eike kleine-benne, dr. arnd heiden, pieter stoutjesdijk@gerstel · we invite you to visit with us...
TRANSCRIPT
17
GERSTEL solutions worldwide / March 2002
16
GERSTEL solutions worldwide / March 2002
News from GERSTEL GmbH & Co. KG · Aktienstraße 232 – 234 · D-45473 Mülheim an der Ruhr · Germany · Phone +49 (0) 208 - 76503-0 · Fax +49 (0) 208 - 7650333
GERSTEL GmbH & Co. KGAktienstraße 232 - 234D-45473 Mülheim an der RuhrGermany
+49 (0) 208 - 7 65 03-0+49 (0) 208 - 7 65 03 [email protected]
GERSTEL Inc.Caton Research Center1510 Caton Center Drive, Suite HBaltimore, MD 21227USA
+1 (410) 247 5885+1 (410) 247 [email protected]
ISS
N 1
619
-007
6
G L O B A L A N A L Y T I C A L S O L U T I O N S
Subject to change.
GERSTEL, GRAPHPACK and TWISTER are registeredtrademarks of GERSTEL GmbH & Co.KG.
Printed in the Fed. Rep. of Germany • 0302b
© Copyright by GERSTEL GmbH & Co.KG
GERSTEL AGEnterpriseSurentalstrasse 10CH-6210 SurseeSwitzerland
+41 (41) 9 21 97 23+41 (41) 9 21 97 [email protected]
GERSTEL on the www:
GERSTEL solutions worldwide Outside
In the past few years, GERSTEL has widened itsinternational activities. The company with its head-quarters in Mülheim an der Ruhr, Germany, has twosubsidiaries, GERSTEL Inc. in the USA and GERSTELAG in Switzerland and is responsible for distribution inmore than 30 countries throughout the world. This hasled to an increase in the requirements for the company,and was reason enough to expand the export department.
SalesBernd Wiesend is an engineer
and came to GERSTEL from theFederal Health Office Germany in1992. He was in charge of the Berlin
Office of the company forthree years, and becameSales Manager for Germa-ny in 1995. In 1999 hebecame responsible fordeveloping the export business. Since Sep-tember 2001, Bernd Wiesend is supported byJan Pieter Stoutjesdijk, who hails from theNetherlands, and was a national sales repre-sentative from 1996 to 1998, before switchingto our Dutch Distributor Analytical Application
Brielle B.V. There he gained experience in export, whichhe can now use in working once more for GERSTEL to
Coordination of worldwide business
Imprint
Published byGERSTEL GmbH & Co. KG,Aktienstrasse 232 – 234,45473 Mülheim an der RuhrGermany
EditorGuido Deußing,ScienceCommunication,Neuss, Germany
Scientific adviserDr. Arnd Heiden,[email protected]
Eike Kleine-Benne,[email protected]
DesignPaura Design, Hagen, Germany
Printed byBasseDruck, Hagen, Germany
www.gerstel.com
Expansion in export department
ThomasAlbinus
Jan PieterStoutjesdijk
BerndWiesend
enlarge the activities of the company, particularly inEurope, Africa and the Eastern.
Contact:[email protected][email protected]
ServiceBernd Wegmann has worked
for GERSTEL for 15 years, and for thepast five years he has been responsi-ble for international service. He is nowresponsible for the technical supportof distributors, and training and sup-port for our instruments and systems,both in the headquarters in Mülheiman der Ruhr and also for distributors on the spot. Becauseof the marked increase in worldwide sales partners, thework has been becoming more and more complex, andmore support was required. Thomas Albinus, a chemicalengineer, now supports Bernd Wegmann. Since 1999,he has been acting as a service en-gineer for the company in Germany.In future, Thomas Albinus will be re-sponsible for Europe and Africa.
Contact:[email protected][email protected]
ISSN 1619-0076
Authors of the scientificarticles contained in this
newsletter are solely respon-sible for their content.
GERSTEL Network
Our distributors in theNetherlands and Italy
Analysis
Trace analysis of taintsin foods and beverages
Formaldehyde Analyzer
Determination in materialsparallel to GC
More time forimportant things
GERSTEL in Show Year 2002
BerndWegmann
32
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
Another is the smoke analyzer, specially de-veloped for the study of cigarette smoke andrealised using two coupled GC 6890s fromAgilent Technologies with the GERSTEL CTS 1and two mass-selective detectors.
The importance to Agilent Technologiesof the partnership is shown by the title awardedto GERSTEL:
Premier Solution Partner – Gold Level.
GERSTEL solutions worldwide Editorial GERSTEL solutions worldwide Cooperation Partners
GERSTEL solutions:More time for the essentials …
The decision of Agilent Technologies Inc. to trans-fer worldwide trading, support and further developmentof the ChemSensor 4440 to GERSTEL indicates a newcloser relationship between the two companies. Bothhave recognised the enormous synergy potential for morethan 15 years: That is, GERSTEL systems specificallydesigned for use with Agilent Technologies instrumentswill open new markets and offer complete »off the shelf«solutions to customers through out the world.
GERSTEL solutions include the Air MonitoringSystem (AMS), consisting of two 6890s with GERSTELTDS G, Easy Cut and CTS 3 for online air monitoring ofpolar and non-polar components during a GC run.
Strong partner with synergy potential
GERSTEL
ChemSensor
System
Infometrix softwareclassifies a sampleusing differentalgorithms
Agilent Technologies and GERSTEL
Infometrix is one of the leading software devel-opers for chemometry in the world. Since 1978, thecompany has been developing chemometric tools,which can be used alone or employed in numerouschemometric solutions. An Infometrix product based onPirouette and developed exclusively for GERSTELcontrols the ChemSensor 4440 and the ChemSensorSystem 4440 and validates the results.
Infometrix Inc. and GERSTELDifferentiating between different colas (regular or
diet), determining the ratio of components in diesel fuel,or determining the origin of an olive oil are simple tasksfor the ChemSensor 4440. This is all made possible bythe wide variety of algorithms available in the softwaredesigned by Infometrix.
OI Corporation and GERSTEL Furtherinformation
GERSTEL: www.gerstel.comAgilent Technologies: www.agilent.comOI Corporation: www.oico.comInformetrix: www.infometrix.com
A promising link. This is the conclusion of the OICorporation, manufacturer and retailer of numerousproducts for gas, ion, and gel permeation chromatogra-phy. With good reason: while OI is mainly concernedwith the detection side of chromatorgaphy, GERSTELconcentrates on sample preparation. It seemed anobvious step to cooperate and to expand. Since the
Smoke Analyzer
Air Monitoring SystemAMS
end of last year, GERSTELhas been the exclusivesales and support providerfor OI Corporation detec-tors and GC systems in theGerman speaking portionof the world.
Ralf BremerTechnical directorof GERSTELGmbH & Co.KG
GERSTEL‘s analytical solutions give you the power to solve the most challengingproblems while allowing you to easily adapt to future needs. GERSTEL‘s approach is tolisten carefully to our customers and to provide them with superior solutions. Thiscustomer-oriented systems design philosophy means that the GERSTEL solution iscomprehensive, encompassing engineering, applications development, and fullinstrument support. Our modular systems approach allows you to expand your capa-bilities as your needs evolve, thus assuring your investment for the future.
We invite you to visit with us in the GERSTEL exhibits at PittCon 2002 in NewOrleans and at Analytica 2002 in Munich. We have some important and exciting newanalytical solutions to share with you, including:
– Our new ChemSensor product line combines technologies from three worldleaders: Agilent Technologies quadrupole mass spectrometry, Infometrix multivariatechemometrics, and GERSTEL sample conditioning and automation. The new Chem-Sensor offers important advantages over conventional electronic nose products.
– New developments with our TDS thermal desorption systems, MPS multi-purpose samplers, and Twister Stir Bar Sorptive Extraction systems that provide evenbetter performance, greater versatility, and productivity-enhancing automation for a widerange of applications.
– Further optimization and enhanced performance of our CIS Cooled Inlet System,which has already proven itself more than a thousand times over!
We think that you will find a visit to the GERSTEL booth to be well worthwhile.The GERSTEL team looks forward to meeting with you.
Yours truly,
In this Issue
Agilent TechnologiesOI CorporationInfometrix
Our Distributor in The Netherlands:Analytical Application Brielle B.V.
Trace analysis of taints in foodsand beverages using Stir BarSorptive Extraction
GERSTEL worldwide
Trade Fair Special: More timefor important things withGlobal Analytical Solutions
Formaldehyde Analyzer –Determination in materialsparallel to GC
Our Distributor in Italy: Abreg S.r.l.
Determination of Herbicidesin Vegetables
GERSTEL: Coordination ofworldwide business
Cooperation Partners Page 3
Overview Page 8 and 9
Network Page 14
Application note Page 15
Outside Page 16
Products / Title Page 10 to 12
Network Page 4
Analysis Page 5 to 7
Innovation Page 13
32
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
Another is the smoke analyzer, specially de-veloped for the study of cigarette smoke andrealised using two coupled GC 6890s fromAgilent Technologies with the GERSTEL CTS 1and two mass-selective detectors.
The importance to Agilent Technologiesof the partnership is shown by the title awardedto GERSTEL:
Premier Solution Partner – Gold Level.
GERSTEL solutions worldwide Editorial GERSTEL solutions worldwide Cooperation Partners
GERSTEL solutions:More time for the essentials …
The decision of Agilent Technologies Inc. to trans-fer worldwide trading, support and further developmentof the ChemSensor 4440 to GERSTEL indicates a newcloser relationship between the two companies. Bothhave recognised the enormous synergy potential for morethan 15 years: That is, GERSTEL systems specificallydesigned for use with Agilent Technologies instrumentswill open new markets and offer complete »off the shelf«solutions to customers through out the world.
GERSTEL solutions include the Air MonitoringSystem (AMS), consisting of two 6890s with GERSTELTDS G, Easy Cut and CTS 3 for online air monitoring ofpolar and non-polar components during a GC run.
Strong partner with synergy potential
GERSTEL
ChemSensor
System
Infometrix softwareclassifies a sampleusing differentalgorithms
Agilent Technologies and GERSTEL
Infometrix is one of the leading software devel-opers for chemometry in the world. Since 1978, thecompany has been developing chemometric tools,which can be used alone or employed in numerouschemometric solutions. An Infometrix product based onPirouette and developed exclusively for GERSTELcontrols the ChemSensor 4440 and the ChemSensorSystem 4440 and validates the results.
Infometrix Inc. and GERSTELDifferentiating between different colas (regular or
diet), determining the ratio of components in diesel fuel,or determining the origin of an olive oil are simple tasksfor the ChemSensor 4440. This is all made possible bythe wide variety of algorithms available in the softwaredesigned by Infometrix.
