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LabSolutions concept

Cross-system platform for HPLC-,UHPLC and GC systems, as well asfor LCMS and LCMS/MS systems

Including part 2 of the bigbreakfast test

SALD-7500

New family member fornanoparticle measurement

Amino acid identification

Fast and easy with the UF-Amino Station for high-throughput analysis

Bitumen – it’s all in the mix – FTIR spectroscopy determines qualitydifferences 4

Searching for elemental traces inpetrochemicals – The high-precisionICPE-9000 inductively coupled plas-ma optical emission spectrometer 9

Exact measurement of color – Newsoftware for color determination 10

Determination of microbial biomass in soils – TOC in soil science 12

Amino acids – fast and simple identi-fication – UF-Amino Station enableshigh-throughput analysis 14

A small, subtle distinction – Trace analysis in polymers using pyrolysis GCMS 16

The daily bread – The big breakfasttest using the EZ Test EZ-X textureanalyzer (part 2) 19

Following the traces of climatechange – Novel plasma technologyoffers new detection possibilities 20

Effect of mobile phase pH on reversed-phase HPLC separations of ionizable compounds 22

Customized TOC analysis – The online TOC-4200 with many options and kits 23

How to make invisible things visible?Worldwide unique: The new HyperVision HPV-X camera 2

New family member, improved possibilties – SALD-7500 for meas -uring nanoparticles 5

New: LabSolutions DB and CS Software 6

New accessory for UV-VIS spectro-photometers TCC-100 8

APPLICATION

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SHIMADZU NEWS 2/2014

INHALT

How to make invisiblethings visible?

Added value for you

U ltra-high-speed recordingswith video cameras havebecome standard tools for

characterizing and quantifying

million frames per second (fps)while maintaining excellent spatialresolution at any recording speed.

of high speed events in order tomake invisible things visible.Shimadzu’s HPV-1 and HPV-2enable recordings at up to one

Worldwide unique: The new Hyper Vision HPV-X camera with 10 million frames per second

... means the best. It is apparent in the de -

tails. And in our employees. Both contribute

to your added value.

... means creating technologies that are

compatible with our lives, our values and

with nature. This will secure our future.

... means overcoming limitations and pre-

conceptions – technical, psychological, social.

This leads to progress.

P roduct and service quality ofthe highest level, easy-to-useinstruments, system perfor -

mance and total costs of owner-ship (TCO) are important param-eters for achieving the best resultsfor maximum cost-effectiveness.With this claim, Shimadzu contin-

uously extends and redefines tech-nological limits. This is confirmedby numerous world premieres andawards. All analyzers are manufac -tured in accordance with interna-tionally established standards (forinstance ISO), so users can workaccording to GLP, GMP, FDA or

Pharmacopoeia. Shimadzu offersinterdisciplinary solutions formany application areas. The mo -tifs shown above representShimadzu’s claims to trade fairs,conferences and symposia – andoffer users the added value in theirwork for their clients.

NEWS – Shimadzu’s customer maga -zine is also available as WebApp(for iOS and Android) via: www.shimadzu-webapp.euor as app for iPhone in the AppStore.

3SHIMADZU NEWS 2/2014

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It is even possible to see the titlesof books that people in the trainare reading.

Many physical phenomena in reallife are much faster than the topspeed of a high-speed train. Dur -ing explosions a sudden increaseof pressure generates a shockwave. To visualize such effects,recording speeds of 1,000,000 fpsor even higher are needed. Shock -wave research is important for the

aerospace industries in order tounderstand the generation and dis -tribution of shockwaves on thewings of airplanes. At supersonicflights with velocities of 343 m/s(1,225 km/h) the shockwaves arethe subjects of intensive studies.

CFRP (carbon fiber reinforcedplastics) have also attracted atten-tion as high-performance compos-ite materials with high strengthand rigidity, yet low in weight.They are applied in various fieldssuch as automobiles and civil en -gineering. With high-speed videocameras it is possible to recordspecimen fracture, allowing cap-ture of image data of the instantthe CFRP material is fractured.

Unique: 10 million fps – in high resolution

Nowadays, many phenomena inscientific applications elapse in aninstant, leaving no clue to theirsolution. Ultra-high-speed videocameras record such moments, en -abling visualization through slow-motion replay.

The latest development in this ap -plication field is the Shimadzu

Figure 1: HPV-X system configuration consisting of camera head and power supply unit (Laptop PC optional accessory)

Hyper Vision HPV-X High-SpeedVideo Camera equipped with anewly developed proprietary high-speed CMOS image sensor, allow-ing ultra-high-speed recordings at10 million frames per second. ThisCMOS sensor is a unique featureand a key differentiator in com-parison to other high-speed cam-eras systems.

The challenge for all ultra-high-speed cameras is the signal pro-

cessing. The conversion from lightto an electric charge can be real-ized in a very fast and efficientway, but the processing of theanalog signal (electric charge) ishowever the most time-consumingstep.

With the high-speed CMOS sen-sor, the photo diode is connecteddirectly to an in situ-memory.Since there is no sequential read-out operation, there is also nooutput amplifier limitation, there-by enabling high-resolution re -cording even at ultra-high speeds.

High speed meets high resolution

The new HPV-X can record 128frames, 20 % more than the HPV-2at a resolution of 400 x 250 pixels.In HP-mode a double-memoryfunction enables recordings of 256consecutive frames for recordingof even longer periods. This givesthe user the choice of prioritizingeither resolution or recordingtime.

While other high-speed camerasystems lower the resolution asrecording speed increases, the

HPV-X maintains the same highresolution even when recordingspeed is increased. Analog data isstored within the sensor andprocessed afterwards. This featureis included in all Shimadzu HyperVision high-speed video cameras,allowing recordings of ultra-high-speed phenomena in far moredetail.

The HPV-X is able to record at aspeed up to five million images

per second using 100,000 pixels orat a speed of ten million imagesper second using 50,000 pixels.

In contrast to other high-speedcamera systems, the HPV-X isvery compact and easy to use. Justlike previous models in the HyperVision series, the simple systemconfiguration consisting of theHPV-X camera head connected bycable to a laptop computer offersa compact and highly portabledesign making on-site setup espe-cially easy. The same HPV soft-ware that has been so popularwith current users all over theworld is also retained. It featuresintuitive and easy-to-understandsetting screens making it easy tocapture ultra-high-speed videos.

The need to capture high-speedphenomena comes from academicinstitutions and research institutesas well as from various manufac-turing industries. Applicationsinclude fuel injection in combus-tion engines, dispersion of inkdrops by inkjet printers, studieson hydrodynamics, destructionprocesses, shock wave develop-ment and visualization of machin-ing processes as well as fast chem-ical reactions.

A simple real-life example helps to illustrate the advantage of theultra-high-speed recording in com -parison to conventional videocamera systems:

When a high-speed train passesthe station at 180 km/h, the hu -man eye hasn`t time to recognizeany detail, neither of the trainitself nor of anything inside. Aconventional video camera with arecording speed of 25 frames persecond cannot record individualpassengers inside this moving train.A high speed video camera with arecording speed of 4,500 fps (180times faster) allows the visualiza-tion of every detail of the trainand every single passenger inside.

APPLICATION

4 SHIMADZU NEWS 2/2014

B itumen is used in manyeveryday products, like car-peting or roofing paper. Bi -

tumen is best known from roadconstruction; together with min-eral additives, bitumen makesasphalt.

The quality of the bitumen alsodetermines its use. Through theaddition of polymers, such aspolypropylene and styrene-buta-diene-styrene, the material canbecome very viscous. The blendwith polypropylene is called APPplastomeric bitumen and theblend with styrene SBS is calledelastomeric bitumen. These blendsare used as sealing materials and in

Bitumen – it’s all in the mixFTIR spectroscopy determines quality differences

Figure 1: Two infrared spectra of a bitumen with additive (above) and an EVA polymer (below)

roofing paper. Another polymer isEVA copolymer (ethylene-vinyl-acetate), which is for instanceapplied in polymer packaging asan odor barrier.

Quality control using FTIR

Bitumen is the residue from vacu-um distillation of mineral oils.The quality of the bitumen is animportant analytical criterion inorder to be able to better controlthe amounts of additive used. Non-destructive infrared spectroscopycan be used for the analysis. Com -bined with single-reflectance ac -cessories from ATR family, thiscan be easily implemented.

As bitumen can be very viscousby nature, a diamond ATR unit isrecommended. Diamond is robustagainst the cleaning proceduresthat are required after measure-ment. One drop of the samplematerial is sufficient for the 2 mmmeasuring window, which mini-mizes complex cleaning proce-dures. The sample is heated tosoften it in order to enable a bet-ter contact with the measuringwindow. This technique makes itpossible to control the productionprocess.

Detection of the additives

In this application, various typesof bitumen (base bitumen), gradedas 1/10 and 70/100, are explored.The values reflect how the bitu-men performs during the specificneedle test. The needle penetratesthe surface, whereby 70/100 refersto a penetration depth between 70 and 100 tenths of a millimeter.A table with typical values for theneedle test and other specifica-tions is presented below (table 1).

