390392 398

GAS DIFFUSION, 274GAS LIQUID

CHROMATOGRAPHY, 97GAS-PHASE, 67 80 277 311GAS PIPE, 277GAS TRANSMISSION, 311GEL, 46 319 326GEL ELECTROPHORESIS, 97GEL PERMEATION

CHROMATOGRAPHY, 50 107113 137 152 169 172 190 200233 259 264 295 310 325 334356 376 383 388 396 399

GELATION, 7 73 134 161 294GLASS, 145 167 276 351GLASS CONTENT, 296GLASS FIBRE, 76 176 197GLASS FIBRE-REINFORCED

PLASTIC, 17 179 202 211 231271 288 296 333

GLASS TRANSITIONTEMPERATURE, 12 15 18 2029 36 49 51 56 74 77 81 85 94101 106 110 114 117 122 135

149 155 161 163 164 170 179207 213 220 249 261 269 280282 287 290 305 308 309 323328 338 357 367 377 382 390394

GLOW DISCHARGE, 343GLOW DISCHARGE

SPECTROSCOPY, 202GRAVIMETRIC ANALYSIS, 23

82 85 93 94 152 189 196 211244 258 296 317 347 377 380

HHEADSPACE ANALYSIS, 311HEADSPACE

CHROMATOGRAPHY, 185HEAT CAPACITY, 20 74 78 125

161 179 220 253 261 276 280287 290 309 324 336 394

HEAT DEGRADATION, 23 26 2975 76 83 152 160 163 189 192194 196 244 266 273 318 325380 381

HEAT FLOW, 36 155 245 252 261276 309 324

HEAT INSULATION, 80 276HEAT RESISTANCE, 11 24 26 57

85 126 163 196 228 266 267269 295 317 377

HEAT STABILITY, 146 196HEAT TREATMENT, 57 119HEATING, 36 179 187 244 266

309 323 348 354HEATING RATE, 36 54 144 179

309 328 332 348 380HELIUM, 57HETEROGENEITY, 25 217 268HETEROGENEOUS, 129 146 170HEXANE, 240 319HIGH DENSITY

POLYETHYLENE, 52 56 57 6387 91 102 109 112 128 132 143164 195 212 214 307 357 372392

HIGH IMPACT PS, 48HIGH PERFORMANCE LIQUID

CHROMATOGRAPHY, 21 3539 46 76 97 165 171 183 195200 222 233 238 239 242 247264 266 286 304 337 366 375383 399 400

HIGH TEMPERATURE, 62 107277 381

HIGH RESOLUTION, 179 209289 340 354 363 389

HINDERED AMINE, 3 31 66 123225

Subject Index


HINDERED PHENOL, 41HIP JOINT, 42HOMOGENEITY, 100 289 340HOT STAGE MICROSCOPY, 2

181HUMIDITY, 44 56 57 309HYDROFLUOROCARBON, 321HYDROGEN BONDING, 77 94

99 114 342 364HYDROGEN CHLORIDE, 34 48

194 228HYDROLYSIS, 34 58 59 165 319

341 352HYDROPHILICITY, 46 51 360HYDROPHOBICITY, 37 46 360

375HYDROXYBENZENE, 75 297

300HYDROXYETHYL

METHACRYLATECOPOLYMER, 46

HYDROXYL GROUP, 36 69

IIDENTIFICATION, 30 79 121 128

132 212 214 353 370 397ILLUMINATION, 311IMAGING, 13 67 88 168 179 275

289 346IMIDAZOLE, 262IMIDISATION, 8 355IMMERSION, 178 223 237IMMISCIBLE, 188 367 394IMMUNOELECTROPHORESIS,

97IMPACT PROPERTIES, 56 63 231

370 388IMPLANT, 219 262 393IMPURITY, 221INDUCTION PERIOD, 41 88INDUCTIVELY COUPLED

PLASMA SPECTROMETRY,351

INELASTIC NEUTRONSCATTERING, 361

INFRARED ABSORPTION, 36274 362

INFRARED CAMERA, 67INFRARED DICHROISM, 284INFRARED SPECTROSCOPY, 1 3

8 11 14 17 24 26 29 33 34 36 3941 43 51 60 63 66 69 72 77 7985 88 92 93 94 98 108 113 126135 142 150 153 156 160 161163 164 165 169 172 173 181184 186 188 189 207 215 216225 226 228 230 244 246 249

250 256 257 259 262 264 269271 274 275 277 284 294 297301 306 316 318 321 328 341343 344 345 353 360 362 364365 371 374 381 383 385 386387 393 399

