Livre Blanc Volume 1 Spectrophotomètrie UV-Visible et ... · Livre Blanc Volume 1 Spectrophotomètrie UV-Visible et Infrarouge « Plus de 70 pages d’applications UV-Vis et FTIR..»

Livre Blanc Volume 1

SpectrophotomtrieUV-Visible et Infrarouge

Plus de 70 pages dapplications UV-Vis et FTIR..

Shimadzu Corporation 2013

Fond en 1875, Shimadzu est un groupe multinational japonais de 3 milliards de dollars ct la bourse de Tokyo. Avec prs de 10000 employs dans le monde Shimadzu Corporation regroupe trois acti-vits principales : linstrumentation analytique et physique, le diagnostic mdical et laronautique. Prsent dans plus de 100 pays, Shimadzu est un fabricant dinstrumentation analytique et dqui-pement de contrle environnemental. En effet Shimadzu dispose dune large gamme dinstru-ments analytiques : Chromatographie liquide et gazeuse, spectromtrie de masse, une gamme complte de Maldi, des robots de prparation, spectromtrie UV-Vis, FTIR, analyse lmentaire.

Shimadzu est aussi un fabricant mondial de machines de caractrisation de matriaux et des-sais mcaniques. En effet Shimadzu offre une large gamme de machines lectromcaniques ou hydrauliques, statiques ou dynamiques, de traction, compression, flexion, pelage, cisaillement fatigue

Fond en 1968 en Allemagne, Shimadzu Europe fourni des solutions analytiques aux scientifiques europens. Aujourdhui Shimadzu Europe reprsente plus de 9 filiales et 13 distributeurs rpartis travers lEurope dont Shimadzu France, filiale de plus de 65 personnes en forte croissance depuis sa cration en 2002.

A propos de Shimadzu

Shimadzu France possde en ses locaux Noisiel (77) plusieurs showrooms reprsentant chaque gamme, dun laboratoire de prparations dchantillons et de salles de formation et de runions.Notre laboratoire vient en complment des 1500m de laboratoire disponibles notre sige eurpen bas Duisburg (Alle-magne) rcemment inuagurs.

Laboratoires de dmonstration

UV-1800Allant bien au-del des normes de la pharmacope, lUV-1800 offre un ventail de fonctionnalits compltes et conviviales. Il peut tre configur en tant quinstrument autonome ou contrl par PC.

Avec la rsolution la plus leve de sa catgorie (1 nm), il rpond aisment la rsolution de longueur donde requise.

Montage optique Czerny-Turner dans un systme compact atteignant une lumire parasite faible, une excellente rptabilit de la longueur donde et une grande stabilit de la ligne de base.

Mesurant seulement 450 mm de large, cest lun des instruments les plus compacts de sa catgorie.

Les cls USB permettent aux utilisateurs danalyser les donnes sur un PC spar en utilisant le logiciel UVProbe standard qui peut galement permettre le contrle total de linstrument.

UVmini-1240LUVmini-1240 est un instrument danalyse faible cot et trs peu encombrant.

Plage de mesure de 190 nm 1100 nm.

Largeur de bande spectrale de 5 nm.

Logiciel de contrle embarqu avec grand cran LCD.

Les oprations incluent la photomtrie, lacquisition spectrale et la quantification.

UV-3600 / SolidSpec-3700Les spectrophotomtres UV-3600 et SolidSpec UV-VIS-NIR ont t conus pour les mesures ncessitant la sensibilit la plus leve possible. Ils incluent tous les deux une technologie trois dtecteurs en transmission et en rflexion, permettant un niveau de performance maximale de lUV au proche Infra Rouge.

Plage de mesure possible de 185 nm 3300 nm (UV-3600) ou 165-3300 nm (SolidSpec-3700).

Trois dtecteurs : PMT, InGaAs et PbS.

Grand compartiment dchantillons 900x700x350 mm (SolidSpec-3700)

Le chemin optique vertical permet un positionnement horizontal de lchantillon. (SolidSpec-3700).

RF-5301Instrument de fluorescence de pointe pour la recherche et le dveloppement, les analyses de routine et lenseignement.

Gamme dynamique de mesure de fluorescence base sur la slection du dtecteur en deux tapes.

Optique double pour les mesures du spectre dexcitation et des missions, notamment lobturation et le choix de deux taux de largeur de bande et de mesure.

Gamme UV-VIS/NIRFL

UORE

SCEN

CE

UV-2600/2700Gce une toute nouvelle gnration de rseaux Low-Ray-Ligh dvelopp par Shimadzu, les spectrophotomtres UV-2600/UV-2700 vous permettront datteindre des niveaux de performance ingals en UV-Visible. Ils regroupent tout le savoir-faire de Shimadzu depuis plus de 65 ans avec un minimum dencombrement.

LUV-2600 est le systme universel quels que soient vos chantillons. Avec une linarit de 0 6 Abs et un bruit de fond infrieur 0,00003Abs, il vous permettra la mesure de tout produit, de la plus infime quantit au produit les plus opaques. Coupl notre nouvelle sphre dintgration ISR-2600Plus, il vous ouvrira les portes du Proche Infra Rouge grce une plage de mesure exceptionnelle allant de 185 1400 nm.

LUV-2700 permet danalyser vos chantillons les plus opaques et les plus absorbants. Avec son double monochromateur, il atteint une linarit maximale jusqu 8 Abs entre 190 et 900 nm, permettant ainsi de travailler sur vos chantillons sans dilutions supplmentaires.
http://www.shimadzu.fr/spectroscopie-uv-visible-nir

IRAffinityLIRAffinity est muni dun systme innovant et unique de protection de loptique. Grce un compartiment tanche muni dune membrane hydrolytique, lIRAffinity est protg de lhumidit en permanence, teint comme allum, sans aucune intervention manuelle tout au long de sa dure de vie. Ajout une optique de haute qualit, il est le spectrophotomtre FTIR le plus performant de sa catgorie.

Rsolution 0,5 cm-1 et dimensions compactes.

Rapport signal/bruit 30000:1 en utilisant une source de source cramique haute densit, et le dtecteur DLATGS temprature contrle.

AIM-8800 MicroscopeLe microscope infrarouge AIM-8800 permet un contrle ais des tapes et un rglage de louverture partir de lcran du PC.

Transmission, rflexion et rflexion totale attnue.

Louverture automatique optimise lclairage infrarouge.

Ltape X-Y automatique simplifie le positionnement de lchantillon.

Mise au point automatique et centrage automatique.

IRPrestige-21 LIRPrestige-21 offre des possibilits dextension rapides allant de linfrarouge proche,

linfrarouge moyen jusqu linfrarouge lointain.

Le systme optique unique avec des miroirs en or permet datteindre des performances de recherche comme un rapport signal/bruit de 40000:1 et une rsolution de 0,5 cm-1.

Optimisation en temps rel de linterfromtre, avec un alignement dynamique avanc.

GladiATR 10Echantillons durs

(Diamant Massif Naturel)

HATR 10Liquides, Polymres, Ptes

MiRacle 10ATR Universel

ATR

ATR Shimadzu vous propose sa gamme dATR srie 10 dernire gnration, optimise pour loptique de lIRAffinity-1. Chaque ATR est quip dune presse avec d-brayage automatique ainsi quun positionnement Plug and Play. Un capteur de pression est aussi disponible en option.

Gamme FTIR
http://www.shimadzu.fr/spectroscopie-ftir-ft-nir

Shimadzu News Article Collection

Volume 1

UV Ultra violet Visible and Near Infrared

Spectroscopy

Blank page

APPLICATION Shimadzu News 1/2011

6

Windows in the spotlight

In the Hitchcock movie RearWindow, the window open-ing onto the courtyard wasopen most of the time. In thisway, James Stewart could toleratethe summer heat of 1954 and alsosee the murder happening in hisneighbors house. But how, inthese times of global warming,can a comfortable indoor climatebe provided during the hot sum-mer months? Climate changeplaces increasingly higherdemands not only on environ-mental behavior, but also on ourway of life.

In addition to the use of air con-ditioning systems, efficient use ofbuilding materials is also helpful,and windows play a significantrole. Use of selected flat glasshelps to prevent as much heat aspossible from entering the room,while still allowing enough lightto pass.

Light transmittance in flat glass

The quality of flat glass in thebuilding industry is testedaccording to DIN EN 410: Glassin building determination ofluminous and solar characteristicsof glazing. In Japan JIS R 3106 isapplied: Testing method onTransmittance, Reflectance andEmittance of Float Glasses andEvaluation of Solar Gain Coeffi-cient. Testing includes lighttransmittance and reflectance inthe visible spectral range of 380to 780 nm, solar transmittanceand reflectance between 300 and2,500 nm as well as normal emit-tance in the 2,000 - 400 cm-1

range (5,000 - 25,000 nm as IRmeasurement).

In the examples shown here,measurements were carried outaccording to the Japanese indus-trial standard JIS R 3106. Formeasurements in the visible

Determination of the transmittance and reflectance of

Figure 1: Display of the Daylight software with calculation of results

Table 1: Instrument measurement parameters according to JIS R3106

Close to parallel

beam of light

incident from the

normal direction

The air layer is

used as the

standard sample,

and its spectral

transmittance is

taken to be 1

300 - 2,500 nm

< 300 nm, 5 nm max. 380 - 780 nm, 10 nm

max. 780 nm and higher, < = 50 nm max.

380 - 780 nm

10 nm max.

Close to parallel

beam of light

incident from the

radiation slit at

an angle not

exceeding 15

degrees

Specular reflector

of reflectance

specified by the

absolute reflec-

tance measurement

method (sample 1),

or specular reflec-

tor of reflectance

specified by

comparison with

sample 1

Close to parallel

beam of light inci-

dent from the radia-

tion slit at an angle

not exceeding 15

degrees.