The presence of the additives canbe easily verified in the infraredspectra. Base bitumens and modi-fied base bitumens are comparedwith each other.

The spectrum of the blend clearlyshows changes in signal structure.The signals at 630 cm-1 that can be

attributed to the EVA polymer,are particularly noticeable. Forcomparison, the 1/10 base bitu-men is shown in figure 2.

An additional group of signals at1,693 cm-1 clearly illustrates thedifference: it is a signal of the car-bonyl group (C = O vibration).Using subtraction spectroscopy, itis possible to isolate the additivefrom the spectrum of the blend.Figure 3 shows the result of thissubtraction and the subsequentlibrary search for the identifica-tion of the EVA polymer. Thesubtraction is performed with afactor 1 and can also be furtherrefined.

Quality control of unknown addi-tives can be carried out with thehelp of infrared spectroscopy,wherein the base bitumen is com-pared with the unknown bitumen.

The base bitumen in the exampleis graded as 70/100. Figure 4shows the base bitumen and amodified base bitumen. Visualcomparison shows deviations at630 cm-1, which cannot be attrib-uted to the EVA polymer.

In comparison with the associatedlibraries, the contamination analy-sis function revealed, cross-linkingto polyethylene as main compo-nents, which does not present anyproblem for bitumen, and addi-tives based on phosphate salts.

Figure 2: Infrared spectrum of a 1/10 grade base bitumen


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New family member,improved possibiltiesSALD-7500 for measuring nanoparticles

The signal at 630 cm-1 correlateswith the vibrations of these salts.

Conclusion

The analysis examples presentedhere clearly show that infraredspectroscopy is suitable for theanalysis of various bitumens. Bi -tumen blends can be analyzed andquality control can be implement-ed via comparison of the infraredspectra. Shimadzu’s IRAffinity-1Sand its Golden Gate single-reflec -tance unit, equipped with a dia-mond window, have been used.

Figure 3: Result of the subtraction of the base bitumen from the modified bitumen and the

result of the subsequent library search for identification of the material

Figure 4: Spectra of a 70/100 grade bitumen with additive (red line) and a base bitumen

(black line)

Pen (dmm)Softening point(°C)Retained pene-tration (%)Increase in Softening point(°C)Viscosity at 135 °C (Pa s)

95 88 26

44.6

0.24

67

4.2

46.2

0.56

80

2.2

56.8

0.87

69

4.0

Bitumen 70/100 Bitumen 70/100+ modified clay Bitumen 20/300

Table 1: Typical influence of the additives in bitumen compared to the base bitumen

T he SALD 7-series has been de -veloped specifically for highlysensitive particle measurement

in the submicron and nanometerrange. The successful SALD-7101 isnow being replaced by the SALD-7500.

The SALD-7500 not only builds uponthe excellent qualities of its predeces-sor – Fourier Optics, one light source,one large detector, and one measur-ing theory – but also adds new andimproved features.

Using additional detector elements,the measuring range is now extendedto 7 nm - 800 μm. Samples can bemeasured in the concentration rangeof 0.1 ppm - 20 %. Through revisedand in part completely new accessoriesand new software, the SALD-7500opens up entirely new applicationareas.

The main application area continuesto be the measurement of nanoparti-cles and nanomaterials that are pres-ent in, for instance, sunscreens, cloth-ing, wall paints and even foods. Thesetiny helpers disinfect or protect thehuman body from hazardous UV-radi-ation, for example.

Nanoparticles also impart new prop-erties to materials. Their effects (so-called nanorisks) on the human bodyare, however, still quite unknown. Theactuality of this problem is illustratedby the fact that the EU has, already inmid-2013, introduced labeling require -

ments for nanoparticles in cosmeticproducts. In 2014, this could be fol-lowed by labeling requirements forfoods. Labeling, risk assessment andmeasurement of nanoparticles willbecome more and more important inthe future.

Accessories increase range of applications

The ‘Aggregation Property EvaluationSystem for Biopharmaceuticals’ (Ag -gregate Sizer) offers the new possibil-ity not only to quantitatively deter-mine particle size of biopharmaceuti-cal products, but also their concentra-tions in the range of 100 nm - 10 μm.With a continuous measuring func-tion, changes in size or mass can bemonitored in real time. Measurementdata can be stored at 1-second inter-vals. Mechanical stimulation acceler-ates the agglomeration process.

Nanobubbles are another excitingnew application. Here, the tiniestlong-term stable air bubbles in waterimpart amazing new properties tothis solvent. Water treated in this waycan even exhibit fat-dissolving prop-erties – as if tensides had been ad -ded. But as the water is free of ten-sides, it is now an ideal cleaning sol-vent for semiconductors.

New and yet fully integrated in thefamily – the SALD-7500 is ready totake on a wide range of applications.

Further information

about the IRAffinity-1S:

www.shimadzu.eu/

iraffinity-1s

PRODUCTS

L abSolutions has been thestandard software for newHPLC, UHPLC and GC

systems for many years. Shimadzu’sLC/MS and LCMS/MS systemsoperate under the same platform.In this way it is possible to mutu-ally utilize functions and systemcontrols, i.e. there are no restric-tions regarding HPLC control orthe use of the photodiode-arraydetector for the MS and MS/MSversion.This simplifies, for instance,accessing or switching to a new orunfamiliar analysis technique.

The aim is to gradually enable allShimadzu’s analytical systems tobe operated under this software. A unified user interface simplifieslaboratory operation.

The new LabSolutions DB and CSsoftware packages are available foruse in conventional chromatogra-phy and Fourier transform infra -red spectroscopy (FTIR) and canbe operated from a common userinterface in a laboratory network.

One software for system operation, data acquisition, processing and storage

An integrated database is the heartof the new LabSolutions DB (da -tabase version) and CS (client/server) software packages. De -pending on varying customer re -quirements in different countries,Oracle as well as MS-SQL is sup-ported.

For the user, little changes at firstglance – method parameters, datadescriptions and re-analysis func-tions remain at the same locationand menu structures also remainunchanged. Users will quickly getused to departing from the file-based structure.

This makes it possible to storedata of all analytical instruments

who must ensure that the entiresystem is compliant. The softwareonly fa cilitates compliance.

It is still possible to integrate datafrom other instruments, e.g. labo-ratory balances and UV spec-trophotometers, in the databasevia the CLASS Agent. Bearing inmind the compliance issue alreadymentioned, this is a convenientsolution for report generationsince it simplifies the compilationof reports, including insertion ofadditional calculations, graphs andresults of various detectors withthe help of Microsoft Excel®. In addition to the Agent reportwhich helps to compile reportsdirectly in Excel while allowingfor adjustments, a multi-data re -port creation function is optional-ly available for the advanced user.

This function can merge all ofthese data into an integrated re -port. At first glance, this seems tobe a complex task. However, thetime invested to explore the vari-ous options is worthwhile, as spe-cific calculations can be imple-mented quickly and in accordancewith individual requirements, andcan be saved as templates. Forentry-level users a Flash anima-tion is available which explainsthe individual steps from the ideaof the report content up to the

21 CFR Part 11: User administra-tion and access rights, audit trailsof all actions carried out on theanalytical data and in the soft-ware, as well as an electronic sig-nature of the data. All of these,features which up to now wereonly available via the CLASSAgent in combination with therespective software.

Existing CLASS Agent systemsand their databases can be inte-grated into a LabSolutions CSdatabase. Just as a reminder: pri-mary responsibility for compli-ance lies not with the softwareitself and its functions, but ratherwith the customer/software user

consistently in a common data-base and to enable faster re trievalin a common report. At the sametime, data backup and recovery arebecoming more user-friendly. Onthe positive side for the user, thismeans one software package onlyfor operating various instruments,their data acquisition, data pro-cessing and data storage. Indivi -dual functions are clearly stilldependent on the analytical sys-tem used, but essential workflowsand routines can be used withoutany additional learning effort.

The new LabSolutions DB and CS packages support all functionsrequired by the FDA guideline


LabSolutions concept – one plat-form for all instrumentsNew: LabSolutions DB and CS Software

Figure 1: Real time window LCMS/MS and LC

Figure 2: Home screen LabSolutions CS

(including IRSolution)

Figure 3: Agent concept


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finished template – with time win-dows for copying and participat-ing. For all users already familiarwith Mircosoft Excel®, the AgentReport and its template based re -porting is still available.

Controlling instruments ofother manufacturers

The distinguishing feature of cur-rent chromatography data systemsis the control of instruments ofother manufacturers – each usercan control their analytical sys-tems via one single software inter-face. This requires an exchange ofsensitive information betweencompetitors, which does not al -ways proceed as quickly and aseasily as all parties would like.

In mid-2013 Shimadzu and Agilentagreed to share the control codesfor their LC and GC instruments.Control of Shimadzu’s prominence

und Nexera is carried out viaAgilent’s OpenLAB Software; con-versely, LabSolutions CS also con-trols Agilent’s LC- and UHPLCsystems. This is possible via theconsistent implementation of theICF/RC.Net concept introducedby Agilent several years ago.

