.~. EASTMAN

A wealth

I of, \ formulating

~ .~ ! options...

18 ~

/

~.~

;J .. ~.,..

,/

? ~

,. .~....." ~ "

. *" " ."'t.

-. :.I.~.",.'..

V\ th Eastman's spectrum of hydrocarbon resins

Hydrocarbon ResinsEastman has been a major supplier of resins for more than40 years and, worldwide, currently markets a large and diverseportfolio of tackifier resins.

We offer technology derived from hydrocarbon and rosinresins that satisfies the application requirements of thecustomer and delivers the desired value to the customer.

This guide presents physical, chemical, and applicationinformation for the most commonly used hydrocarbon resinsoriginating from our Jefferson, Pennsylvania, and Longview,Texas, manufacturing plants. Eastman also produceshydrocarbon resins at its European plant in Middelburg, TheNetherlands, and in Nanjing, China.

The products featured in this guide are suitable for use ina variety of applications, including adhesives, graphic arts,and rubber and plastic modifications.

We continue to examine worldwide market trends to determineappropriate uses for our products and guide new productdevelopment. Focusing on the requirements of major marketsas part of our long-range strategy will enable us to sustainour position as a major resin supplier.

Values in this guide are average values of typical samplesand should not be interpreted as product specifications. Forapplications requiring specific FDA clearances, please contactyour local Eastman sales representative.

Should you require samples or additional informationon these or any other products supplied worldwide byEastman, please contact your Eastman representative orone of the offices listed on the back cover.

Contact your Eastman representative at:Corporate HeadquartersTelephone:U.S.A.and Canada, 800-EASTMAN(800-327-8626)Fax: (1) 423-229-1193

Other locations

Telephone: (1) 423-229-2000Fax: (1) 423-229-1193

2

...:: ...(.,

.f .f .f .f .f'"

Softening point, 6 95 100 101 112(I).- R&B,O(

(alar, Gardner 3 2 2 2 2(I)c.. Tg, O( (midpoint)

- 43 47 46 58

0J.. MMAp,O( 92 94 94 96 99

a.. DA(P,O( 43 52 57 62 69- OMS(P,O( <-50 <-40 <-40 <-40 <-40faV Mz 3,800 3,500 4,950 8,250 15,900.- Mw 1,750 1,700 2,150 2,900 3,800c.. Mn 800 800 900 950 1,100

Mw/Mn 2.1 2.1 2.4 3.0 3.4

A!ipl, at. I"f.,. :A:::JII ,

Aliphatic ResinsPiccotac 1020This liquid resin is manufactured from mixed monomersof petroleum-derived origin. Piccotac1020 gives an excellentbalance of tack and adhesive properties in pressure-sensitiveand hot melt systems. This product is stabilized with 0.05%antioxidant.!

Piccotac 1095, 1098, 1100, and 1115These resins are manufactured from mixed monomers of

petroleum origin and are available in softening points rangingfrom 95° to 115°C (203° to 239°F). Because of their excellentcolor and unique ranges of molecular weight, they find utilityin adhesive, hot melt traffic marking, paint, waterproofing,rubber, paper saturation, and coatings applications. Theseproducts are stabilized with 0.1 % antioxidant.!

General Product CharacteristicsThese are neutral resins with < 1 add number and <2

saponification number. The relative degree of unsaturationcan vary, with bromine numbers ranging from 20 to 40.In general, the specific gravity as measured at 25°C (77°F)will be 0.91 to 0.97. Flash points as measured by cae are>1700e (>338°F). For specific data on individual products,refer to the product data sheet.

I:''Tetrakis[methylene(3,5di-tert-butyl-4-hydroxyhydrocinnamate)]methane.

