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The Evolution of Gas Chromatographic Instrumentation at PerkinElmer

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Published on the occasion of the 50-year anniversary of PerkinElmer’s first gas chromatograph, introduced in 1955. The Evolution of Gas Chromatographic Instrumentation at PerkinElmer
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Published on the occasion of the

50-year anniversary of

PerkinElmer’s first gas chromatograph,

introduced in 1955.

The Evolution ofGas Chromatographic

Instrumentationat PerkinElmer

laboratories helped in learning the principles of thenew technique. Based on this information, an extensivedevelopment program was initiated in the company’sheadquarters, in Norwalk, Connecticut. The conclusionof this development work was the Model 154 VaporFractometer, introduced in May 1955. Its basic features,unique at that time, were: the use of an air thermostat(the “oven”), permitting to keep the temperature of theseparation column adjustable between room tempera-ture and 150 ˚C; a flash vaporizer, allowing syringeinjection of liquid and gas samples through a rubberseptum into the carrier gas stream; and a thermistor-type thermal-conductivity detector. Also, the companyprovided a number of standardized columns with awide range of separation characteristics, permitting theuse of the instrument for the successful analysis ofdiverse samples.

The instrument was an instant success. An editorial in Analytical Chemistry characterized it as “a splendidexample of automatic analysis” and the chromatogramsobtained “a delight to behold.” Soon after the introduc-tion of the instrument, Perkin-Elmer also published asimple 31-page booklet, explaining the principles ofgas chromatography and how to select the operationalparameters. Analytical Chemistry praised this text in anew editorial, calling it “a compact and very informa-tive summary,” helping “in disseminating scientificand technical information.”

Naturally, development work did not stop with the intro-duction of the Model 154. By the beginning of 1956, animproved version was introduced; this was the Model154-B. In this new version, the temperature range wasextended to 225 ˚C, and an optional rotary-type valve,with variable sample loops, was added for the introduc-tion of gas samples. It is noteworthy that all the rotary-type, multiport-sampling and switching valves inexistence today, supplied by a large number of com-panies, can be traced back to the design of this valve.

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achievements in gas chromatography

In 2005, PerkinElmer celebrates the 50th anniversary of the Model 154 Vapor Fractometer, the first gaschromatograph (GC) developed by The Perkin-ElmerCorporation. This instrument heralded the era of thisversatile technique, which changed the way chemicalanalysis is carried out. It also represented the first trulyautomated, complex analytical instrument that did notneed specially skilled scientists for its operation andcould be used by practically every laboratory.

The Model 154 represented the first in a series of gaschromatographs, descendants of which are still manu-factured by the Life & Analytical Sciences division ofPerkinElmer. On the occasion of this anniversary, wewould like to review the evolution of gas chromato-graphic instrumentation at PerkinElmer.

The saga of the Model 154

In 1953-54, Perkin-Elmer’s representatives heard for thefirst time about the pioneering GC work done in England,by A.T. James and A.J.P. Martin, in the laboratories ofthe British Medical Council, London, and by C.S.G.Phillips at the University of Oxford. Visits to their

The Model 154-B Gas Chromatograph. The column oven is behind the door on the left-hand side of the unit. On the right-hand side, heating controls are on the toppanel; pneumatic controls, as well as controls of the thermal-conductivity detector,are on the lower-right panel, while a flow meter is installed in the middle. The heatedinjection port for syringe injection is at the lower left. The potentiometric recorderwas usually housed in a separate, equal-size cabinet. The Model 154-A had the samelook as this instrument.

The simplicity and ease of operation of the Model 154series was a significant factor in the exponential growthof gas chromatography. Soon, every large analyticallaboratory included GC among the techniques employed,and laboratories having a number of these instrumentswere not uncommon.

Over five years after its introduction, the Model 154 andits improved versions were the most widely used gaschromatographs. From 1962 on, new and more sophis-ticated instruments were introduced, yet the Model 154series and its European counterparts continued to beproduced until the late 1960s. Many laboratories kepttheir old instruments in use for decades. The unparal-leled history of this instrument is the best testimonyof the foresight of its developers.

The year 1958 saw the invention of open-tubular (cap-illary) columns by Perkin-Elmer’s Dr. M.J.E. Golay, oneof the most respected scientists in the field of scientificinstrumentation and, especially, gas chromatography.The next version of the instrument, the Model 154-C,introduced at the 1959 Pittsburgh Conference, providedthe capability of using capillary columns and the newlydeveloped flame-ionization detector.