OI Corporation and GERSTEL Furtherinformation
GERSTEL: www.gerstel.comAgilent Technologies: www.agilent.comOI Corporation: www.oico.comInformetrix: www.infometrix.com
A promising link. This is the conclusion of the OICorporation, manufacturer and retailer of numerousproducts for gas, ion, and gel permeation chromatogra-phy. With good reason: while OI is mainly concernedwith the detection side of chromatorgaphy, GERSTELconcentrates on sample preparation. It seemed anobvious step to cooperate and to expand. Since the
Smoke Analyzer
Air Monitoring SystemAMS
end of last year, GERSTELhas been the exclusivesales and support providerfor OI Corporation detec-tors and GC systems in theGerman speaking portionof the world.
Ralf BremerTechnical directorof GERSTELGmbH & Co.KG
GERSTEL‘s analytical solutions give you the power to solve the most challengingproblems while allowing you to easily adapt to future needs. GERSTEL‘s approach is tolisten carefully to our customers and to provide them with superior solutions. Thiscustomer-oriented systems design philosophy means that the GERSTEL solution iscomprehensive, encompassing engineering, applications development, and fullinstrument support. Our modular systems approach allows you to expand your capa-bilities as your needs evolve, thus assuring your investment for the future.
We invite you to visit with us in the GERSTEL exhibits at PittCon 2002 in NewOrleans and at Analytica 2002 in Munich. We have some important and exciting newanalytical solutions to share with you, including:
– Our new ChemSensor product line combines technologies from three worldleaders: Agilent Technologies quadrupole mass spectrometry, Infometrix multivariatechemometrics, and GERSTEL sample conditioning and automation. The new Chem-Sensor offers important advantages over conventional electronic nose products.
– New developments with our TDS thermal desorption systems, MPS multi-purpose samplers, and Twister Stir Bar Sorptive Extraction systems that provide evenbetter performance, greater versatility, and productivity-enhancing automation for a widerange of applications.
– Further optimization and enhanced performance of our CIS Cooled Inlet System,which has already proven itself more than a thousand times over!
We think that you will find a visit to the GERSTEL booth to be well worthwhile.The GERSTEL team looks forward to meeting with you.
Yours truly,
In this Issue
Agilent TechnologiesOI CorporationInfometrix
Our Distributor in The Netherlands:Analytical Application Brielle B.V.
Trace analysis of taints in foodsand beverages using Stir BarSorptive Extraction
GERSTEL worldwide
Trade Fair Special: More timefor important things withGlobal Analytical Solutions
Formaldehyde Analyzer –Determination in materialsparallel to GC
Our Distributor in Italy: Abreg S.r.l.
Determination of Herbicidesin Vegetables
GERSTEL: Coordination ofworldwide business
Cooperation Partners Page 3
Overview Page 8 and 9
Network Page 14
Application note Page 15
Outside Page 16
Products / Title Page 10 to 12
Network Page 4
Analysis Page 5 to 7
Innovation Page 13
54
GERSTEL Aktuell Titel
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
GERSTEL solutions worldwide Network
Since 1991, Analytical Applications has beeninvolved in specialist application-support for analyticallaboratories. We are a »Value Added Business Partner«of Agilent Technologies, GERSTEL and other vendors.In close cooperation with our contract partners weconcentrate on the field of GC, HPLC, GC/MS andLC/MS applications.
The offices of Analytical Applications are locatedin Brielle, The Netherlands, and Farnborough, UnitedKingdom (U.K.). Our Dutch office has recently movedinto a new building with brand new facilities including aseparate seminar area equipped for classroom training,a spacious application lab, and storage space allowinginstruments for rental and leasing programmes to bedispatched to the customer immediately from stock.The offices are thus perfectly designed to handle themajor business activities of Analytical Applications:System Integration, Rentals & Leases and SupportServices. The U.K. office has recently cooperated withthe Food Research Institute in Leatherhead, and areport on this also appears in this issue.
Doing business with Analytical Applicationsmeans doing business with an enthusiastic experiencedteam, giving personal service and advice. Our SalesDepartments, in both The Netherlands and the U.K.,offer clients advice and integrated analytical solutions.The Sales Department is complemented by SupportServices, looking after installations, maintenance andrepairs and training. All telephone calls and orders areprocessed immediately by our administrative staff.
System IntegrationThrough close cooperation with Contract Partners
such as GERSTEL, Analytical Applications offers thecustomer multi-vendor solutions and therefore com-plete system integration. For the customers this resultsin a so called One-Stop-Shop.
Rentals & LeasesRenting & Leases GC, GC/MS, LC or LC/MS
systems, including full service, can be the ideal solutionin case of limited budget availability or emergencies. Theequipment is immediately available from stock. Afterrenting the equipment for 1 to 12 months, the systemcan be purchased or returned.
Support ServicesAfter thorough consultation about the application,
systems are specifically tailored for and demonstratedto customers in the modern laboratory by AnalyticalApplications’ own Applications Chemists. Installation,training and maintenance of the equipment is providedby the Support Engineers. In addition to technicalconsultancy, the Support Department also providesdemonstration workshops and training in analyticalinstrumentation.
Market SegmentsThe market segments Analytical Applications
serves and will continue to serve from its new premises,are predominantly in the fragrances, food and pharma-ceutical industries. In addition we are active in the areasof chemical, petrochemical, agricultural, environmentaland pyrolysis applications.
GERSTEL service and support network: Our Distributor in Benelux and UK
Analytical Applications Brielle B.V.
Further informationAnalytical Applications Brielle B.V.P.O. Box 673230 AB Brielle +31 181 416 555 +31 181 418 600 [email protected] www.anaplications.com
AuthorsChris Offen and Dr Adrian Squibb,Leatherhead Food RA, Randalls Road,Leatherhead, Surrey KT22 7RY, United Kingdom.
Introduction
Stir Bar Sorptive Extraction (SBSE) is a novel tech-nique for sample extraction.1, 2 Analyte extraction isbased on a small glass stir bar (10 or 20 mm in length)coated with a 1 mm thick layer of polydimethylsiloxane(PDMS). The 10 mm SBSE has a PDMS volume of 24 µL,which compares with an solid phase micro extraction(SPME) fibre, typically coated with less than 0.5 µL ofadsorbent. Within the glass bar is a metal strip to enablemagnetic stirring. After sampling, the stir bar is removed,washed and placed in a thermal desorption unit. Theanalytes are thermally desorbed by heating and deter-mined by GC-MS.
This work describes a comparative study on theanalysis of contaminating compounds associated withtaints in foods and beverages based on SBSE andSPME. The presence of contaminants resulting inorganoleptic problems of off-odour and taint in foodproducts can result in considerable economic loss to amanufacturer in terms of sales and product reputation.
The first study compares the analysis of a „cock-tail mixture“ of 11 volatile compounds commonly asso-ciated with problems of taint in foods and beverages.The second involves the analysis for halophenols andhaloanisoles in water and alcoholic beverages.
Experimental
InstrumentationAll analyses were performed on a GC (6890
Agilent Technologies) with mass selective detection(5973 Agilent Technologies). For SBSE analysis, the GCwas equipped with a Thermal Desorption unit (TDS 2,GERSTEL), and a cooled injection system (CIS 4,GERSTEL). For SPME analysis, the PDMS (100 mm)fibre was desorbed directly in the CIS 4, configured foroperation as a GC injector.
Cocktail mixtureStandards were prepared by spiking 11 com-
pounds into water. The water had been previouslyboiled and cooled to removing residual volatiles. Sam-pling was undertaken on 10 mL aliquots for 30 min atambient temperature (20 oC). Desorption from SPME fibreand SBSE stir bars were undertaken at 200 oC. The GC-MS analysis was undertaken using a 30 m x 0.25 mm i.d.,
Trace analysis of taints in foodsand beverages using Stir BarSorptive Extraction (SBSE)
Let’s twist again
Karel LundDirector of AnalyticalApplications Brielle B.V.
The staff From left to right:
Ben Baars(Service Engineer),
Frank van Schooten(Service Engineer),
Fanina Zwart(Order Processing),
Jeroen Weijts(Service Engineer),
Hans Anderson(Sales Engineer),
Stefanie van Oyen(Marketing
Communications),Richard Keizer
(Service Engineer),Sylvia de Koning
(Human Resources),Edwin van Trigt
(Sales Engineer),Karel Lund (Director)
GERSTEL-
Twister
In combination withGERSTEL TDS forthe determinationof flavour and off-flavour compounds
GERSTEL solutions worldwide Analysis
54
GERSTEL Aktuell Titel
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
GERSTEL solutions worldwide Network
Since 1991, Analytical Applications has beeninvolved in specialist application-support for analyticallaboratories. We are a »Value Added Business Partner«of Agilent Technologies, GERSTEL and other vendors.In close cooperation with our contract partners weconcentrate on the field of GC, HPLC, GC/MS andLC/MS applications.
The offices of Analytical Applications are locatedin Brielle, The Netherlands, and Farnborough, UnitedKingdom (U.K.). Our Dutch office has recently movedinto a new building with brand new facilities including aseparate seminar area equipped for classroom training,a spacious application lab, and storage space allowinginstruments for rental and leasing programmes to bedispatched to the customer immediately from stock.The offices are thus perfectly designed to handle themajor business activities of Analytical Applications:System Integration, Rentals & Leases and SupportServices. The U.K. office has recently cooperated withthe Food Research Institute in Leatherhead, and areport on this also appears in this issue.
Doing business with Analytical Applicationsmeans doing business with an enthusiastic experiencedteam, giving personal service and advice. Our SalesDepartments, in both The Netherlands and the U.K.,offer clients advice and integrated analytical solutions.The Sales Department is complemented by SupportServices, looking after installations, maintenance andrepairs and training. All telephone calls and orders areprocessed immediately by our administrative staff.
System IntegrationThrough close cooperation with Contract Partners
such as GERSTEL, Analytical Applications offers thecustomer multi-vendor solutions and therefore com-plete system integration. For the customers this resultsin a so called One-Stop-Shop.
Rentals & LeasesRenting & Leases GC, GC/MS, LC or LC/MS
systems, including full service, can be the ideal solutionin case of limited budget availability or emergencies. Theequipment is immediately available from stock. Afterrenting the equipment for 1 to 12 months, the systemcan be purchased or returned.
Support ServicesAfter thorough consultation about the application,
systems are specifically tailored for and demonstratedto customers in the modern laboratory by AnalyticalApplications’ own Applications Chemists. Installation,training and maintenance of the equipment is providedby the Support Engineers. In addition to technicalconsultancy, the Support Department also providesdemonstration workshops and training in analyticalinstrumentation.
Market SegmentsThe market segments Analytical Applications
serves and will continue to serve from its new premises,are predominantly in the fragrances, food and pharma-ceutical industries. In addition we are active in the areasof chemical, petrochemical, agricultural, environmentaland pyrolysis applications.