Close to parallel

bundle of rays

incident from nor-

mal direction

Specular reflector

of reflectance

specified by the

absolute reflec-

tance measurement

method (sample 1),

or specular reflec-

tor of reflectance

specified by

comparison with

sample 1

IRAffinity-1 FTIR

spectrophotometer

and SRM-8000, an

accessory for spec-

ular reflection

5 - 25 m

4 cm-1

Light radiation

at an angle not

exceeding 15

degree

Aluminum-coated

mirror with

certified absolute

reflectance (float

flat glass with

vacuumdeposited

aluminum film)

Visible range Solar range

Transmittance Reflectance Transmittance ReflectanceNormal

Emittance

UV-3600 UV-VIS-NIR spectrophotometer ISR-3100 Integration sphere

(Ulbricht sphere) with three detectors

Analytical

instrument

Measurement

wavelength

range

Resolution

Incident light

conditions

Standard sample

for comparison

Close to parallel

beam of light

incident from the

normal direction

The air layer is

used as the stan-

dard sample and

its spectral trans-

mittance is taken

to be 1

7

APPLICATIONShimadzu News 1/2011

UV-VIS spectroscopy

as well as in the solar range, Shimadzus UV-3600 with theISR-3100 integration sphere wasused. The companys IRAffinity-1with a directed SRM-8000 reflec-tance unit was applied for thedetermination of the normalemittance. Both instruments canbe used in the infrared range(thermal radiation). The UV-VIS-NIR UV-3600 system covers thenear infrared (NIR) range, andthe FTIR system covers the mid-infrared range (MIR).

According to JIS R 3106, themeasurement parameters can belisted as shown in table 1.

Evaluation of results is carriedout in accordance with JIS R3106. A spreadsheet program oroptimized software can be usedfor calculation. Parameters forthe visible (te) and solar (tv)transmittance as well as re-flectance determined as pe andpv, can be listed using ShimadzusDaylight software.

The following standard valuescan be determined optionally (see table 3).

As an example, the visible andsolar transmittance and the chro-maticity values for five types ofglass were calculated according to

flat glass in the building industry according to DIN EN 410/JIS R 3106

Table 3: Tristimulus values which can be determined using the

Daylight software

Figure 2: UV-VIS-NIR spectra of glasses in transmittance: black corresponds to

Glass-0, red to Glass-1, blue to Glass-2, green to Glass-3 and violet to Glass-4

Table 2: Visible and solar transmittance for five flat glass samples with Standard Illuminant D65 calculated under an observation

angle of 2

JIS R 3106. The values are listedin table 2 and the UV-VIS-NIRspectra are shown in figure 2. TheStandard Illuminant D65 wasselected for the calculation as thisrepresents daylight according tothe CIE (International Commis-sion on Illumination). An angleof observation of 2 was selected.The results presented show just asmall extract of the determinationrange. [1][2]

[1] Shimadzu Application News No.

A396, Daylight Transmittance

Application Data of Glass Plate

[2] Shimadzu Application News No.

A404, Glass Plate Analysis in

Accordance with JIS R 3106

1/nm

T%

-9,112

0

50,000

100,123

300 500 1,000 1,500 2,000 2,100

x

1

2

3

4

5

86.756

36.167

31.559

9.164

8.108

90.672

29.913

27.223

1.527

1.389

85.830

28.586

25.912

9.124

8.267

90.672

29.912

27.223

1.525

1.387

98.478

60.079

54.484

48.573

44.027

GLASS-0

GLASS-1

GLASS-2

GLASS-3

GLASS-4

Sample number te tv y z File name

te, pe dte, tpe

tv, pv

dtv, dpv

User X, Y, ZdX, dY, dXx, ydx, dydWL

Daylight transmittance, reflectance (JIS R 3106)Difference of daylight transmittances, reflectances (JIS R 3106)Visible light transmittance, reflectance (JIS R 3106, JIS Z 8722)Difference of visible light transmittances, reflectances (JIS R 3106, JIS Z 8722) Calculated by user defined weighted factor fileTristimulus Value X, Y, Z (JIS Z 8722)Difference of X, Y, ZChromaticity Coordinates x, y (JIS Z 8722)Difference of x, yDominant Wavelength dWL (JIS Z 8701)

We will gladly send you further information. Please note

the appropriate number on your reply card or order via the

News App resp. News WebApp. Info 392


4

Photons and holes are termscommonly used in photovoltaics.Rays of sunlight (photo-effect)hitting a solid-state body such asa solar cell, will release positiveand negative charge carriers. Asolar cell contains p-conductingand n-conducting semiconductorlayers, resulting in p-n transitionswhere these two layers meet.

Free electrons and holes becomeactivated based on their chargedifferences. When p-n-transitionsoccur, electrons and holes formpairs. As a result, the n-dopedarea acquires a positive chargedue to lack of electrons. At the

of solar energy due to back-reflection from the surface (bycomparison: a simple glass sur-face already reflects 4 % of theincident energy).

The finite supply of fossilfuels and high costs ofenergy as well as CO2emissions have recently brought awell-known alternative technolo-gy back into prominence: photo-voltaics, which harvests energyfrom the sun. Photovoltaics con-verts solar energy instantly intoelectrical energy.

An important component of solarenergy technology is silicon,which is one of the most abun-dant chemical elements. Underthe influence of solar radiation,silicon exhibits electrical proper-ties and acts as a semiconductor.

same time, the p-doped area islacking positively charged holesand acquires a negative charge.Between these oppositely chargedareas an electrical field is generat-ed which becomes stronger asmore electron-hole pairs areformed.

Sunlight activates the flow ofelectrons, which is the first steptowards generation of an electri-cal current. A voltage can betapped off the electrodes. Figure 1shows a schematic representationof a solar cell.

Anti-reflection film increasesefficiency

Although the efficiency of a solarcell has often been the subject offierce criticism, the performanceof solar cells has been optimizedcontinuously. One step in theoptimization of solar cells is toensure that they can accommo-date all incident solar irradiation.High conversion yields can beobtained by coating the solar cellsurface with an anti-reflectionfilm. This film prevents any loss

Figure 1: Configuration of a solar cell

Figure 2: Schematic representation of the polarization levels of non-polarized and

polarized light

Figure 3: Schematic representation of the planes of incidence of p-polarized and

s-polarized light

Figure 4: Shimadzus UV-3700 spectro-

photometer, a UV-VIS-NIR system with

three-detector configuration and large

sample compartment

This application note discussesthe reflectance measurement ofthe anti-reflection coating of aSi3Ni4 (silicon nitrate) solar cell.In this study, the spectrum in theUV-VIS-NIR range (300 2200nm) was investigated using themethod of absolute specularreflectance.

5


0.0

20.0

40.0

60.0

80.0

100.0

300.0 500.0 1000.0 1500.0 2000.0

nm

R %

0.0

20.0

40.0

60.0

80.0

100.0

300.0 500.0 1000.0 1500.0 2000.0

nm

R %

Figure 7: UV-VIS-NIR spectra recorded using s-polarized light and specular

total reflectance

Figure 8: UV-VIS-NIR spectra recorded using p-polarized light and absolute

specular total reflectance

Figure 5: Absolute specular reflec-

tance attachment with variable angle

of incidence

Figure 6: The inner compartment of

the UV-3700 with built-in variable abso-

lute reflectance attachment. The solar

cell sample is placed in the holder.

Absolute reflectance is that partof specular reflectance withoutthe contribution of diffuse orstray-light phenomena. In thisseries of measurement, incidentangles of 5 60 were used.When carrying out this measure-ment technique under higherangles of incidence, polarizationeffects can occur. A polarizer wastherefore used to generate p- ands-polarized light. Depending onthe angle of incidence and therefractive index, non-linear influ-ences on the reflectance resultswere observed.

The component of light on theplane of incidence is called p-polarized light (parallel-polar-ized); s-polarized light (vertical-ly-polarized) strikes the plane ofincidence vertically. The plane ofincidence is the direction of theincident light and the line per-pendicular to the reflective sur-face.

For small angles of incidence,hardly any difference in reflec-tion with respect to polarizationcould be observed. For largeangles of incidence the influenceof polarization increased and apolarizer should therefore beused during measurement.

Highest sensitivity using the UV-3700

Using this reflectance technique,it is possible to find the optimumangle of solar radiation incidenceon a silicon surface in order toobtain the highest conversionyield for the solar cell. The fol-lowing measuring results wereobtained using Shimadzus UV-3700. Its three-detector-configu-ration enables highly accurateand sensitive measurement in the

300 2200 nm measuring range.The large sample compartment ofthe UV-3700 facilitates the inte-gration of a variable reflectanceattachment with integrationsphere.

Measurements were carried outusing s- and p-polarized light.The measured results which weredependent on the angles of inci-dence, are shown in Figures 7 and 8.

The following angles of incidencehave been selected for measure-ments and the associated spectraare indicated according to linecolour: green 5, red 15, blue30, black 45 and purple 60.

The results for the s-polarizedlight and the p-polarized light areshown in the above figures. Theleast amount of reflection occursin the range of 500 to 600 nm.From the measured results it isapparent that the anti-reflectionfilm minimizes reflection mainlyin the visible wavelength range.

We will gladly send you further informa-

tion. Please note the appropriate number

on your reply card. Info 347

CNT1.3 - 1.4

45

Looking into tubes with spectroscopy The world of carbon nanotubes 2

What is purging? POC measuring process 5

Low flows high potential prominence Nano-pump 8

Analysis of primary amino acids 12

Highly efficient Determination of environmental contaminants 14

A global challenge State-of-the-art water analysis 16

How paper tells medieval stories Antiquarian books as a source of environment historical data 18

FTIR spectrometry in traditional Chinese medicine 19

Antarctic expedition 10

Frost & Sullivan awards Shimadzu Europa 9

Silver Jubilee Medal 2008 for Luigi Mondello 17

Installation kit for HPLC systems 27

Teddy bears and Jelly bears Universal testing machines 20

One box for all purposes New valve techniques for GC 22

More is better MOC-120H 24

prominence UFLC-XR in MS software 27

A matter of taste Determination of dimethyl sulfide in wort 25

European Symposium on Atomic Spectroscopy 26

Dinner for all 40 years Shimadzu Europe 28

APPLICATION

INTERNAL

ANNIVERSARY

CONFERENCE

READ FOR YOU

PRODUCTS

TELEGRAM

The best in class FTIR system IRAffinity-1: MultipleChoice.