3

4

t? ;;q- t§>

,r ,r !It\" ,rtf tf tf tf

.f .f .f .fq; q; q; q;'"

Softeningpoint, 94 105 95 50(I).- R&B,°C

Color. Gardner 3 2 3 3(I)C. !9.. °C (midpoint) 42 52 41 7

2 MMAP,°C 88 92 76 65Q. DACp,°C 47 60 38 7- OMSCp,°C -22/<-50 <-40 <-50 <-40

toU Mz 4,250 9,750 5,500 1,730.- Mw 1,900 3,200 2,200 980C. Mn 850 1,000 850 600

Mw/Mn 2.3 3.2 2.6 1.7

. =I . oJ,

Aliphaticl Aromatic ResinsPiccotac 9095, 9105, 8095, and 7050 ResinsThese resins are manufactured with varying proportions ofpetroleum-derived monomers and are available in softeningpoints ranging from 50° to 105°C (122° to 221°F). Thisvariation in aliphatic and aromatic composition accountsfor solubility differences that enable these products to beuseful in natural rubber, styrene-butadiene rubber (SBR),nitrile-butadiene rubber (NBR),block copolymers, andethylene-vinyl acetate (EVA)for hot melt systems. Theseresins are stabilized with an antioxidant.2

General Product CharacteristicsThese are neutral resins with <1 acid number and <2saponification number. The relative degree of unsaturationcan vary, with bromine numbers ranging from 15 to 30.In general, the specific gravity as measured at 25°C (77°F)will be 0.96 to 1.04. Flash points as measured by cae andSetaflash are >200oe (>392°F). For specificdata on individualproducts, refer to the product data sheet.

'\'0.10% tetrakis[methylene(3,5 di-tert-butyl-4-hydraxyhydrodnnamate)]methane.

5

...

T

6

§,y.

e e e e e'" il.f il. il.f il.f il.f

CD Softeningpoint, 103 119 141 104 113.- R&B,°C

CD Color,Gardner 12 12 12 11 12

C.T9' °C (midpoint) 43 60 84 46 55

0MMAp, °C 34 23 23 30 45a.. DACP,°C 44 10 10 10 49- OMSCp,°C 120/100 75/58 75/58 75/58 95/87

toU Mz 3,600 5,300 6,000 5,300 3,500.-C. Mw 1,400 1,800 2,300 1,800 1,300

Mn 450 550 750 550 450

MwfMn 3.1 3.3 3.1 3.3 2.8

Aromatic ResinsPicco ResinsThese products are manufactured using a mixture of petroleum-derived feed streams. Softening points range from 103°to141°C(217° to 286°F). In general, these products are lightamber to dark brown in color. With varying degrees ofaromatic content, these resins will find utility in adhesives,rubber compounding, printing inks, coatings, paints, concretecuring, waterproofing, and sealant compounds. They arecompatible in useful proportions with styrene-butadienerubber (SBR),polar elastomers, chlorinated rubber, andchlorinated paraffins. The resins contain an antioxidant.3

General Product CharacteristicsThese are neutral resins with <1 acid number and <2saponification number. The relative degree of unsaturationcan vary, with bromine numbers ranging from 5 to 20 forPicco5000 and 6000 series resins. In general, the specificgravity as measured at 25°C (77°F)will be 108 to 110. Flashpoints as measured by cae are >232°C (>450°F). For specificdata on individual products, refer to the product data sheet.

'Contains 0.75% Te7Takis[methylene(3.5 di-tert-buty/-4-hydroxyhydrocinnamate)}methane.

7

8

IV IV

f.r;: r;:'rt

'"Softeningpoint, 121 140

CV.- R&B, °C

Color, YID 11 13CVC. !9., DC(midpoint) 43 840

MMAp, DC 8 9a.. DACP,DC <-50 -44- OMSCp,°C >180 >180toU Mz 8,500 13,000.-

Mw 3,800 5,200C. Mn 1,150 1,350Mw/Mn 3.3 4.0

.

Light-Colored ResinsPlastolyn 240 and 290 ResinsThese are water-white, highly color-stable aromatic resinsmade from pure monomer feed streams. There are twosoftening point grades: 120°C (240°F) and 140°C (290°F).They are recommended for use as flow modifiers in suchpolymers as polyviny1chloride (PVC),acrylonitrile-butadiene-styrene (ABS),and block copolymers. Other applicationsinclude paints, caulking compounds, laminating and hotmelt adhesives, and coatings.