In the Model 154-C, the flame-ionization detector amplifier was in a separate box. This was then con-solidated into the Model 154-D, first shown at the 1960 Pittsburgh Conference. This instrument alsoprovided a more sophisticated inlet system for cap-illary columns. Finally, in 1961, a simplified version of the original design, the Model 154-L, was intro-duced, specially developed for light gas analysis.

The Model 154 also served as the basis of other successful instruments at Perkin-Elmer’s Europeansubsidiaries in Germany (Models 116 and 116E) andEngland (Models 451 and 452).

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Dr. M.J.E. Golay (1902-1989), pioneering scientist in scientificinstrumentation and the inventor of open-tubular (capillary) columns.

The first advertisement of the Model 154-C Gas Chromatographshows the instrument with the oven door open. The capillarycolumn and the flame ionization detector are mounted in the oven. The amplifier of the FID is in a separate box. The chromato-ogram illustrates the full separation of ethylbenzene and the three xylene isomers.

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The Model 188

Very soon after the introduction of gas chromatography,chemists (mainly in the petroleum industry) wanted toanalyze wide boiling-range samples. For this type ofanalysis, the operating range of a single, isothermal in-strument was not enough. At that time, temperature pro-gramming of the column was not yet developed andtherefore, another approach was suggested: to havemultiple columns in series, each at a different temper-ature, with separate flow-through (thermal-conductivity)detectors at the end of each column. Such an instru-ment was Perkin-Elmer’s Model 188, introduced in 1957,which, in essence, was three Model 154 oven-and-detector systems, combined in series. However, thisinstrument was short-lived. Within a few years, tem-perature programming of a single column proved to be a much simpler solution for such applications.

New instruments in the early 1960s

In 1959-61, various new innovations extended the rangeof gas chromatography. Perkin-Elmer pioneered thedevelopment of a number of new instruments, driving a higher level of results.

We have already mentioned that temperature program-ming started to be popular in this period. To adapt theModel 154 GCs (which only permitted isothermalanalysis) for this need, a separate unit, the Model 222,was developed and introduced at the 1961 PittsburghConference. This instrument, which housed theseparation column and was connected to the Model154 utilizing its detector, had two unique features:

The first was that the (packed) column was resistanceheated, permitting 39 program rates from 0.5 to 52 °C/min. Recently, resistance heating was reintroducedand claimed as a new development. This is, however,not true – the technique was pioneered 43 years ago by Perkin-Elmer. One of the reasons why resistanceheating was utilized in the Model 222, was a resultof the poor design of early temperature-programmedovens, where significant thermal lag was reportedbetween set and actual column temperatures. Thisproblem was eliminated by resistance heating. Thecolumn follows instantaneously with the set program.

The combination of the 222/154 system had a secondfeature which was important in those early stages oftemperature programming, since relatively low-boiling

The Model 188 Triplestage Gas Chromatograph. The sample wasintroduced through the injection port of the leftmost unit and wasthen conducted by the carrier gas through three columns in series,each in a separate oven at different temperatures. Each had a thermalconductivity detector at the column outlet, making separate recordsof the particular fraction analyzed in that column.

Routine gas chromatography laboratory at Esso R&D Co., in early1958. This room contained at that time eight Model 154 Gas Chro-matographs. Except for the unit attended by the operator, the po-tentiometric recorders were placed directly under each chromatograph.(From W.A. Dietz, Instrument News, Spring 1958 edition.)

1955 1957

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substances (truly “liquid” phases) were used as thestationary phase. With such columns, an excessivebaseline drift was observed during programming, due to the exponential increase of vapor pressure withtemperature, causing a similar “bleeding” from thecolumn into the detector. In the 222/154 system, ashort column coated with the same phase as the sepa-ration column was installed in the Model 154’s oven, in series with the temperature-programmed separationcolumn. The temperature of this scrubber column was kept isothermally, at the maximum of the pro-gram. This way, the stationary phase concentration inthe carrier gas, due to the bleeding, equilibrated andbecame constant toward the detector – thus, the base-line drift was eliminated.