LabSolutions goes iPad

In modern networks, it is com-mon to make all applications avail-able to all users via one terminalserver in order to avoid the needfor installation of memory-and-resource intensive programs onmany PC’s, while ensuring a highdegree of data security. Moreover,this method offers the advantagethat in a regulated environmentonly one PC needs to be validat-ed, as all users log on to this PC(terminal server) and do not workwith the data and this program on

their local computers. When in -stalled on a terminal server, theLabSolutions CS software offersthe possibility to start data acqui-sition or re-analysis and data evalu-ation.

In such a network setup, it is alsopossible to use the LabSolutionssoftware on an iPad via specialapps – an attractive option whenworking in a confined laboratoryspace. And since electronic labora-tory notebooks and protocolshave already been implemented ine-lab notebook applications, con-nection with a chromatographydata system is surely only a matterof time.

The new DB and CS versions ofthe LabSolutions software meet awide range of requirements: anattractive entry-level version(LabSolutions LITE), a standardworkstation for LC/GC up to adatabase as well as networkdesign. Since upgrades to higherversions are possible for all ver-sions, a user can switch from a‘simpler’ version to a more com-

Figures 4a and 4b: Multi data report and Flash screenshot

Figures 5a and 5b: Screenshot of Agilent’s LC control

plex software version dependingon available budget and the task at hand.

LabSolutions DIRECT – the smartphone can carry out LC

Whoever prefers to remotelyoperate and monitor the HPLCsystems can control via the cur-rent LabSolutions software ver-sion 5.57 (and of course also laterversions) the LC instruments,browser-based and wireless viasmartphone.

The following instruments andsystems are currently supported:iPhone 4S, iPhone 5, iPod touch(4th generation), iPad (1st to 4th

generation) as well as Android 2.3to 4.0; for LC systems a new sys-tem firmware may be required.

PRODUCTS


P art of Shimadzu’s vast rangeof accessories for UV-VISNIR-spectrophotometers is

the wide variety of cell holders.They are available with or withouttemperature control and allowsystem configurations tailor-madefor all requirements of the envi-ronmental, pharma, food and lifescience applications, and manymore. Whether a single standardcell at room temperature is usedor a cell holder for high tempera-ture measurements is required –the Shimadzu product portfoliocovers each analytical problem.

The latest release in the Europeanmarket is the TCC-100, a thermo-electrically temperature-controlledsingle cell holder. The TCC-100

Figure 1 shows the UV-1800 incombination with CPS-100. Fur -thermore, the TCC-100 can beused in the following spectropho-tometers: UVmini-1240 series,UV-2600/UV-2700 and UV-3600.

includes a reference cell using aPeltier element for temperaturecontrol and does not require anexternal cooling water device. Thetemperature control range is from7 °C to 60 °C with a precision of+/- 0.1 °C.

In combination with a spectro -photometer such as UV-1800work ing in kinetics mode, the sys-tem can be used to measure en -zyme activity. Tests like these arevery sensitive to temperature. It istherefore absolutely necessary tomaintain a stable temperature dur-ing the sample measurement. Theideal solution for regulating thecell temperature is a Peltier-con-trolled cell holder, without exter-nal water circulator.

New accessory for UV-VISspectrophotometersTCC-100 – thermoelectrically temperature-controlled cell holder

Figure 1: UV-1800 with TCC-100

measurement of trace levels byreducing the background noisefrom the organic solvent, which isnow separated more easily.

The oxygen kit can be helpful withmany different types of organicsolvents, such as kerosene, xylene,methyl isobutyl ketone (MIBK),isopropyl alcohol (IPA), and ethylalcohol.

To show some typical limits ofquantification (LOQ), differentelements were analyzed in toluene(figure 2). In this case, the limit ofdetection (LOD) was about a thirdof the LOQ.


APPLICATION

T o evaluate elemental pollu-tion in petrochemical appli-cations, it is necessary to

measure organic samples in a di -rect way without any dilution,since concentrations may alreadybe very low. For fast multi-ele-ment analysis, Shimadzu’s ICPE-9000 is most suitable.

The Ar/O2 Mixed Gas Supply Kitis recommended for obtaininghighest sensitivity in the measure-ment of organic solvents. This kituses a special 4-way Quadrupletorch (figure 1). An additional gas(Ar + O2) is mixed with the carri-er gas flow, resulting in high oxi-dizing power. This allows the

Searching for elemental traces in petrochemicalsThe high-precision ICPE-9000 inductively coupled plasma optical emission spectrometer

Figure 1: Sample introduction and torch

Figure 2: Calibration and LOQ of some elements in toluene

An application note focussing onhighest sensitivity of tin (Sn) intoluene is available by scanning theQR code:

www.shimadzu.eu/sites/default/files/AN_SCA_115_021%20Toluene%20Oxygen%20Kit.pdf

Simply scan the QR code.

Application Note ‘Deter -

mination of Trace Elements

in Toluene using ICPE-9000

and Oxygen Kit’

APPLICATION

C olor can be of decisive sig-nificance for the marketingsuccess of a product. Espe -

cially when using natural or recy-cled raw materials with fluctuatingchemical composition, color canvary strongly – for instance in theproduction of packaging glasses.Continuous and objective controlof the color effect is therefore anessential precondition for an un -changing and reproducible quality.

Color measurement

Color is a not just physical char-acteristic of materials but rather a

To this day, these so-called color-matching functions have been thebasis for color determinationaccording to ISO 11664 and otherstandards.

For the calculation of color val-ues, a suitable spectrophotometer(for instance Shimadzu’s UV-1800)was used to record a transmissionor a reflection spectrum (depend-ing on the application) in the visi-ble range of the electromagneticspectrum (380 to 780 nm). Thisspectrum is subsequently weight-ed against a standardized lightsource (D65 for daylight or A for

sensory perception that is stronglydependent on environmental con-ditions (especially on lighting) andthe observer (human). Color isper ceived, so to speak, in the eyeof the observer. For objective de -termination of color values, thespectral sensitivity of the humaneye for the three primary colorsred, green and blue (there is a cor-responding number of sensory celltypes in the retina) was deter-mined by empirical experiments inthe 1930’s, and the CIE ColorSpace was published by the Inter -national Commission on Illumi -nation.


Exact measurement of colorNew software for color determination in the industrial sector with direct control using Shimadzu’s UV-VIS spectrophotometers

incandescent light) in order totake into account the influence ofthe illumination. Subsequently, thespectrum is successively weightedagainst the three CIE color-match -ing functions to determine the redcomponent (X), the green compo-nent (Y) and the blue component(Z) of the spectrum. Using thesethree values, any color can beunequivocally characterized.

In practice, however, the tristimu-lus values X, Y and Z are usuallynot applied directly. Instead theCIELAB system, in which colorperception is specified by the

Figure 1: All measurement parameters necessary for measurement are summarized

in methods

Figure 2: During measurement, the corrected spectrum is displayed in addition to the

raw data


APPLICATION

three values L* (brightness), a*(red-green ratio) and b* (blue-yel-low ratio) has become established.These values, however, are mathe-matically derived from the tristim-ulus values X, Y and Z so that theinformation content is the same.Alternatively, the CIExy systemin which color perception is ex -pressed by three values DWL (do -minant wavelength), S (saturation)and A (brightness) is still appliedin many industrial sectors. Butthese values are also based on thetristimulus values X, Y and Z.

Industrial practice

In industrial production processes,color is usually determined at ran-dom on the basis of representativesamples. Color measurement isoften carried out in an on site labo-

ratory, but more frequently colordetermination is moving closer tothe production line, in order to beable to react faster in case of colordeviations. Personnel, which hasbeen specially trained for this task,is often not available at the pro-duction line, whereby the demandson the software significantly in -crease. The software must be easyto use, fast to operate and must beable to rule out operating errors aswell as possible. In order to recog-nize trends quickly and to be ableto immediately intervene, statisticalevaluation in the form of qualitycontrol charts is indispensible. Thedata should, therefore, be automat-ically transferred to an on site dataacquisition system. Ideally, thesoftware itself features an integrat-ed database and correspondingevaluation options.

Color measurement using Chroma

The Chroma software was devel-oped to fulfill the above require-ments in routine analysis. Theprincipal feature of the software isthe clearly structured user inter-face that is tailored to the work-flow and user roles. All requiredmeasuring parameters for themeasurement are summarized inso-called methods (figure 1). Priorto measurement, only the missingsample parameters must be added– for example the sample thick-ness for transmission measure-ments. The transformations de -fined in the method, such as con-version to a fixed standard thick-ness, are already taken into ac -count during the measurementand the corrected spectrum is dis-played in addition to the rawspectrum.

After data storage the user is au -to matically directed to the analy-sis mode, in which all results areexpressed in terms of numbersand graphs (figure 3). Here, thepossibility exists to print the re -sults or to export them to otherprograms for additional process-ing. Furthermore, certain parame-ters can be modified later on inthe analysis mode, without affect-ing the results that are alreadystored in the database.