General Product CharacteristicsPlastolyn240 and 290 are neutral resins with <1 acid numberand <2 saponification number. The relative degree ofunsaturation can vary, with bromine numbers ranging from2 to 8. Specificgravity as measured at 25°C (77°F)will be1.04 to 1.10. Flash points are >232°C (>4S0°F)as measuredby COCo

For specific data on individual products, refer to the productdata sheet.

9

Pure Monomer ResinsEndex ResinsThese resins are manufactured as a copolymer of modifiedstyrenes, with softening points grades of 153°and 159°C(307°to 318°F).The specificmolecular weight and solubilityof these resins make them particularly suited to reinforcethe styrenic domains of block copolymers in hot melt andpressure-sensitiveadhesive applications.

Kristalex ResinsThese resins are water-white and highly color stable, withsoftening points ranging from 70° to 139°C(158°to 284°F).They are manufactured as a copolymer of varying ratios ofpure monomers. These aromatic resins find utility as reinforcingresins for the styrenic domain of block copolymer systems.Other uses include paints, caulking compounds, laminatingand hot melt adhesives, textile dry sizes, coatings, andplastic modification.

10

4'" " j j jj j . . .

<i; <i;'"

Softening point, 153 159 119 70 85CV-- R&B,o(

Color, GardnerCVC. Color,YID 5 8 7 7 4

0 , °C (midpoint) 99 105 60 32 41

Q. MMAp,°C 16 16 5 0 1- DACP,o( -23 -15 -35 <-50 <-50IU OMSCp,°C 129/121 149/140 >180 8/3 36/32U-- Mz 13,850 18,400 7,600 1,450 1,900C. Mw 6,950 8,600 2,800 950 1,150

Mn 2,400 2,500 800 650 650

Mw/Mn 3.0 3.6 3.5 1.5 1.8

Piccolastic ResinsThese resins are manufactured from styrenic monomers, withsoftening points ranging from 5° to 125°C(41°to 257°F).Thelow molecular weight versions are useful as plastidzers andas paper saturants. Higher softening versions are used inadhesive formulations, shoe construction, hot melt applications,investment castings, and in xerographic applications. In blockcopolymer systems,they would be compatible with the styrenicphase but would not be expected to generate significant tack.

Piccotex ResinsThese products are manufactured as a copolymer of modifiedstyrenes that result in a range of softening points from75° to 120°C (167°Fto 248°F).Aliphatic solubility decreasesproportionally as softening point increases. They are usedin coatings and adhesives as well as dry size agents and inbaking enamels.

General Product CharacteristicsThese are neutral resins with <1 add number and <2saponification number. The relative degree of unsaturationcan vary, with bromine numbers ranging from 2 to 8. Ingeneral, the spectficgravity as measured at 25°C (77°F)willbe 1.04 to 1.10. Flash points as measured by cae are >232°C(>450°F) [except for PiccolasticA5 at 166°C(330°F)].Becauseof their inherent stability, these products do not contain anantioxidant. For specific data on individual products, referto the product data sheet.

11

,§ .{' ...,§,;- lI) () .{' v. . . ..., "' '''

;; ;; ;;;§ ;§ -:..'b' -:..'b' If If If If. . 8 8 8 .f .f .f .f

4.S 4.S

100 139 5 74 126 75 91 98 118

- - 2 1 2 - -5 4 - - - 6 8 6 5

53 85 - 35 64 32 46 50 70

5 9 -6 6 13 1 3 7 11<-50 -48 <-50 <-50 -32 <-50 <-50 <-50 -3576/68 >180 - 74170 >180 -9/-10 -71-9 26/20 53/46

2,550 12,100 550 2,250 179,000 1,700 2,200 3,600 6,4001,500 4,900 350 1,300 37,400 1,100 1,350 2,200 3,500700 1,500 300 700 1,300 650 750 1,000 1,4502.1 3.3 1.2 1.9 28.5 1.7 1.8 2.2 2.4

II~ \

12

§ § §

'" qf qf qfGJ

Softening point, 19 87 95--R&B.°C

GJ Color,YID 6 2 2C.0 , °C (midpoint) -22 34 40J...

a.. MMAp,°C 64 87 84- DACP,oC 14 43 59"' OMSCp,°C <-40 -11 <-40U--C. Mz 500 1,500 1,350

Mw 350 1,000 850Mn 300 600 550Mw/Mn 1.2 1.6 1.6

ti:.,vuroYl:.l1 3t(ir:.