The Model 222 was short lived for two reasons. Thedual-column, baseline-compensation method, describedin 1961 by E.M. Emery and W.E. Koerner of MonsantoChemical Co. for the elimination of baseline drift duringprogramming, proved to be simpler than the systemused in the 222/154 combination. Perkin-Elmer imme-diately realized the importance of this technique anddeveloped an instrument for its utilization. However,

the company went one step further. While Emery andKoerner utilized a thermal-conductivity detector, withits standard two channels, Perkin-Elmer developed adifferential flame-ionization detector for this use. TheModel 800, introduced at the 1962 Pittsburgh Conference,was the first instrument permitting baseline compensa-tion with an FID, also including capillary columns. Thisinstrument also had a significantly improved ovendesign, assuring constant temperature along the columnand a minimal thermal lag during programming.

The Model 800 could be used with both packed andcapillary columns. A few months after its introduction, a modified version, the Model 801 became available.This instrument was specially designed for the growingbiochemical-clinical market, providing all-glass sys-tems including glass on-column injectors and glasspacked columns.

In the next few years, further versions of the Model 800 were available, with both the differential FID (the Models 810 and 880) and thermal-conductivitydetectors (the Model 820). These instruments also had all-glass versions: the Models 811 and 881.

The Model 154-D. In this unit, the amplifier of the flame-ionizationdetector was incorporated in the upper part of the recorder cabinet(right). The rotary-type gas sampling valve, originally introduced withthe Model 154-B, is mounted on the left side of the instrument cabinet.

1959 1960

The Model 213 Hydrocarbon Analyzer. It was a portable unit, permit-ting the analysis of atmospheric samples for the total organics content,with help of a flame-ionization detector.

Parallel to the Model 800, Perkin-Elmer’s Germanaffiliate introduced the Model F-6 gas chromatograph.This was the first truly modular GC based on a build-ing-block system, with multi-detector possibilities,permitting both isothermal and programmed-tempera-ture operation. Two years later, in 1964, a dual-columnversion, the Model F-7, also became available.

Both the Models 800 and F-6/7 series were general-purpose instruments, although they permitted the use of both packed and capillary columns. The applicationof capillary columns, however, expanded in a numberof fields; an instrument specially designed for capillary-column work became necessary. This instrument, theModel 226, was also introduced at the 1962 PittsburghConference. It had a unique design, eliminating the needfor a column oven: the thin-walled capillary columnswere embedded in a flat metal disk and heated by directcontact with a similarly shaped flat heater. This systemprovided extremely accurate temperature control and analmost zero lag between set and actual temperatures inboth isothermal and programmed-temperature operations.

In 1964, another highly successful gas chromatographwas introduced by Perkin-Elmer, the Model F-11, de-signed by the company’s British affiliate. This compact,low-cost, modular instrument could be expanded froma simple single-column, single-detector, isothermal in-strument to a temperature-programmed, multi-detectorversion. This instrument and its later version, theModel F-33, were sold worldwide for over a decade.Another low-cost GC, the Model F-20, was introduced in 1965 for the German market. This instrument and itsimproved version, the Model F-22, were also producedfor over a decade.

Instruments of the second decade

In the first decade of commercial gas chromatography,almost every year saw the introduction of a new, im-proved model of the popular series of instruments.However, by the mid-1960s, the field started to settledown. The instrument-design principles were consol-idated. Improvements then occurred in the areas ofelectronics and engineering components, such aspressure controls and flow regulators. These advancesalso permitted optimization of instrument design for

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The Model 222 Temperature Program-ming Accessory for the Model 154 GasChromatographs. The resistance-heatedcolumn is behind the vertical “chim-ney.” The injection port (for syringeinjection) is just below the chimney.

The Perkin-Elmer-Shell Model 212 Sorptometer was developed for thedetermination of the surface area of solids according to the BET method,using a GC-type measurement. The sample holder was placed in theDewar flask on the right where adsorption took place at liquid-nitrogentemperature.

1960 1961

both packed and capillary columns. A certain designcould last for a number of years with only minorenhancements that did not change the overall features of the instrument. The Models F-11 and F-20 alreadyrepresented such long-lasting designs, successfullymarketed for over a decade. However, both were, bydefinition, relatively simple, low-cost instruments,aiming for the routine analysis market.