INFRARED THERMOGRAPHY,67

INJECTION MOULDING, 67 160231 296 357

INK, 239INSULATION, 80 276INTERACTION, 90 167 178 235

249 285 311 318 341 342 364INTERACTION PARAMETER,

220 235 285INTERCHAIN PACKING, 135INTERFACE, 178 179 182 206 229

236 322 341 342 346 367 394INTERFACIAL ADHESION, 333INTERFACIAL DEBONDING, 167INTERFACIAL INTERACTION,

90 167 178INTERFACIAL PROPERTIES, 81

90 111 141 167 178 249 320 342INTERFEROMETRY, 13 275 363INTERNAL MOULD RELEASE,

202INTRINSIC VISCOSITY, 29 172

266 330INVERSE GAS

CHROMATOGRAPHY, 81 90141 143 191 217 235 339 382390

ION CHROMATOGRAPHY, 97218

ION CYCLOTRON RESONANCE,397

ION EXCHANGE, 50 97 351IONISATION, 46 50 206 222 379IRON OXIDE, 112IRRADIATION, 4 40 92 153 358IRRADIATION DEGRADATION,

133ISOELECTRIC POINT, 46 333ISOMERISATION, 11 288ISOPHORONE DIISOCYANATE,

121ISOTACHOPHORESIS, 46ISOTACTIC, 129 133 274 314ISOTHERM, 67 178 309 339ISOTHERMAL, 36 78 117 125 276

317 338 348 375ISOTROPY, 117

KKAOLIN, 226 306

KEVLAR, 191KINETIC, 8 10 45 73 83 125 377KINETICS, 3 23 52 73 75 94 144

149 302 317 323 332 363 380381

LLAC RESIN, 352LACQUER, 185LAMELLAE, 78 139LAMINATE, 56 57 168 182 266

342LAMINATED FILM, 57 168 266

293LANGIVIN EQUATION, 3 46 50

60 75LASER, 62 212 236 298 351 397LASER INDUCED

DECOHESIONSPECTROSCOPY, 236

LASER INTERFEROMETRY, 363LASER IONISATION MASS

SPECTROMETRY, 6LASER LIGHT SCATTERING, 35

200LASER RAMAN

SPECTROSCOPY, 168LATERAL FORCE

MICROSCOPY, 308LATEX, 46 156 174 193 198LEACHING, 183LEAD, 201LEAST-SQUARES ANALYSIS,

70 214 345LENS, 219 265LIFETIME PREDICTION, 108

255 377LIGHT ABSORPTION, 229 274LIGHT DEGRADATION, 3 40 129

153 196 274 288LIGHT MICROSCOPY, 181 295LIGHT SCATTERING, 111 116

117 172 203 238 260 310 396LIGHT STABILISER, 3 31 123

132 288LIGHT STABILITY, 3 288LIGNOCELLULOSE, 82LINEAR LOW DENSITY

POLYETHYLENE, 57 92 107139 186 216 225 324 386

LINEAR REGRESSIONANALYSIS, 144

LIQUID CHROMATOGRAPHY,21 25 35 39 46 50 55 76 97 103105 108 124 159 165 171 183195 200 203 206 210 222 229233 238 239 240 241 242 243

Subject Index


247 264 266 285 286 299 304319 337 353 355 366 375 379383 384 395

LIQUID CRYSTAL POLYMER,309 367 387

LIQUID NITROGEN, 358LOW DENSITY

POLYETHYLENE, 3 57 86 87139 143 164 168 186 207 214266 324 325 348 372 373 386

LOW FREQUENCY, 126 363LOW MOLECULAR WEIGHT,

128 375

MMAGIC ANGLE, 209 268 283 291

300 340MAGNESIUM-25, 359MALDI-TOF SPECTROSCOPY,

28 103 127 137 158 159 166 204310 322 335 356 376

MALEIC ANHYDRIDE, 82MALEIC ANHYDRIDE

COPOLYMER, 28 341MAPPING, 69 275 289 339 342

344MASS SELECTIVE DETECTOR,

76 218MASS SPECTROMETRY, 4 6 13

28 30 50 75 103 107 112 127132 178 186 192 194 204 222229 266 278 307 311 376 379382 392 396 397 398

MASS SPECTROSCOPY, 28 66 7284 86 103 121 124 127 128 137153 158 159 166 177 185 190195 202 204 206 244 250 270273 303 310 312 322 335 356376 399

MATRIX, 36 82 141 178 182 351359

MATRIX-ASSISTED LASERDESORPTION, 28 103 127 137158 159 166 204 310 322 335356 376

MDI, 9MECHANICAL DEGRADATION,

266MECHANICAL PROPERTIES, 9

40 41 56 61 62 63 65 67 82 8486 91 114 115 126 151 163 168178 179 182 207 231 249 256269 271 277 281 288 289 296309 315 316 324 325 333 353365 370 388

MECHANICAL RECYCLING, 195MECHANICAL SPECTROSCOPY,

325MEDICAL APPLICATION, 42 262MELAMINE-FORMALDEHYDE

RESIN, 159 365MELT, 54 170 254 282 290 354MELT TRANSITION, 267MELTING, 2 24 54 78 79 136 155

179 209 252 309 332MELTING POINT, 12 52 56 63 94

114 164 266 295 324MELTING TEMPERATURE, 20 57

179 207 309 323 332 370MEMBRANE OSMOMETRY, 396METAL, 177 179 298 341METAL ADHESION, 62 223 341METAL COATING, 62 255METAL SALT, 352METALLISED FILM, 168 266 387METHACRYLATE COPOLYMER,

190METHACRYLIC ACID

COPOLYMER, 15 63 259METHACRYLIC ESTER

COPOLYMER, 190METHACRYLIC ESTER

POLYMER, 45 245METHANOL, 39 56 76 171 266METHANOLYSIS, 39METHYL ACETATE, 185METHYL ACRYLATE

COPOLYMER, 33 172 299 395METHYL ETHYL KETONE, 285METHYL METHACRYLATE, 288METHYL METHACRYLATE

COPOLYMER, 28 33 166 198308 384

METHYLBENZENE, 56 185 241261

METHYLENE CHLORIDE, 266MICROANALYSIS, 179 231 289MICROBIAL DEGRADATION, 5MICROCALORIMETRY, 154MICRODIELECTROMETRY, 9MICROEXTRACTION, 71 185MICRORAMAN

SPECTROSCOPY, 168 346MICROSCOPY, 2 13 16 27 38 41

58 59 61 98 111 125 126 142145 168 179 181 213 231 256257 277 289 295 308 324 387