Looking into tub


2

What are nanotubes?

A nanotube is a cylindrical struc-ture with a diameter within thenanometer-range and several millimeters in length. There aretwo main types: the SWNT (sin-gle-walled nanotube) and theMWNT (multi-walled nanotube).Nanotubes belong to the familyof fullerenes; they are cylindricaland typically capped with a half-sphere at one end of the cylinder.The known and various manifes-

The world of carbon nanotubes

Carbon nanotubes (CNTs)are tube-like structures thatconsist entirely of carbon(Figure 1). They were dis-covered in 1991 by SumioIijima.

Depending on the struc-ture of the tube, carbonnanotubes are eithermetallic or semiconducting. Dueto these two important character-istics, CNTs are of great interestto the industry.

Figure 1: Picture of a nanotube

Table 1: Comparison of CNT with steel properties

PropertyDensity [g/cm3]Tensile strength [GPa]

Steel7.82

IMPRINTShimadzu NEWS, Customer Magazine of Shimadzu Europa GmbH, Duisburg

Publisher:Shimadzu Europa GmbHAlbert-Hahn-Str. 6 -10 D - 47269 DuisburgPhone: +49 - 203 - 7687- 0 Telefax: +49 - 203 - 766625Email: [email protected]: www.shimadzu.eu

Editorial Team:Uta Steeger Phone: +49 - 203 - 7687- 410 Ralf Weber, Angela Bhren

Design and Production:m/e brand communication GmbH GWADsseldorf

Circulation:German: 7,600 English: 22,000

Copyright:Shimadzu Europa GmbH, Duisburg, GermanyNovember 2008

Windows is a Trademark of Microsoft Corporation

es with spectroscopy

3


of the excellent mechanical prop-erties of CNTs is the density ofapproximately 1.3 1.4 g/cm3 incombination with an extraordi-nary tensile strength that exhibitsa 135-fold better density/tensilestrength ratio than steel (Table 1).

For the electronics industry, theelectrical charge density as well asthe thermal conductivity, whichat room temperature amounts tovirtually twice that of diamond(CNT 6000 W/m*K and diamond3320 W/m*K), are of interest.

The CNT optical transitionsoccur in the following sequence,as seen from the low energeticside of the spectrum: semicon-ductor semiconductor metal.On decreasing nanotube diame-ter, the absorptions will shift tothe higher energetic side of thespectrum. At increasing diameter,

Figure 2: Various manifestations of carbon (carbon allotropes): (a) diamond,

(b) graphite, (c) lonsdaelite, (d) C60, (e) C540, (f) C70, (g) amorphous carbon and

(h) carbon nanotube

Figure 3: Depending on the rolling mechanism, nanotubes with either metallic pro-

perties (armchair) or semiconductor properties are formed. During rolling the point

labelled (0,0) will join with another point (10.0, 10.5 or 10.10). The names armchair

and zigzag originate from the way the C-atoms are rolled along the axis connecting

the two points (emphasized atoms).

the absorption will result inbroader absorption bands.

Spectroscopy visualizesenergy states

Energy states can be visualizedwith the aid of UV-VIS/NIRspectroscopy. Several examples ofdifferent CNT-states are shownbelow:

spectroscopy is the method ofchoice for the analysis of thethree signals, as these will be displayed very sharply. This isattributed to the nature of theCNTs and is also described asVan Hove singularities.

A typical SWCNT spectrum isshown in Figure 4 (Page 4). M1 isthe metallic property and S1 andS2 represent the semiconductorproperties. Figure 5 shows thespectrum in the nanometer scale,whereas Figure 4 is expressed inelectron Volts (eV). Typically, the

signals are found between 0.5 and1.2 eV for SWCNTs. This corre-sponds to a tube diameter of 0.8up to 1.5 nm.

tations of carbon, the origin ofCNTs, are shown in Figure 2.

A carbon nanotube is formedwhen a graphene layer joinstogether. Depending on the waythe hexagonal graphene networkis rolled up, CNTs with eithermetallic or semiconductor char-acteristics are formed. The threedifferent variants are clearlydefined. They are called zigzag,chiral or armchair and displaydifferent characteristics. The arm-chair type, for instance, is alwaysmetallic.

Of interest to the electronics industry

In theory, metallic nanotubespossess an approximately 1000-fold better electrical currentdensity when compared withmetals like silver or copper. One


4

The CNTs are assembled accord-ing to various procedures. Twoprocedures for the assembly HiP-Co (high-pressure CO conver-sion) (Figure 6) and CoMoCAT(Figure 7) result in different spec-tra.

At the University of Oklahoma,USA, the catalytic CoMoCATprocedure was developed inorder to manufacture SWCNTsin high yields (Figure 7). Thespectra shown were recordedusing Shimadzus SolidSpec-3700,whereas the instrument wasequipped with an integratingsphere.

Another example is transmissionspectroscopy carried out in solu-tion using the UV-3600. Thespectrum of the liquid sample CNT diluted in N-methyl-2-pyrrolidon (NMP) is shown inFigure 8. The fluid matrix exhib-its better stray light behavior.This leads to improved quality ofthe spectra and higher detectionlimits in the UV-VIS/NIR meas-uring range.

The Van Hove singularities canbe identified clearly in the spec-trum. The signals and the conver-sion to electron volts are listed inTable 2.

The suspension consisting ofCNT and NMP was filled into a10 mm quadratic quartz cell. The pure NMP solvent was usedas reference and was filled intothe reference position of the Shimadzu UV-3600.

Literature and references

1. Recommended practice guide for

Nano Carbon tubes characterization,

Michael E. Itkis, Robert C. Haddon,

University of California

2. Mr. Iijima is Professor in Meijo

University and belongs to AIST and

NEC Corporation

Instrument and sample preparation

Instrument: UV-3600 with threedetectors

Slit width: 1 nmScan speed: mediumCell: two 10 mm quartz

cells

The measurement took place inthe range of 350 to 1700 nm asthe dilution agent exhibits astrong absorption in the wave-length range > 1700 nm.

Conversion into electron volts isnecessary for the determinationof the CNT diameter. The DOS(electronic density of states) canbe calculated according to fixedparameters:

S1 = 2a/dS2 = 4a/dM1 = 6a/d

Where a = carbon-carbon bondlength (nm), = energy in the porbitals (~2.9 eV) and d = SWNTdiameter.

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.5 1.0 1.5 2.0 2.5 3.0 3.5

Photon Energy [eV]

Abs

0.000

0.100

0.200

0.300

0.400

0.500

190.0 500.0 1000.0 1500.0 2000.0 2500.0

Wavelength [nm]

Abs

Figure 4: Typical spectrum of an SWCNT (single-wall carbon nanotube) wherein the

absorption is plotted against the energy scale

Figure 5: UV-VIS/NIR spectrum of an SWCNT dispersed onto a quartz substrate.

Measurement was carried out using an integrating sphere.

[eV]0.86130.94931.06211.15061.2486

[nm]1439.513061167.41077.6993

CNT 1-D

Figure 6: Representation of the

UV-VIS/NIR spectrum of a HiPCo (high-

pressure carbon monoxide) measured

using Shimadzus UV-3700

Figure 7: Representation of the

UV-VIS/NIR spectrum of a CoMoCAT

measured using Shimadzus UV-3700

Table 2: Analytical wavelength of the

carbon nanotube (CNT) in the UV-VIS/NIR

range

Figure 8: Representation of the CNT

spectrum in the NMP matrix measured

using Shimadzus UV-3600

0.00

1.50

0.75

350.0 1075.0 1800.0

nm

Abs

0.00

0.03

0.01

350.0 1075.0 1800.0

nm

Abs

0.2278

0.5000

1.0000

1.5381

305.19 1000.00 1700.00

nm

Abs

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4

Mineral water in a diffe

With 130 liters consump-tion per capita and peryear in Germany, theyare an important food source inour daily nutritional intake, sup-plying important minerals andtrace elements, both sparklingand still mineral waters. Theirlabels are their trademarks andbusiness cards as they containspecific information on the con-tents. These labels testify to thequality of the mineral waterspring where the water comesfrom. Interestingly, the labels donot mention the actual test dateof the water, as the informationcannot be printed fast enough onthe labels. When checking theimprints on the bottles, one findsa date that differs by severalmonths from the mineral analysisof the well itself.

Drinking water is one of themost tested food sources. It issubject to continuous monitoringaccording to national and Euro-pean drinking water ordinances.Monitoring includes, among oth-ers, the analysis of minerals andtrace elements. These analyses are

usually carried out using atomicabsorption spectroscopy or ICP-OES methods. The total organiccarbon content is determinedusing TOC methods; nitrate andnitrite content can be determinedusing UV spectroscopy. Manyfoods are also characterized usingNIR spectroscopy, a measuringtechnique that is not quite assuitable for the identification ofmineral water.

UV spectroscopy also for the identification ofspring waters

The following application showsthat UV spectroscopy is suitablenot only for the determination ofelements and their salts, but alsofor straightforward identificationof spring waters. Waters fromvarious sources exhibit differ-ences and these differences can berevealed using absorption spec-troscopy and UV spectra, as wellas NIR measurements. As miner-al waters are all transparent in thevisible range, special attentionwas focused on the ultravioletand near-infrared ranges.

Quality control using UV spectroscopy

0.0

0.5

1.0

1.5

1.8

190.0 200.0 220.0 240.0 250.0 nm

Abs

Figure 1: Ultraviolet spectra of four different still mineral waters

5


Sample (theoretical) A Water (%) B Water (%) C Water (%)

104020

C Water (%)9.72

39.9219.91

123

Sample (calculated)123

103020

A Water (%)10.3630.1220.41

803060

B Water (%)79.9029.9659.68

Standard A Water (%) B Water (%) C Water (%)

12345

205030

050

30205050

0

5030205050

rent light

Analysis in the ultra-violet range

Spectra of four store-bought stillmineral waters were measured inthe ultraviolet range of 190 - 250nm using Shimadzus UV-3600spectrophotometer. The result isshown in figure 1. A 10 mm thickquartz cuvette was used for themeasurements, and deionizedwater was used and measured asreference sample. When compar-ing the spectra, one can see aclear difference between thecurves, which can be attributed tothe individual characteristics ofthe mineral waters.