By the mid-1960s, it was clear that a new major, top-of-the-line gas chromatograph was needed, which wouldprovide high sophistication and flexibility and couldbe used in both research and routine analysis. A specialrequirement, raised at that time by users, was thepossibility of using two columns and multiple detec-tors. The Model 900, introduced at the 1967 PittsburghConference, fulfilled this need. This instrument, whichwe consider one of the finest GCs ever built, set thestandard for high-performance gas chromatography.With the enhanced Model 990 introduced three yearslater, the 900 series was one of the dominating gaschromatographs of the decade. Even 38 years after itsintroduction, many can still be found operational inlaboratories around the world.

The 900/990 series was phased out in 1974 by the Model 3920, one of the most successful instruments in the medium-price range. In addition to updatedelectronics, a new feature was the N/P detector,selective to nitrogen- and phosphorus-containingorganic compounds. This detector became very impor-tant in drug screening, particularly at the Olympic Games.The debut of its application was at the 1976 WinterGames in Innsbruck, Austria, where Perkin-Elmerprovided the instrumentation needed for routinetesting of the athletes.

Meanwhile, Perkin-Elmer Ltd., the company’s Britishaffiliate, was also engaged in GC development, with theaim of replacing the Model F-11 with a more up-to-datedesign and, at the same time, designing a top-of-the-line instrument. The Model F-11 was eventually replacedin 1974 by the Model F-33, while in 1971 the Model F-30, a superb, high-performance gas chromatographwas introduced. This instrument was the basis of thedevelopment of the Model F-17, a highly versatile,medium-priced GC, introduced in 1973, that enjoyedconsiderable success in Europe.

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Configuration of the capillary column and heater of the Model 226Gas Chromatograph. The heater is the disk at the bottom, while thecapillary column is embedded in the disk above it.

1962 1963

The Model 810/820 Gas Chromatographs. These represented advancedversions of the Model 800 Gas Chromatograph, originally introducedin 1962, offering, for the first time, dual-column baseline compensationin programmed-temperature operation, with differential flame-ionizationdetectors or with a dual thermal-conductivity detector. The Model 810 (onthe left) is the FID and the Model 820 (on the right) is the TCD version.

Instruments of the electronic age

By the mid-1970s, electronic technology had ad-vanced to such an extent that it permitted the devel-opment of an entirely new line of microprocessor-controlled instruments, replacing all existing GCs. Thisrapid advance has continued ever since. As a result,instrument lines were replaced periodically by newerdesigns, incorporating the latest achievements in com-puter technology.

In the last 30 years, PerkinElmer has developed fourdistinct GC instrument lines, always corresponding to the newest advances.

The Sigma series

The first new line of gas chromatographs was representedby the highly successful Sigma series of instruments,developed in 1975-77. During development, some of thenew features had already been incorporated into theModel 910, an upgraded version of the Model 3920,introduced in 1976. The whole line of new instrumentswas introduced at the 1977 Pittsburgh Conference.

Four versions were offered with interchangeablecomponents and accessories, from a simple, isothermalGC, the Sigma 4, to the very sophisticated, complex,automated instrument, the Sigma 1. Further improve-ments in 1980 led to the Sigma B series. The Sigma 1Bwas also enlarged to include full data-handling capa-bilities; the result was the Sigma 115, introduced in1981. Based on the Sigma 2B, the Sigma 2000, an ad-vanced, flexible, high-performance instrument ofmodular design, was developed. Introduced in 1982,this instrument remained highly popular for almost adecade. The moderate-cost Sigma 3B was also furtherimproved in 1983, resulting in the Sigma 300.

The 8000 series

The next phase of GC innovation was the 8000 series,incorporating real-time screen display of the chromato-gram with built-in method development and data-handling capability. The instruments were developedat Perkin-Elmer’s British affiliate. The first of this serieswas the Model 8300, a simple, single-channel gas

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The Model 3920 Gas Chromatograph. Its design represented anadvanced version of the system originally incorporated in theModel 900.

1967 1974

The Model 900 Gas Chromatograph. The column oven opens on thetop left, with two FIDs in the wire cage to its right. Behind this are thecontrols for three gases, the carrier gas (helium), as well as hydrogenand air for the FIDs. The dual injection port is left of the name plate.The various knobs represent temperature controls and controls for thedetector electronics.

chromatograph, introduced in 1983. This was thenfollowed by three models with increasing capabilities:the Models 8400 and 8500 (1986) and the Model 8700(1987). Unique features of these instruments were the sliding oven door, optional installation of addi-tional injectors and detectors, and automated bleedcompensation.