MICROSTRUCTURE, 13 58 60168 170 198 274 370 388 392

MICROTOMY, 168MICROWAVE, 112 128 262MICROWAVEABLE, 266 387MID-INFRARED

SPECTROSCOPY, 362MIGRATION, 46 65 183 264 266

288 387MINERAL FILLER, 45 288 289

324MISCIBILITY, 12 64 77 98 125 146

209 213 220 309 367 390 391394

MOBILE PHASE, 50 375 395MODEL, 28 105 149 152 172 216

290 311 319 336 341 360 381382 394

MODULATED DIFFERENTIALSCANNING CALORIMETRY,10 36 74 125 131 135 161 220261 282 309 377 394

MODULATED TEMPERATURETHERMOMECHANICALANALYSIS, 20

MOISTURE CONTENT, 6 51 148266 309

MOLAR MASS, 25 35 102 103 107140 159

MOLECULARCONFIGURATION, 117 130135 168 328 338 355 367

MOLECULAR INTERACTION,178 220 342 375

MOLECULAR MOBILITY, 26 268301 389

MOLECULAR ORIENTATION,257 281 284 327 360

MOLECULAR STRUCTURE, 1 812 16 25 31 47 49 51 53 56 6668 72 73 77 80 83 89 93 98 101102 103 107 114 130 133 140146 152 158 159 164 166 168172 180 197 198 200 211 213222 228 229 232 243 264 268269 274 275 277 283 284 286289 291 300 301 308 310 317318 328 331 334 337 355 356364 365 368 370 376 382 391

MOLECULAR WEIGHT, 1 28 2942 46 50 52 54 55 62 73 89 102112 113 114 116 120 127 128130 158 164 166 172 185 190200 204 210 222 224 235 239243 285 310 314 319 322 323325 330 332 334 337 355 356375 376 378 381 382 388 395396

MOLECULAR WEIGHTDISTRIBUTION, 102 116 190200 204 224 310 314 319 322325 356 375 381 396

MONITORING, 5 70 149 174 188223 261 272 298 311 321 348

MONOETHYLENE GLYCOL, 39266

Subject Index


MONOMER, 124 229 269 270 387MORPHOLOGY, 2 13 54 61 63 98

115 118 136 191 213 256 309319 346 367 391 394

MOULDING, 134 225 343MULTI-ANGLE LASER LIGHT

SCATTERING, 35 200MULTILAYER, 168 266 344 387MULTILAYER FILM, 57 168MULTIPLE PULSE NMR, 291MULTIVARIATE ANALYSIS, 216MUNICIPAL WASTE, 128

NN-METHYL-2-PYRROLIDONE,

355NANOCOMPOSITE, 62NAPHTHA, 215NATURAL FIBRE, 82NATURAL FIBRE-REINFORCED

PLASTIC, 141NATURAL POLYMER, 232 352NEAR-INFRARED

CORRELATIONSPECTROSCOPY, 364

NEAR-INFRAREDSPECTROSCOPY, 14 36 215225 362 371

NITROCELLULOSE, 46 79 185NITROGEN, 57 76 95NITROGEN-CONTAINING

POLYMER, 250NON-DESTRUCTIVE TEST, 19

32 67 106 126 157 327NOVOLAC RESIN, 73 300NUCLEAR MAGNETIC

RESONANCE, 1 22 28 30 3132 34 57 60 68 73 77 100 108113 114 123 130 138 148 162169 172 180 189 193 201 209212 246 248 251 265 268 272283 291 297 300 314 331 334340 350 359 370 372 376 383388 389 391 392