Water in the near infrared range

In the infrared range of 100 -1800 nm using a layer thicknessof 2 mm, the same waters did notexhibit any individual character-istics for the water absorptionsignal at 1440 nm (Figure 2). Thisis due to the strong absorptionby water in the NIR range, as canbe seen in figure 2. This value lies within the linear measuring

Table 1: Mixing ratios for measurements using the UV-3600 of three different still

mineral waters (see Figure 3).

Table 2: The result of a model calculation with respect to four analytical wavelengths

and three samples

0.0

1.0

2.0

3.0

3.3

1000.0 1200.0 1400.0 1600.0 1800.0nm

Abs

Figure 2: Near-infrared spectra of 4 still mineral waters, measured using a 2 mm

thick cuvette

0.0

0.5

1.0

1.5

1.7

190.0 200.0 220.0 240.0 250.0 nm

Abs

Figure 3: Five UV absorption spectra of mixtures of three mineral waters.

The different mixing ratios are listed in Table 1; red = standard 1, blue = standard 2,

black = standard 3, green = standard 4, brown = standard 5

range of the instrument. The dif-ferences among the water samplescannot be determined using NIR,as the NIR range is representedby -CH, -OH and -NH vibra-tions. Minerals are inorganic innature.

Multiple linear regression

To verify the assumption that theultraviolet range reveals differ-ences, multiple linear regressionwas carried out at four analyticalwavelengths in the UV range.The wavelengths 200, 205, 210and 215 were selected and a cali-bration was carried out. Calibra-tion standards were prepared bymixing 3 mineral waters (Tab. 1).Figure 3 shows five UV spectraof these standards.

The result from this straightfor-ward multiple-component analy-sis model (Table 2) shows that themineral waters are distinguish-able. It should be noted that mul-tiple-component analysis can alsobe applied in the UV spectros-copy range of 190 to 250 nm.

This evidently requires an instru-ment technology which stilldelivers reliable results in thisrange. Shimadzus UV-VIS-NIRUV-3600 spectrophotometer isparticularly suitable for thesetypes of analysis.

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information. Please enter the cor-

responding number on the reply

card or order via Shimadzus News

App or News WebApp. Info 396

The purple colored UV-VIS-NIRspectrum shows filtering at 800nm and an inflection point at awavelength of 737 nm, as well asthe highest reflectance in the NIRrange of 2,500 up to 750 nm com-pared to other textiles. The textilesample shown in figure 2 is espe-cially UV reflecting (orange-redspectrum). Both surfaces (silverand cream colored surface) showweaker reflectance in the visiblerange. These surfaces show goodheat-reflecting properties in theNIR range.

The spectrum of the grey sample(light brown spectrum) exhibitseven lower thermal radiation aswell as reduced light transmissi-bility in the visible range. This iscertainly a suitable textile fordarkening a room. Furthermorethe various organometallic com-pounds in combination with thepolymer generate a NIR spec-trum that enables identificationof the polymer. The fibers consistof polyester plus an intelligentmetallic dye.

With the Shimadzu UV-3600triple-detector system and theassociated ISR-3100 integratingsphere with three detectors, the


6

light, respectively sunlight. Forthis purpose, materials with twodifferent surfaces have been in-vestigated. An example of a silverand a cream colored surface isshown in figure 2.

The behavior of the material,when light, heat and strong UVradiation hits the textile, is ofspecial interest.

Instrument and measuringconditions

For analysis, a UV-VIS-NIRinstrument was used. The UV-3600 spectrophotometer con-tains an integrating sphere (Ul-bricht sphere). It is equipped withthree detectors in order to meas-ure the entire range from UV toNIR with higher sensitivity. Instrument: UV-3600 Integrating sphere: ISR-3100

with three detectors.

Measurements were carried outunder 0 reflectance conditions.This method leads to the determi-nation of diffuse reflectance ofthe sample surface. Figure 3 pro-vides a short description of thereflectance of light at a surfacewith specularly reflected light and

I n Europe the previousdecade was the warmestsince recording of tempera-ture in Germany which approxi-mately began 130 years ago. Tem-peratures have also been risingaround the rest of the globe. Thisdoes not lead to energy-savinghowever, as air conditioning sys-tems are used during the summerto cool living spaces and workplaces. These require much elec-tricity, which also increases costs.Ideas are welcome on how toreduce warming of living andworkspaces resulting from solarirradiation.

Suitable textiles already exist forcars or commercial buildings andoffices. Glass panes coated withlight-reflecting layers are alsoavailable to reduce heat or toprovide anti-glare shields forwindows. At the same time,roller blinds or sun blinds canserve as screens.

The surfaces of these types oftextiles, as used for sun blinds,are shown in figure 2.

This article shows how textilescan be used to allow or to blockdifferent wavelength ranges of

diffusely transmitted light, at anincident light angle of 45. Inorder to block specularly reflect-ed light, an incident light angle of0 is applied. Figure 4 schemati-cally shows the alignment of thesample to the integrating spherewhen only the diffusely transmit-ted light is measured.

Measuring results

Under these measuring condi-tions, several textiles were ana-lyzed in order to determine thebest properties of the materialunder the aspects of heat trans-missibility and UV transmissibi-lity.

Intelligent textiles reduce warmiworkspaces Advantages of the triple-detector integratin

Figure 1: A typical window blind a vertical blind Figure 2: Textile with two surfaces, a silver and a cream colored layer of a roller

blind material

Figure 3: Reflectance of light at a

surface

7

TELEGRAMShimadzu News 1/2010

entire UV-VIS-NIR range can beinvestigated with high measuringsensitivity in one single measure-ment.

Legend

UV = Ultraviolet too much UV

light can cause skin cancer

and eye damage

ing of ng sphere

Figure 4: Alignment of the experiment

VIS = Visible light this is the work-

ing range of the human eye

NIR = IR is the thermal radiation;

NIR is the near-infrared spec-

tral range of the radiation.

-5.004

0.000

50.000

98.274

190.00 500.00 1000.00 1500.00 2000.00 2500.00nm.

R %

orange-red = sample with silver and cream

colored surfaces

purple = sample with green surface

blue = sample with brown surface

green = sample with grey surface

light brown = low-density grey sample

Figure 5: UV-VIS-NIR spectra of various textiles composed of polymer and metal

layering

New integrated FTIR accessoriesIRAffinity-1

FTIR instruments with attenuated total reflectance (ATR) for surface meas-urements have revolutionized infrared spectroscopy. The ATR measuringtechnique requires an easy sample preparation and post-processing. Identi-fication or quality control can be carried out simply, effectively and quickly.

The ATR technique has been further advanced through its single reflec-tance accessories. Now, even less sample quantity and time are needed forsample preparation and post-processing than ever before. In addition, due totheir small sample plate surface area, these accessories are extremelyrobust. Sample plates manufactured out of diamond are almost indestructi-ble. This leads to higher sample throughput and to any possible contamina-tion of the sample compartment.

In order to meet the demands of high sample throughput and fast measure-ment, a new accessory concept has been developed for the IRAffinity-1. In 2010, Shimadzu will introduce its new integrated accessories for theIRAffinity-1. The accessories originate from the single reflectance and theHATR-techniques. A single reflectance unit, for instance, enables the pro-cessing of large samples as the measuring position is situated on top of theinstrument housing. These accessories expand the already wide range ofproducts. More news will be available at analytica 2010.

15

APPLICATIONShimadzu News 2/2001INTERNAL Shimadzu News 2/2001

14

Highlighted Piece by Piece Determination of hydroxyproline content in meat and meat products according to 35 LMBG

Shimadzu Biotech has beencreated to bring together astrong solutions-based offer-ing to accelerate the progress ofbiotechnology research and devel-opment.

Shimadzu Biotech captures, with-in one dedicated organisation, thebest expertise and technologyfrom within Shimadzu Corpora-tion and its subsidiary, KratosAnalytical.

The groups initial offering will bebased on delivering a wide rangeof key products covering tech-nologies from DNA sequencingto high performance mass spec-trometry to provide an integratedapproach to the fast growing pro-teomics and genomics markets.Proteomics is rapidly becomingthe focal point of biopharmaceu-tical research and is predicted togrow by 20 % to a total of $ 10billion over the next 5 years.

Kratos Analyticals new MALDI-TOF (Matrix-Assisted Laser Des-orption Ionisation Time-of-Flight) and MALDI IT-TOF(Quadrupole Ion Trap Mass Spec-trometer) represent the cuttingedge of mass spectrometry akey technology ideally suited tofuture developments in pro-teomics.

Other applications that the newunit will be supporting includecombinatorial chemistry, micro-satellite DNA and SNP analysis.

Shimadzu Biotech will be head-quartered in Kyoto and will oper-ate in the USA, Japan and Centraland Northern Europe under thestrategic direction of an interna-tional management team, headedby Dr Ichikawa who joins Shimadzu Biotech from his previ-ous position as head of life sci-ence at Shimadzu Corporation.

Dr Ichikawa commented, We seean excellent strategic fit betweenour know-how and the criticalsuccess factors that will be essen-tial to the future of the biotechindustry. Shimadzu Biotech is oursolution to guaranteeing that we

can deliver this expertise to thesector.

The new business unit will pro-vide a full service offering usingdedicated sales teams, supportedby full applications and serviceback-up.

In addition to bringing togetherproducts from both ShimadzuCorporation and Kratos Analyti-cal to provide scientists with aunified solution to the drug dis-covery process, Shimadzu Biotechwill also be a vehicle for evaluat-ing and developing exciting newtechnologies to advance researchin this field. A key part of thiswill be the creation of strategicpartnerships, such as the Pro-teomics Alliance. This combinesShimadzu Biotech, Proteome Sys-tems and Sigma-Aldrich into asingle force focused on providingintegrated practical solutions forproteomics.