GERSTEL service and support network: Our Distributor in Benelux and UK
Analytical Applications Brielle B.V.
Further informationAnalytical Applications Brielle B.V.P.O. Box 673230 AB Brielle +31 181 416 555 +31 181 418 600 [email protected] www.anaplications.com
AuthorsChris Offen and Dr Adrian Squibb,Leatherhead Food RA, Randalls Road,Leatherhead, Surrey KT22 7RY, United Kingdom.
Introduction
Stir Bar Sorptive Extraction (SBSE) is a novel tech-nique for sample extraction.1, 2 Analyte extraction isbased on a small glass stir bar (10 or 20 mm in length)coated with a 1 mm thick layer of polydimethylsiloxane(PDMS). The 10 mm SBSE has a PDMS volume of 24 µL,which compares with an solid phase micro extraction(SPME) fibre, typically coated with less than 0.5 µL ofadsorbent. Within the glass bar is a metal strip to enablemagnetic stirring. After sampling, the stir bar is removed,washed and placed in a thermal desorption unit. Theanalytes are thermally desorbed by heating and deter-mined by GC-MS.
This work describes a comparative study on theanalysis of contaminating compounds associated withtaints in foods and beverages based on SBSE andSPME. The presence of contaminants resulting inorganoleptic problems of off-odour and taint in foodproducts can result in considerable economic loss to amanufacturer in terms of sales and product reputation.
The first study compares the analysis of a „cock-tail mixture“ of 11 volatile compounds commonly asso-ciated with problems of taint in foods and beverages.The second involves the analysis for halophenols andhaloanisoles in water and alcoholic beverages.
Experimental
InstrumentationAll analyses were performed on a GC (6890
Agilent Technologies) with mass selective detection(5973 Agilent Technologies). For SBSE analysis, the GCwas equipped with a Thermal Desorption unit (TDS 2,GERSTEL), and a cooled injection system (CIS 4,GERSTEL). For SPME analysis, the PDMS (100 mm)fibre was desorbed directly in the CIS 4, configured foroperation as a GC injector.
Cocktail mixtureStandards were prepared by spiking 11 com-
pounds into water. The water had been previouslyboiled and cooled to removing residual volatiles. Sam-pling was undertaken on 10 mL aliquots for 30 min atambient temperature (20 oC). Desorption from SPME fibreand SBSE stir bars were undertaken at 200 oC. The GC-MS analysis was undertaken using a 30 m x 0.25 mm i.d.,
Trace analysis of taints in foodsand beverages using Stir BarSorptive Extraction (SBSE)
Let’s twist again
Karel LundDirector of AnalyticalApplications Brielle B.V.
The staff From left to right:
Ben Baars(Service Engineer),
Frank van Schooten(Service Engineer),
Fanina Zwart(Order Processing),
Jeroen Weijts(Service Engineer),
Hans Anderson(Sales Engineer),
Stefanie van Oyen(Marketing
Communications),Richard Keizer
(Service Engineer),Sylvia de Koning
(Human Resources),Edwin van Trigt
(Sales Engineer),Karel Lund (Director)
GERSTEL-
Twister
In combination withGERSTEL TDS forthe determinationof flavour and off-flavour compounds
GERSTEL solutions worldwide Analysis
76
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
0.25 mm film thickness HP5 column, with a temperatureprogram of 50 oC (2 min) – 10 oC/min – 220 oC. The MSwas set to scan mass range 40-300 m/z.
Halophenols and haloanisoles
Samples of water, wine simulant (10 % ethanol) andwhite wine were spiked with the following: 2,4,6-trich-loroanisole (2,4,6-TCA), 2,4,6-trichlorophenol (2,4,6-TCP), 2,4,6-tribromoanisole (2,4,6-TBA) and 2,4,6-tribromophenol (2,4,6-TBP), at levels corresponding to0, 0.001, 0.01, 0.1 and 1 ppb (µg/mL). Each samplewas also spiked with 2,3,6-trichloroanisole (2,3,6-TCA)and 2,3,6-trichlorophenol (2,3,6-TCP) at 0.1 ppb(µg/mL) as internal marker standards.
Sampling was undertaken on 10 mL aliquots for30 min at ambient temperature (20 oC). Desorption fromSPME fibre and SBSE stir bars was undertaken at280 oC and 220 oC, respectively. The GC-MS analysiswas undertaken using a 30 m x 0.25 mm i.d., 0.25 mmfilm thickness HP5 column, temperature programmed120 oC (1 min) – 3 oC/min – 200 oC. The MS was set tomonitor the following 8 mass ions (195, 210, 196, 198,330, 332, 344 and 346 m/z) as a single group. The massion dwell time was 80 millisecs.
Results and Discussion
Cocktail mixtureThe responses of 11 components of „cocktail
mixture“ analysed by SPME-GC-MS and SBSE-GC-MS were determined. Based on mass ion peak areameasurements from RIC data, comparison of analyte le-vel of responses by SPME headspace and direct immer-sion SBSE analyses (spiked at 10 ppb) can be made (Table 1).
The SBSE GC/MS (tic) chromatogram for taintcocktail mix (10 ppb spike) in water is shown in Figure 1.
Overall, the data show that, for the majority of com-pounds, a higher response value was obtained withSBSE than with SPME. Higher levels of extraction canbe seen for less volatile components such as indole andskatole, which gave at least a 100-fold improvement inthe level of response.
Investigation of the detection of the „taint cocktailmix“ spiked in milk was also undertaken. Based ondefinitive mass spectra data, the following compoundswere identified at a 10 ppb (10 µg/mL) spiking level:hexanal, styrene, 2-ethyl-3-methylpyrazine, 6-chloro(ortho) cresol (6-COC), diallyl disulfide, indole andskatole. The mass spectra of styrene and 6-COC areshown, respectively, in Figure 2 and 3. Figure 3 alsoshows the RIC for the molecular ions of 6-COC(142 m/z) and the coeluting diallyl disulfide (146 m/z).
Halophenols and haloanisoles
Water, wine simulant (10 % ethanol) and whitewine samples were spiked with 2,4,6-TCA and 2,4,6-TCP at levels of: 0, 0.001. 0.01, 0.1 and 1 ppb (µg/mL).2,3,6-TCP and 2,3,6-TCA were added as an internalmarker standard (0.1 ppb).
Under the analytical conditions used, 2,4,6-TCAand 2,4,6-TBA were detectable in water, wine simulantand white wine at 10 ppt spiking level by SBME GC/MS(Fig. 4). 2,4,6-TCP and TBP were also detectable at thisspiking level in water and wine simulant. However,although 2,4,6-TBP was detectable at 10 ppt spikinglevel, owing to co-eluting interferences 2,4,6-TCP wasnot detectable in white wine at this spiking level.
Figure 5 shows the corresponding GC/MS SIMmass ion chromatograms for 2,4,6-trichloroanisoles/phenols, spiking at a 10 ppt level sampling by directimmersion SPME. The 2,3,6-TCA internal markerstandard (0.1 ppb) is the only component detected.2,4,6-TCP and 2,4,6-TBP were detectable by SPME(direct immersion) in samples spiked at 1 ppb (Fig. 6).
The studies show that detection of haloanisoles(i.e. 2,4,6-TCA and 2,4,6-TBA) in the above matrices isimproved ten-fold when sampling by SBSE comparedwith SPME, where the fibre is directly immersed in theaqueous matrices. In the case of halophenols (i.e. 2,4,6-TCP and 2,4,6-TBP), the level of detection by SBSEwas of the order of 10 ppt. This was 100 times bettercompared with direct immersion SPME (i.e. 1 ppb).
Regression data show that the calibration curvefor halophenols and anisoles at the sub parts per billionlevel (0-1000 ppt) is linear. The correlation coefficientvalues (r2) for halophenols and anisoles are given below(Table 2).
Conclusions
SBSE is a rapid and easy method for determiningtainting compounds in aqueous foods and beverages.This study has demonstrated the applicability of samplingat the low and sub part per billion levels for tainting conta-minants. The results show that, for certain contaminants,the level of detection can be improved by a factor of atleast 100 compared with sample extraction by directimmersion solid phase micro extraction (SPME).
Matrix 2,4,6-TCP 2,4,6-TBP 2,4,6-TCA 2,4,6-TBA
Water 0.9944 0.9995 0.9996 0.9985
Wine simulant 0.9994 0.9933 0.9971 0.9972
Wine 0.9976 0.9961 0.9995 0.9917
Table 2Correlation coefficient (r2)
values for halophenols andhaloanisoles spiked in
different matrices
References
[1] Baltussen E, Sandra P, David F and Crammers C, „StirBar Sorptive Extraction (SBSE), a novel extraction techniquefor aqueous samples theory and principles“, Journal ofMicrocolumn Separations, September. 1999, 11, 737-747.
[2] Hoffmann A and Heiden A, „Determination of flavourand off-flavour compounds in dairy products using Stir BarSorptive Extraction (SBSE) and thermal desorption GC/MSD/PFPD“, App Note 5/2000, Gerstel, 2000.
GERSTEL solutions worldwide Analysis
Table 1Relative SBSE
response comparedwith SPME for „taint
cocktail mix“compounds
Figure 1SBSE GC/MS (tic) of taint cocktailmix (10 ppb) spiked in water
Figure 2SBSE GC/MS analysis of styrene (10 ppb)spiked in milk
Figure 3SBSE GC/MSanalysis of 6-COC(10 ppb) spiked in milk
Figure 4SBSE GC/MSanalysis of 2,4,6-trichlorophenols/anisoles(0.01 ppb) spiked in water
Figure 5SPME (directimmersion) GC/MSanalysis of 2,4,6-trichlorophenols/anisoles(0.01) ppb spiked in water
Figure 6SPME (directimmersion) GC/MSanalysis of 2,4,6-TCA/TCP spikedat 1 ppb level
Compound Retention Molecular Ratiotime (min) mass ion (m/z)
Allyl methylsulphide 2.8 88 *
Hexanal 4.0 82 6.4
Diallyl sulfide 4.9 114 0.7
Styrene 5.5 104 1.5
2-Ethyl-3-methyl
pyrazine 7.4 122 24.6
m-Cresol 8.5 108 *
6-Chloro(ortho)cresol (6-COC) 8.6 142 8.0
Diallyl disulfide 8.6 146 4.9
Guiacol 8.8 124 18.1
Indole 11.9 117 103.6
Skatole 13.2 131 202.2
* not detected.
GERSTEL solutions worldwide Analysis
76
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
0.25 mm film thickness HP5 column, with a temperatureprogram of 50 oC (2 min) – 10 oC/min – 220 oC. The MSwas set to scan mass range 40-300 m/z.