.lite

;\O OiTl rl" "=( - ,. ....

Hydrogenated PureMonomer Resins

Regalrez ResinsThese products are manufactured by selective hydrogenationof base resins polymerized using styrenic-based comonomers.Degrees of hydrogenation range from 30% to 100%. Softeningpoints vary from 19° to 141°C (66° to 286°F). These productsare highly UV and oxidative resistant and do not containany stabilizers.

Regalrezresins generate excellent tack and reduce sealantviscosity without significantly reducing slump resistance.Becauseof their excellent color and stability, these productsare broadly compatible with block copolymers, oils, waxes,alkyds,and plastics.Usesinclude adhesives,caulks and sealants,film, rubber, plastics, and coatings.

General Product CharacteristicsThese are neutral resins with <1 acid number and <2saponification number. (The relative degree of unsaturationcan vary, with bromine numbers ranging from 2 to 8.) Ingeneral, the specific gravity as measured at 25°C (77°P)will be 0.95 to 1.05. Plash points as measured by cae are>232°C (>450°F) except for Regalrez1018 [149°C(300°F)].Por specific data on individual products, refer to the productdata sheet.

13

;y ;y ;y ;y ;y§ § § § §,§{ ,§{ ,§{ ,§{ ,§{

124 130 141 108 102

67 72 84 55 51

92 104 109 53 2476 - 79 25 -15

<-40 -23/<-40 -10/<-40 -14/<-40 <-40

2,050 3,900 5,200 2,300 2,3501.250 2,500 3,100 1,400 1,450700 1.350 1.350 750 8001.8 1.9 2.3 1.8 1.8

V' ..........I ./ .

14

§

rr rr rr rr rr{f {f {f {f (f

?;: ?;: ?;: ?;: ?;:

'" Softeningpoint, 100 100 100 100 115

Q) R&B,°C--1:: Color,Gardner 5 1.5 - - 5

Q) Color,YID - - 18 8

c..,oC (midpoint) 44 44 44 41 61

2MMAp,°C 77 79 78 81 80c.. DACp,°C 61 68 65 69 70- OMSCp,°c <-50 <-50 <-50 <-50 <-50

toV Mz 2,450 2,550 2,300 2,150 2,600--c.. Mw 1,050 1,050 1,000 1,000 1,050

Mn 450 450 450 450 450

Mw/Mn 2.3 2.3 2.2 2.2 2.3

l1' 1r(Jg€. I f-e.. j'nS-Eas!'.'!--:1

Hydrogenated Resins-EastotacEastotac ResinsProduced from petroleum feedstockfollowedby hydrogenation,these resins are characterized by low color, low odor, excellentheat stability, and good compatibility with most polymers.Four color levels ranging from 100° to 142°C(212°to 288°F)softening points allow the selection of the most suitable resinfor a particular application. These resins are used as tackifyingresins for pressure sensitive adhesives, hot melt adhesives,caulks, and sealants.

General Product CharacteristicsThese are neutral resins with <1 acid number. The relativedegree of unsaturation is low. In general, the specific gravitymeasured at 25°C (77°F)will be 1.04. Flash points as measuredby cae are >243°C (>470°F). For specificdata on individualproducts, refer to the product data sheet.