All measurement results in theChroma software are archived inan integrated database and can beretrieved and evaluated at any

time. To organize the measure-ments, it is possible to define anyattribute according to which canbe filtered in the archive (figure 4).Alternatively to display in tabularformat, the data can also be graphi -cally displayed in the form oftrend diagrams (figure 5). Thisway, it is possible to easily recog-nize trends in the development ofcertain color values and to takesuitable measures.

Summary

Using the Chroma software pack-age and a Shimadzu UV/VIS spec-trophotometer, spectral character-istics of glasses and other materi-als can be accurately determinedand color values can be calculatedand graphically displayed. Chro -ma combines measurement andevaluation with a high-perform-ance database in which all resultsare stored in a structured manner.Chroma fulfills the requirementsin routine analysis and qualitycontrol and meets the highestdemands in research and develop-ment through its flexible evalua-tion options and statistical func-tions. Chroma is always intuitive,simple and reliable to use.

Author:Henning Katte, ilis GmbH Erlangen

Figure 3: In the analysis mode, all results are numerically and graphically displayed in a

well-organized manner

Figure 4: All measurement results are archived in an integrated database

Figure 5: The trend view shows the development over time of a selected color value

treated with chloroform gas in asuitable apparatus (e.g. a desicca-tor) over an extended period oftime of at least 24 hours. This de -stroys the cell walls and kills offthe microorganisms. After fumiga-tion, the chloroform remaining inthe soil is removed.

DOC is determined first

Subsequent to fumigation, eachfumigated subsample and onenon-fumigated soil sample ismixed with a 0.5 M (mol/L) po -tassium sulfate solution and thenshaken. After filtration of the elu-ate, the DOC (dissolved organiccarbon) of the extracts is deter-mined. Since experience has shown,not all cells are destroyed and ex -tracted, and an empirical correc-tion factor is additionally applied.(An exact description of the fumi-gation-extraction method is foundin the EN ISO 14240-2:2011 stan-dard).

DOC analyses of the potassiumsulfate extracts are carried outusing a TOC analyzer. In thisprocedure, the extract is mixedwith an acid to remove the inor-ganic carbon fraction, wherebycarbonates and hydrogen carbon-ates are converted to CO2. Thecarbon dioxide is purged from thesample using a purging gas. Analiquot of the pretreated extract issubsequently injected onto a hot

APPLICATION

F ertile soils contain a multi-tude of microorganisms.They are responsible for the

degradation of organic substancesand protection of the nutrientcycle. To evaluate soils in terms oftheir biodegradability and theirfertility, the microbial biomass ofthe soil, i.e. the organic carbonfraction that is bound to thesetiniest organisms, is determined.

The fumigation-extraction methodis a commonly used method forthe determination of microbialbiomass in soils. The microbialbiomass is described regardingextractable organic carbon com-pounds before and after killing offthe microorganisms.

In the fumigation-extraction meth -od, a subsample of the soil is


Determination of microbial TOC in soil science

Concentration [mg/L]

Are

a

Figure 1: Automated NPOC calibration in the range of 1 to 10 mg/L

0

21

28.8915

14

7

0 11108642


APPLICATION

platinum catalyst, whereby theorganic substances are oxidized toCO2. A carrier gas transfers thecarbon dioxide to an NDIR detec-tor, which detects the amount ofCO2.

Kit for high salt loads

For many TOC analyzers, thehigh salt loads of the extracts can,however, cause problems. The ex -traction solution alone has a saltload of approximately 87 g/L.High salt loads can lead to clog-ging of the catalysts and the com-bustion tubes. When the combus-tion temperature is too high, thesalts form a melt that blocks theactive sites of the catalyst.

Therefore, Shimadzu’s TOC-Luses a catalytic combustion tem-perature of 680 °C, which is lower

biomass in soils

Sign

al [

mv]

Time [min]

Figure 2: Injection 1 - 20

-20

20

14

7

0 40302010

Sign

al [

mv]

Time [min]

Figure 3: Injection 581 - 600

-20

20

14

7

0 40302010

than the melting point of mostsalts. In addition, a special kit forhigh salt load samples is availablefor such measuring tasks. It con-sists of a combustion tube featur-ing a specific geometry and aunique catalyst mixture. This par-ticular catalyst can handle up to12 times more salt than a conven-tional catalyst.

Long-term test with 600 injections

A long-term test should show thatan application, such as the analysisof soil extracts from a 0.5 M po -tassium sulfate solution can becarried out problem-free using akit for high salt load samples. Forthis test, a 0.5 M K2SO4 solution(corresponding to 87 g/L) wasinjected 600 times onto the kit forhigh-salt samples.

Method parameters

NPOC preparation: automated usingthe ISP module of the TOC-L analyzer

Acidification: 2 %

Sparging: 6 minutes

Injection volume: 50 μL

Calibration: 6-point calibrationusing the automated dilution func-tion, from a stock solution in therange of 0.5 mg/L to 10 mg/L.

Results

Even after 600 injections, the peakshapes remain exactly the same asat the start of the injection series.The results remain stable over theentire time period. As one can see,the TOC-L in combination withthe kit for high salt load samplesis highly suitable for TOC deter-mination of salt-containing sam-ples, such as soil extracts from a0.5 M potassium sulfate solution.

Figure 4: Sequence (area and concentration) of the 600 injections

02468

101214161820

116 31 46 61 76 91

106

121

136

151

166

181

196

211

226

241

256

271

286

301

316

331

346

361

376

391

406

421

436

451

466

481

496

511

526

541

556

571

586

Table 1: Statistical evaluation of the 600 injections

Mean valueStandard deviationStandard deviation in %

17.010.3922.3

6.660.1532.3

Area NPOC concentration [mg/L]

IMPRINT

Shimadzu NEWS, Customer Magazine of Shimadzu Europa GmbH, Duisburg

PublisherShimadzu Europa GmbHAlbert-Hahn-Str. 6 -10 · D-47269 DuisburgPhone: +49 - 203 - 76 87-0 Fax: +49 - 203 - 76 66 [email protected]

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CopyrightShimadzu Europa GmbH, Duisburg, Germany – April 2014.

Windows is a trademark of Microsoft Corporation. ©2014

Apple Inc. All rights reserved. Apple, theApple logo, Mac, Mac OS and Macintoshare trademarks of Apple Inc.

APPLICATION

A mino acids are of vital im -portance for human life.They are the basis for each

and every metabolic pathway inthe body, since they serve as trans -port or storage medium. Aminoacids are components of protein-containing foods and are also usedin cosmetics, such as skin care pro -ducts and shampoos.

Proteinogenic amino acids are thebuilding blocks of proteins in liv-ing organisms. The 20 L-aminoacids are each encoded by threenucleic acids. Of these, 12 aminoacids are synthesized by the hu -man body, for instance by micro -organisms that live in the humandigestive tract. The remaining 8amino acids are essential for hu -mans, meaning that they must beabsorbed from foods containinganimal proteins or a suitable com-bination of plant proteins.

Valine, methionine, leucine, iso -leucine, phenylalanine, trypto-phan, threonine and lysine areessential amino acids for humans.Semi-essential amino acids, how-ever, only need to be absorbedfrom foods in certain situations,for instance during growth or se -rious injury. The remaining aminoacids are either synthesized direct-

bolic pathways for standard ami -no acids.

Amino acid analysis

There are many possibilities foranalyzing amino acids. The mostcommonly used methods are car-ried out via automated pre-col-umn or post-column derivatiza-tion. The UF-Amino Station, de -veloped in cooperation with theinternational food manufacturerAjinomoto, uses automated pre-column derivatization with a spe-cial reaction reagent.

Figure 2 shows the schematic de -sign of the UF-Amino station. Allnecessary reagents such as aminoacid standards, internal standard,reaction reagents and eluents arecommercially available from WakoChemicals, Neuss, Germany. Af -ter mixing of all the reagents, theproduct mixture is left standing inthe reaction unit for a short timeat 60 °C to complete the derivati-zation. The derivatizated aminoacids obtained are injected ontothe analytical column (ShimpackUF-Amino 2.0 μm, 2.1 x 100 mm)via an injection loop, installedwithin a switching valve, and sub-sequently detected using the

ly or derived from other aminoacids through modification andare, therefore, referred to as non-essential.

In addition to 20 standard aminoacids, there are many non-stan-dard amino acids which often oc -cur as intermediates in the meta-


Amino acids – fast and simple iden -tification UF-Amino Station enables high-throughput analysis

Figure 1: UF-Amino Station

Figure 3: AmiNavi™ Software

Figure 4: Analysis – Color highlighting of the

individual sample positions of the batch

Figure 5: Processing – Calibration curve of

the individual substances

Figure 6: Overview table of the concen-

trationsFigure 2: Flow diagram for derivatization and injection


APPLICATION

The calibration curve is createdautomatically according to thepreset method and can, wheneverrequired, be very easily modifiedor adapted via manual integration.An overview table which showsthe concentrations of the individ-ual amino acids can be printed as a report

Investigation of a standard mix-ture containing 38 amino acidswith the UF-Amino Station resultsin good separation between theindividual substances and goodsensitivities for identification andquantification – which can beevaluated very easily using theAmiNaviTM software.

Figure 7 shows the correspondingchromatograms as depicted withthe LabSolutions software.