Halophenols and haloanisoles
Samples of water, wine simulant (10 % ethanol) andwhite wine were spiked with the following: 2,4,6-trich-loroanisole (2,4,6-TCA), 2,4,6-trichlorophenol (2,4,6-TCP), 2,4,6-tribromoanisole (2,4,6-TBA) and 2,4,6-tribromophenol (2,4,6-TBP), at levels corresponding to0, 0.001, 0.01, 0.1 and 1 ppb (µg/mL). Each samplewas also spiked with 2,3,6-trichloroanisole (2,3,6-TCA)and 2,3,6-trichlorophenol (2,3,6-TCP) at 0.1 ppb(µg/mL) as internal marker standards.
Sampling was undertaken on 10 mL aliquots for30 min at ambient temperature (20 oC). Desorption fromSPME fibre and SBSE stir bars was undertaken at280 oC and 220 oC, respectively. The GC-MS analysiswas undertaken using a 30 m x 0.25 mm i.d., 0.25 mmfilm thickness HP5 column, temperature programmed120 oC (1 min) – 3 oC/min – 200 oC. The MS was set tomonitor the following 8 mass ions (195, 210, 196, 198,330, 332, 344 and 346 m/z) as a single group. The massion dwell time was 80 millisecs.
Results and Discussion
Cocktail mixtureThe responses of 11 components of „cocktail
mixture“ analysed by SPME-GC-MS and SBSE-GC-MS were determined. Based on mass ion peak areameasurements from RIC data, comparison of analyte le-vel of responses by SPME headspace and direct immer-sion SBSE analyses (spiked at 10 ppb) can be made (Table 1).
The SBSE GC/MS (tic) chromatogram for taintcocktail mix (10 ppb spike) in water is shown in Figure 1.
Overall, the data show that, for the majority of com-pounds, a higher response value was obtained withSBSE than with SPME. Higher levels of extraction canbe seen for less volatile components such as indole andskatole, which gave at least a 100-fold improvement inthe level of response.
Investigation of the detection of the „taint cocktailmix“ spiked in milk was also undertaken. Based ondefinitive mass spectra data, the following compoundswere identified at a 10 ppb (10 µg/mL) spiking level:hexanal, styrene, 2-ethyl-3-methylpyrazine, 6-chloro(ortho) cresol (6-COC), diallyl disulfide, indole andskatole. The mass spectra of styrene and 6-COC areshown, respectively, in Figure 2 and 3. Figure 3 alsoshows the RIC for the molecular ions of 6-COC(142 m/z) and the coeluting diallyl disulfide (146 m/z).
Halophenols and haloanisoles
Water, wine simulant (10 % ethanol) and whitewine samples were spiked with 2,4,6-TCA and 2,4,6-TCP at levels of: 0, 0.001. 0.01, 0.1 and 1 ppb (µg/mL).2,3,6-TCP and 2,3,6-TCA were added as an internalmarker standard (0.1 ppb).
Under the analytical conditions used, 2,4,6-TCAand 2,4,6-TBA were detectable in water, wine simulantand white wine at 10 ppt spiking level by SBME GC/MS(Fig. 4). 2,4,6-TCP and TBP were also detectable at thisspiking level in water and wine simulant. However,although 2,4,6-TBP was detectable at 10 ppt spikinglevel, owing to co-eluting interferences 2,4,6-TCP wasnot detectable in white wine at this spiking level.
Figure 5 shows the corresponding GC/MS SIMmass ion chromatograms for 2,4,6-trichloroanisoles/phenols, spiking at a 10 ppt level sampling by directimmersion SPME. The 2,3,6-TCA internal markerstandard (0.1 ppb) is the only component detected.2,4,6-TCP and 2,4,6-TBP were detectable by SPME(direct immersion) in samples spiked at 1 ppb (Fig. 6).
The studies show that detection of haloanisoles(i.e. 2,4,6-TCA and 2,4,6-TBA) in the above matrices isimproved ten-fold when sampling by SBSE comparedwith SPME, where the fibre is directly immersed in theaqueous matrices. In the case of halophenols (i.e. 2,4,6-TCP and 2,4,6-TBP), the level of detection by SBSEwas of the order of 10 ppt. This was 100 times bettercompared with direct immersion SPME (i.e. 1 ppb).
Regression data show that the calibration curvefor halophenols and anisoles at the sub parts per billionlevel (0-1000 ppt) is linear. The correlation coefficientvalues (r2) for halophenols and anisoles are given below(Table 2).
Conclusions
SBSE is a rapid and easy method for determiningtainting compounds in aqueous foods and beverages.This study has demonstrated the applicability of samplingat the low and sub part per billion levels for tainting conta-minants. The results show that, for certain contaminants,the level of detection can be improved by a factor of atleast 100 compared with sample extraction by directimmersion solid phase micro extraction (SPME).
Matrix 2,4,6-TCP 2,4,6-TBP 2,4,6-TCA 2,4,6-TBA
Water 0.9944 0.9995 0.9996 0.9985
Wine simulant 0.9994 0.9933 0.9971 0.9972
Wine 0.9976 0.9961 0.9995 0.9917
Table 2Correlation coefficient (r2)
values for halophenols andhaloanisoles spiked in
different matrices
References
[1] Baltussen E, Sandra P, David F and Crammers C, „StirBar Sorptive Extraction (SBSE), a novel extraction techniquefor aqueous samples theory and principles“, Journal ofMicrocolumn Separations, September. 1999, 11, 737-747.
[2] Hoffmann A and Heiden A, „Determination of flavourand off-flavour compounds in dairy products using Stir BarSorptive Extraction (SBSE) and thermal desorption GC/MSD/PFPD“, App Note 5/2000, Gerstel, 2000.
GERSTEL solutions worldwide Analysis
Table 1Relative SBSE
response comparedwith SPME for „taint
cocktail mix“compounds
Figure 1SBSE GC/MS (tic) of taint cocktailmix (10 ppb) spiked in water
Figure 2SBSE GC/MS analysis of styrene (10 ppb)spiked in milk
Figure 3SBSE GC/MSanalysis of 6-COC(10 ppb) spiked in milk
Figure 4SBSE GC/MSanalysis of 2,4,6-trichlorophenols/anisoles(0.01 ppb) spiked in water
Figure 5SPME (directimmersion) GC/MSanalysis of 2,4,6-trichlorophenols/anisoles(0.01) ppb spiked in water
Figure 6SPME (directimmersion) GC/MSanalysis of 2,4,6-TCA/TCP spikedat 1 ppb level
Compound Retention Molecular Ratiotime (min) mass ion (m/z)
Allyl methylsulphide 2.8 88 *
Hexanal 4.0 82 6.4
Diallyl sulfide 4.9 114 0.7
Styrene 5.5 104 1.5
2-Ethyl-3-methyl
pyrazine 7.4 122 24.6
m-Cresol 8.5 108 *
6-Chloro(ortho)cresol (6-COC) 8.6 142 8.0
Diallyl disulfide 8.6 146 4.9
Guiacol 8.8 124 18.1
Indole 11.9 117 103.6
Skatole 13.2 131 202.2
* not detected.
GERSTEL solutions worldwide Analysis
PolandCHROMTECChromatographia ApparatureAkcesoriaUl. Rakowiecka02532 WarszawaPoland
0048 (22) 6 06 38 830048 (22) 8 49 10 [email protected]
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GERSTEL worldwide
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0049 (0)208 – 7 65 03-250049 (0)208 – 7 65 [email protected]
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0049 (0)89 – 93 08 65 140049 (0)89 – 93 08 61 [email protected]
Technical officesGermany
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0061 (417) 62 76 670061 (7) 55 25 28 [email protected]
Benelux and UKAnalytical Applications Brielle B.V.Amer 93232 HA BrielleThe Netherlands
0031 (181) 41 65 550031 (181) 41 86 [email protected]
ChinaTegent Technology Ltd.Room 2103-05, Westin Centre26 Hung To RoadHong Kong
00852 - 27 59 21 8200852 - 27 58 38 [email protected]
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00420 4440-24 2400420 4440-25 [email protected]
If your country is notshown in our list ofdistributors, pleasecontact one of ourExport Managers:
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PolandCHROMTECChromatographia ApparatureAkcesoriaUl. Rakowiecka02532 WarszawaPoland
0048 (22) 6 06 38 830048 (22) 8 49 10 [email protected]
South AfricaChemetrix (Pty) Ltd.Block C, Siltek Park505 15th Road, Randjespark1685 MidrandRepublic South Africa
0027 (11) 4 44 30 00-1020027 (11) 4 44 30 03
TaiwanGreat EngineeringTechnology Corp.11F-1, No. 372 Chung Cheng1st Rd.Kaohsiung Taiwan R.O.C.Taiwan
00886 – 7 711 – 22 05 10100886 – 7 711 – 46 [email protected]
ScandinaviaImpressed ABHumanistgatan 8 B21456 MalmöSweden
0046 (40) 30 92 130046 (40) 6 72 69 02
SloveniaChemass d.o.o.Baznikova 401000 LjubljanaSlovenia
00386 (1) 4 27 75 6000386 (1) 4 27 75 [email protected]
SpainAndaluza De Intrumentacion S.L.Manufactura 8 EdificioBoudere I 2a PlantaPoligono PISA41927 Mairena de Aljarafe –SevillaSpain
0034 (95) 5 60 01 170034 (95) 4 18 20 [email protected]
KoreaYoung In Scientific Co., Ltd.Young-Wha Bldg. 547Shin Sa-Dong, Kang Nam-KuSeoul, 135-120Korea
0082 (2) 5 19 73 000082 (2) 5 19 74 [email protected]
IndiaTritech10, Ellora, Shradhanand RoadNear Telephone Exchange, VileParle (E)Mumbai – 400 057India
0091 (22) 401 72 440091 (22) 401 72 [email protected]
IsraelEldan ElectronicInstrument Co. Ltd.Idan twin buildingNew industrial park Afek21 Ha’Melacha st.48091 Rosh Ha‘AyinIsrael
00972 (3) 9 02 13 3000972 (3) 9 02 13 [email protected]
ItalyAbreg s.r.l.Via Montello, 2015100 AlessandriaItaly
0039 (131) 32 51 240039 (131) 51 09 [email protected]
JapanYokogawa Analytical Systems Inc.Sales Department / Gas PhaseProductsMitaka Takagi Bldg.1-15-5 Nakacho, Musashino.shi180 TokyoJapan
0081 (422) 56 93 930081 (422) 56 94 [email protected]
HungaryKromat Kft.Fehérvári út 1441116 BudapestHungary
0036 (1) 4 63 07 770036 (1) 2 06 29 [email protected]
GreeceHELLAMCO S.A.Scientific Laboratory Equipment7 Marathonos str. &Macedonias15233 Chalandri AthensGreece
0030 (1) 6 89 52 600030 (1) 6 80 16 [email protected]
FranceResearch Institutefor Chromatography7, Place Antonin Poncet69002 LyonFrance
0033 – 0620 – 73 45 580033 – 0478 - [email protected]
GERSTEL Inc.Caton Research Center1510 Caton Center DriveSuite HBaltimore, MD 21227United States of America
001 (410) 2 47 58 85001 (410) 2 47 58 [email protected]
GERSTEL AGEnterpriseSurentalstraße 106210 SurseeSwitzerland
0041 (41) 9 21 97 230041 (41) 9 21 97 [email protected]
GERSTEL worldwide
BerlinHarriet Diedering
0049 (0)30 – 21 90 98 280049 (0)30 – 21 90 98 [email protected]
BremenMichael Gröger
0049 (0)421 – 3 47 56 240049 (0)421 – 3 47 56 [email protected]
KarlsruheKlaus Klöckner
0049 (0)721 – 9 63 92 100049 (0)721 – 9 63 92 [email protected]
Mülheim an der RuhrDetlef Bergemann
0049 (0)208 – 7 65 03-250049 (0)208 – 7 65 [email protected]
MünchenHelmut Boljahn
0049 (0)89 – 93 08 65 140049 (0)89 – 93 08 61 [email protected]
Technical officesGermany
Support ManagerAsia/Pacific
Dr. Fred Schwarzer0081 (422) 60 29 580081 90 77 – 07 05 [email protected]
GERSTEL GmbH & Co. KGAktienstraße 232-23445473 Mülheim an der RuhrGermany
0049 (0)208 – 7 65 03-00049 (0)208 – 7 65 [email protected]
Head office Subsidiaries Distributorsworldwide
AustraliaLasersan Pty.Ltd.P.O.Box 3279Robina Town Centre, 4230QueenslandAustralia
0061 (417) 62 76 670061 (7) 55 25 28 [email protected]
Benelux and UKAnalytical Applications Brielle B.V.Amer 93232 HA BrielleThe Netherlands
0031 (181) 41 65 550031 (181) 41 86 [email protected]