15

4=' ;; §.... :!J :!J :!J :!J....,r ,r ,r ,r ,r ,r ,r ,r ,r

If If If If If If If If If?f ?f ?f ?f ?f ?f ?f ?f ?f

</J </J </J </J </J </J </J </J </J

115 115 115 130 130 130 130 142 142

1.5 - - 5 1.5 - - 1.5

18 8 - - 18 8 - 8

53 60 56 . 66 73 75 78 87 88

82 82 80 78 81 83 83 82 8576 75 68 72 70 77 76 74 76

<-50 <-50 <-50 <-50 <-50 <-50 <-50 <-50 <-50

2,450 2,400 2,100 2,350 2,400 2,350 2,200 2,300 2,0001,050 1,000 950 1,050 1,050 1,050 1,000 1,050 950450 450 450 500 500 500 500 500 5002.3 2.2 2.1 2.1 2.1 2.1 2.0 2.1 1.9

Neat Resin ViscosityFormulated adhesive viscosity with temperature behavioris affected by 2 main factors: 1) the viscosity of eachindividual component, and 2) the interactions betweenthe components. Although it is somewhat difficultto predict formulated viscosity without consideringcomponent interactions, there is an occasional needfor viscosity data of the resins themselves. Viscositydata for Eastman resins with temperature is highlydependent on the softening point. Figure 1 providesthe approximate viscosity of a resin with a certainsoftening point and at a certain temperature.

Neat Resin Color

All resin color measurements were conducted bydissolving the resins in a 50% toluene solution(by weight), pladng the solution in a 5 cm pathlengthcell and measuring with a colorimetric method.

Cloud Points and

Their ApplicationsCompatibilityThe performance characteristics of a resin in an adhesiveare directly related to the compatibility characteristicsof the resin in the polymer. To produce an adhesivehaving aggressive tack, for example, a resin must be foundthat has good compatibility with a suitable polymer.When a compatible resin is added in the correctconcentration to the polymer, tack will be produced.An incompatible resin may also be added to a polymersystem to impact other desirable properties, butincompatibility will not produce tack properties in apolymer system. The "fine-tuning" of adhesive systemsis often made by the addition of a resin having limitedcompatibility, thus produdng perhaps a lower tacklevel with higher cohesive strength characteristics thana fully compatible resin.

Figure 1. Viscosity vs. Temperature and Softening Point (R&B)

100,000

10,000

CLU

~"Vi0uV1

:>

1,000

1000 20 40 200 220 240 260 280 300

16

The Cloud Point ConceptSoftening point and resin concentration are familiarconcepts that are recognized by the formulator asbeing essential information, but this alone will notdetermine the influence the resin has on performance.Compatibility data is also required to complete thepicture. A convenient method to characterize resincompatibility is by determination of cloud points insuitable solvent systems. From the cloud point valuesobtained, the resin may be characterized as beingaliphatic, aromatic, or a combination of both, polaror nonpolar, and having a high or low molecularweight. Unlike rosin resins, hydrocarbon resins displaywide variation in cloud point values. Thus, the cloudpoint concept is a useful method to characterizehydrocarbon resins.

Choice of Solvent SystemsEastman uses three solvent systems to determine cloudpoints of hydrocarbon resins. They are:

.1:2 mixture of methylcyclohexane and aniline(MMAP).. 1:1 mixture of xylene and 4-hydroxy-4-methyl-2-pentanone (DACP)..Odorless mineral spirits, a mixture of various aliphaticmineral solvents (OMS).

The determination of MMAp, DACP, and OMS cloudpoints gives rise to values measured in °C. The methodis the same for all three solvent systems.

A standard weight of resin is dissolved in the solvent at

high temperature and allowed to cool with mixing. Thetemperature at which the resin begins to separate out asan extra phase is determined to be the cloud point.This may be seen in the mixture as a cloudiness in thepreviously clear solution.

Cloud Points and Resin CompatibilityFor practical purposes, the cloud points may be relatedto compatibility as follows:

.MMAP is a measurement of aromatic solubility anddetermines the aliphatic/aromatic character of theresin. The lower the MMAP value, the more aromaticthe resin.

.DACP determines the polarity of the resin due tothe highly polar nature of the solvent system. Sincespecific adhesion is related to the polarity of a resin,the DACP cloud point can be used as a specificadhesion indicator. The lower the DACP value, thebetter the specific adhesion of a resin.

.OMS-This determination is only meaningful foraromatic resins since other resin types give OMSvalues lower than -30°C (-22°F). Most laboratoriesare not equipped to operate at such low temperatures,therefore the method becomes impracticable.