As an example for one of manyapplications, figure 8 shows theamino acids contained in culturemedia. Here, it is possible to in -vestigate continuous monitoringof the amino acid. An example forthe amino acids contained in meatis shown in figure 9. This methodcan be used for quality control inthe food industry.

High-throughput analysis

The fully automated derivatiza-tion by the UF-Amino Stationand the easy-to-use AmiNaviTM

software for starting and evaluat-ing sample sequences enableshigh-throughput analysis of up to38 amino acids. Compared to oth -er methods, fast chromatographyand automatically performed, par-allel derivatization can result inconsiderable savings in time peranalysis, as illustrated in figure 10.

LCMS-2020 single-quadrupolemass spectrometer.

Specifically developed software

The AmiNaviTM software, specifi-cally developed for the UF-AminoStation, supports users in settingup complete analyses and evalua-tion of samples. After enteringsample names, a batch with thedesired number of standards,blank injections and samples iscreated automatically. This is thenillustrated via color highlightingof the positions of the individualsubstances in a deep-well plate, sothat filling of the wells is greatlysimplified.

[1] Paula Yurkanis Bruice: Organic Chemistry,

Pearson Education Inc., 2004, 4th Edition,

p. 960 - 962

Minutes

Figure 7: 38 Amino acids

0

1,000,000

2,000,000

3,000,000

4,000,000

5,000,000

6,000,000

7,000,000

8,000,000

9,000,000

10,000,000

11,000,000

12,000,000

13,000,000

14,000,000

15,000,000

0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0

Minutes

Figure 8: Amino acids in culture media

0

250,000

500,000

750,000

1,000,000

1,250,000

1,500,000

1,750,000

2,000,000

2,250,000

2,500,000

2,750,000

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5

Figure 9: Amino acids in meat

0

50,000

100,000

150,000

200,000

250,000

300,000

350,000

400,000

450,000

500,000

Minutes0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5

Table 1: 20 standard amino acids – *essential for children and pregnant women

AlanineArginineAsparagineAspartic acidCysteineGlutamineGlutamic acidGlycineHistidineIsoleucineLeucineLysineMethioninePhenylalanineProlineSerineThreonineTryptophaneTyrosineValine

AlaArgAsnAspCysGlnGluGlyHisIleLeuLysMetPheProSerThrTrpTyrVal

non-essentialsemi-essentialnon-essentialnon-essentialnon-essential*non-essentialnon-essentialnon-essentialsemi-essentialessentialessentialessentialessentialessentialnon-essentialnon-essentialessentialessentialnon-essential*essential

9.0 %4.7 %4.4 %5.5 %2.8 %3.9 %6.2 %7.5 %2.1 %4.6 %7.5 %7.0 %1.7 %3.5 %4.6 %7.1 %6.0 %1.1 %3.5 %6.9 %

Amino acid Three-lettercode Comment Ø in proteins*

Figure 10: Time comparison of various amino

acid analysis methods

0.00.51.01.52.02.53.03.54.04.55.05.56.06.57.07.58.08.59.0

(x 10.000.000)

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5 35.0

Figure 2: Pyrogram of the elastomer sample A, butyl rubber (result of the library search

of several significant peaks: 1. Isobutene; 2. Isoprene; 3. 1,3-Pentadiene, 2,4-dimethyl-;

4. 1-Pentene,2,4,4-trimethyl-; 5. 2-Pentene,2,4,4-trimethyl-; 6. Hept-2-ene 2,4,4,6-tetrame-

thyl-; 7. l-Limonene).

Figure 3: Pyrogram of the elastomer sample D, butadiene rubber (result of the library

search of several significant peaks: 1. Cyclobutene; 2. Benzene; 3. 1,3-Cyclohexadiene;

4. Benzene, methyl-; 5. Cyclohexene, 4-ethenyl-; 6. Styrene).

0.00

0.25

0.55

0.75

1.00

1.25

1.50

1.75

2.00

2.25

2.50

2.75

3.00

3.25

3.50

(x 10,000,000)

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0

APPLICATION

concentrations of the starting ma -terials and additives can be detect-ed.

During pyrolysis GCMS, approxi-mately 200 μg of the sample mate-rial is decomposed directly in apreheated furnace at temperaturesbetween 400 and 800 °C typically.The resulting pyrolysis productsare separated chromatographicallyon a GC capillary column andsubsequently detected using amass spectrometer. Due to theway of sample introduction andthe chromatographic separation, itis possible not only to analyzevery small amounts but also toobtain valuable, detailed addition-al information – in comparisonwith other methods in polymeranalysis such as FTIR, TGA orHPLC.

Selecting the detector

Characteristic chromatograms or‘pyrograms’ are obtained using aflame ionization detector (FID) aswell as via mass spectrometry de -tection. These pyrograms act as‘fingerprints’ and are used to iden -tify polymers unequivocally viacomparison. When using an FID,it is only possible to use retention

used, specialized progressive ana-lytical methods are applied.

Pyrolysis GCMS (coupled gaschromatography-mass spectrome-try) is an excellent technique forthe analysis and characterizationof polymers. Using this technique,which avoids time-consumingsample preparation, minimal dif-ferences between two samplessuch as impurities or fluctuating

ble, inert to solvents, and fire re -sistant. This is why verification ofthe desired properties duringmaterial development or post-pro-duction control is of great inter-est.

Physical and chemical test meth-ods help to characterize polymerproperties. In order to determinethe chemical composition of aplastic or the type of additive


A small, subtle distinctionTrace analysis in polymers using pyrolysis GCMS

Figure 1: Pyrolysis GCMS

S ynthetic polymers or plasticsare omnipresent. They areprocessed into products such

as polyethylene garbage bags, poly -propylene bicycle helmets or high -ly specialized materials for medi -cal technology, sports, construc-tion or research.

Initially, they were only used assubstitutes for valuable or rarematerials. But they also possessunusual properties that other ma -terials do not offer. For instance,plastics can be tailored to specificapplication areas in order to attaincertain chemical, mechanical orelectrical characteristics. This isachieved through selection ofstarting materials, the addition ofadditives and the production pro -cess. Chemical additives such asantioxidants, stabilizers or flame-retardants can change the charac-teristics of a product already invery low concentrations.

Polymer characterization via pyrolysis

Expectations of the material prop-erties of plastics are high – de -pending on the application area,they should be resistant to weath-ering, shape-and-temperature sta-


APPLICATION

times for the identification of in di -vidual peaks. Mass spectrometrydetection yields a mass spectrumfor every peak, pro viding informa-tion on the structure of a substance.By comparing the mass spectrawith those stored in specializedlibraries, in dividual componentscan be definitely iden tified. Usingcharacteristic mass traces, it is alsopossible to detect and quantifyvery low concentrations of sub-stances in highly complex pyro-grams.

Trace analysis in rubber samples

The following example demon-strates the performance of a pyro -lysis GCMS system in the detec-tion of traces of a compound in apolymer sample. Figure 2 showsthe pyrogram of an elastomer sam-ple A. The sample is a butyl rub-ber (copolymer of 95 - 99 % iso -butene and 1 - 5% isoprene). Elas -tomer sample D is a pure butadi-ene rubber (see figure 3), which isused widely in the rubber world.Sample C is also a butadiene rub-ber, as can quickly be identifiedbased on its virtually identical fin-gerprint (see figure 4). But thiselastomer is a blend of butadieneand butyl rubber. The concentra-tion of the butyl rubber is be -tween 0.5 - 3 %, which is in thetrace range. Is it possible to detectthis minimal amount in the pyro-gram of sample C?

The pyrograms of the three sam-ples were directly compared.

When looking closely at individ-ual enlarged sections, peaks can befound in sample C that are un -equivocally identified as pyrolysisproducts of a butyl rubber.

To illustrate this peak assignmentmore clearly, a certain mass trace(here: m/z 112) is calculated fromthe TIC (total iron current) andthe corresponding section of thepyrogram is enlarged. At retentiontimes 12.17 and 12.56 seconds,there are two peaks that can onlybe detected in sample A (blackmass trace) and in sample C (redmass trace) but not in sample D(blue mass trace) – see figure 5.

Comparison of the mass spectra in figures 5a and 5b shows that itis clearly the same substance. Inthis way, additional peaks can befound that confirm the presence oftraces of butyl rubber in the buta-diene rubber (see figures 6 and 6a).

Data reproducibility

An important requirement for thisefficient trace analysis is data re -producibility. In pyrolysis, thisdepends greatly on the heating-uptime of the sample.

Characteristic for a furnace pyro -lyzer is the preheated, accuratelytemperature-controlled furnace inwhich the sample falls (free fall)and is heated in a fraction of amillisecond. �

Figure 4: Pyrogram of the elastomer sample C, butadiene rubber with traces of butyl

rubber. (Results of the library search of several significant peaks: 1. Cyclobutene;

2. Benzene; 3. 1,3-Cyclohexadiene; 4. Benzene, methyl-; 5. Cyclohexene, 4-ethenyl-;

6. Styrene).

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5(x 1,000,000)

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5 30.0 32.5

Figure 5a: Comparison of mass spectra of the peaks at 12.17 minutes

Figure 5b: Comparison of mass spectra of the peaks at 12.56 minutes

(x 1,000,000) Base Peak: 57/2,199,753

0.0

1.0

2.0

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

m/z Abs. Inten. Rel. Inten.