The AutoSystem instruments

In 1990, Perkin-Elmer introduced the AutoSystem™ GC, a high-performance instrument, incorporating thenewest advances in chromatography and electroniccontrol, with a fully integrated autosampler, capable of handling up to 83 samples and injections of differentvolumes. In October 1995, an advanced model, theAutoSystem XL™ GC, was introduced with an auto-mated programmable pneumatic control for tempera-ture-programmable split/splitless or on-column sampleintroduction, as well as large-volume injection and a

number of universal and selective detectors. This in-strument provided the highest-quality gas chromato-graphic instrumentation available at that time.

The Clarus 500 GC

Following a change in ownership, the company –renamed PerkinElmer, Inc. – introduced a new GCplatform in the form of the Clarus® 500 GC and Clarus500 GC/MS in July 2002. Both feature a revolutionaryplatform design, incorporating the easy-to-learn, touch-screen user interface. The Clarus 500 GC offers a wholenew approach to the way users interact with the instru-ment – the intuitive graphical user interface featuresreal-time signal display and eight-language support.The Clarus 500 GC retains the analytical performanceof the AutoSystem GC, and the Clarus 500 MS incor-porates all the high-performance technology of theTurboMass™ Gold mass spectrometer.

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The microprocessor-controlled Sigma 1 Gas Chromatograph is shownwith its data system on the right.

1977 1982

The Sigma 2000 was an electronically controlled gas chromatographwith a built-in display of the method and the actual conditions.Shown in the middle are the four injection ports that permitted theinstallation of four columns simultaneously.

Mass spectrometry (MS) had always been considered the ultimate identification technique for organiccompounds. However, early mass spectrometers werelarge, complex and expensive. Also, for some time,direct coupling of a GC with an MS was practicallyimpossible, due to the large carrier gas flow and thesmall concentrations of the sample components to be investigated.

In 1963, Perkin-Elmer started to be involved in GC/MS,first by taking over the marketing of the mass spectrom-eters produced by Hitachi, Japan. These were stand-alone instruments that could be successfully coupledwith Perkin-Elmer gas chromatographs, using theWatson-Biemann type separator, consisting of a porousquartz tube through which helium molecules diffused.The heavier organic molecules remained in the gasstream in the tube and were conducted into the MS.Then, in 1967, Perkin-Elmer introduced the Model 270, a double-focusing, magnetic-sector mass spectrometerdeveloped at Perkin-Elmer, which was directly com-bined with a gas chromatograph. This instrument wasdiscontinued in the first part of the 1970s.

The next major involvement of Perkin-Elmer in massspectrometry was the introduction of the Ion TrapDetector™ in 1986. This was a benchtop unit, directlyinterfaced to the 8000 series gas chromatographs via anopen split interface, permitting the identification of thesample components eluting from a capillary column.This was then replaced in 1990 by the Q-Mass 910™

Quadrupole Mass Spectrometer, another benchtop unitwhich was interfaced with the AutoSystem GC.

In the 1990s, Perkin-Elmer started the development of a mass spectrometric detector that could serve as anintegral part of the gas chromatography system. Thenew instrument, the TurboMass Mass Spectrometer, was introduced in the fall of 1997 and could be directlycoupled to the AutoSystem XL GC.

As a further improvement in mass spectrometricdetection, PerkinElmer introduced the TurboMass Gold™

Mass Spectrometer in March 2001. By combining thetechnology with the Clarus 500 GC to form the Clarus500 GC/MS, it represents the highest performanceavailable today.

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The Q-Mass 910 Quadrupole Mass Spectrometer coupled with theAutoSystem GC. The Q-Mass 910 offered the fastest pumpdown in the industry, providing the analytical laboratory high uptime andefficiency of operation.

1983 1990

The 8000 series instruments permitted realtime screen graphics, data handling and method development through the control of asingle keyboard.

successes in GC mass spectrometry

These and the successive instruments were capable of handling a large number of samples and of carryingout the sampling and analysis according to a prepro-grammed schedule.