The OMS value is related to molecular weight andmolecular weight distribution. In addition, OMS candetermine compatibility characteristics of a resin/polymer system, especially in ethylene-vinyl acetate(EVA)polymer. For anyone generic type of resin, thehigher the OMS cloud point, the greater the molecularweight and the molecular weight distribution. Inparticular, high OMS values can indicate the presenceof high molecular weight material (M.).

17

Cloud Point CompatibilityWhen cloud point values are graphically displayed,compatibility application windows may be determined forresin compatibility with various polymers.

Cloud Point MappingFigure 2 displays the MMAP and DACP cloud point regionsfor hydrocarbon resins. A region for rosin-derived resins isshown for comparison. Tackification regions for SBS/(SB)nand styrene-butadiene-styrene (SIS)-type block copolymershave been identified that indicate the resin type required toproduce tack in the respective polymer. It should be notedthat the pure monomer, styrene-based resins and the aromaticresins are compatible only with the styrene end block in theblock copolymer and do not produce tack in block copolymers,while the modified aromatic resins act in a similar manner torosin-derived resins, producing tack.

Figure 2. MMAP and DACP Cloud Point Regions for

Hydrocarbon, and Rosin-Based Resins

AliphaticResins

ModifiedAliphatic Resins

HydrogenatedMixed Resins

Highly Modified- AromaticResins

0

IPureMonomerResins'!AromaticResins''ModifiedAromaticResins

SBS/(SB)"ISISTackification

Region

515 TackificationRegion

Rosin-DerivedResins

-10<-30 -30 -20 -10 0 10 20 30 40 50

DACPCloud Point, 'c60 70

, Thesegroups of resinsare styrene-compatible only Theresinsdo not produce tack in block copolymers.Somemay produce tack in EVA.

18

80 90 100

120

110

100

90

80

}-i 70-c.0 60"-":::J

.2u 50"-«

40

30

20

10

Eastman Hydrogenated andAliphatic ResinsIn Figure 3, the MMAP-DACP cloud points of hydrogenated,aliphatic, and modified aliphatic hydrocarbon resins are shownas point values for individual resin grades. These values areaveraged, and in reality, there is a small spread of values foreach resin. Compatibility application windows for SBS andSIS block copolymers have been added to demonstrate theusefulness of the concept.

Figure 3. MMAP and DACP Cloud Point Values of

Eastman Hydrogenated and Aliphatic Resins

110

= ='" = e.SBS/(SB)"ISIS

Tackification Regip,n iP"".~ =

'"

CD

l'ure.MODOlJ1er..Bpsios."'.6:fdmatic'Resin"S' =....Modified Aromatic Resins

Rosin-Derived Resins

iii

-10--50 -30 -10 10 30 50

DACP Cloud Point, °C

70 90

Note: The values displayed are typical values and may not represent shipments of resin received.

19

0 Regalrez 1139. Piccotac 1115. Piccotac 1100

0 Piccotac9105. Piccotac1098

0 Piccotac 1095. Piccotac9095

0 Piccotac 1020

0 Regalrez 1085

G Piccotac8095. Regalrez1094G Eastotac H-1 OOR

(9 Eastotac H-130R

e EastotacH-142R

e Piccotac7050

110 . Regalrez1018. Regalrez 6108

CD Regalrez3102

90

Y+-'" 70c'0c...

-0:J 50.2uc...

<{

30

10

Eastman Aromatic Resins

Figure 4 displays the MMAP and OMS cloud points of aromaticand modified aromatic hydrocarbon resins. Similar to othercloud points, an individual resin type does not have a singledefinite cloud point value but a small spread. This is illustratedusing the Kristalex, Endex, Piccotex, and Picco resin ranges.

The practical usefulness of the cloud point concept may beshown by the Kristalex region. The MMAP cloud point valueshave little spread due to a constant aromaticity, whilethe OMS values vary due to differences in molecular weightdistribution. A higher OMS cloud point would indicate agreater contribution of higher molecular weight material inthe resin.