Data 1: Sample_A03.qgd · R.T. [12.143 –> 12.217] - [12.300 –> 12.350] · Scan# · [3584 –> 3606] - [3631 –> 3646]

(x 10,000) Base Peak: 57/11,314

0.0

0.5

1.0

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0


Data 2: Sample_C03.qgd · R.T. [12.163 –> 12.240] - [12.323 –> 12.370] · Scan# · [3590 –> 3613] - [3638 –> 3652](x 10,000) Base Peak: 66/32,682

0.01.02.03.0

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0


Data 3: Sample_D03.qgd · R.T. [12.143 –> 12.217] - [12.300 –> 12.350] · Scan# · [3584 –> 3606] - [3631 –> 3646]

(x 1,000,000)

0.0

0.5

1.0

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 1: Sample_A03.qgd · R.T. [12.537 –> 12.607] - [12.677 –> 12.797] · Scan# · [3702 –> 3723] - [3744 –> 3780]

Base Peak: 97/1,207,648

m/z 311,70 Abs. Inten. 1 Rel. Inten. 0,00

(x 1.000)

0.02.55.07.5

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 2: Sample_C03.qgd · R.T. [12.560 –> 12.672] - [12.697 –> 12.820] · Scan# · [3709 –> 3729] - [3750 –> 3787]

Base Peak: 97/8,153


(x 10,000)

0.0

1.0

2.0

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 3: Sample_D03.qgd · R.T. [12.537 –> 12.607] - [12.677 –> 12.797] · Scan# · [3702 –> 3723] - [3744 –> 3780]

Base Peak: 54/21,317


Figure 5: Detail of the comparison of mass traces m/z 112 of 11.8 to 13 minutes of

sample A (black), sample C (red) and sample D (blue)

(x 10,000)

-0.10.00.10.20.30.40.50.60.70.80.91.0

11.8 11.9 12.0 12.1 12.2 12.3 12.4 12.5 12.6 12.7 12.8 12.9 13.0

FID_Sample_E_repro02.gcdFID_Sample_E_repro03.gcdFID_Sample_E_repro05.gcdFID_Sample_E_repro06.gcdFID_Sample_E_repro07.gcdFID_Sample_E_repro08.gcdFID_Sample_E_repro09.gcdFID_Sample_E_repro10.gcdFID_Sample_E_repro11.gcdFID_Sample_E_repro12.gcdAverage% RSDMaximumMinimumStandard Deviation

9.3149.3149.3259.3169.3149.3129.3219.3159.3179.3199.3170.0409.3259.3120.004

1160042131302715958181308772153422210950071516246131804413969711512641137507912,110

15958181095007166521

22.11521.30022.28121.75321.34422.26522.45921.94021.94722.11221.9521.765

22.45921.3000.387

ID#1 Compound name: C

Data file Ret. time Area Con. [%]

APPLICATION


The sample is placed in a deacti-vated stainless steel cup that iscleaned quickly and easily via redheating with a small torch.

Due to the minimal heating-uptime, the loss of volatile compo-nents is prevented and high repro-ducibilities can be achieved. Theoptimized interface between pyro -lyzer and gas chromatograph min-imizes dead volumes and coldspots, thereby preventing poorlyreproducible peaks.

Figure 7 demonstrates the excel-lent reproducibility of the pyroly-sis GCMS system in eight consec-utive measurements of a styrene-butadiene polymer blend. If de -sired, the system can be equippedwith an additional FID (flame ion-ization detector). Reproduci bilitymeasurements of the sty rene-buta -diene polymer blend were also car -ried out using this detector.

Table 1 lists some statistical detailsof the evaluation of one significantpeak (peak C: butadiene dimer).Quantification was carried out viathe area normalization or area %method, which can yield verygood results even when the indi-vidual samples could not beweighed. For quantitative analysisof pyrolysis GCMS data, quantifi-cation of characteristic SIM masstraces (single ion monitoring)using the internal standard meth -od is recommended

Valuable time savings using an autosampler

For all measurements shown here,an autosampler was used to intro-duce the samples in the EGA/PY-3030D pyrolyzer. Autosamplersoffer a great advantage when manysamples need to be analyzed. Thesample carousel can be loadedwith 48 stainless steel cups, and

programming of a sequence tabletakes place via a simple, user-friendly interface.

Summary

Pyrolysis GCMS is a modern,high-performance technique foraccurate characterization andquantification of synthetic poly-mers and biopolymers. The appli-cation possibilities are extensiveand range from plastics manufac-turing and processing, automotiveand paper industry, wood andresins analysis to paints, varnishes,adhesives and applications in fo -rensics, art and archaeology.

This application provides just aglimpse of the capabilities of theEGA/PY-3030D pyrolyzer fur-nace. Using the specialized sam-plers, it is also possible to selectvarious sampling methods such asthe double-shot technique, reac-tive pyrolysis or sample irradiat-

Figure 6: Detail of the comparison of mass traces m/z 97 from 19.5 to 27 minutes of

sample A (black), sample C (red) and sample D (blue). Presence of the butyl rubber can

be found at 20.45 and 25.92 minutes.

0.51.01.52.02.53.03.54.04.55.05.56.06.57.07.58.08.5

(x 100,000)

19.5 20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0 24.5 25.0 25.5 26.0 26.5 27.0

Figure 6a: Comparison of the mass spectra of the peaks at 20.45 minutes

(x 1,000,000) Base Peak: 97/4,134,504

0.0

2.5

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 1: Sample_A03.qgd · R.T. [20.410 –> 20.500] · Scan# · [6064 –> 6091]


(x 10,000) Base Peak: 97/37,902

0.0

2.5

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 2: Sample_C03.qgd · R.T. [20.410 –> 20.500] · Scan# · [6064 –> 6091]


(x 10,000) Base Peak: 97/37,322

0.0

2.5

25.0 50.0 75.0 100.0 125.0 150.0 175.0 200.0 225.0 250.0 275.0 300.0 325.0 350.0 375.0 400.0 425.0 450.0 475.0 500.0

Data 3: Sample_D03.qgd · R.T. [20.410 –> 20.500] · Scan# · [6064 –> 6091]


Figure 7: Comparison measurements (8 runs) of a styrene-butadiene polymer blend

using pyrolysis GCMS

0.00

0.25

0.50

0.75

1.00

1.25

1.50

1.75

2.00

2.25

2.50

2.75

3.00

3.25

(x 100,000,000)

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 30.025.0 27.5

ing with UV-light in order to sim-ulate aging processes. In addition,standard EGA (evolved gas analy-sis) measurements using an ex -tremely short capillary columnwithout stationary phase are pos-sible, for instance to determine theoptimum pyrolysis temperature ofa sample.

Table 1: Statistical evaluation of comparison measurements (10 runs) using pyrolysis FID

F oods as a basic need of hu -man existence are subject toconstant inspection. The

Shimadzu News reports regularlyon new analytical capabilities.

In addition to taste and the inspec -tion of ingredients, questions arealways raised on the physical pro -perties of our food: how quicklydoes our bread get stale? Howcrisp are our sausages? What arethe differences between eggshellsoriginating from different eggfarming methods? ... These are thequestions that will be addressed inthis and in subsequent issues ofthe Shimadzu News – using thefoods that make up a continentalbreakfast.

due to drying out of baked goodsthat were packaged in paper bags.Only in the case of the crusty ryebread bought at the supermarketcould a lower value be measuredafter 24 hours of storage.

As a slight increase could also bemeasured for the crusty breadobtained from the bakery, it canbe concluded that the crumbs inthese baked goods have a muchhigher moisture content comparedto the small baked goods. Thisensures that the bread dries outmuch more slowly. For bakedgoods from the discount super-market, the crust apparently soft-ened over 24 hours. This is why adecrease in force was registered.This could, however, also indicatethat the baking time was too shortso that the bread was not com-pletely baked.

Overall, it can be concluded thatthe measured values for productspurchased at the supermarket andthe bakery were similar and werestill edible after 24 hours. Signifi -cant changes could only be ob -served after 72 hours. Many prod-ucts had by then become so hardthat they were no longer fit forconsumption. Another proof ofwhy Europeans like to enjoy theirbaked goods freshly baked eachday ...

To be continued ...*

*For those of you who cannot wait for the

next breakfast test, the entire text can be

downloaded in advance.

www.shimadzu.eu/breakfast-test

mately 66 kg/year, Europe holds aleading position in the worldwideconsumption of bread. With near-ly 70 percent, fresh baked breaddominates, prior the frozen bak-ery products, fast food bread andlong-life bakery products.

Bakery or supermarket – whichoffers the freshest products?

It is not surprising that freshlybaked goods are usually found atthe European breakfast table.Depending on local tastes, thesecould be breads, baguettes or cia-battas; the main issue is the fresh-ness of the products. In additionto traditional bakeries, freshlybaked goods from on site bakingovens are increasingly being offeredin supermarkets.