NUMBER-AVERAGEMOLECULAR WEIGHT, 130375 378

NYLON, 33 56 57 79 125 164 168192 199 207 225 231 309 331

NYLON 1010, 24NYLON-12, 294 364NYLON-6, 33 56 57 132 207 387NYLON-6,6, 17 33 57 130 231 329

OODOUR, 57 183 307

OIL, 194 277OLIGOMER, 26 46 103 124 172

190 192 238 242 264 266 335ON-LINE MEASUREMENT, 314OPTICAL FIBRE, 36 188 292OPTICAL MICROSCOPY, 2 13 41

98 125 142 181 213 289 324387

OPTICAL PROPERTIES, 1 3 4757 162 181 199 200 206 263274 288 292 293 323 332 350362 375

OPTIMISATION, 50 102 105 171233 318 373

ORGANOLEPTIC PROPERTIES,57 183

ORIENTED, 104 117 283 284 361387

ORTHOPAEDIC APPLICATION,393

OSCILLATING DIFFERENTIALSCANNING CALORIMETRY,7

OSMOMETRY, 29 46 200 378OVEN STABILITY, 266OXIDATION, 40 41 61 66 88 94

104 129 152 153 205 266 269274 288 325 329 348 381 393

OXYGEN, 57 104 153 262 274311

OXYGEN ABSORPTION, 104387

OXYGEN BARRIER, 56 57 168

PPACKAGING, 5 57 128 131 168

212 264 266 278 323 387PACKAGING FILM, 57 168 266

387PAINT, 62 174 185 217 255 298PAPER, 266 387PAPER CHROMATOGRAPHY, 97PARACRYSTALLINE, 102 207

213 315PARTIAL LEAST SQUARES, 215

216PARTICLE BEAM ANALYSIS,

206PARTICLE PACKING, 324PARTICLE SIZE, 13 45 50 81 225

233 319 324 372 375PARTICLE SIZE

DISTRIBUTION, 62 324PEAK INTENSITY, 168 178 260

289 392PELLET, 216 266 296 373PERMEABILITY, 56 57 168 237

PERMITTIVITY, 338PEROXIDE, 294 326PEROXY COMPOUND, 393PESTICIDE, 373PH, 46 50 130 183PHARMACEUTICAL

APPLICATION, 46 221PHASE BEHAVIOUR, 267 340

365PHASE SEPARATION, 110 125

156 391 394PHENOL, 75 297 300PHENOL-FORMALDEHYDE

RESIN, 73 297 300PHENOLIC ANTIOXIDANT, 183PHENOLIC RESIN, 83 199 300PHOSPHORUS, 95 312 373PHOTOACOUSTIC

SPECTROSCOPY, 249 288 344PHOTOCALORIMETRY, 377PHOTOCHEMICAL

DEGRADATION, 288PHOTOCROSSLINKING, 45 187PHOTODEGRADATION, 16 19

65 66 274 279PHOTOELECTRON

SPECTROSCOPY, 13 37 48100 104 121 167 175 176 196197 202 205 277 279 298 308312 316 320 333 343

PHOTOINITIATOR, 27 312PHOTOISOMERISATION, 288PHOTOLYSIS, 153PHOTON CORRELATION

SPECTROSCOPY, 224PHOTOOXIDATION, 40 129 153

274 288PHOTOVOLTAIC PROPERTIES,

38PHTHALATE, 288PHTHALOCYANINE GREEN, 65PHYSICAL AGEING, 101 135 213

309 338PHYSICAL PROPERTIES, 12 42

52 56 63 94 114 164 188 215216 236 259 266 295 324 353382

PIGMENT, 65 121 181 217 225236 237 325 399

PIPE, 52 183 277 307 329PLANT FIBRE, 82PLASMA TREATMENT, 61 69

106 230 262 298 343PLASTICISATION, 36 56 301 348PLASTICISER, 33 34 120 184 258

277 353 387 399PLASTICS WASTE, 87 211 212PLATE-OUT, 6

Subject Index


POLARISATION, 256 257 284POLARISED CONFOCAL

RAMAN MICROSCOPY, 257POLARISED FLUORESCENCE,

284POLARISED LIGHT

MICROSCOPY, 181POLARISED OPTICAL

MICROSCOPY, 13POLARISING MICROSCOPY,

168POLARITY, 50 203 339POLYACETAL, 164POLYACRYLAMIDE, 46 240POLYACRYLATE, 245 269POLYACRYLIC, 249 343POLYACRYLIC ACID, 46 172 342POLYACRYLIC IMIDE, 387POLYACRYLONITRILE, 33 79

119 342POLYALPHA-

METHYLSTYRENE, 153POLYAMIC ACID, 355POLYAMIDE, 33 56 57 79 125

164 168 192 199 207 225 231309 331

POLYAMIDE-1010, 24POLYAMIDE-12, 159POLYAMIDE-6, 33 56 57 132 165

207 387POLYAMIDE-6,6, 17 130POLYAMIDE-IMIDE, 316POLYAMINE, 46 272POLYANILINE, 46 115POLYARAMIDE, 191 339POLYARYL ETHER KETONE,

213POLYARYLATE, 367POLYBENZIMIDAZOLE, 79POLYBENZYL

METHACRYLATE, 35POLYBIBENZOATE, 309POLYBISGLYCIDYL

METHACRYLATE, 247POLYBUTYL ACRYLATE, 156

394POLYBUTYL METHACRYLATE,

21 376POLYBUTYL THIOPHENE, 327POLYBUTYLENE

NAPHTHALATE, 98POLYBUTYLENE

TEREPHTHALATE, 164 273POLYCAPROLACTONE, 147 267

390POLYCARBONATE, 14 57 62 72

79 99 101 199 207 245 273 280309 340 356 363 367 382 398

POLYCYANATE, 11POLYCYANURATE, 317POLYDEUTEROPOLYETHYLENE,

361POLYDICYANATE, 11POLYDIMETHYLPHENYLENE

OXIDE, 356POLYDIMETHYLSILOXANE,

140POLYDISPERSITY, 29 35 127 137

204 224 325 335 356POLYEPICHLOROHYDRIN, 390POLYEPOXIDE, 10 20 32 36 47

62 68 144 145 149 151 157 161178 179 182 199 200 222 249255 269 272 282 292 305 309312 320

POLYESTER RESIN, 199 204 288POLYESTER-URETHANE, 114POLYESTERIMIDE, 355POLYETHER, 54 66 158 235 238

242 384 398POLYETHER SULPHONE, 75

125 151 356POLYETHER-ETHERKETONE,

54 79 126 213 295 315POLYETHER-URETHANE, 90POLYETHERETHERKETONE, 79

126POLYETHERIMIDE, 64 79 98 192

296 367 387POLYETHERSULPHONE, 75 125

151 356POLYETHYL ACRYLATE, 58POLYETHYL METHACRYLATE,

390POLYETHYLENE, 42 52 56 57 60

61 63 65 79 87 91 92 99 102107 109 112 128 132 139 143146 148 154 157 164 168 181186 188 195 199 207 212 214216 225 249 256 260 263 266267 283 293 307 315 324 325344 348 357 361 365 366 368370 372 373 386 392 393 398400