Figure 4 also shows regions of polymer compatibility for naturalrubber, SBR, and EVAcontaining 28% vinyl acetate (VA). Inaddition, there is a region of thermoplastic rubber end blockreinforcement. Resins in this region will reinforce the cohesivestrength of a thermoplastic block-copolymer-based adhesive.

Figure 4. MMAP and OMS Cloud Point Values ofEastman Aromatic Resins

48

46

44

42

40

38

36

34

32

30

28

26

~ 24+-;

"6 22Q.." 20::>8 18

~ 16-r.2 142

12

10

8

6

4

2

0-50 -25

. Picco2215 EVA(28%VA)

Incompatible

. Picco 2100

. . Endex160Endex155

0 25 50 75 100 125OMS Cloud Point, .C

150 175 200

20

Molecular Weight andWeight DistributionThe molecular weight and weight distribution of anyonegeneric type of resin has a strong influence on its compatibilityin any polymer. In general, a resin with a similar chemistryto a polymer will be compatible with that polymer onlywhen the molecular weight is not too great and the molecularweight distribution not too broad. In addition, a resinwith dissimilar chemistry may well be compatible with thepolymer when the molecular weight is low enough and itsdistribution narrow.

Gel Permeation Chromatography (GPC)GPCis a chromatographic method that measures the molecularweight and molecular weight distribution by comparing resinsamples to a polymer of known parameters. The methodinvolves using a thin metal column packed with a specialgel, having a specified volume and distribution of pore sizes.The resin is injected as a solvent solution into the columnand allowed to diffuse under pressure through the gel medium.During diffusion, the larger molecules are not captured bythe gel pores and travel quickly through the gel. The smallermolecules permeate into the pores and are thus hindered.They eventually emerge from the column after the largermolecules.

The emerging molecules are measured by special detectorsand a chromatogram is produced of the molecular weightdistribution. In theory, the chromatogram should have theform of a Gaussian curve (Figure 5), but in practice, a typicalmolecular weight distribution curve would look similarto Figure 6.

21

Figure5. Idealistic MolecularWeight DistributionCurve of a Resin

......>:en

"OJI-'"'"OJCL

Time

Figure 6. Typical Molecular Weight DistributionCurve of a Resin

I I

IMwi

......>:en"OJI-'"'"OJCL

Time

Calculationof MolecularWeight ParametersMD' Mw, Mz, and PdThe numerical results obtained are reported as Mll1Mw, M"and Pd values. These values give specific information con-cerning the molecular weight and distribution of the resin.

. Mn (Number Average)-This is a simple arithmetical aver-age and provides information about the lower molecularweight parts of the resin.

. Mw(Weight Average)-This indicates the average molecularweight of the resin. This value would be quoted when themolecular weight of the resin is requested.

. Mz(Z-Average)-This value is used as an indication of thehigh molecular weight tail in the resin, which has a verypronounced effect on compatibility and, hence, adhesiveproperties.

As mentioned on the previous page, gel permeation chro-matography is a comparative method using a known molecu-lar weight standard polymer as reference. Thus, GPC resultsmay only be compared with each other if one single refer-ence sample has been used for all resin measurements. GPCanalyses made at different times using a different referencesample will show a considerable random error, especially inthe Mz value calculation. Consequently, a spread of100/0-15% in Mz values should be regarded as normal.

.Pd (Poly-Dispersity)-This value describes the broadness ofthe molecular weight distribution and is calculated as theratio Mw/Mn; the greater the value, the broader the molecu-lar weight distribution.

22

The values of Mn' Mw,Mz.and Pdare calculatedby the following equations:

Mn = L(ni x Mi)L(ni x Mi1-1)

Mw = L(ni x Mi2)L(ni x Mi2-1)

Mz = L(ni x Mi3)L(ni x Mi3-1)

Pd = Mw/Mn

Where:ni is the number of molecules;andMiisthe massof the moleculeswith number ni.

Figure7. Illustration of MolecularWeight Distribution

Resin A..........................~.