Yet, how fresh are these bakedgoods and are there any differ-ences in texture and shelf life?Shimadzu has tested several bakedgoods from a bakery and super-market chosen at random.

To get upon the freshness’ track

Various baked goods were sub-jected to a compression test usingthe EZ Test-X Texture Analyzer,where pressure plates simulate apressure test applied with thepalm of a hand. In this way, thestiffness/chewiness of the crust aswell as the crumb is tested. Thebaked goods were removed fromtheir commercial packaging, andeach set was tested one hour afterpurchase, thereafter 24 hours and72 hours after purchase:

As expected, a very strong in -crease in the texture of all breadshas been measured. This is mainly

Bread has been a basic food in theWestern world for thousands ofyears. With an average bread con-sumption per capita of approxi-

The daily breadThe big breakfast test using the EZTest EZ-X texture analyzer (part 2)

Figure 1: Bread firmness test using Texture Analyzer EZ-Test-LX with ø 50 mm compression jig

Table 1: Compression test of bread


APPLICATION

Croissant

Ciabatta

Wheat bread rolls

Multigrain roll

Baguette

Crusty rye bread

ABABABABABAB

54.54736353065

10050473620

1624

255291

5744

142160125100

3226

8582

700305160

801,7001,900

670520125

90

Bakery productsDiscount supermar-ket (A) – bakery (B)

Max. force (N)after 1 hour

Max. force (N)after 24 hours

Max. force (N)after 72 hours

APPLICATION

C limate change due to globalwarming is taking placemuch faster than expected

[1] – according to the clear warn-ing in the most recent report ofthe ‘Intergovernmental Panel onClimate Change’ (IPCC). This is areason for developing more effi-cient methods for monitoring

Through innovative technology, ahighly sensitive universal detec-tion system with a hitherto unsur-passed long-term stability has beendeveloped. In this way, the BIDbridges an application gap to theflame ionization detector (FID),the most commonly used detectorin gas chromatography.

The FID is popular because of itsexceptional combination of sensi-tivity, reproducibility and long-term stability. Unfortunately, theFID detection spectrum lacks per-manent gases such as oxygen, ni -trogen and carbon dioxide. Sensi -tive measurement of permanentgases in the presence of volatilehydrocarbons, therefore requirescomplex GC configurations usingmultiple detectors.

As the BID is up to 100 timesmore sensitive than a thermal con-ductivity detector (TCD) andtwice as sensitive as a FID, it of -fers an ideal solution for such ap -plications without any significant

plified to a gas chromatographicsystem with only one column andone detector (Tracera System, fig -ure 1).

Innovative plasma technology

The barrier ionization dischargedetector (BID) is a helium ioniza-tion detector based on a novelplasma technology. The heliumplasma is generated inside a quartztube, which serves as a dielectricbarrier (figure 2). In this way, theelectrodes used for plasma genera-tion are protected against possiblecontamination due to columnbleeding, the sample and the plas-ma itself, which considerably im -proves the long-term stability ofthe detector. The light emittedfrom the plasma has an ionizationenergy of 17.7 eV, which enablesthe BID to detect all substancesexcept helium and neon. The ion-ized substances are detected viaelectrodes made of a specially de -veloped Kovar alloy.

contributors to the greenhouseeffect, such as methane (CH4),carbon dioxide (CO2) and nitrousoxide (N2O).

Up to now, this seemingly straight -forward task required a consider-able analytical effort. This is dueto the strongly varying concentra-tions of these components in theatmosphere, which range from thehigh ppm range for carbon diox-ide, to ppm and ppb levels formethane, and even lower to thetrace level below 100 ppb for ni -trous oxide. To meet these analyti-cal requirements, complex GCsystems were needed using two orthree detectors. With the new bar-rier discharge ionization detector(BID), this approach can be sim-


Following the tracesof climate changeNovel plasma technology offers new detection possibilities

Figure 1: GC-2010 Plus with barrier ionization

discharge detector (BID, Tracera System)

The Analytical Scientist – Innovations

Award 2013

Figure 2: Cross sectional drawing though a barrier ionization discharge detector. The lower

half of the detector contains the capillary column and Kovar electrodes for detection. Plasma

generation takes place inside the quartz tube in the upper half of the detector.


APPLICATION

loss in precision or long-term sta-bility. For this reason, leadingEuropean scientists voted the BIDat rank four of the most innova-tive products in the year 2013 [2].

uV (x 1,000)

Minutes

Figure 3: Chromatogram of the standard, 500 ppb methane, carbon dioxide and nitrous

oxide in helium

-1.0

-0.5

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0

uV (x 10,000)

Minutes

Figure 4: Real ambient air sample from the vicinity of the city of Duisburg, Germany

0.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0

Trace analysis of greenhousegases

The chromatographic separationof methane from oxygen and ni -trogen in ambient air represents achallenge to the capacity of anycapillary column. To achieve detec -tion limits below 100 ppb, split-analysis is not a common alterna-tive. For direct analysis of vol-umes greater than 500 μL, PLOT(porous layer open tubular) col -umns with an internal diameter of0.53 mm are often overloaded bynitrogen and oxygen, and separa-tion from methane can no longerbe satisfactorily achieved.

The best results in terms of detec-tion limit and chromatographicseparation were obtained using a 2 m 1/16’’ micro-packed ShinCarbon ST column. This al -lows injection volumes of 1,000 μL

and thus detection limits wellbelow 100 ppb. Sampling andinjection was carried out using aVALCO six-port valve. As leak-age of the valve in the trace range

can lead to sample variation byambient air, the valve was equippedwith a helium-purged rotor hous-ing.

1,000 μL of sample was injecteddirectly from the sample looponto the column. Helium with apurity of 6.0 was used as carriergas and for gas discharge of theBID. The carrier gas flow waskept constant at 15 mL/min and ahelium flow rate of 80 mL/minwas set for the BID discharge gas.

The best chromatographic separa-tion was achieved using a temper-ature program starting at 30 °C.Depending on the characteristicsof the ShinCarbon ST column, astarting temperature of 40 °C isalso possible (Temperature pro-gram: 30 °C for 5 minutes isother-mally, followed by a rate of 10 °C/min to 120 °C). The long isotherm

MethaneCarbon dioxideNitrous oxide

6.23611.6713.132

23,25113,35616,997

2,1921,4481,857

575757

382532

436551

ppbppbppb

Name Ret. Time Area Height Noise S/N DL Unit

Table 1: Evaluation of the standard sample in figure 3. Detection limits (DL) are calculated

at a signal-to-noise ratio of 3.3.

Table 2: Results of the real sample in figure 4

MethaneCarbon dioxideNitrous oxide

6.20311.66413.138

77,362932,381

8,972

6,1441,060,978

1,010

1,664371,820

264

ppbppbppb

Name Ret. Time Area Height Conc. Unit

at 30 °C is necessary to sufficient-ly separate methane from the ni -trogen/oxygen signal.

Results

A standard of 500 ppb methane,carbon dioxide and nitrous oxidein helium was used for calibration(see chromatogram in figure 3).Regardless of the low standardconcentration, a reproducibility ofthe measurement results with astandard deviation of 1.1 % forCH4, 1.4 % for CO2 and 1.1 %for N2O could be determined.Based on a signal-to-noise ratio of 3.3, a detection limit below 100 ppb could be calculated for all components (table 1).

Figure 4 shows the chromatogramof a real ambient air sample fromthe vicinity of the city of Duis -burg, Germany. Methane is suffi-ciently separated, not only fromthe matrix but also from an un -known substance that elutes im -mediately following methane (res-olution R = 0.92). Low N2O con-centrations are also well separatedfrom a nearly 400-ppm broadCO2 signal (resolution R > 400).Additional results of the real sam-ple are listed in table 2.

To date, sensitive measurement ofgreenhouse gases often requiredcomplex gas chromatographic sys-tems equipped with a thermalconductivity detector (TCD),flame ionization detector (FID)and electron capture detector(ECD). Using the barrier ioniza-tion discharge detector (BID), theGC system could be simplified to

one column and one detector, with -out having to accept any loss inprecision and detection limit.

Reference literature

[1] 5th IPCC Report Final Draft (accepted):

http://www.climatechange2013.org/report/

review-drafts/

[2] The Analytical Scientist, Volume 11,

December 2013, The Analytical Scientist

Innovation Awards 2013

Additional information to this article can

be obtained via the QR code or by sending an

email to [email protected].

Effect of mobile phase pH onreversed-phase HPLC separationsof ionizable compounds

away from the analyte pKa, wherea compound is 50 % ionized. Thiscan give rise to split peaks, due todifferent retention behavior of theionized and non-ionized form.