POLYETHYLENE GLYCOL, 46233 310 369 378

POLYETHYLENE GLYCOLTEREPHTHALATE, 26

POLYETHYLENENAPHTHALATE, 387

POLYETHYLENE OXIDE, 125154 235 337

POLYETHYLENETEREPHTHALATE, 2 12 2639 40 57 63 64 74 76 79 106117 118 131 136 157 164 168

207 212 214 257 261 263 266269 283 293 309 323 336 357358 382 388 398

POLYFLUOROETHYLENE, 79164 180 279 296

POLYHYDROXYBUTYRATE, 59POLYHYDROXYBUTYRIC

ACID, 246POLYHYDROXYETHYL

METHACRYLATE, 172 248POLYHYDROXYKETONE, 349POLYHYDROXYSTYRENE, 77

367POLYIMIDE, 5 23 79 196 199 320

355POLYIONENE, 57 276POLYISOCYANATE, 9POLYKETONE, 54POLYLACTIC ACID, 267POLYMERIC FLAME

RETARDANT, 218 273POLYMERIC MOULD RELEASE

AGENT, 202POLYMETHACRYLATE, 45 245

398POLYMETHACRYLIC ACID, 15

141POLYMETHACRYLONITRILE,

141POLYMETHYL

METHACRYLATE, 14 21 116132 137 141 159 166 178 204219 220 221 224 229 240 241284 285 289 299 301 304 314319 335 338 343 363 375 382384 394 397 398

POLYMETHYLENE OXIDE, 79POLYOL, 84 110POLYOXYETHYLENE, 154POLYOXYMETHYLENE, 79POLYPHENYLENE, 398POLYPHENYLENE ETHER, 79

152 220 367POLYPHENYLENE OXIDE, 79

152 220 357 367 394POLYPHENYLENE SULPHIDE,

79 170 296 320 328POLYPHENYLENE

TEREPHTHALAMIDE, 339POLYPHENYLMETHACRYLATE,

367POLYPHENYLSULPHONE, 79POLYPROPYLENE, 31 41 57 59

79 87 88 91 102 104 109 112118 123 128 129 132 133 168171 183 188 205 206 207 212214 249 264 281 284 289 293329 330 370 380 381 398

Subject Index


POLYPROPYLENE GLYCOL,334

POLYPROPYLENE GLYCOLMALEATE, 288

POLYPROPYLENE OXIDE, 103POLYPYRROLE, 46POLYSTYRENE, 14 21 35 46 48

57 58 79 82 85 87 118 141 153156 159 160 164 166 203 207212 214 220 230 245 278 290299 304 308 315 334 351 363367 375 382 394 395 398

POLYSULPHONE, 75 79 99 125331

POLYTETRAFLUOROETHYLENE,79 164 180 279 296 363

POLYTETRAMETHYLENEOXIDE, 384

POLYTHIOPHENE, 38POLYURETHANE, 19 66 79 80 84

89 110 157 158 163 169 187199 207 255

POLYVINYL ACETATE, 79 199209 220 268 270 367 394

POLYVINYL ALCOHOL, 1 46 5157 284 342

POLYVINYL CARBAZOLE, 162POLYVINYL CHLORIDE, 6 7 17

57 79 87 108 141 145 146 167184 194 201 207 212 214 227228 254 262 315 326 353 374385 392 394

POLYVINYL ESTER, 320POLYVINYL METHYL ETHER,

363POLYVINYL PHENOL, 77 367POLYVINYL PYRROLIDONE, 46

77 248 250 340POLYVINYLBENZENE, 79 85 87

118 153 212 290 315POLYVINYLCARBAZOLE, 162POLYVINYLIDENE CHLORIDE,

57 168 387POLYVINYLIDENE FLUORIDE,

12 79 277 390POLYVINYLPYRROLIDONE, 46

77 248 250 340PORE SIZE, 50 241 285 319 375POROSITY, 50 126 142 203 241

285 319 367 375POSITRON ANNIHILATION

LIFETIME SPECTROSCOPY,19 99 338 367

POST-CONSUMER, 195 214 266373

POTABLE WATER, 183 307POTASSIUM BROMIDE, 262 271POWDER, 126 175 194

POWDER COATING, 222PRE-TREATMENT, 176 197 215

223 351PRECIPITATION, 35 266PRESSURE, 50 56 171 194 206

222 236 395PRINCIPAL COMPONENTS

ANALYSIS, 216PROBE, 179 339 382PROBLEM PREVENTION, 30

181 296 303PROCESSING, 115 168 199 207

209 231 254 261 323 325 329373 388

PROPYLENE, 264PROPYLENE COPOLYMER, 18

22 69 102PROPYLENE-ETHYLENE

COPOLYMER, 69 274 370PROTECTIVE COATING, 217

255PROTON MAGNETIC

RESONANCE, 265 291 314388

PROTON SPIN RELAXATION,209 268

PULSED NMR, 272PURITY, 120 192PYROLYSIS, 4 75 83 87 119 192

194 212 234 270 273 296 303374 380 392

PYROLYSIS GASCHROMATOGRAPHY, 4 96107 132 198 218 221 232 250270 392

PYROLYSIS-IRSPECTROPHOTOMETRY, 4

PYROLYSIS MASSSPECTROMETRY, 4 192

QQUALITATIVE ANALYSIS, 195QUALITY, 183 311 361QUALITY CONTROL, 67 131 329

347 353 357 386QUANTITATIVE ANALYSIS, 102

171 179 184 195 221 278 373QUENCHING, 101 117 135 261

363

RRADIATION CURING, 269RADIO FREQUENCY

DISCHARGE, 343RADIOLYSIS, 4RAMAN SPECTROSCOPY, 16 27

30 33 42 47 69 70 108 109 129140 151 168 182 212 214 215216 256 257 263 281 284 288293 300 342 346 365 369 393