The previous three models were complete instruments,including not only the sample thermostat and the sam-pling unit, but also the gas chromatograph. The ModelF-20 and F-22 GCs were used for this purpose. Afterthe introduction of the Sigma series of gas chromato-graphs, the design concept was changed by having theheadspace sampler as an attachment to the prevailinggas chromatographs. The first such unit was a small,manually operated system, the Model HS-6 introducedin 1978, capable of handling six samples. Subsequently,a series of fully automated HS systems have been de-veloped, capable of handling a large number of samplesand combined with the PerkinElmer® gas chromato-graphs. These were the Model HS-100 (1983) to theSigma Series, the HS-101 (1986) to the 8000 series, the HS 40 (1991) to the AutoSystem and the HS 40XL (1996)to the AutoSystem XL gas chromatographs. In addition to the gas chromatograph for which they were optimized,these headspace samplers differed from each other by theincreasing degree of sophistication of the programmer

PerkinElmer is a pioneer in the development of two major sample handling systems, permittingheadspace analysis and the use of automatic ther-mal desorption sampling.

Headspace analysis

The analysis of volatile components present in anessentially non-volatile matrix is fairly difficult. Such a sample cannot be directly introduced into a gaschromatograph and, therefore, sample pretreatment(e.g., extraction) is necessary. This problem can beovercome by the direct sampling of the gas phase inequilibrium with the sample (static headspace). Thetechnique of headspace-gas chromatography (HS-GC)was originally invented by Professor G. Machata of theUniversity of Vienna in Austria. The proper instrumen-tation for the practical realization of the technique wasdeveloped by Perkin-Elmer’s German affiliate, using aunique pressure-balanced, time-based sampling of theheadspace of the thermostatted sample vials. The firstinstrument, the Model F-40 was introduced in the fallof 1967; it was then followed by the Model F-42 in 1975and the Model F-45 in 1978. The individual units mainlydiffered in the upper temperature of the thermostatwhich, in the Model F-45, was extended to 150 °C.

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The HS 40XL Automatic Headspace Sampler was the seventh genera-tion of headspace samplers. On the left is the carousel where thesamples are placed. The tower on the right side is where the vials are heated and the volatiles transferred to the gas chromatograph.

1996 1997

accomplishments in GC sample handling

The TurboMass Mass Spectrometer is a quadrupole benchtop massspectrometer with a standard mass range of 2-1200 daltons. It interfacesthrough the left side of the AutoSystem XL Gas Chromatograph, asshown in this photo.

controlling the automatic analytical sequence and theavailability of additional techniques to further extend therange of HS-GC.

In March 2000, PerkinElmer introduced the TurboMatrix™

series, a new generation of headspace samplers. Theintuitive touch-screen graphical user interface provideseasy control of the sampler in eight languages. Buildingon more than 40 years of experience in GC sample han-dling and introduction, TurboMatrix Headspace Samplersincorporate proven pressure-balanced sampling forbetter performance. The TurboMatrix series includesthree models:

• TurboMatrix HS 16, providing 16 positions

• TurboMatrix HS 40, providing 40 positions

• TurboMatrix HS 110, providing 110 positions

These instruments provide integrated, programmablepneumatics control, platform technology and fully auto-mated operation. The three models have complete up-gradeability, expanding with the user’s needs.

In 2003, PerkinElmer further improved the TurboMatrixHS 40 and HS 110 headspace samplers with patentedbuilt-in-trap technology, a key differentiator in headspacesampling. This system provides the ability for completeheadspace extraction with built-in preconcentration,

allowing up to 100 times lower detection limits thanstandard headspace samplers.

Automated thermal desorption sampling

The aim of the Automated Thermal Desorber (ATD) isto permit the automatic handling of sorbent-filled air-sampling tubes for the determination of the adsorbedvolatile compounds (e.g., VOCs in air) in concentra-tions from ppt to percent values. However, it can alsobe used for the determination of volatiles present in a solid sample, which can be vaporized upon heating.These instruments were developed by the company’sBritish affiliate. The first unit, the Model ATD-50, wasintroduced in 1981. It was followed in 1990 by theModel ATD-400. Each can automatically handle 50sampling tubes. The difference is in the upper desorptiontemperature, which was 250 °C in the Model ATD-50and 400 °C in the Model ATD-400.

In 2000, PerkinElmer introduced a new generation ofinstruments, the TurboMatrix TD thermal desorbers.These allow the choice of single-shot analysis of onesampling tube, or the use of an autosampler capable ofhandling 50 tubes and, similarly to the TurboMatrixheadspace samplers, provide complete upgradeability to grow with user requirements.

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The Clarus 500 GC/MS system includes a quadrupole MS with themass range of 1-1200 daltons, providing very fast scan speed, up to 60 scans/second, and permits Selected Ion Full Ion (SIFI™) monitoringin the same run, simultaneously acquiring data in full scan togetherwith Selected Ion Monitoring (SIM).