Instrumentation: Nexera X2 seriesUHPLC system, wide pH version

Column: ACE Excel 3 Super C18, 100 x 2.1 mm

Mobile phase: a) acidic: A: 10 mMHCOONH4, pH 2.8 in H2O and B: in MeCN/H2O (90 : 10 v/v)b) basic: A: 0.1 % NH3, pH ~ 10 inH2O and B: in MeCN/H2O (90 : 10 v/v)

Gradient: 3 - 100 % B in 7 min

Cycle time: 11 min

Flow rate: 0.42 mL/min

Temperature: 40 °C

Injection volume: 2 μL

Sample: ~ 0,3 mg/mL of each com-pound in MeCN/H2O (5 : 95)

C hanging the pH of a mobilephase is a powerful tool toobtain significant changes in

the selectivity of a reversed-phaseHPLC separation. Ionizable com-pounds, meaning acidic, basic orzwitterionic analytes will showextreme changes in retention de -pending on their pKa and pH ofthe mobile phase. Therefore, awide pH range of the HPLCequipment offers additional possi-bilities for HPLC method opti-mization by exploiting selectivitychanges at low, intermediate andhigh pH.

The mobile phase pH reflects thehydrogen ion [H+] concentrationin solution. An acidic pH < 7 rep-resents an increased [H+] concen-tration, while adding a base to pH> 7 lowers the [H+] concentrationand suppresses ionization of basicanalytes, as shown in the exampleof N-acetylprocainamide in figure 1and methylparabene in figure 2.

As the extent of analyte ionizationchanges, so does the retention be -havior in reversed-phase HPLCseparations. Since the ionizedform is more polar, it is retainedless on alkylated, non-polar sta-tionary phases. Ion suppressionby decreasing the pH for acids, orincreasing it for basic analytes willsignificantly lengthen retention asdemonstrated in the applicationexample shown in figure 3.

A mixture of seven pharmaceuti-cals was separated in acidic or ba -sic mobile phase conditions. Whilethe neutral analytes showed nomarked change in retention time,the basic analytes, namely nizati-dine, N-acetylprocainamide andreserpine were retained muchlonger in basic conditions. Methyl -parabene moved forward once thephenol group was ionized (figures2 and 3).

Ion suppression can also be usedto considerably improve the peakshape of ionizable compounds, ascharged analytes undergo second-ary interactions with the station-ary phase, which can lead to strongpeak tailing. Neutral or unchargedcompounds will normally elute assharp, symmetrical peaks. In anycase, care should be taken to ad -just the mobile phase pH in arange that is about 2 pH units

N-acetylprocainamide, pKa ≈ 8.3

O

O

N+

H

pH = 2.8

O

O

N

pH = 10NH

NH

NH

NH

Figure 1: Ionization of N-acetylprocainamide in acidic or basic pH

Methylparabene, pKa ≈ 8.4

CH3O

pH = 2.8

O

OH

CH3O

pH = 10

O

O-

Figure 2: Ionization of methylparabene in

acidic or basic pH

Minutes

Figure 3: Separation of seven pharmaceuticals in a) acidic or b) basic mobile phase

conditions

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5

APPLICATION



APPLICATION

Figure 1: The TOC-4200

Customized TOC analysisThe online TOC-4200 with many options and kits

I n monitoring of wastewatersor quality control of ultrapurewater – wherever the organic

load of water plays a major role,TOC analyses are used. The TOC(Total Organic Carbon) sum para -meter defines the carbon concen-trations in organic compounds ina matrix and is therefore consid-ered to be a measure of contami-nation by organic compounds.

However, different applicationsand measurement tasks also placedifferent demands on the analyzer.Some waters contain high concen-trations of organic substanceswhile other waters contain hardlyany, or only very small amountsof TOC. Some waters are clear,others contain particulate matter,still others contain large amountsof salt or inorganic carbon com-pounds such as carbonates or hy -drogen carbonates.

Process analysis enables fast response

It is often important to monitorwater quality very closely and inreal-time. Conventional laborato-ry analyses will not be adequatehere. It often takes too much timefrom collecting a sample and ana-lyzing it in the laboratory to hav-ing the results available. Processanalysis has been developed forsuch cases. Here, a special analyz-er operates at close distance to awastewater discharge line or aprocess, to withdraw a sample pe -riodically (for instance every tenminutes), process it, and analyzeand evaluate it. The analyzer thensends the analysis value automati-cally to a process control system.The wastewater plant can nowrespond promptly to any changesor abnormalities.

The TOC parameter can be deter-mined easily and securely in on -line process analysis. The analyzerwithdraws an aliquot of the sam-ple and mixes it with an acid. Theacid decomposes inorganic carbon

examined for possible organicimpurities. In critical applica-tions, this also needs to be moni-tored around the clock.

• To cool industrial processes orplant components, water fromflowing watercourses is oftenused. This water is subsequentlyled back. It is hard to imaginewhat environmental damagecould occur when plant compo-nents start to leak and let envi-ronmentally hazardous sub-stances enter our watercourses –

such as carbonates and hydrogencarbonates compounds. The re -sulting CO2 is sparged from thesample using a sparge gas.

Subsequently, an aliquot of thesample is injected onto a hot plat-inum catalyst (680 °C). The or -ganic carbon compounds are oxi-dized to carbon dioxide and trans-ferred by the carrier gas to anNDIR detector, which detects theamount of CO2 produced. A sin-gle analysis takes about 3 to 4min utes, so the TOC can also bemeasured in the shortest time in -tervals.

Numerous applications for process analysis

• Wastewater treatment plantinflow is monitored to preventdamage to the biology of theplant by high organic loads withassociated high costs. To checkthe operation of the wastewatertreatment plant, the plant’s out-flow is also examined.

• In industrial applications, theorganic load in a wastewater isoften used to calculate the sew -age charge. Therefore, the waste-water streams are often moni-tored online.

• In the steam-water cycle of apower plant, the water is allowedto evaporate and condense againand again. The organic sub-stances can accumulate and dam-age the components of the tur-bines. Online monitoring of thecondensate protects the plantcomponents from damage.

• During cold spells, aircrafts aretreated with de-icing agentsshortly before takeoff. Thisresults in wastewater with veryhigh concentrations of organicsubstances. Airport operatorstherefore examine their waste-water streams during the wintermonths using online TOC sys-tems.

• In some applications, the TOCserves as a quality parameter.Starting materials or products are

not to mention the damage to theplant and the company’s reputa-tion. Here also, online TOC ana-lyzers are of great help in pro-tecting the environment as wellas the company.

These are just some examples ofthe many application areas of TOCprocess analyzers. �

APPLICATION

24

Wire07.04. - 11.04.2014Duesseldorf, Germanywww.wire.de

Control06.05. - 09.05.2014Stuttgart, Germanywww.control-messe.de

Setac11.05. - 15.05.2014Basel, Switzerlandwww.basel.setac.eu

ISCC18.05. - 23.05.2014Riva del Garda, Italywww.chromaleont.it /iscc

EXTECH25.05. - 28.05.2014Crete, Greecewww.extech2014.tuc.gr

Nordic Plasma01.06. - 04.06.2014Loen, Norwaywww.nordicplasma.com

EPRW Pesticide30.06. - 04.07.2014Dublin, Irelandwww.eprw2014.com

IMSC24.08. - 29.08.2014Geneva, Switzerlandwww.imsc2014.ch

WOTS 2014 (former HET)30.09. - 03.10.2014Utrecht, The Netherlandshttp://wots.nl /

Pyrolysis19.05. - 23.05.2014Birmingham, Great Britainwww.pyro2014.co.uk

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To meet the requirements of eachapplication, one needs systemsthat can be customized to the re -spective measurement task. To doso re quires many special optionsand kits.

Universally applicable andadaptable

Shimadzu’s TOC-4200 is a TOCprocess analyzer featuring all ofthese characteristics. The univer-

sal system can be customized toany measuring task using manyaccessories. Various types ofsampling systems are available.There are samplers with homoge-nizers that homogenize particle-containing wastewaters as well asspecial sampling stations for ultra -pure water. Various rinsing sys-tems such as an acid or base rinsecan be used to clean the samplingsystem. Sample stream exchang-ers enable monitoring of up tosix different sample streams usinga TOC-4200.

The analyzer also features anautomatic dilution function. Thisnot only increases the alreadywide measuring range, but alsoenables the creation of multi-point calibrations from a stan-dard solution.

Process analyzers must be able tolargely operate autonomously.Maintenance requirements shouldbe as low as possible and servicelife as long as possible. High saltloads in the sample reduce themaintenance interval. A high-saltkit has been developed specifical-ly for this purpose. It consists ofa catalyst tube with a specific ge -ometry and a special catalyst mix -ture that can handle up to twelvetimes the amount of salt-contain-ing sample, compared to a con-ventional catalyst. In addition,the dilution factor can also helpto reduce sample matrix effects.A TN module enables the simul-

taneous determination of thetotal amount of nitrogen com-pounds.

Communication supports versatility

The communication options ofthe analyzer are also versatile. Inaddition to the conventional 4 -20 mA line, the TOC-4200 alsofeatures Modbus communication.This enables wired communica-tion between multiple analyzersand the control room. An addi-tional web-based option enablesaccess to measurement resultsand the status of the analyzerfrom any networked computer.

It is clear that the many optionsand kits make the TOC-4200 auniversally applicable analyzersuited to any measuring task.

Figure 2: TOC Applikation Handbook

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