RAPID SCAN, 344 345REACTIVITY, 151 274 388 392REARVIEW MIRROR, 67RECLAIM, 289RECOVERY, 319RECRYSTALLISATION, 54 136

309 332RECYCLABILITY, 57 88 266 387RECYCLATE, 64 91 122 195 329

373RECYCLING, 39 57 64 88 91 122

128 165 195 211 212 231 266373 387

REFLECTANCESPECTROSCOPY, 257 343

REFRACTIVE INDEX, 1 106 190200 229 292 375

REFRIGERATOR, 80REGRESSION ANALYSIS, 144

214 215 216 224 345REINFORCED PLASTIC, 13 17

36 79 81 90 100 134 141 176178 179 182 196 197 199 202211 231 234 271 281 288 296318 320 333 339 357 377

RELATIVE HUMIDITY, 44 56 57309

RELAXATION, 74 282 287 290309 363

RELAXATION MAP ANALYSISSPECTROSCOPY, 377

RELAXATION SPECTRA, 325RELAXATION TIME, 209 291

340RELAXATION TRANSITION,

290RELEASE AGENT, 202REPEATABILITY, 347REPRODUCIBILITY, 6 46 347

375RESIDENCE TIME, 266 325 357RESIDUAL ADDITIVE, 221RESIDUAL CATALYST, 129RESIDUAL STRESS, 67 316RESOLUTION, 50 118 229RETENTION TIME, 119 222RETENTION VOLUME, 143 375REVERSE OSMOSIS, 97REVERSE-PHASE

CHROMATOGRAPHY, 50 195233

REVIEW, 13 55 59 71 79 107 199205 212 283 284 310 350 363364 365 367 372 377 383 387

Subject Index


390 391 396RHEOLOGICAL PROPERTIES,

10 20 29 41 46 73 149 161 163217 266 295 324 325 338 354

RHEOMETRY, 10 324 325RHEOPHOTOACOUSTIC

SPECTROSCOPY, 249ROPE, 281ROTATING FRAME, 209 268 340ROUND ROBIN TEST, 173

SSAMPLE PREPARATION, 13 72

123 124 207SAMPLE SIZE, 72 124 143SAMPLING, 13 71 72 123 124 207

233 351SAN, 110 147 207 220 284 315

345SATURATED POLYESTER, 26 49

106 114 204 229 267 322 336367 376 388 398

SCANNING ELECTRONMICROSCOPY, 2 5 6 13 59 6162 63 82 98 108 129 181 202231 289 316 324 358

SCANNING PROBEMICROSCOPY, 59 179

SCISSION, 4 152 274 380SCRAP POLYMER, 122 128 214

231SEALANT, 247SEALING, 387SEAT, 274SECONDARY AMINE, 36 151SECONDARY ANTIOXIDANT,

93SECONDARY ION MASS

SPECTROSCOPY, 13 121 178202 312

SECONDARY STABILISER, 228SEMICONDUCTOR, 321SEMICRYSTALLINE, 102 106

122 207 213 235 315SENSITIVITY, 118 291SENSOR, 20 292SEPARATION, 35 55 97 105 128

243 341 351 370 375 384SEQUENCE ANALYSIS, 50SHEAR, 9 178 182 324 325 333SHEET, 186SHEET MOULDING

COMPOUND, 202 211SHELF LIFE, 57 311 387SHELLAC, 232 352SHIFT FACTOR, 209SIDING, 385

SILICA, 6 21 40 45 46 90 203 289319 375

SILICA GEL, 241 319SILICATE, 65 81SILICONE POLYMER, 204 284SIMULATED BODY FLUID, 34SIMULATION, 34 134 149 323

362 367SIZE EXCLUSION

CHROMATOGRAPHY, 28 2934 35 40 50 52 55 60 97 102103 108 112 114 116 158 166204 229 239 240 243 299 314322 334 375 381

SIZING, 176SMALL-ANGLE, 117 291 354SMOKE EMISSION, 76 150 173SOFTENING TEMPERATURE,

179SOFTWARE, 67 195 344SOL-GEL, 53SOLAR ENERGY

APPLICATION, 38SOLID STATE, 193 209 268 283

291 300 340 359 389SOLUBILITY, 56 79 90 97 114

115 160 372 375SOLUTE, 50 235 382SOLUTION, 21 46 55 77 115 116

130 178 224 268 291 351 367389

SOLUTION CASTING, 94 262367

SOLUTION VISCOSITY, 396SOLVENT, 21 29 35 56 113 124

130 185 203 210 235 259 261266 285 349 360 366 369 375388

SOLVENT EXTRACTION, 266331

SOLVENT PERMEABILITY, 56SOXHLET EXTRACTION, 112SPECIFIC HEAT, 20 122 207 309

324 354SPECIFIC VOLUME, 18SPIN-PROBE ANALYSIS, 45SPIN RELAXATION, 209 268 300SPOILAGE INDICATOR, 311STABILISER, 3 40 41 66 86 183

184 201 225 228 288 372STABILITY, 24 26 57 85 126 163

196 228 266 267 269 295 317324 377

STANDARD, 120 183 184 392STAR-BRANCHED, 35STARCH, 112 267 348STARCH POLYMER,STATIC HEAD SPACE GAS

CHROMATOGRAPHY, 71STATIONARY PHASE, 50 203

235 375STEEL, 223 341STEP-SCAN PHOTOACOUSTIC

SPECTROSCOPY, 344STEREOREGULARITY, 168STERIC EXCLUSION

CHROMATOGRAPHY, 41STERILISATION, 42 393STORAGE, 309 311STORAGE TIME, 311STRAIN, 315 325 365STRENGTH, 9 167 269 315STRESS, 67 168 182 281 289 315