ChinaTegent Technology Ltd.Room 2103-05, Westin Centre26 Hung To RoadHong Kong
00852 - 27 59 21 8200852 - 27 58 38 [email protected]
Czech RepublicHPST, s.r.o.K zatácce 518/814300 Prag 4Czech Republic
00420 4440-24 2400420 4440-25 [email protected]
If your country is notshown in our list ofdistributors, pleasecontact one of ourExport Managers:
Bernd Wiesend0049 (0)208 – 7 65 03-310049 (0)208 – 7 65 03-33,[email protected]
Jan Pieter Stoutjesdijk0049 (0)208 – 7 65 02-720049 (0)208 – 7 65 [email protected]
1110
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
GERSTEL solutions worldwide Trade Fair Special GERSTEL solutions worldwide Trade Fair Special
More time for important thingswith Global Analytical Solutions
Numerous business areas are increasingly usingelectronic noses for quality assurance, and in monito-ring products and processes. From the small group ofmarket-ready systems, one stands out: the GERSTEL-ChemSensor 4440. The instrument has been used suc-cessfully for more than three years, mainly in monitoringproduction lines for sensory determination of volatileheadspace components. A crucial difference determines
The Thermo Desorption System TDS 2 productfamily from GERSTEL has grown: thanks to a change inthe internal dimensions of the heating chamber, the newTDS 2-7, besides using the standard TDS tubes fromGERSTEL, allows use of thermal desorption basedpassive sampling tubes in sizes 1/4” x 3.5” from othermanufacturers for the first time. Automation was accom-plished by modifying the proven TDS A with a newmicroprocessor controlled tube lift mechanism designedto easily handle the different tube sizes. The mechanicallift was replaced by a microprocessor controlled lift arm.
success: in contrast to conventional electronic noses, theChemSensor 4440 does not work with relatively solidstate sensors, but is based on quadrupole massspectrometry technology. The headspace volatiles aretransferred directly to the mass selective detector (MSD)with elective scan mass ranges resulting is fast analysistime. The resulting mass spectrum is used as a finger-print to train the ChemSensor with acceptable samples.
Products that do match this fingerprint areeasily recognized. For example, for quali-
tative analysis a simple good/bad out-put could be used. For quantitativeanalysis measurement of compo-nent content could be made usingpercentage terms. Differences bet-ween samples are also found usingthe GC/MS configuration, which is
ideal for R&D applications. Discriminatingions previously determined with the 4440can be search in the GC/MS and the diffe-
rentiating compounds could easily be found.ChemSensor software developed exclusively for theGERSTEL ChemSensor 4440 by Infometrix Inc. allowsthe visualization of these mass spectra with patternrecognition techniques. The software is capable ofcontrolling the hardware as well as creating chemo-metric models in an integrated package.
ChemSensor System
Now also for passive sampling tubes
Thermo Desorption System TDS 2-7
GERSTEL in Show Year 2002
GERSTEL ChemSensor 4440Based on well-known mass spectrometryquadrupole technology.
Electronic nose based on MSThe product range of the most frequently used universal
injectors for all tasks in gas chromatography has been extended. Inaddition to the current GERSTEL Cooled Injection Systems (theCIS 3 and CIS 4), two new versions will be available soon. The CIS 6is the new universal injector designed specifically for AgilentTechnologies’ 6850 and 6890 gas chromatographs, and the CIS 5 isfor use in other manufactures’ gas chromatographs. The new CISinlets have been improved through the optimization of constructionand improved heating technology. For the first time they offerprogrammable heating to 600 °C. The new inlets will come with achoice of LN
2, LCO
2, Peltier or cryostatic cooling.
Heating to 600 °Cfor the first time
Individualcalibration gases
Standard GasPreparation System SPS
GERSTEL
CIS 6Designed for theAgilent Technologies6850 and 6890 gaschromatographs
GERSTEL
TDS 2-7First time for thermaldesorption basedpassive samplingtubes in sizes1/4‘‘ x 3.5‘‘ fromother manufacturers
Cooled Injection System CIS 6
The patented dynamic Standard Gas PreparationSystem SPS from GERSTEL allows rapid and cost-effective production of any desired gaseous calibrationmixture for thermal desorption. The system (currently
undergoing final testing) is analternative to calibration gas mixesstored in gas cylinders. Until now,these have been the best, but
most expensive sources for calibra-tion gas mixtures. Because of pro-duction-related long supply timesfor individual gases, many usershave stopped using these sources.Besides this, some mixtures are notcommercially available because theyare not stable in pressurised gas
contaniners. The precision and accuracy of the SPS ispossible thanks to a piezocrystal controlled microdropsystem – also used in colour inkjet printers – the indivi-dual drops of the calibration solution are sprayed at aprecisely defined rate into a highly purified gas stream(N2 or air); the process is carried out under normalpressure. Because of the small drop diameter of 30 to60 µm, the components vaporise completely. By con-trolling the frequency, the piezocrystal allows injection of1 to 2000 drops per second with a volume of approximately15 picolitres (10-12 L) into the gas stream: the digitallydetermined drop frequency allows calibration over threeorders of magnitude – with no mechanical changes tothe system or changes in the gas flow.
1110
GERSTEL solutions worldwide / March 2002GERSTEL solutions worldwide / March 2002
GERSTEL solutions worldwide Trade Fair Special GERSTEL solutions worldwide Trade Fair Special
More time for important thingswith Global Analytical Solutions
Numerous business areas are increasingly usingelectronic noses for quality assurance, and in monito-ring products and processes. From the small group ofmarket-ready systems, one stands out: the GERSTEL-ChemSensor 4440. The instrument has been used suc-cessfully for more than three years, mainly in monitoringproduction lines for sensory determination of volatileheadspace components. A crucial difference determines
The Thermo Desorption System TDS 2 productfamily from GERSTEL has grown: thanks to a change inthe internal dimensions of the heating chamber, the newTDS 2-7, besides using the standard TDS tubes fromGERSTEL, allows use of thermal desorption basedpassive sampling tubes in sizes 1/4” x 3.5” from othermanufacturers for the first time. Automation was accom-plished by modifying the proven TDS A with a newmicroprocessor controlled tube lift mechanism designedto easily handle the different tube sizes. The mechanicallift was replaced by a microprocessor controlled lift arm.
success: in contrast to conventional electronic noses, theChemSensor 4440 does not work with relatively solidstate sensors, but is based on quadrupole massspectrometry technology. The headspace volatiles aretransferred directly to the mass selective detector (MSD)with elective scan mass ranges resulting is fast analysistime. The resulting mass spectrum is used as a finger-print to train the ChemSensor with acceptable samples.
Products that do match this fingerprint areeasily recognized. For example, for quali-
tative analysis a simple good/bad out-put could be used. For quantitativeanalysis measurement of compo-nent content could be made usingpercentage terms. Differences bet-ween samples are also found usingthe GC/MS configuration, which is
ideal for R&D applications. Discriminatingions previously determined with the 4440can be search in the GC/MS and the diffe-
rentiating compounds could easily be found.ChemSensor software developed exclusively for theGERSTEL ChemSensor 4440 by Infometrix Inc. allowsthe visualization of these mass spectra with patternrecognition techniques. The software is capable ofcontrolling the hardware as well as creating chemo-metric models in an integrated package.
ChemSensor System
Now also for passive sampling tubes
Thermo Desorption System TDS 2-7
GERSTEL in Show Year 2002
GERSTEL ChemSensor 4440Based on well-known mass spectrometryquadrupole technology.
Electronic nose based on MSThe product range of the most frequently used universal
injectors for all tasks in gas chromatography has been extended. Inaddition to the current GERSTEL Cooled Injection Systems (theCIS 3 and CIS 4), two new versions will be available soon. The CIS 6is the new universal injector designed specifically for AgilentTechnologies’ 6850 and 6890 gas chromatographs, and the CIS 5 isfor use in other manufactures’ gas chromatographs. The new CISinlets have been improved through the optimization of constructionand improved heating technology. For the first time they offerprogrammable heating to 600 °C. The new inlets will come with achoice of LN
2, LCO
2, Peltier or cryostatic cooling.
Heating to 600 °Cfor the first time
Individualcalibration gases
Standard GasPreparation System SPS
GERSTEL
CIS 6Designed for theAgilent Technologies6850 and 6890 gaschromatographs
GERSTEL
TDS 2-7First time for thermaldesorption basedpassive samplingtubes in sizes1/4‘‘ x 3.5‘‘ fromother manufacturers
Cooled Injection System CIS 6
The patented dynamic Standard Gas PreparationSystem SPS from GERSTEL allows rapid and cost-effective production of any desired gaseous calibrationmixture for thermal desorption. The system (currently
undergoing final testing) is analternative to calibration gas mixesstored in gas cylinders. Until now,these have been the best, but
most expensive sources for calibra-tion gas mixtures. Because of pro-duction-related long supply timesfor individual gases, many usershave stopped using these sources.Besides this, some mixtures are notcommercially available because theyare not stable in pressurised gas
contaniners. The precision and accuracy of the SPS ispossible thanks to a piezocrystal controlled microdropsystem – also used in colour inkjet printers – the indivi-dual drops of the calibration solution are sprayed at aprecisely defined rate into a highly purified gas stream(N2 or air); the process is carried out under normalpressure. Because of the small drop diameter of 30 to60 µm, the components vaporise completely. By con-trolling the frequency, the piezocrystal allows injection of1 to 2000 drops per second with a volume of approximately15 picolitres (10-12 L) into the gas stream: the digitallydetermined drop frequency allows calibration over threeorders of magnitude – with no mechanical changes tothe system or changes in the gas flow.