The three companies will worktogether to provide quality coreproducts that meet the demandsof protein scientists from front-end chemicals to protein identifi-cation and informatics.

Other key relationships that havebeen formed include the multi-million dollar agreement betweenLumiCyte, Inc. of Fremont Cali-fornia and Kratos (part of thenewly formed Shimadzu Biotech)to supply mass spectrometers tosupport LumiCytes ground-breaking proteomics work. Underthis arrangement, LumiCyte willpurchase a minimum of 105 AXIMA-CFR MALDI-TOF sys-tems over the next thirty monthsto incorporate into its ProteinBioChip data aggregation facili-ties worldwide.

Customer defined equation Setting of Pass/Fail criteria

Common experience showsthat meat is the most nutritious of all foods according to Justus von Liebig,one of the best-known chemistsin Germany. As a main food itemon our plates, meats and meatproducts must be constantly sub-jected to stringent quality control.

One of the analytical methodsused is UV-VIS spectrophotome-try. This article describes the determination of hydroxyprolineaccording to the German standard 35 LMBG. Hydroxyproline is aparameter for the metabolism ofcollagen. Via the hydroxyprolinecontent, the collagen content canbe calculated, which in turn is anindication of the meat content inmeats and meat products.

For the determination of hydroxy-proline a double-beam UV-1700UV-VIS spectrophotometer withUV-Probe software is used. In addition to the quantification ofhydroxyproline via a calibrationcurve, it is also possible to usevarious arithmetic calculationfunctions and to define pass/failcriteria. A report generator facili-tates printing of the results. Thephotometric determination is car-

ried out via solutions of red 4-dimethyl aminobenzaldehyde ata wavelength of 560 nm. Themethod can be automated using aperistaltic sipper in combinationwith a flow cell. The data is eval-uated via a 6-point calibrationcurve.

During measurement it is possibleto switch between standard andsample measurements. The stan-dards therefore, do not have to bedetermined before the actual sam-ples but can be included in thesample analysis.

With the use of user definablearithmetic calculation functions, it is possible, for instance, torecalculate the hydroxyprolinecontent from units in g/0.1 mL

to g/100 g. This way the collagencontent can be calculated directlyfrom the hydroxyproline content.

The pass/fail function of the soft-ware allows the definition of vari-ous control criteria. The sampletables show whether a measuredvalue meets these criteria. Thepass/fail function is employedduring method development inorder to test whether the sampleconcentration lies within the cali-bration range. In addition to thehydroxyproline method, the UV-1700 spectrophotometer issuitable for other meat qualitycontrol methods: the determina-tion of nitrite/nitrate in cold cutsor the determination of totalphosphate in meats and meatproducts.

We will gladly send you further information. Please note the appropriate number on your reader reply card. Info 245

g/0.1 mL

Fail: Concentration above calibration area Probe 3: Conc > 3.8 g/0.1 mL (highest Standard) Probe 4: Conc > 0.3 g/0.1 mL (lowest Standard)

g/100 g

New Biotech Unit

w w w . s h i m a d z u - b i o t e c h . n e t

Blank page

Extinction using the fibre-optical immersion probe

UV-1700

Extinction using the 10 mm quartz cuvette

260 nm

0.210

0.430

0.856

1.744

2.599

0.205

0.425

0.851

1.739

2.648

350 nm

0.161

0.326

0.644

1.281

1.938

0.157

0.320

0.635

1.289

1.928

15


It is often necessary to moni-tor the quality of products orraw materials located remote-ly from the UV-VIS spectropho-tometer. Fibre-optics technologymakes this possible. In this arti-cle the performance of a fibre-optical probe is demonstrated bycomparing the transmissionmeasurements of a stronglyabsorbing solution, successfullyachieved with a routine system.

Shimadzus UV-1700 is a high-performance, application-orient-ed and compact spectrophotome-ter and in combination with theHELLMA fibre-optical probeand fibre-optic enables fast andprecise measurements of UV-VISspectra. The UV-1700 (190 - 1100 nm) can be operated as astand-alone instrument or via theuser-friendly UVProbe software.Using the standard SUPRASIL

300 dip probe and the quartz fibre-optic (monofibre) for theUV-VIS, a spectral range of 220 nm up to 1100 nm is attain-able. HELLMA offers a fibre-optic adapter that can be attached

via the standard cuvette holder(Figures 1 and 2) connecting the fibre-optic probe to the UV-1700.

Performance

In order to verify the perform-ance of the system, potassiumdichromate (K2Cr2O7) solutionsof differing concentrations wereexamined. As a reference theequivalent spectra of the 10 mmquartz cell measurements were

used. The absorption path lengthof the dip probe used was also 10 mm. Due to the constructionof the dip probe, where the lightbeam is passed through the sam-ple only once, the measuringprinciple applied is the same as incuvette measurements. A total offive different concentratedK2Cr2O7 solutions in 0.01 n(0.005 M) H2SO4 were used.

The complete UV-VIS spectrumwas acquired for each solution


14

l within reachFar away, but stil

and the absorbances at the char-acteristic wavelengths at 1 = 260 nm and 2 = 350 nm weremeasured. Figure 3 shows a com-parison of the spectra obtainedfor the cuvettes and the dipprobe with a 2 m fibre-opticprobe for the dichromate meas-urement.

It is clear that above 270 nmthere is very good correspon-dence between the spectraobtained via both techniques.Only below 270 nm is a decreasein transparency of the fibre-opticobserved for the highest concen-trations, with a correspondingslight decrease in the signal tonoise ratio of the absorption sig-nal. To get a complete overview,the absorbances at 260 nm and350 nm are shown in Table 1.

Application area

The spectra obtained using thestandard dip probe and the 2 mUV-VIS fibre-optic with fibre-optic adapter correspond verywell with the 10 mm quartzcuvette measurements over theentire spectral range of 220 up to1100 nm. Shimadzus UV-1700with fibre-optic and dip probe istherefore very well suited forspectroscopic measurements thatneed to be carried out at a dis-tance from the sample.

This includes measurements ofraw materials for manufacturingprocesses at production site aswell as measurements that due totheir hazardous nature cannot becarried out directly in the spec-trophotometer. Furthermore,measurements in hazardous explosive environments are included, measurements of high-

ly toxic and radioactive com-pounds as well as measurementsin highly contaminated areas.

The fibre-optic system presentedhere can also be used in unal-tered form for the UVmini-1240,MultiSpec-1501, UV-1650PC,UV2401PC and UV2501PC.

We will gladly send you further infor-

mation. Please note the appropriate

number on your reader reply card.

Info 292

Figure 1: UV-1700 with UV-VIS fibre-optic and

fibre-optic adapter

Figure 2: Fibre-optic adapter for standard cuvette holder

Table 1: Absorbances at 260 nm and 350 nm of the five dichromate solutions

of different concentrations.

Figure 3: Comparison of UV-VIS

measurements of a K2Cr2O7 solution

in 0.01 n (0.005 M) H2SO4.10 mm

quartz cuvettes and dip probe measu-

rements are shown together

Figure 4: Comparison of the 10 mm cuvette- and the dip probe measurements

at 260 nm (black graph) and at 350 nm (blue graph). Equal wavelengths have the

same colour.

The deviations from the cuvette measurement, even at the highest concentrations

are less than 2 % (260 nm), and less than 1 % (350 nm)

optics Successful analyses using routine systemsUV-VIS measurements with fibre-

Concentration (mg/L)

K2Cr2O7

15

30

60

120

180

15

30

60

120

180

nm.

220.00 300.00 400.00 500.00 550.000.000

3,000

2,000

1,000

Ext

inct

ion

(K2Cr2O7)/mg/L

0 25 50 75 100 125 150 175 2000.0

0.5

1.0

1.5

2.0

2.5

3.0

Ext

inct

ion

Extinction using the fibre-optical immersion probe

UV-1700

Extinction using the 10 mm quartz cuvette

260 nm

0.210

0.430

0.856

1.744

2.599

0.205

0.425

0.851

1.739

2.648

350 nm

0.161

0.326

0.644

1.281

1.938

0.157

0.320

0.635

1.289

1.928

15


It is often necessary to moni-tor the quality of products orraw materials located remote-ly from the UV-VIS spectropho-tometer. Fibre-optics technologymakes this possible. In this arti-cle the performance of a fibre-optical probe is demonstrated bycomparing the transmissionmeasurements of a stronglyabsorbing solution, successfullyachieved with a routine system.

Shimadzus UV-1700 is a high-performance, application-orient-ed and compact spectrophotome-ter and in combination with theHELLMA fibre-optical probeand fibre-optic enables fast andprecise measurements of UV-VISspectra. The UV-1700 (190 - 1100 nm) can be operated as astand-alone instrument or via theuser-friendly UVProbe software.Using the standard SUPRASIL

300 dip probe and the quartz fibre-optic (monofibre) for theUV-VIS, a spectral range of 220 nm up to 1100 nm is attain-able. HELLMA offers a fibre-optic adapter that can be attached

via the standard cuvette holder(Figures 1 and 2) connecting the fibre-optic probe to the UV-1700.

Performance

In order to verify the perform-ance of the system, potassiumdichromate (K2Cr2O7) solutionsof differing concentrations wereexamined. As a reference theequivalent spectra of the 10 mmquartz cell measurements were

used. The absorption path lengthof the dip probe used was also 10 mm. Due to the constructionof the dip probe, where the lightbeam is passed through the sam-ple only once, the measuringprinciple applied is the same as incuvette measurements. A total offive different concentratedK2Cr2O7 solutions in 0.01 n(0.005 M) H2SO4 were used.

The complete UV-VIS spectrumwas acquired for each solution


14

l within reachFar away, but stil

and the absorbances at the char-acteristic wavelengths at 1 = 260 nm and 2 = 350 nm weremeasured. Figure 3 shows a com-parison of the spectra obtainedfor the cuvettes and the dipprobe with a 2 m fibre-opticprobe for the dichromate meas-urement.