316 325STRESS CRACKING, 271STRESS-STRAIN PROPERTIES,

61 231 281 325STRUCTURAL ADHESIVE, 62STRUCTURAL ANALYSIS, 168STRUCTURE-PROPERTY

RELATIONSHIP, 209 269 389STYRENE, 199 278 288STYRENE-ACRYLONITRILE

COPOLYMER, 72 110 147 207220 284 315 345

STYRENE COPOLYMER, 28 69127 198 299 308 363 395

STYRENE-ISOPRENE-STYRENE BLOCKCOPOLYMER, 394

STYRENE-METHACRYLICACID COPOLYMER, 81

SUB-GLASS TRANSITION, 170SUBSTRATE, 126 223 236 262

285 298SULPHUR DIOXIDE, 75SUPERCRITICAL, 39SUPERCRITICAL FLUID

CHROMATOGRAPHY, 50 372SUPERCRITICAL FLUID

EXTRACTION, 97 171 372373

SUPERCRITICAL GAS, 301SURFACE ANALYSIS, 19 30 37

38 44 58 59 62 67 69 118 175178 179 202 219 289 324 333

SURFACE AREA, 197 324SURFACE CHEMISTRY, 93 298

319SURFACE ENERGY, 52 141 217

235 277 339SURFACE PROPERTIES, 42 44

106 118 179 191 196 217 219277 308 312 360 383

SURFACE TREATMENT, 61 6281 168 176 178 182 197 205

Subject Index


223 230 262 277 298 343 371SURFACTANT, 46 65 233SURGICAL APPLICATION, 219

393SWELLING, 15 237 250 326 360SYNCHROTRON RADIATION,

291SYNTHETIC FIBRE-

REINFORCED PLASTIC, 281

TTALC, 65 318 324TAPE, 284TAPPING MODE ATOMIC

FORCE MICROSCOPY, 58TASTE, 57TEMPERATURE DEPENDENCE,

49 99 135 146 147 170 196 259269 308 336 354 364 382

TEMPERATURE GRADIENTINTERACTIONCHROMATOGRAPHY, 304375

TEMPERATURE MODULATEDDIFFERENTIAL SCANNINGCALORIMETRY, 54 78 136252 253 280 287 290 309 336

TEMPERATURE PROFILE, 67324

TEMPERATUREPROGRAMMEDANALYTICAL PYROLYSIS,273

TEMPERATURE RANGE, 207317 364 380 382

TEMPERATURE RISINGELUTION FRACTIONATION,370 396

TENSILE PROPERTIES, 40 41 6163 65 86 114 115 231 277 315333

TEREPHTHALIC ACID, 76TERTIARY AMINE, 36 151TEST SPECIMEN, 236 346 351

358TESTING, 19 43 58 59 62 71 79

96 108 112 120 123 124 134145 174 182 183 184 185 195206 208 254 255 270 288 293304 315 321 329 332 345 347357 363 365 379 382 398

TETRAHYDROFURAN, 29 35240 241 319 395

TEXTILE APPLICATION, 371THERMAL AGEING, 88 152THERMAL ANALYSIS, 7 20 26

36 54 56 67 78 83 92 95 110

133 134 144 147 149 154 155170 179 186 187 189 207 245252 258 267 269 270 305 309313 324 325 367 377 383 386394

THERMAL CONDUCTIVITY, 80179 309 324 377

THERMAL DEGRADATION, 2326 29 75 76 83 85 152 160 163189 192 194 196 244 258 266273 318 325 380 381

THERMAL DIFFUSIVITY, 179324 394

THERMAL FIELD-FLOWFRACTIONATION, 35

THERMAL HISTORY, 57 135 136207 245 254 262 287 309

THERMAL IMAGING, 67THERMAL INSULATION, 80 276THERMAL MECHANICAL

ANALYSIS, 196 377THERMAL RELAXATION, 282

290THERMAL RESISTANCE, 196THERMAL STABILITY, 11 24 26

57 85 126 163 196 228 266 267269 295 317 377

THERMAL TRANSITION, 56 78220 282 290 309

THERMAL VOLATILISATIONANALYSIS, 189

THERMALLY STIMULATEDCURRENT, 323 377

THERMOANALYTICAL, 348THERMODYNAMIC

PROPERTIES, 21 90 122 155169 172 220 235 290 339

THERMOGRAM, 36 67 323 348370

THERMOGRAVIMETRICANALYSIS, 2 8 12 15 17 23 2426 29 48 82 83 85 93 94 98 146152 163 164 189 192 194 196211 228 231 244 258 267 269295 296 316 317 318 326 330347 348 377 380 381 398