,

'. ................. ...............~

"..............................~ ....... ...... .......................................................................................................500 molecules at 1 mg = 500

2 molecules at 250 mg = 500

Total weight = 1,000 mg

(500 x 1)+ (2 x250) = 1,000500 2 502

= 1.99 Mn

(500 X 12)+ (2 x 2502) = 125,500(500 x1) (2X250) 1,000

= 125.5 Mw

(500X13) + (2X 2503) = 31,250,500 = 249.0Mz(500X12) (2X2502) 125,500

125.51.99

= 63.07 Pd

The difference between Mn, Mw, and Mz may beillustrated by the example of two hypothetical resinsamples with the same total mass of 1,000 mg butwith a different size distribution. (See Figure 7.)

The Mn values of both resins are very similar, indicatingboth have similar low molecular weight fractions; fivehundred I-mg molecules versus four hundred I-mgmolecules.

The Mw values show large value differences, 125.5versus 4. The average molecular weight of Resin A isconsiderably influenced by the two, very large moleculespresent; while that of Resin B is less affected by the

large, 6-mg molecules.

The Mz value of Resin B is close to its Mw value. Thus,

the system has little high molecular weight material.Resin A has a very high Mz value and thus a large massof high molecular weight material.

Resin B

w:.: V:e: V:.: V:e: V:.:.......................... ... ... ... ... ..~...~...~ ~u:e:V:e:V:e:V:e:V:e:'........................'. '...~ . ' . ' . ' .~~:e:~:e:~:.:V:.:~:.:~...~...~ ~..~. ... ... ... ......8i."'.8i."'.~."'.~."'.~ .~

I=..:e:~:e:~:e:~:e:~:e:~...~...~...~...~..~:.:A:.:A:.:A:.:A:':.'400 molecules at 1 mg =400

100 molecules at 6 mg =600

Total weight =1,000 mg

(400x1)+(100X6) = 1,000400 100 500

= 2.0 Mn

(400 X 12) + (100 x 62) = 4,000 = 4.0 Mw(400X1) (100X6) 1,000

(400XP) + (100 X 63) = 22,000 = 5.5 Mz(400X12) (100X62) 4,000

4.02.0

= 2.0 Pd

The Pd value of Resin A is very large, indicating abroad molecular distribution; while the value of Resin Bshows its narrower molecular weight distributioncharacteristics.

Resin A could be described as a high molecular weight,with a very broad molecular weight distribution, resin;while Resin B has a low molecular weight with a narrowmolecular weight distribution.

Practical AspectsIt may be envisaged that both resins are of the samegeneric type, i.e., of similar chemistry. Resin B, dueto its low molecular weight together with a very lowMzvalue, would be compatible with a certain polymer.Resin A, although it has the correct chemistry to becompatible, would be incompatible. This is due tothe very high molecular weight material preventing theresin from mixing intimately with the polymer molecules.

23

Figure 8. Eastman Correlation Chart of Various Color Scales

10,000

5,0004,0003,000

2,000

1,000

500400300

200

100

- - - - - - - - - 1_~ - - - ? - - -543-------2

Iodine1,000

Dichromate

100

10

543

2504030

20

- - - - -.-

Gardner,50%Resinin Toluene

18

17

16

15141312

11

10

9

8

7

65432

Gardner, Neat16151413

12

11

109876543

NWG

WWX

XAX8

- .- - - ><C

Barrett

85

USDADEF

GH

I

K

84

83

82

10

81

M

80.5

LilyWhite

Standard White

----------------------

- - - - - - -. - - - - - - - - -

543

2

Prime White

- - - - - - - - - -+20

Water White

0.5Hunterlab b- - - - - - - - - - - - - - - - - - - - _+25

+30

NOTE: Correlations are approximate. No responsibility will be accepted for the resultsobtained by the application of this information.

Test Methods:

Dichromate: mg/1,000 ml H2SO4, H-90-2cSaybolt: ASTM D156Iodine: mg/100 ml H2O

24

Gardner: ASTM D1544-80

Hunterlab: ASTM E450USDA: R-25-4a

Yellowness Index: ASTM D1925

YellownessIndex

11

10

9

6

2

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