It is clear that above 270 nmthere is very good correspon-dence between the spectraobtained via both techniques.Only below 270 nm is a decreasein transparency of the fibre-opticobserved for the highest concen-trations, with a correspondingslight decrease in the signal tonoise ratio of the absorption sig-nal. To get a complete overview,the absorbances at 260 nm and350 nm are shown in Table 1.

Application area

The spectra obtained using thestandard dip probe and the 2 mUV-VIS fibre-optic with fibre-optic adapter correspond verywell with the 10 mm quartzcuvette measurements over theentire spectral range of 220 up to1100 nm. Shimadzus UV-1700with fibre-optic and dip probe istherefore very well suited forspectroscopic measurements thatneed to be carried out at a dis-tance from the sample.

This includes measurements ofraw materials for manufacturingprocesses at production site aswell as measurements that due totheir hazardous nature cannot becarried out directly in the spec-trophotometer. Furthermore,measurements in hazardous explosive environments are included, measurements of high-

ly toxic and radioactive com-pounds as well as measurementsin highly contaminated areas.

The fibre-optic system presentedhere can also be used in unal-tered form for the UVmini-1240,MultiSpec-1501, UV-1650PC,UV2401PC and UV2501PC.




Info 292

Figure 1: UV-1700 with UV-VIS fibre-optic and

fibre-optic adapter

Figure 2: Fibre-optic adapter for standard cuvette holder

Table 1: Absorbances at 260 nm and 350 nm of the five dichromate solutions

of different concentrations.

Figure 3: Comparison of UV-VIS

measurements of a K2Cr2O7 solution

in 0.01 n (0.005 M) H2SO4.10 mm

quartz cuvettes and dip probe measu-

rements are shown together

Figure 4: Comparison of the 10 mm cuvette- and the dip probe measurements

at 260 nm (black graph) and at 350 nm (blue graph). Equal wavelengths have the

same colour.

The deviations from the cuvette measurement, even at the highest concentrations

are less than 2 % (260 nm), and less than 1 % (350 nm)

optics Successful analyses using routine systemsUV-VIS measurements with fibre-

Concentration (mg/L)

K2Cr2O7

15

30

60

120

180

15

30

60

120

180

nm.

220.00 300.00 400.00 500.00 550.000.000

3,000

2,000

1,000Ext

inct

ion

(K2Cr2O7)/mg/L

0 25 50 75 100 125 150 175 2000.0

0.5

1.0

1.5

2.0

2.5

3.0

Ext

inct

ion

d = x12

12

1

m

2n2 sin2


20

olProduction quality contr

The UV spectroscopy canbe applied for the non-destructive determinationof layer thicknesses of thin films.This determination is based onthe simple physical phenomenonof interference, resulting fromstanding waves between twophase boundaries. In order tomake this possible in UV spec-troscopy, the materials under in-vestigation must exhibit layerthicknesses of approximately 0.3to 60 m. The refractive index of

where d is the film thickness, mis the number of peaks in thefixed wavelength range, n is theindex of refraction, is the angleof incidence of the light on thesample surface, and 1 and 2 arethe initial and final wavelength ofthe respective range.

The calculation for two samples,a 10 m polyvinyl chloride filmand a 46 m polycarbonate film,with different film thickness is

production, where process con-trol of the thicknesses of theapplied SiO2 films is critical.Wide variations in film thicknessresult in high failure rates duringfurther processing.

The transmission mode is appliedfor thin films on a transparentsubstrate, for instance in the man-ufacture of foils. In the transmis-sion mode it is also possible toanalyze films consisting of onlyone material.

Theory

An example is presented toexplain the physical principle ofreflectance spectroscopy. Lightstriking a film at an angle of inci-dence invokes an interaction/interference of the incident sur-face A with an angle of reflec-tance of the opposite surface B(bottom), as shown in Figure 1,which results in a spectrum withinterference patterns (Figure 2).Counting the number of peaks(or valleys) in this pattern in afixed wavelength range, the filmthickness can be calculatedaccording to the following equa-tion:

the material must be known to beable to carry out this determina-tion.

Reflectance spectroscopyand transmission measure-ment

There are basically two UVmeasuring modes reflectanceand transmittance spectroscopy which enable interference meas-urement in application areas suchas thin films deposited ontomaterials or transparent filmsconsisting of a single material.

Thin films can be present on non-transparent carrier materials. Theuniformity of the surface film canbe determined using reflectancespectroscopy. The sample surfacemust be smooth and mirror-like.Rough surfaces are not suitable,as the diffuse reflectance takingplace at the surface prevents theformation of an interference pat-tern.

A typical example of this appli-cation is film thickness determi-nation of wafers during chip

Film thickness determination using UV spectroscopy

Figure 1: Principle of interference

Figure 2: Screenshot of the film thickness software and an example of the selection

criteria for film thickness determination

NEWS 01.2009_01_GB 11.03.2009 12:55 Uhr Seite 21

Now also Vista compatible

Most valued features of theTOC-Control V software

21

TELEGRAMShimadzu News 1/2009

olntrcopy

Figure 3: Reflectance measurement of a polyvinyl chloride film with a

film thickness of 10 m

TOC-Control V software 2.1

Figure 4: UV reflectance spectrum of a polycarbonate film with a

film thickness of 46 m

0.00

5.00

10.00

15.00

600.0 700.0 800.0 900.0

Wavelength (nm)

Refle

ctan

ce (%

R)

5.00

6.00

8.00

10.00

12.00

14.00

15.00

600.0 700.0 800.0 900.0

Wavelength (nm)

Refle

ctan

ce (%

R)

presented below. Figure 3 showsthe interference pattern of the 10m PVC film in the wavelengthrange of 600 to 900 nm. This iscompared with the higher filmthickness sample of 46 m. Theresult is an excellent exampledemonstrating that thin films leadto wide amplitudes and thickerfilms to narrower amplitudes.

The calculation can be easily car-ried out using the film thickness

determination tool featured in the software. When all physicalparameters such as refractiveindex, angle of incidence andwavelength range are known, thefilm thicknesses are calculatedautomatically (Figure 2).

Most valued features of theTOC-Control V software

Now also Vista compatible

An update (version 2.1) for Windows Vista is now available for the TOC-Control V software successfully introduced last year. Among the featuresmost valued by our users are:

Adding additional samples during ongoing operationAny number of samples, calibration curves or control samples may beadded in the edit mode. Previously measured samples can be recalculatedand reports can be printed. During activation of the edit mode the ongoingmeasurement cycle continues running.

Other users can take over during ongoing operationIn access-controlled systems, it is important that change of personnel dur-ing shift operation allows users to log in and out without interrupting theongoing measuring cycle. This can be configured in the user authorizationrights for each user.

Simplified recalculation in a single stepIn the past, recalculation of previously measured samples using anothercalibration curve had to be carried out individually for each sample. In theTOC-Control V version 2.00 software, however, the respective samples aretagged in the sample table before a new calibration curve is selected andthe recalculation is carried out.

Simple operationSample tables can be established via a simple drag & drop operation.Using the mouse, the desired elements are dragged into the sample tablefrom a list of the established calibration curves, measuring methods, con-trol samples and measuring sequences. The right mouse button containsmany functions which greatly simplify operation.

The use of shorter Wizards enables even faster establishment of cali-bration curves and measuring methods as well as improved templates forsample tables in routine analyses.

NEWS 01.2009_01_GB 11.03.2009 12:55 Uhr Seite 22

9


Figure 1: Two camera objectives from

different manufacturers, featuring a stan-

dard lens and a macro lens

Figure 2: UV-VIS spectra of a zoom

objective at a setting of 25 mm (green)

and 300 mm (blue)

Figure 3: UV-VIS spectra and compari-

son of the light transmittance of a fixed

objective (black) of 50 mm with a zoom

objective (green) at a setting of 25 mm

Everything within viewQuality control of camera objectives with UV-2600and MPC-2600

Testing two objectives

In the experiment shown here,two objectives from different man-ufacturers were tested. Since theobjectives have been designed fordifferent uses, they have differentcharacteristics:1. Fixed lens system, 50 mm F/1.22. Macro lens, 28-300 mm F3.5 -

6.3 DG Macro (F = focal length,1.2 or 3.5 -6.3 are aperture val-ues.)

The objectives were measuredusing the UV-2600 and MCP-2600sample compartment. The objec-tives were placed on the V-table ofthe MPC-2600 and were broughtto the measuring position. Themeasuring assembly simulates theincident light for imaging withinthe camera. The objectives weremeasured with the incident lightfrom outward to inward.

The detector (photomultiplier) islocated in an integrating sphere(Ulbricht sphere) and displays thetransmittance, i.e. the light of thetransmittance of the object (objec-tive). Furthermore, absorptions bysealings can be expected, as well aseffects of reflections and antire-flective coatings.

Discussion of the spectra

When the focal length is increased,the light transmittance decreasesdue to the reduction of the field ofview, as can be seen in Figure 2.The spectra displayed are the lighttransmittance at 28 mm (70.6 %)and 300 mm (37 %). Due to thereduced light transmittance, takinga photograph using the zoom set-ting needs a longer exposure time,a larger aperture or additionallighting in order to obtain morelight intensity.

The quality of the objectives variesaccording to the function of the

In addition, it is also possible tocheck the specifications that char-acterize the objective. The goal is,after all, to manufacture high-quality objectives. There are sever-al criteria in photography that canbe met by implementing suchquality control: the visible range of an objective

for the image quality of the colors, or depth of field in thephotographs

the quality of the coatings onglasses and lenses

sensitivity in the red or blueranges.

In addition, a UV-VIS spectro-photometer can be used to qualifycamera accessories such as polariz-ing filters or UV filters.