THERMOLYSIS, 189THERMOMECHANICAL

DEGRADATION, 266THERMOMECHANICAL

PROPERTIES, 179 269THERMOOXIDATIVE

DEGRADATION, 41 94 152269 348

THERMORHEOLOGICALPROPERTIES, 338

THICKNESS, 27 56 62 67 168 179236 255 257 263

THIN LAYERCHROMATOGRAPHY, 97 399

TIE LAYER, 168TIME, 54 61 94 135 209 223 253

261 268 277 289 317 338 354394

TIME DEPENDENCE, 125 196360

TIME OF FLIGHT, 103 127 137158 159 166 178 202 204 229310 312 322 335 356 376

TIME RESOLVEDSPECTROSCOPY, 170

TITANIUM DIOXIDE, 40 65 217237 325

TOLUENE, 56 185 241 261 319TOTAL ORGANIC CARBON, 183TOXICITY, 173 195TRACE ELEMENT, 177TRANSITION PHENOMENA,

254TRANSITION PROPERTIES, 203

269 340 354TRANSITION TEMPERATURE,

179TRANSMISSION ELECTRON

MICROSCOPY, 2 5 13 59 6382 108 129 181 213 289 331358

TRANSMISSIONSPECTROSCOPY, 234 292 362

TRANSPARENCY, 57 236 323TRANSPORT PROPERTIES, 56

115TRIAZINE, 40TRICHLOROBENZENE, 29TRICHLOROMETHANE, 29TRIETHYLAMINE, 298TRIFLUOROACETIC ACID, 388TROUBLESHOOTING, 30 181

296 303TWO-DIMENSIONAL, 55 58 209

233 242 275 283 344 345 364365

UUHMWPE, 260 393ULTRA-HIGH RESOLUTION

SPECTROSCOPY, 363ULTRASONIC, 112 126 272ULTRAVIOLET ABSORPTION,

229 274ULTRAVIOLET CURING, 27 269

349ULTRAVIOLET DEGRADATION,

16 19 196ULTRAVIOLET IRRADIATION,

Subject Index


19 40 44 196ULTRAVIOLET RESISTANCE,

57 196ULTRAVIOLET SPECTRA, 3 41

65 86 157 264 372 383 399ULTRAVIOLET

SPECTROSCOPY, 1 3 41 46 6586 115 157 288 372

ULTRAVIOLET STABILISER,225 288 399

UNIT CELL, 13 168UNPLASTICISED POLYVINYL

CHLORIDE, 254UNSATURATED POLYESTER,

82 199 204 288 333UV VIS SPECTROSCOPY, 1 46

115 288

VVACUUM DISTILLATION, 97

185VACUUM PYROLYSIS, 87 194VAPOUR PERMEABILITY, 56

168VAPOUR PHASE OSMOMETRY,

396VAPOUR PRESSURE

OSMOMETRY, 29 200 378VARNISH, 174VEHICLE BONNET, 329VEHICLE MIRROR, 67VIBRATIONAL

SPECTROSCOPY, 14 16 17 2627 30 33 36 39 42 43 47 51 6970 85 108 109 129 140 142 150151 156 164 168 172 173 182184 186 188 207 212 214 215216 225 226 230 244 256 257263 269 274 281 284 288 293297 300 318 342 345 346 353365 369 393

VINYL ACETATE, 251 270VINYL ACETATE COPOLYMER,

209 359 389VINYL ACETATE-ETHYLENE

COPOLYMER, 100 270 341359

VINYL CHLORIDE, 199 392VINYL CYANIDE, 119VINYL CYANIDE COPOLYMER,

57

VINYL ESTER RESIN, 320VINYL GROUP, 274VINYL PYRROLIDONE

COPOLYMER, 46VISCOELASTICITY, 20 219 308VISCOMETRY, 29 200 203 355VISCOSITY, 10 29 46 149 172 266

324 325 330VISIBLE SPECTROSCOPY, 1 46

115 288VITRIFICATION, 78 161 290VOLATILE CONTENT, 72 185VOLATILE ORGANIC

COMPOUND, 84 174 185 255278 321

VOLATILISATION, 72 97VOLUME FRACTION, 13 227

231 324 332 367

WWASTE, 87 122 128 211 212 266

387WATER, 39 56 61 266 360WATER ABSORPTION, 51 56 237

309WATER CONTENT, 6 51 148WATER PERMEABILITY, 56 237WATER PIPE, 307 329WATER TREE GROWTH RATE,

148WATER VAPOUR

PERMEABILITY, 56 168WAVE NUMBER, 168WAVELENGTH, 44 207 288WAX, 232WEATHERING, 44 62 86 92 222

385WEIGHT AVERAGE

MOLECULAR WEIGHT, 375WEIGHT CHANGE, 348WEIGHT FRACTION, 176 394WEIGHT GAIN, 56WEIGHT LOSS, 56 94 164 267

296 347 380WETTABILITY, 37 343WIDE ANGLE, 117 213 260WIDE ANGLE X-RAY

SCATTERING, 24WINDOW, 7WOOD FIBRE-REINFORCED

PLASTIC, 9 82 141 258

XX-RAY ANALYSIS, 6 108 129 212

231 289 328 383X-RAY DIFFRACTION, 13 41 57

83 92 95 117 213 260 277 291327 328 398 399

X-RAY FLUORESCENCE, 17 399X-RAY FLUORESCENCE

SPECTROSCOPY, 108X-RAY NEAR EDGE

ABSORPTIONSPECTROSCOPY, 358

X-RAY PHOTOELECTRONSPECTROSCOPY, 13 37 48100 121 145 167 175 176 196197 202 277 279 298 308 312316 320 333 343

X-RAY RESISTANCE, 104 279X-RAY SCATTERING, 13 24 41

57 83 92 95 117 213 260 277291 327 328

X-RAY SPECTROSCOPY, 13 3748 63 100 108 121 167 175 176196 197 202 277 279 298 308312 316 320 328 333 343 354358

XENON LIGHT, 274

YYELLOWING, 288YOGHURT POT, 278YOUNG’S MODULUS, 40 114

168 231 256 269 309 365

ZZEOLITE, 307ZIEGLER CATALYST, 102 129ZINC, 298ZINC BORATE, 359ZIRCONOCENE, 365

Subject Index


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