13
GERSTEL solutions worldwide / March 2002
12
GERSTEL solutions worldwide / March 2002
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GERSTEL solutions worldwide Trade Fair Special
Thanks to the new membrane extrac-tion, even dirty aqueous matrices can be stu-died chromatographically without numerous
sample preparation steps.The functional principle ofmembrane extraction is ba-sed on a physical mecha-nism: the distribution bet-ween two phases corre-sponds to the distribution
MultiPurposeSampler MPS 2 and 3:
New features for the MPS family
Twister optionfor MPS 2
Back extraction using Twister is the firstmethod to automate the SBSE liquid desorp-tion step of the Twister, and to inject the liquidextract with the aid of the Multi Purpose Sam-pler MPS 3 directly into a HPLC system. Thisrequires using 250 µL vials and the samplepreparation option of the GERSTEL MAStersoftware. This allows complete flexibility ofMPS 3 control for method development.
A case study: for enrichment of PAHs,10 mL of the water sample to be investigatedare placed in a 10 mL glass vial, containingthe Twister. It is extracted for about 60 minu-tes at 100 rpm at room temperature. TheTwister is then removed from the vial usingclean forceps, dried with a lint-free wipe, andtransferred in a conical glass insert to a 2 mLsample vial, which is closed with a magneticcap or a plastic screw cap with an applied
Save time and money when using gas chromatography. With this in mind,GERSTEL concentrated on developing asimple desorption unit for the Twister, a pa-tented stir bar with a PDMS coating. Withthe Twister, organic components can beextracted from any aqueous matrices rapidlywith up to 1000 times lower detection limitsthan SPME.
As a result of its efforts, GERSTEL isnow in the final stages of testing the Twister
Membrane Extraction for the MPS
Twister Back Extraction for the MPS 3
Determination of the formaldehyde concentration inmaterials has until now been carried out photometricallyafter extraction and derivatisation with acetylacetone inaqueous solution. Liquid gas chromatography deter-mination of formaldehyde could only be performed afterextaction and derivatisation, and so liquid chromato-graphy using UV/VIS or fluorescence detection has beenpreferred; the derivatisation is carried out according toDIN 53315 at acidic pH with 2,4-dinitrophenylhydrazinein acetonitrile.
The automobile, furniture, packaging and food in-dustries predominantly use the so-called flask method(VDA recommendation 275 / DIN EN 717-3): in a cham-ber atmosphere, released formaldehyde enriches anaqueous solution until equilibrium is achieved, and theformaldehyde is determined after derivatisation withacetylacetone.
Besides formaldehyde, the whole spectrum ofvolatile organic compounds in a material, or its emissionspectrum, is usually also of interest. Thanks to the combi-
nation of a GERSTEL Thermo Desorption System TDS 2with GC-MSD and the parallel use of the FormaldehydeAnalyzer from AERO-Laser, Garmisch-Partenkirchen,Germany, the emission potential according to VDA 278from the material being studied cannow for the first time be measureddirectly using thermal extraction.
In detail: the selective detec-tion of formaldehyde is based on the reaction of formal-dehyde with acetylacetone and NH3 in aqueous phase.This leads to formation of a-a’-dimethyl-b-b’-diacetylpy-ridine, which is excited at 400 nm (Hg lamp) and detec-ted at 510 nm in the fluorescence cell (Figure 1).
The gaseous formaldehyde from the CIS split exit ismixed in a strip cell with the reaction solution with definedflow rates and contact times. Gas and reaction solutionare separated at the exit from the cell, and the solution isled to the fluorescence measurement cell.
The working range so far established statistically fordetermination of formaldehyde with the formaldehydeanalyzer is a total of 10 ng to 100 ng. However, the linearrange extends to more than 1000 ng (1 µg). With materialcontents according to VDA 278 the following workingranges, related to the material, can be used analytically:
Another advantage of the formaldehyde analyzer isthe low cross-reaction, such as to phenol, as observedwith the flask method (see Table 2). In order to discoverthe extent to which formaldehyde measurement with theformaldehyde analyzer is affected by cross-reaction withphenol, aqueous standard solutions containing increa-sing concentrations of phenol were prepared andmeasured. The same solutions were determined photo-metrically with the acetylacetone procedure according toVDA 275. The results of the measurements with both me-thods are compared in the Table 2.
Appendix
AERO-Laser and GERSTEL started cooperatingthis year to study formaldehyde emissions from materialsdirectly using thermal extraction in addition to other liquidorganic compounds. The result of this cooperation is aspecial adaptation of the AERO-Laser AL 4021 Form-aldehyde analyzer to GERSTEL Thermo DesorptionSystems, which is marketed by GERSTEL. By adaptationof the formaldehyde analyzer to the GERSTEL Thermo-Extractor, the pure formaldehyde emission of a materialcan be measured simply without sample preparation. Thiswork was carried out by Dr. Hans-Peter Schlegelmilch atimat-uve in Neuss, who largely managed this project.
Desorption Unit (TDU). The TDU is based on the sameprinciple as the very successful TDS 2, but is significantlysmaller with a thermal desorption oven designed spe-cifically for the Twister. Automation of up to 200 Twisteranalyses is made possible by simply using an adap-tation kit for the GERSTEL MPS 2.
metal ring. Usually, this is the onlymanual step; addition of the desorp-tion solution, shaking of the vial,removal and injection of theextract occur automatically.
The combination of theStir Bar Sorptive Extraction(SBSE) with solvent desorp-tion followed by LC fluore-scence detection allowssensitive and reproducibledetermination of PAHs in aqueous samples. Thanksto the MPS 3, manual steps are greatly reduced. Theprocedure is robust and easy to carry out. Samples canbe extracted in parallel, automatically processed andanalysed, giving higher sample througput. The Backextraction with Twister can be used for other organiccompounds, such as the determination of pesticides,herbicides and phenols.
coefficients combined with the exchange between the twophases through a permeable membrane.
In detail: the sample is transferred to a 20 mL head-space vial and sealed. The vial cap contains a membranewhich will be filled automatically by the MPS with an extrac-tion solution. After a suitable exchange time with supportby heating and shaking the vial in the agitator, the organiccomponents are enriched in the solvent phase dependingupon their distribution coefficients; the MPS takes analiquot and injects it into the GC or HPLC – automatically.
Twister Desorption Unit TDUThe combination with MPS 2 for desorption of theTwister is an alternative to the TDS 2 plus TDS A
Determination in materials parallel to GCFormaldehyde Analyzer
Dr. Hans-Peter Schlegelmilch
IMAT - UVE GmbHTilsiter Straße 11D-41460 NeussGermany
+49 - 2131 - 268501+49 - 2131 - [email protected]
Table 2Cross-reaction with phenol after normalisation of measurementwithout interference (without phenol addition) to 500 µg/L.
Table 1 Working ranges
Material Recommended Workingcontents range
accordingto VDA 278 µg / g
Foam / leather / varnish 15 mg 0.67 – 66.7
Compound materials /foil-like materials 30 mg 0.33 – 33.3
Fibre compound materials 60 mg 0.17 – 16.7
HCHO Phenol Combination: UV-VISconcentration addition TDS 2 / GC-MSD / VDA 275
Formaldehyde[µg/L] [µg/L] Analyzer [µg/L] [µg/L]
500 0 500 500
500 10 499 514
500 50 498 508
500 500 493 522
500 5000 490 523
500 50000 493 525
500 500000 494 540
500 1000000 495 557
Figure 1Reaction offormaldehyde withacetylacetone andNH3 in an aqueousphase forming a-a’-dimethyl-b-b’-diacetylpyridine.
GERSTEL solutions worldwide Innovation
The Author
13
GERSTEL solutions worldwide / March 2002
12
GERSTEL solutions worldwide / March 2002
www.gerstel.com
You can find further information
on times, services and products
on our internet home page at
www.gerstel.com
MarchLifeCom 2002Heinrich Heine UniversitätDüsseldorf, Germany,from 12. to 14.03.2002Pittcon 2002New Orleans, USA,from 17 to 21.03.2002ForumLabo 2002Paris, France,from 26. to 29.03.2002
AprilPALABFa. Novartis,Basel, Switzerland,from 08. to 09.04.2002ANALYTICA 2002Neue Messe München,Germany,from 23. to 26.04.2002
May25th InternationalSymposium onCapillary ChromatographyRiva, Italy,from 13. to 17.05.2002
JuneInstitute ofFood Technologists (IFT)Anaheim, USA,from 15. to 19. 06.2002
AugustAmerican ChemicalSociety (ACS)Boston, USA,from 18. to 22. 08.2002
SeptemberAnalytica China 2002Shanghai, China,from 03. to 06.09.2002Japan Analytical InstrumentsManufactures Association(JAIMA)Japan,from 05. to 07.09.2002
NovemberHet InstrumentUtrecht, The Netherlands,from 04. to 08.11.2002
GERSTEL isthere for you.
GERSTEL solutions worldwide Trade Fair Special
Thanks to the new membrane extrac-tion, even dirty aqueous matrices can be stu-died chromatographically without numerous
sample preparation steps.The functional principle ofmembrane extraction is ba-sed on a physical mecha-nism: the distribution bet-ween two phases corre-sponds to the distribution
MultiPurposeSampler MPS 2 and 3:
New features for the MPS family
Twister optionfor MPS 2
Back extraction using Twister is the firstmethod to automate the SBSE liquid desorp-tion step of the Twister, and to inject the liquidextract with the aid of the Multi Purpose Sam-pler MPS 3 directly into a HPLC system. Thisrequires using 250 µL vials and the samplepreparation option of the GERSTEL MAStersoftware. This allows complete flexibility ofMPS 3 control for method development.
A case study: for enrichment of PAHs,10 mL of the water sample to be investigatedare placed in a 10 mL glass vial, containingthe Twister. It is extracted for about 60 minu-tes at 100 rpm at room temperature. TheTwister is then removed from the vial usingclean forceps, dried with a lint-free wipe, andtransferred in a conical glass insert to a 2 mLsample vial, which is closed with a magneticcap or a plastic screw cap with an applied
Save time and money when using gas chromatography. With this in mind,GERSTEL concentrated on developing asimple desorption unit for the Twister, a pa-tented stir bar with a PDMS coating. Withthe Twister, organic components can beextracted from any aqueous matrices rapidlywith up to 1000 times lower detection limitsthan SPME.