With the introduction of the new generationof LO-RAY-LIGHgratings in Shimadzus new UV-2600/UV-2700 UV-VIS spec-trophotometer series, many appli-cation areas in the field of opticscan now be covered. In addition to single optical elements such aslenses and glasses, composite ma-terials or single-coated systemsand even entire assemblies cannow be analyzed. Camera objec-tives are small optical benches,equipped with different lenses andglasses with protective coatings orsurface finishes. The quality of anobjective is determined by its lightintensity and low optical aberra-tions.

The light intensity can be deter-mined spectroscopically. By com-bining the UV-2600 or UV-2700with a MPC-2600 extra large sam-ple compartment, non-destructiveanalysis of entire camera objectivesis possible. This sample compart-ment is equipped with a V-shapedholder, ensuring stable positioningof the objective. The holder can bepositioned in all three dimensions,so that the analytical irradiationhits the center of the objective op-tics and passes through the opticalbench, while the spectrophotome-ter measures the incident lightintensity, which is displayed in theform of transmittance spectra.These spectra show not only thelight throughput in percentagesbut also the transmission range asa function of wavelength for visi-ble and ultraviolet light.

Quality determination of objectives and cameraaccessories

Using this combination of instru-ments, it becomes possible to es-tablish a quality determinationprocess that allows productioncontrol of a production series.

50,000

0

-8,873

97,530

nm.

T %

190.0 400.0 600.0 800.0 900.0

50,000

0

-8,873

97,530

nm.

T %

190.0 400.0 600.0 800.0 900.0

objective. An objective with fixedfocal length can result in goodlight transmittance with few com-ponents. Figure 3 shows two verydifferent representative examples.

The light transmittance of thefixed focal length results in a valueof 86.7 % while the variable focallength results in a transmittance ofup to 70.6 %. Assuming the lossof 4 % of the original energy at allsurfaces based on the physics offlat glass, it might be concludedthat the fixed objective consists of4 glass components.

With extrapolation, four glasscomponents should result in a lossof approx. 15 % of transmittance.This corresponds approximately tothe measured value of 86.7 %. Butthis is, of course, a rough estimatefor an unknown object in whichother aspects, e.g. filtering surfacecoatings, can have an influence.

Both objectives are distinguishedby their wavelength range. Theobjective with fixed focal length

features a high light transmittance.In addition, a profile maximum atapprox. 520 nm corresponding tothe green wavelength range is ap-parent. In comparison, the zoomobjective is optimized for wave-lengths in the red range (approxi-mately 620 nm).

Blank page

Cap

Cell

Mirror

Pipette

Window

Samplesolution


4

orAdvances in UV-VIS absShimEvaluation of low DNA/RNA sample volumes on the

spectrophotometer using a Hellma TrayCell

In the last years, new tech-nologies have emerged foraccurate UV-VIS spec-trophotometric measurements ofsample volumes in the microliterrange. In this respect, the HellmaTrayCell is a more recent opticaldevice that provides, in combina-tion with a standard single beamspectrophotometer, a cost-effec-tive option for assessing sampleconcentration with undiluted,minimal volumes. Hellma Tray-Cell is a highly innovative toolbased on fibre-optics and inte-grated beam deflection technolo-gy (Figure 1).

Nucleic acid measurements

The study focused on nucleicacid measurements at 260 nm,using a plasmid DNA sample. Itsconcentration was arbitrarilyconsidered as reference whenmeasured with the classical 10mm-path ultra micro cuvette.Readings were performed at fourdilutions factors (1 : 50, 1 :100,1 : 200 and 1 : 400) and an averagesample concentration of 1.725g/L was obtained (CV = 4.3 %)(Table 1). The concentration wasfurther estimated on the HellmaTrayCell with 4 L of undilutedsample. With the 0.2 mm-pathcap an average absorbance of0.664 was obtained (n = 4, CV =3.7 %), corresponding to an aver-age concentration of 1.661 g/L(Table 2). The linearity of theabsorbance readings with theHellma TrayCell/0.2 mm cap set-ting was next assessed, making

Most importantly, its dimensionsare equivalent to a standardcuvette allowing its use in con-ventional spectrophotometers.However, two exchangeable mir-ror caps create defined opticallight path of only 0.2 or 1 mm,which at the sample level trans-lates into virtual dilution factorsof 1 : 50 and 1 : 10 respectively.Higher concentrated sampleswhich cannot be estimated direct-ly with the more classical cuvettes(5 or 10 mm optical path) can bemeasured with the Hellma Tray-Cell without prior dilution.

The sample is placed directly onthe surface of the optical window,and recommended volumes areonly 0.7- 4 L for the 0.2 mm capor 3- 5 L for the 1 mm cap.Another valuable feature is thatthe Hellma TrayCell remains inthe photometer during sampleloading, retrieval or cleaning,ensuring not only optical stabilitybut also higher turn around timeof the measurements. Theretrieved sample can be used forfurther analysis if desired.

The aim of this preliminary studywas to compare absorbance read-ings with the Hellma TrayCell onthe Shimadzu UVmini-1240 spec-trophotometer against readingswith a classical 10 mm ultra microcuvette. The latter is of blackbody style with a 10-mm opticalpath, a 2.5 x 2 mm measurementwindow and a minimum requiredsample volume of 70 L. TheUVmini-1240 spectrophotometeris a single beam optics systemwith concave holographic gratingas monochromator, a 5 nm spec-tral band width and silicon pho-todiode detector.

Figure1: The Shimadzu UVmini-1240 spectrophotometer and the Hellma TrayCell.

The UVmini-1240 is a stand-alone UV-VIS single beam spectrophotometer with an optical

band width of 5 nm. The system uses a concave holographic grating as monochromator and

has a silicon photodiode detector. The measurement wavelength range is 190 to 1100 nm.

On-board software contains basic menus including photometric mode for fixed wavelengths,

spectrum mode for wavelength scanning and quantitation mode for single component analy-

sis. In addition, several optional program packs are available with dedicated research applica-

tions such as multiwavelength measurements, kinetics and protein analysis.

The Hellma TrayCell is a micro cell with fibre optic cables and integrated beam deflection.

Due to these features the sample is placed directly on the surface of the optical window and

readings can be performed either with the 0.2 mm or the 1 mm light path mirror cap,

depending on sample concentration.

Cristiana Stefan, Clin. Chem., Ph.D, Cath. University of Leuven, Faculty of Medicine, Department of Oncology, Belgium; Pascal Mannaert, Shimadzu Benelux, BBs Hertogenbosch, The Netherlands

*NEWS 01.2007 GB 21.02.2007 15:39 Uhr Seite 5

0.6410.6900.6460.68

AverageSDCV

9864321

1234

No.

Dilution factor

Dilution factor

0 0.2 0.4 0.6 0.8 1.0 1.20

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

A 2

60 n

m

1/ Dilution factor

y = 0.6951x 0.0023R2 = 0.9992

Window

Sampleolution

5


orbance measurementsbsShimadzu UVmini-1240the

Figure 2a: Evaluation of absorbance linearity with the UVmini-1240 and the Hellma TrayCell/

0.2 mm cap setting Absorbance readings and calculated concentrations

Figure 2b: Linearity curve

Table 1: Evaluation of the DNA sample concentration with the UVmini-1240 and the classical

10 mm-path ultra micro cuvette setting

A 260 nm = absorbance at 260 nm SD = standard deviation CV = coefficient of variation

g/L = [A260 nm (10 mm) x dilution factor x 50 g/mL] /1000

Table 2: Evaluation of the DNA sample concentration with the UVmini-1240 and the Hellma

TrayCell/0.2 mm cap setting

A 260 nm = absorbance at 260 nm SD = standard deviation CV = = coefficient of variation

g/L = [A260 nm (0.2 mm) (correction for 10 mm path) x dilution factor x 50 g/mL] /1000

use of various sample dilutions(n = 7) (Figure 2). In this analysis,the absorbance values covered the0.069 to 0.69 unit interval andaverage sample concentration was1.694 g/L (n = 7, CV = 6.4 %).Correlation analysis showedexcellent linearity parameters(r2 = 0.9992, y = 0.6951 x -0.0023),indicating that readings with theundiluted sample were within alinear range. Measurements werealso taken with the 1 mm cap insimilar studies, and an averagesample concentration of 1.614g/L (n = 5, CV = 2.7 %) wasfound.

In conclusion, the Hellma Tray-Cell delivers its promises whenused with the Shimadzu UVmini-1240 spectrophotometer: accurateanalysis of small volumes withremarkable reproducibility. Thisstudy was selected as representa-tive and follows a complex sys-tem check procedure.

Accurate measurement of smallvolumes of undiluted nucleic acidsamples is of particular value fortranslational clinical researchfocussing on gene expressionstudies, where small amounts ofpatient specimen, such as biop-

ment rlands

sies, allow only for limited vol-umes of DNA/RNA-containingsamples to be measured. The useof a standard spectrophotometer-Hellma TrayCell setting forabsorbance measurement is alsojustified even when larger vol-umes of DNA/RNA samples areavailable due to elimination ofdilution-related errors and fasterresults through a higher turnaround time.

We will gladly send you further information.