2000 2002

The TurboMatrix HS 110 (left) and TurboMatrix Automated ThermalDesorber (right). An intuitive, color touch-screen user interface providesinstant access to system functionality. They can be interfaced to almostany GC system, giving access to PerkinElmer’s proven technology,regardless of the GC brand or model.

The PerkinElmer-Arnel Model 4088 Beer Analyzer. This systemincludes a PerkinElmer-Arnel Clarus GC with FID detector, coupledwith a TurboMatrix HS Trap for off-flavor testing.

The TurboMatrix HS 110 Trap provides built-in analyte-trappingcapabilities that maximize the extraction and transfer of headspacevapor into the GC column, thereby lowering the detection limits by up to 100 times.

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2003 2005

The principles of gas chromatography have also been applied to instruments aiming at some specialapplications. GC has also been combined either withspecial sampling techniques or with other major in-strumental analytical techniques used for the iden-tification of sample components separated in the gaschromatograph. PerkinElmer has been active in thedevelopment and marketing of a number of such dedicated systems. Below is a brief summary of the most important units.

Preparative GC

The potential of using gas chromatography to obtainsample components in pure form had been realizedpractically since the beginnings of GC. The primaryaim was to have pure fractions available for identi-fication, using ancillary analytical techniques such asinfrared, ultraviolet, mass spectroscopy or chemicalreactions and not to “produce” substances in pureform. Thus, when speaking about “preparative” GC, we essentially consider analytical gas chromatographs or instruments with somewhat increased throughputand fraction-collection capability.

Perkin-Elmer had already provided an accessory in1956 to the Model 154-B Gas Chromatograph to collecteluted, pure sample components as they emerge fromthe instrument’s outlet, and heated collection systemswere also available for successive gas chromatographs.

In the 1960s, Perkin-Elmer also introduced two instru-ments specially developed for preparative GC. The firstwas the Model 222P, a scaled-up version of the Model222, utilizing resistance heating of the column. The in-strument, introduced at the 1963 Pittsburgh Conference,also included a thermal-conductivity detector and asample-collection system with two heated exit ports towhich metal or glass collection traps could be attached.Columns of 1-inch OD, up to 10 feet long, could be usedin the system, even with temperature programming.The reason for selecting resistance heating, was that therapid heat-up, or particularly, temperature programmingof such a big mass represented by these columns in anair thermostat, would have been almost impossible.However, this instrument was not popular – it rep-resented an about 16-fold scale-up of sample sizeswhich, as already mentioned, was more than mostlaboratories required.

contributions to special applications

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The second preparative gas chromatograph was devel-oped by Perkin-Elmer’s German affiliate. This was theModel 21 introduced in 1966. This instrument had an advanced design, where higher throughput wasachieved by automatic, repetitive sample introductionand fraction collection into a standard or somewhatlarger (e.g., about 1/3 inch instead of 1/4 inch) analyticalcolumn, rather than by injecting a single, large samplevolume into a significantly scaled-up column. A fewyears after the introduction of the Model 900, a specialaccessory permitting the same technique (automaticrepetitive sample introduction and fraction collection)also became available for this instrument.

By the beginning of the 1970s, interest in “preparative”gas chromatography (i.e., fraction collection for subse-quent analysis) diminished. It was slowly replaced bythe direct connection of a gas chromatograph (the GCcolumn) to another instrumental analytical technique(mainly mass spectrometry) for component identification.

Sorptometer

The Sorptometer was a special instrument, permittingthe determination of the specific surface area of pow-dered or granulated solids according to the BET theory,utilizing a GC-like technique instead of a vacuum systemfor adsorption-desorption measurements. It was originallydeveloped at Shell Development Co., in Emeryville,California, and Perkin-Elmer was licensed to design aninstrument and further develop the technique. Theoriginal instrument, the Model 212, was introduced atthe 1960 Pittsburgh Conference. In subsequent years,improved models such as the Models 212-B, 212-Cand 212-D were introduced. The Sorptometer enjoyedconsiderable success as the only instrument of its kind. However, its field of application was very limited. Toward the end of the decade, its mar-keting was discontinued.