As a result of its efforts, GERSTEL isnow in the final stages of testing the Twister
Membrane Extraction for the MPS
Twister Back Extraction for the MPS 3
Determination of the formaldehyde concentration inmaterials has until now been carried out photometricallyafter extraction and derivatisation with acetylacetone inaqueous solution. Liquid gas chromatography deter-mination of formaldehyde could only be performed afterextaction and derivatisation, and so liquid chromato-graphy using UV/VIS or fluorescence detection has beenpreferred; the derivatisation is carried out according toDIN 53315 at acidic pH with 2,4-dinitrophenylhydrazinein acetonitrile.
The automobile, furniture, packaging and food in-dustries predominantly use the so-called flask method(VDA recommendation 275 / DIN EN 717-3): in a cham-ber atmosphere, released formaldehyde enriches anaqueous solution until equilibrium is achieved, and theformaldehyde is determined after derivatisation withacetylacetone.
Besides formaldehyde, the whole spectrum ofvolatile organic compounds in a material, or its emissionspectrum, is usually also of interest. Thanks to the combi-
nation of a GERSTEL Thermo Desorption System TDS 2with GC-MSD and the parallel use of the FormaldehydeAnalyzer from AERO-Laser, Garmisch-Partenkirchen,Germany, the emission potential according to VDA 278from the material being studied cannow for the first time be measureddirectly using thermal extraction.
In detail: the selective detec-tion of formaldehyde is based on the reaction of formal-dehyde with acetylacetone and NH3 in aqueous phase.This leads to formation of a-a’-dimethyl-b-b’-diacetylpy-ridine, which is excited at 400 nm (Hg lamp) and detec-ted at 510 nm in the fluorescence cell (Figure 1).
The gaseous formaldehyde from the CIS split exit ismixed in a strip cell with the reaction solution with definedflow rates and contact times. Gas and reaction solutionare separated at the exit from the cell, and the solution isled to the fluorescence measurement cell.
The working range so far established statistically fordetermination of formaldehyde with the formaldehydeanalyzer is a total of 10 ng to 100 ng. However, the linearrange extends to more than 1000 ng (1 µg). With materialcontents according to VDA 278 the following workingranges, related to the material, can be used analytically:
Another advantage of the formaldehyde analyzer isthe low cross-reaction, such as to phenol, as observedwith the flask method (see Table 2). In order to discoverthe extent to which formaldehyde measurement with theformaldehyde analyzer is affected by cross-reaction withphenol, aqueous standard solutions containing increa-sing concentrations of phenol were prepared andmeasured. The same solutions were determined photo-metrically with the acetylacetone procedure according toVDA 275. The results of the measurements with both me-thods are compared in the Table 2.
Appendix
AERO-Laser and GERSTEL started cooperatingthis year to study formaldehyde emissions from materialsdirectly using thermal extraction in addition to other liquidorganic compounds. The result of this cooperation is aspecial adaptation of the AERO-Laser AL 4021 Form-aldehyde analyzer to GERSTEL Thermo DesorptionSystems, which is marketed by GERSTEL. By adaptationof the formaldehyde analyzer to the GERSTEL Thermo-Extractor, the pure formaldehyde emission of a materialcan be measured simply without sample preparation. Thiswork was carried out by Dr. Hans-Peter Schlegelmilch atimat-uve in Neuss, who largely managed this project.
Desorption Unit (TDU). The TDU is based on the sameprinciple as the very successful TDS 2, but is significantlysmaller with a thermal desorption oven designed spe-cifically for the Twister. Automation of up to 200 Twisteranalyses is made possible by simply using an adap-tation kit for the GERSTEL MPS 2.
metal ring. Usually, this is the onlymanual step; addition of the desorp-tion solution, shaking of the vial,removal and injection of theextract occur automatically.
The combination of theStir Bar Sorptive Extraction(SBSE) with solvent desorp-tion followed by LC fluore-scence detection allowssensitive and reproducibledetermination of PAHs in aqueous samples. Thanksto the MPS 3, manual steps are greatly reduced. Theprocedure is robust and easy to carry out. Samples canbe extracted in parallel, automatically processed andanalysed, giving higher sample througput. The Backextraction with Twister can be used for other organiccompounds, such as the determination of pesticides,herbicides and phenols.
coefficients combined with the exchange between the twophases through a permeable membrane.
In detail: the sample is transferred to a 20 mL head-space vial and sealed. The vial cap contains a membranewhich will be filled automatically by the MPS with an extrac-tion solution. After a suitable exchange time with supportby heating and shaking the vial in the agitator, the organiccomponents are enriched in the solvent phase dependingupon their distribution coefficients; the MPS takes analiquot and injects it into the GC or HPLC – automatically.
Twister Desorption Unit TDUThe combination with MPS 2 for desorption of theTwister is an alternative to the TDS 2 plus TDS A
Determination in materials parallel to GCFormaldehyde Analyzer
Dr. Hans-Peter Schlegelmilch
IMAT - UVE GmbHTilsiter Straße 11D-41460 NeussGermany
+49 - 2131 - 268501+49 - 2131 - [email protected]
Table 2Cross-reaction with phenol after normalisation of measurementwithout interference (without phenol addition) to 500 µg/L.
Table 1 Working ranges
Material Recommended Workingcontents range
accordingto VDA 278 µg / g
Foam / leather / varnish 15 mg 0.67 – 66.7
Compound materials /foil-like materials 30 mg 0.33 – 33.3
Fibre compound materials 60 mg 0.17 – 16.7
HCHO Phenol Combination: UV-VISconcentration addition TDS 2 / GC-MSD / VDA 275
Formaldehyde[µg/L] [µg/L] Analyzer [µg/L] [µg/L]
500 0 500 500
500 10 499 514
500 50 498 508
500 500 493 522
500 5000 490 523
500 50000 493 525
500 500000 494 540
500 1000000 495 557
Figure 1Reaction offormaldehyde withacetylacetone andNH3 in an aqueousphase forming a-a’-dimethyl-b-b’-diacetylpyridine.
GERSTEL solutions worldwide Innovation
The Author
15
GERSTEL solutions worldwide / March 2002
14
GERSTEL solutions worldwide / March 2002
User’s Guide for CIS and TDSThe GERSTEL Thermo Desorption System TDS 2
(in all its available forms) is an extremely sensitivethermal desorption system. It can be used for classicalthermal desorption or for direct thermal extractionwithout sample preparation. The GERSTEL CooledInjection System CIS is the most frequently usedseptum-less sampling head in the world for all injectiontechniques in gas chromatography: split, splitless,on-column, large volume up to 1000 µL.
For both systems, the first edition of a compactuser’s guide is available in booklet form, describing theprocedures and possible uses. The texts are short andconcise; numerous tables and figures enable rapidunderstanding and thus make it easy to convert basictheory into practice.
GERSTEL solutions worldwide News
During the last quarter of 1999 we started to workon the idea of pooling our professional experience in acommon plan, which has found its own shape andmotivation in ABreg. Each of the founders has had along career in sales and assistance in the field of analy-tical devices distributed by HP then Agilent ChemicalAnalysis Group.
The aim that sustained our project was to fulfil theever-increasing number of requests and requirements
of customers for instrumentsable to provide global solutions.For this reason we searched fora company that could offer itsown instruments with Agilenthigh compatibility.
GERSTEL was a naturalchoice because of the stronglong-term partnership. In Twisterwe saw great potential forsuccess, and for the last year
we have progressively been introducing GERSTEL tothe Italian market. The promotional initiative for GERSTELproducts has resulted in ABreg giving a number of de-monstrations where real samples of different typessupplied by customers have been examined.
We have had a high success rate with the»demos« and many potential customers who visited us
Our Distributor in Italy: ABreg S.r.l.GERSTEL service and support network
with their samples have now adopted GERSTEL solutions.In certain specific cases we promoted Agilent to increasesales of their products further.Our experience has increasedrapidly, and our sales staff hasdetails of more than 80 analy-ses performed on different kindof samples.
Analyses of pesticides contai-ned in food products performed usingTwister were found to be highly sensitiveand reproducible, as well as easy to use.As we approach the end of our first year as aGERSTEL distributor, we are looking forwardto new challenges in the future, after the greatsuccesses of the past year.
AuthorRoberto GaitaABREG S.r.l. (VAR), Via Montello 20,I-15100 Alessandria AL
Introduction
A carrot obtained from a supermarket chain wasanalysed in order to detect herbicides by means of aclassic method of solvent extraction, purification on asilica gel column, concentration under vacuum andanalysis by GC-MS.
GERSTEL solutions worldwide Application note
Instrumentation and conditions of analysis
� Stir Bar Sorptive Extraction Twister (GERSTEL)� Thermo Desorption System TDS 2 (GERSTEL)� Cooled Injection System CIS 4 (GERSTEL)� Gas chromatograph 6890 A (Agilent Technologies)� Mass spectrometer 5973N (Agilent Technologies)� MS Chemstation software (Agilent Technologies)� MASter software (GERSTEL)
GERSTEL INSTRUMENTATION
Thermo Desorption System TDS 2Mode : SplitlessDesorp. Profile: 30 °C initial temp.
40 °C per min290 °C final temp10 min final time
CIS 4 Cooled Injection System
Mode: Solvent ventVent flow 30 mL/min
Temp/Flow profile: - 60 °C initial temp12 °C/sec ramp290 °C final temp
AGILENT INSTRUMENTATION
GC 6890Column = HP5MS 30 m 0.25 mm 0.25 mm film thiknessFlow = Constant flowOven profile = 30 ° C initial temp
1‘ min initial time20 °C per min120 °C final temp 18 °C per min290 °C final temp 2
MSD 5973N
MS parameterAcquisition mode = scan 50 - 550 AMUThreshold = 150Scans/sec = 2.86
TemperaturesTransfer line = 280 °CMS quad = 120 °CMS source = 230 °C
ABreg represents GERSTELAt the most important analytical
exhibition in Italy (Milan) in October 2001
The sample turned out to contain 52 ppb ofTrifluralin (alpha, alpha, alpha-trifluoro-2,6-di-nitro-N,N-dipropyl-p-toluidine, CAS number 001582-09-8), a wellknown herbicide, which may be absorbed by carrots ifused incorrectly, excessively or if the latency time is notobserved.
The same sample was used to evaluate the SBSE(Stir Bar Sorptive Extraction) extraction method based onthe Twister stir bar.
Experimental
10 g carrot was gratedinto a common cookingshaker with 40 g pure waterand then transferred toge-ther with a Twister (length 1cm, phase thikness 0.5 mm)to a flask placed on a stirringplate set at about 700 rpm.