Please note the appropriate number on your

reply card. Info 319

0.0690.0770.1230.1730.2290.350.69

AverageSDCV

1.5521.5401.8451.7301.7171.7501.7251.6940.1096.4

A 260 nm (0.2 mm) g /L

6.78.63.46.0

0.0850.1800.3530.652

400200100

50

AverageSDCV

0.0060.0160.0120.039

1.7001.8001.7681.6311.7250.0754.3

A 260 nm (10 mm)(Average of two readings) SD CV (%) g/L

1.6021.7251.6151.71.6610.0243.7

A 260 nm (0.2 mm) g/L

*NEWS 01.2007 GB 21.02.2007 15:39 Uhr Seite 6

Shimadzu NEWS, Customer Magazine of Shimadzu Europa GmbH, Duisburg

Publisher:Shimadzu Europa GmbHAlbert-Hahn-Str. 6 -10 D - 47269 DuisburgPhone: +49 - 203 - 76 87- 0 Telefax: +49 - 203 - 76 66 [email protected]

Editorial Team:Uta Steeger Phone: +49 - 203 - 76 87- 410 Ralf Weber, Tobias Ohme

Design and Production:m/e brand communication GmbH GWADsseldorf

Circulation:German: 9,175 English: 22,920

Copyright:Shimadzu Europa GmbH, Duisburg, GermanyNovember 2009

Windows is a Trademark of Microsoft Corporation

IMPRINT

The color sells the tea Color testing using UV-VIS spectroscopy 2

Fast, easy, accurate Three-step TOC determination in solid materials 4

White Gold Salt in foods 6

FTIR lemon squeezer extracts citrus fragrance Single-reflection unit and FTIR spectrophotometer 8

Inside Polymers GPC for monitoring polymerization kinetics 10

TOC analysis traces efficiency of photocatalysts 12

Drinking water at risk World Water Forum 2009 14

Composite materials how do they react? 17th ICCM in Edinburgh 5

White wine and coffee Flavour profiling of food samples with SPME-GCMS and On-Column injection 15

Excellence Plus The new GC-2010 Plus Even excellence can be better 18

Three turbos for GC Advanced Flow Technology 20

Recognizing harmful substances in the body Using graphite furnace AAS in biomonitoring 22

AGS-X the popular tester Shimadzus new universal testing machine 24

Pilot study Online TOC for ozonation of treated wastewaters 23

APPLICATION

TELEGRAM

PRODUCTS

CONFERENCE

New TOC draft normDIN EN 15936


2

The color sells t

Green camomile tea doesnttaste. This might be thefirst reaction of a tea con-noisseur who discoversgreen-colored instead of yel-low tea in his cup.

Although the tea tastes likecamomile, the consumer may notbe able to associate the taste ofhis chosen drink with camomiletea. Not only the taste but alsothe color must be right, since thehuman brain automatically asso-ciates colors with certain fra-grances or aromas. This is whymanufacturers should stick to thecolor of a product when aimingfor a positive taste association.

Perception of colors is a difficulttask for the human eye and, inconsequence, for manufacturers.Their classification dependsstrongly on experience, and it issubjective and hardly applicablein an industrial production pro-cess. This is why a standardizedcolor system was established fornatural minerals. The color tablesenable consistent reproduction ofa required color and support

industrial processes. In naturalproducts, free of artificial color-ing, these color scales are suitablefor the control of technically created color blends, for instance. In the case described below, acamomile tea and its color arecorrelated to the brewing timerecommended by the manufac-turer.

The determination of color is oneof the main applications in UV-VIS instrumental measuring tech-niques. This method, indepen-dently of the human eye, enablesthe use of effective classificationmethods instead of subjectiveassessments.

In this application, a tea bag wasextracted with distilled water atroom temperature. The tea bag

was placed in a 50 mL beakerwithout shaking or stirring.Approximately 3 mL of theextract was transferred to aquartz cuvette suitable for UV-VIS spectroscopy measurementand a UV-VIS spectrum was sub-sequently obtained. Additionalmeasurements were carried outafter 5, 10 and 15 minutes. Thetest was carried out under totaltransmission conditions with thehelp of an integrating sphere of150 mm diameter.

Instrumentation:UV-3600, LISR-3100, transmission integrating sphereattachment, 10 mm quartz cells, 50 mL beaker

Total transmission using anintegrating sphere

In direct transmission measure-ments, the energy of the lightsource is measured before andafter it has been transmittedthrough the sample.

In standard measurement of clearsamples, the detection elementrecords directly transmitted lightleaving the sample. The samplesare transparent. In the case ofnatural products and extractsfrom tea bags, a certain turbidityarising from very small particlesis assumed to occur. An integrat-ing sphere was used to measurescattered light effects as well asdirectly transmitted light. Thissphere captures scattered opticalphenomena and focusses themback towards the detector. Byplacing a measuring cell directlyin front of an integrating sphere,it is possible to measure the totaltransmission, which is the sum of

Figure 1: Dried and crushed camomile from a tea bag

Figure 2: Representation of directly transmitted light

Extraction time [min]

0

5

10

20

3


he tea Color testing using UV-VIS spectroscopy

directly transmitted and scatteredlight.

Visual perception of color ischaracterized via standardizedcolor tables. The yellownessindex and the dominant wave-length in a UV-VIS spectrum canbe determined using the CIEstandard color space (since 1931)and the XYZ tristimulus values,specifically in the visible spectralrange. Table 1 shows some of theproperties and time-dependenttrends. Special attention shouldbe paid to the yellowness indexYI and the dominant wavelengthdWL. Figures 5 and 6 show bothvalues as a function of time. Thecolor values were calculated forthe CIE standard illuminant C,which represents daylight with-out UV radiation under an obser-vation angle of 2.

Results

The values measured show a defi-nite trend: the tea is ready todrink after approximately 6 min-utes brewing time. This experi-

ment confirms the manufacturersrecommendation of 6 minutesbrewing time, since in this periodthe dWL as well as the YI (Fig-ures 5 and 6) reach their mathe-matical inflection point in thecurve, after which saturation setsin. This is the point where thegraph reaches a plateau.

The characteristics with respectto the dominant wavelengthchange in time, as the absorptionof the soluble and less solublecomponents in tea are added sub-sequently in time. The observa-tion that the tea extract looksgreen rather than yellow is con-firmed by the analytical wave-length of 570 nm.


mation. Please note the corresponding

number on your reply card. Info 359

Table 1: Calculation result from the color tables, using standard illuminant C and a

standard observation angle of 2

Figure 3: Placement of the sample in the optical path for measurement of total

transmission in an integrating sphere

Figure 4: UV-VIS spectrum of camomile tea

Figure 5: Representation of the time dependence of the dominant wavelength dWL

for the extraction of camomile tea

Figure 6: Representation of the extraction time dependence of the color yellow for

a camomile tea

-10.048

0.000

50.000

100.000

110.275

300.00 400.00 600.00 800.00 900.00

Wavelength [nm]

R %

Black represents the start time

red = 5 minutes

green = 10 minutes

olive = 20 minutes

In order to avoid subjective analyses, color

scales were applied to indicate the chroma-

ticity of the tea. The represented measuring

range is 300 nm to 900 nm. This corre-

sponds to the visible spectral range.

566

568

570

572

574

576

0 5 10 15 20 25

Time [min]

Dominat wavelength for tea over a time period

0

10

20

30

40

50

60

0 5 10 15 20 25

Time [min]

Development of Yellowness Index for tea

X Y Z dWL Yl

96.71

84.12

72.86

67.48

98.79

87.84

76.87

71.28

115.97

81.75

55.47

44.01

566.8

573.1

574.0

574.6

0.88

23.93

44.82

55.74

Wav

elen

gth

[nm

]YI

Yel

low

ness

Inde

x

11


After measurements are com-pleted, the concentrations aredisplayed immediately.

The application example descri-bed above offers an overview ofthe current state-of-the art in thedetermination of hazardous com-pounds in electrical and electron-ic equipment as well as electricalscrap materials according toWEEE and RoHS. The thresholdvalues for lead, mercury, chro-mium, polybrominated biphenylsand polybrominated diphenylethers are determined as 1,000 mg/kg and for cadmium as100 mg/kg, corresponding toconcentrations already used inthe earlier ELV directive.

Hardware and software for accurate determination of hazardous substances

Shimadzu offers an extensiveproduct range featuring a com-plete hardware and software solution for accurate determina-tion of hazardous substances, as well as the competence andknow-how of a market leader inanalytical instrumentation.

Please have a look at the European

seminar tour dates on page 17.




Info 302


10

ccording to the RoHS guidelinesChromium (VI) analysis a

The European Union hasofficially announced in its official bulletin of 13February 2003, new directivesregulating electrical and electron-ic used equipment (WEEE, WasteElectrical and Electronic Equip-ment) as well as the Restrictionof the use of certain HazardousSubstances in electrical and elec-tronic equipment (RoHS). Thismarks the ratification of bothdirectives in the EU (2002/95/ECand 2002/96/EC) which wereadopted into national law in Jan-uary 2005.

According to the RoHS guide-lines, as of 1 July 2006, a thresh-old value will apply for lead,mercury, cadmium, hexavalentchromium, polybrominatedbiphenyls (PBB) and polybromi-nated diphenyl ethers (PBDE).However, RoHS does not applyto all ten equipment categorieslisted in WEEE. According toArticle 2 of the RoHS directivethe equipment categories 8 (med-ical devices) and 9 (monitoringand control instruments) as wellas certain other equipment classes(computer servers, memory sys-tems and network infrastructurein telecommunications) are cur-rently exempted from the direc-tives under RoHS guidelines.

um (VI) oxidizes 1.5-diphenylcarbazide to 1.5-diphenyl carba-zone, forming a red/violet-col-ored complex with chromium.The extinction of the dye is linearwith respect to the chromium(VI) concentration (Figures 3and 4).

Pentavalent vanadium (V5+),trivalent iron (Fe3+) and tetra-valent molybdenum (Mo4+) alsoreact with 1.5-diphenyl carbazideand, in the presence of the reac-tion solution, result in an appar-ently higher Cr6+ concentration.The concentrations of these ionsmust therefore be determined in a preliminary experiment.

Summary

UV-VIS spectrometry is highlysuitable for fast and straightfor-ward determination of hexavalentchromium and can be applied in routine analysis using theUVmini-1240. The UVmini offersthe following advantages for theanalysis of ions in aqueous solu-tions using the specially devel-oped water analysis programpack:

Fast and accurate analysis of selected ions in aqueoussolutions.

55 measuring programs(optional water analysis pro-gram pack) for 34 different ionsincluding hexavalent chromium.

All analysis parameters includ-ing the analytical wavelength,calibration curve, measuringtime etc. are adjusted automati-cally by the selected measuringprogram.

and using electrothermal atomisa-tion mode in a concentrationrange of 0.1 up to 20 g/L.

Photometric quantification ofhexavalent chromium (Cr 6+) can be carried out with theUVmini-1240 (Figure 1) using 1.5-diphenyl carbazide (Figure 2)as reactant to form coloredchromium complexes.

This procedure is suitable for thedetermination of c

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