FID for total organics analysis

The introduction of the flame-ionization detector (FID)in gas chromatography – 40 years ago – coincided with

the start of air-pollution research. At that time, theimportance of determining the total organic content of the atmosphere or other gases (e.g., automobile ex-haust) was identified by a few far-seeing researchers.It was also evident that the FID, which senses allorganic compounds (and the response of which isessentially proportional to the total concentration ofthe organics present in the sample gas), could be usedfor this purpose.

To facilitate such investigations, Perkin-Elmer devel-oped a portable instrument, the Model 213 Hydro-carbon Analyzer, which was introduced in late 1959. In 1961, a benchtop version, the Model 223, also be-came available. Both instruments were based on theFID design of the Model 154-C, but no column wasused and the sample gas (e.g., atmospheric air) waspumped through the detector at a constant flow rate in lieu of the carrier gas. The detector response, ascompared to having a pure inert gas (nitrogen or helium)flow, was proportional to the total concentration of theorganic compounds present in the sample gas.

Specialized gas chromatographs

In some cases, a general-purpose instrument is so extensively used for one special application, that it justifies customizing it. PerkinElmer has a long-standing relationship with Arnel™, a marketleader in customized chromatography solutions, toprovide, install and support proven dedicated sys-tems for a wide range of the applications and stan-dard methods, including light-gas analysis throughtransformer-oil gas analysis, simulated distillation and detailed hydrocarbon analyses. PerkinElmer alsoprovides customized solutions to industries down-stream from petrochemical processes, for example,lubricants, polymers, fine chemicals and beverages.

One of the most recent additions to the PerkinElmer-Arnel customized GC offering is the Model 4088 BeerAnalyzer (introduced in 2005), specialized for off-flavor testing.

www.perkinelmer.com 15

AutoSystem

AutoSystem XL

Clarus500

Clarus500 MS

TurboMatrixHS Trap

About the author

Dr. Leslie S. Ettre, a graduate of theTechnical University ofBudapest, Hungary, hasbeen active in the fieldof gas chromatographyfor almost 50 years, inboth research and in-strument development.His main field had beenin the theory and prac-tice of open-tubular(capillary) columns.

Dr. Ettre had been associated with The Perkin-ElmerCorporation for over 40 years, retiring at the end of1990, as a senior scientist. From 1988 until last year, he has been associated with the Department ofChemical Engineering of Yale University, first as an adjunct professor and, since 1995, as a researchaffiliate. In 1994, he was a guest professor atJohannes Kepler University, in Linz, Austria. Dr. Ettre has lectured throughout the world onchromatography and received numerous national and international awards. He is best known as the co-author of the basic textbook Static Headspace Gas Chromatography and the contributor of theseries on Milestones in Chromatography publishedregularly in LC•GC Magazine.

For a complete listing of our global offices, visit www.perkinelmer.com/lasoffices

©2005 PerkinElmer, Inc. All rights reserved. The PerkinElmer logo and design are registered trademarks of PerkinElmer, Inc. AutoSystem, AutoSystem XL, Q-Mass 910, SIFI,TurboMass, TurboMass Gold and TurboMatrix are trademarks and Clarus and PerkinElmer are registered trademarks of PerkinElmer, Inc. or its subsidiaries, in theUnited States and other countries. Arnel is a trademark of Arnel, Inc. All other trademarks not owned by PerkinElmer, Inc. or its subsidiaries that are depicted herein arethe property of their respective owners. PerkinElmer reserves the right to change this document at any time without notice and disclaims liability for editorial, pictorial ortypographical errors.

006068C_01 KG020505 Printed in USA

PerkinElmer Life and Analytical Sciences710 Bridgeport AvenueShelton, CT 06484-4794 USAPhone: (800) 762-4000 or (+1) 203-925-4602www.perkinelmer.com

The future

Evolution of scientific instruments never stops. Ad-vances in gas chromatography, in the field of elec-tronics, computer and microprocessor technology, as well as in production techniques, provide boththe possibility and the need for continuous improve-ments in design and performance.

Fifty years have passed since the introduction of thefirst PerkinElmer gas chromatograph. During thisperiod, many instruments have evolved, representing a continuous, unbroken line. Each instrument logi-cally followed its predecessor, retaining its goodfeatures, while incorporating the newest advances.This continuity in instrument evolution and theaccumulated knowledge of PerkinElmer’s chem-ists, engineers and physicists is the best guaranteefor excellence in scientific instrumentation in the21st century.

PerkinElmer, Inc.


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