The solution was stirredfor 60 minutes at room tem-perature (in accordance withstandard analyte absorptionon Twister) with adequatesealing of the container.
The Twister was was-hed in purified water, driedwith absorbant paper andtransferred into the ThermoDesorption System TDS 2, connected to the GC-MS, pre-viously employed for the analysis with the classic method.
Results
A number of volatile and semi-volatile componentswere extracted from the sample, constituting the aromaand perfume of the carrot.
Extracting the characteristic ions of the Trifluralin wedetected its retention time and the spectrum was sear-ched using the Agilent pesticide’s spectra library. Thisgave a „match quality“ of 95 %, which increased to 97 %after the background subtraction.
The signal to noise ratio calculated on the analysisperformed with the classic extraction gave a RMS result ofalmost 500/1 while the SBSE method exceeded 5000/1.
Determination of Herbicides in Vegetables
Herbicedes in carrotsExtracting the characteristicions of the Trifluralin we detected itsretention time and the spectrumwas searched using the Agilentpesticide’s spectra library.
FurtherinformationABREG S.r.l. (VAR)Via Montello 20I-15100 Alessandria AL
0039 0131 3251240039 0131 [email protected]
15
GERSTEL solutions worldwide / March 2002
14
GERSTEL solutions worldwide / March 2002
User’s Guide for CIS and TDSThe GERSTEL Thermo Desorption System TDS 2
(in all its available forms) is an extremely sensitivethermal desorption system. It can be used for classicalthermal desorption or for direct thermal extractionwithout sample preparation. The GERSTEL CooledInjection System CIS is the most frequently usedseptum-less sampling head in the world for all injectiontechniques in gas chromatography: split, splitless,on-column, large volume up to 1000 µL.
For both systems, the first edition of a compactuser’s guide is available in booklet form, describing theprocedures and possible uses. The texts are short andconcise; numerous tables and figures enable rapidunderstanding and thus make it easy to convert basictheory into practice.
GERSTEL solutions worldwide News
During the last quarter of 1999 we started to workon the idea of pooling our professional experience in acommon plan, which has found its own shape andmotivation in ABreg. Each of the founders has had along career in sales and assistance in the field of analy-tical devices distributed by HP then Agilent ChemicalAnalysis Group.
The aim that sustained our project was to fulfil theever-increasing number of requests and requirements
of customers for instrumentsable to provide global solutions.For this reason we searched fora company that could offer itsown instruments with Agilenthigh compatibility.
GERSTEL was a naturalchoice because of the stronglong-term partnership. In Twisterwe saw great potential forsuccess, and for the last year
we have progressively been introducing GERSTEL tothe Italian market. The promotional initiative for GERSTELproducts has resulted in ABreg giving a number of de-monstrations where real samples of different typessupplied by customers have been examined.
We have had a high success rate with the»demos« and many potential customers who visited us
Our Distributor in Italy: ABreg S.r.l.GERSTEL service and support network
with their samples have now adopted GERSTEL solutions.In certain specific cases we promoted Agilent to increasesales of their products further.Our experience has increasedrapidly, and our sales staff hasdetails of more than 80 analy-ses performed on different kindof samples.
Analyses of pesticides contai-ned in food products performed usingTwister were found to be highly sensitiveand reproducible, as well as easy to use.As we approach the end of our first year as aGERSTEL distributor, we are looking forwardto new challenges in the future, after the greatsuccesses of the past year.
AuthorRoberto GaitaABREG S.r.l. (VAR), Via Montello 20,I-15100 Alessandria AL
Introduction
A carrot obtained from a supermarket chain wasanalysed in order to detect herbicides by means of aclassic method of solvent extraction, purification on asilica gel column, concentration under vacuum andanalysis by GC-MS.
GERSTEL solutions worldwide Application note
Instrumentation and conditions of analysis
� Stir Bar Sorptive Extraction Twister (GERSTEL)� Thermo Desorption System TDS 2 (GERSTEL)� Cooled Injection System CIS 4 (GERSTEL)� Gas chromatograph 6890 A (Agilent Technologies)� Mass spectrometer 5973N (Agilent Technologies)� MS Chemstation software (Agilent Technologies)� MASter software (GERSTEL)
GERSTEL INSTRUMENTATION
Thermo Desorption System TDS 2Mode : SplitlessDesorp. Profile: 30 °C initial temp.
40 °C per min290 °C final temp10 min final time
CIS 4 Cooled Injection System
Mode: Solvent ventVent flow 30 mL/min
Temp/Flow profile: - 60 °C initial temp12 °C/sec ramp290 °C final temp
AGILENT INSTRUMENTATION
GC 6890Column = HP5MS 30 m 0.25 mm 0.25 mm film thiknessFlow = Constant flowOven profile = 30 ° C initial temp
1‘ min initial time20 °C per min120 °C final temp 18 °C per min290 °C final temp 2
MSD 5973N
MS parameterAcquisition mode = scan 50 - 550 AMUThreshold = 150Scans/sec = 2.86
TemperaturesTransfer line = 280 °CMS quad = 120 °CMS source = 230 °C
ABreg represents GERSTELAt the most important analytical
exhibition in Italy (Milan) in October 2001
The sample turned out to contain 52 ppb ofTrifluralin (alpha, alpha, alpha-trifluoro-2,6-di-nitro-N,N-dipropyl-p-toluidine, CAS number 001582-09-8), a wellknown herbicide, which may be absorbed by carrots ifused incorrectly, excessively or if the latency time is notobserved.
The same sample was used to evaluate the SBSE(Stir Bar Sorptive Extraction) extraction method based onthe Twister stir bar.
Experimental
10 g carrot was gratedinto a common cookingshaker with 40 g pure waterand then transferred toge-ther with a Twister (length 1cm, phase thikness 0.5 mm)to a flask placed on a stirringplate set at about 700 rpm.
The solution was stirredfor 60 minutes at room tem-perature (in accordance withstandard analyte absorptionon Twister) with adequatesealing of the container.
The Twister was was-hed in purified water, driedwith absorbant paper andtransferred into the ThermoDesorption System TDS 2, connected to the GC-MS, pre-viously employed for the analysis with the classic method.
Results
A number of volatile and semi-volatile componentswere extracted from the sample, constituting the aromaand perfume of the carrot.
Extracting the characteristic ions of the Trifluralin wedetected its retention time and the spectrum was sear-ched using the Agilent pesticide’s spectra library. Thisgave a „match quality“ of 95 %, which increased to 97 %after the background subtraction.
The signal to noise ratio calculated on the analysisperformed with the classic extraction gave a RMS result ofalmost 500/1 while the SBSE method exceeded 5000/1.
Determination of Herbicides in Vegetables
Herbicedes in carrotsExtracting the characteristicions of the Trifluralin we detected itsretention time and the spectrumwas searched using the Agilentpesticide’s spectra library.
FurtherinformationABREG S.r.l. (VAR)Via Montello 20I-15100 Alessandria AL
0039 0131 3251240039 0131 [email protected]
17
GERSTEL solutions worldwide / March 2002
16
GERSTEL solutions worldwide / March 2002
News from GERSTEL GmbH & Co. KG · Aktienstraße 232 – 234 · D-45473 Mülheim an der Ruhr · Germany · Phone +49 (0) 208 - 76503-0 · Fax +49 (0) 208 - 7650333
GERSTEL GmbH & Co. KGAktienstraße 232 - 234D-45473 Mülheim an der RuhrGermany
+49 (0) 208 - 7 65 03-0+49 (0) 208 - 7 65 03 [email protected]
GERSTEL Inc.Caton Research Center1510 Caton Center Drive, Suite HBaltimore, MD 21227USA
+1 (410) 247 5885+1 (410) 247 [email protected]
ISS
N 1
619
-007
6
G L O B A L A N A L Y T I C A L S O L U T I O N S
Subject to change.
GERSTEL, GRAPHPACK and TWISTER are registeredtrademarks of GERSTEL GmbH & Co.KG.
Printed in the Fed. Rep. of Germany • 0302b
© Copyright by GERSTEL GmbH & Co.KG
GERSTEL AGEnterpriseSurentalstrasse 10CH-6210 SurseeSwitzerland
+41 (41) 9 21 97 23+41 (41) 9 21 97 [email protected]
GERSTEL on the www:
GERSTEL solutions worldwide Outside
In the past few years, GERSTEL has widened itsinternational activities. The company with its head-quarters in Mülheim an der Ruhr, Germany, has twosubsidiaries, GERSTEL Inc. in the USA and GERSTELAG in Switzerland and is responsible for distribution inmore than 30 countries throughout the world. This hasled to an increase in the requirements for the company,and was reason enough to expand the export department.
SalesBernd Wiesend is an engineer
and came to GERSTEL from theFederal Health Office Germany in1992. He was in charge of the Berlin
Office of the company forthree years, and becameSales Manager for Germa-ny in 1995. In 1999 hebecame responsible fordeveloping the export business. Since Sep-tember 2001, Bernd Wiesend is supported byJan Pieter Stoutjesdijk, who hails from theNetherlands, and was a national sales repre-sentative from 1996 to 1998, before switchingto our Dutch Distributor Analytical Application
Brielle B.V. There he gained experience in export, whichhe can now use in working once more for GERSTEL to
Coordination of worldwide business
Imprint
Published byGERSTEL GmbH & Co. KG,Aktienstrasse 232 – 234,45473 Mülheim an der RuhrGermany
EditorGuido Deußing,ScienceCommunication,Neuss, Germany
Scientific adviserDr. Arnd Heiden,[email protected]
Eike Kleine-Benne,[email protected]
DesignPaura Design, Hagen, Germany
Printed byBasseDruck, Hagen, Germany
www.gerstel.com
Expansion in export department
ThomasAlbinus
Jan PieterStoutjesdijk
BerndWiesend
enlarge the activities of the company, particularly inEurope, Africa and the Eastern.
Contact:[email protected][email protected]
ServiceBernd Wegmann has worked
for GERSTEL for 15 years, and for thepast five years he has been responsi-ble for international service. He is nowresponsible for the technical supportof distributors, and training and sup-port for our instruments and systems,both in the headquarters in Mülheiman der Ruhr and also for distributors on the spot. Becauseof the marked increase in worldwide sales partners, thework has been becoming more and more complex, andmore support was required. Thomas Albinus, a chemicalengineer, now supports Bernd Wegmann. Since 1999,he has been acting as a service en-gineer for the company in Germany.In future, Thomas Albinus will be re-sponsible for Europe and Africa.
Contact:[email protected][email protected]
ISSN 1619-0076
Authors of the scientificarticles contained in this
newsletter are solely respon-sible for their content.
GERSTEL Network
Our distributors in theNetherlands and Italy
Analysis
Trace analysis of taintsin foods and beverages
Formaldehyde Analyzer
Determination in materialsparallel to GC
More time forimportant things
GERSTEL in Show Year 2002
BerndWegmann