16
IJ-VTD 03/2010 Your European Distribution Partner Austria VWR International GmbH Graumanngasse 7 1150 Wien Tel.: 01 97 002 0 Fax: 01 97 002 600 E-mail: [email protected] Belgium VWR International bvba Researchpark Haasrode 2020 Geldenaaksebaan 464 3001 Leuven Tel.: 016 385 011 Fax: 016 385 385 E-mail: [email protected] Denmark VWR - Bie & Berntsen Transformervej 8 2730 Herlev Tel.: 43 86 87 88 Fax: 43 86 87 90 E-mail: [email protected] Finland VWR International Oy Pihatörmä 1 C 1 02240 Espoo Tel.: 09 80 45 51 Fax: 09 80 45 52 00 E-mail: [email protected] France VWR International S.A.S. Le Périgares – Bâtiment B 201, rue Carnot 94126 Fontenay-sous-Bois cedex Tel.: 0 825 02 30 30 (0,15 EUR TTC/min) Fax: 0 825 02 30 35 (0,15 EUR TTC/min) E-mail: [email protected] Germany VWR International GmbH Hilpertstraße 20a D - 64295 Darmstadt Tel.: 0180 570 20 00* Fax: 0180 570 22 22* E-Mail: [email protected] (*0,14 €/Min. aus d. dt. Festnetz, Mobilfunk max. 0,42 €/Min.) Hungary Spektrum-3D Ltd A VWR International Company Simon László u. 4. 4034 Debrecen Tel.: (52) 521 131 Fax: (52) 470 069 E-mail: [email protected] Ireland VWR International Ltd Orion Business Campus Northwest Business Park Ballycoolin Dublin 15 Tel.: 01 88 22 222 Fax: 01 88 22 333 E-mail: [email protected] Northern Ireland VWR International Ltd A10 Harbour Court, 7 Heron Rd Sydenham Business Park Belfast BT3 9HB Tel.: 028 9058 5800 Fax: 028 9080 7812 E-mail: [email protected] Italy VWR International s.r.l. Via Stephenson 94 20157 Milano (MI) Tel.: 02 332 03 11 Fax: 800 152 999 E-mail: [email protected] The Netherlands VWR International B.V. Postbus 8198 1005 AD Amsterdam Tel.: 020 4808 400 Fax: 020 4808 480 E-mail: [email protected] Norway VWR International AS Haavard Martinsensvei 30 0978 Oslo Tel.: 0 2290 Fax: 815 00 940 E-mail: [email protected] Portugal VWR International - Material de Laboratório, Lda Edifício Neopark Rua Tomás Ribeiro, 43- 3 D 2790-221 Carnaxide Tel.: 21 3600 770 Fax: 21 3600 798/9 E-mail: [email protected] Spain VWR International Eurolab S.L. Ronda Can Fatjó, nº 11 Edifici Tecnopark, III Parc Tecnològic del Vallès 08290 Cerdanyola del Vallès Barcelona Tel.: 902 222 897 Fax: 902 430 657 E-mail: [email protected] Sweden VWR International AB Fagerstagatan 18a 163 94 Stockholm Tel.: 08 621 34 00 Fax: 08 621 34 66 E-mail: [email protected] Switzerland VWR International AG Lerzenstrasse 16/18 8953 Dietikon Tel.: 044 745 13 13 Fax: 044 745 13 10 E-mail: [email protected] UK VWR International Ltd Customer Service Centre Hunter Boulevard Magna Park Lutterworth Leicestershire LE17 4XN Tel.: 0800 22 33 44 Fax: 01455 55 85 86 E-mail: [email protected] Go to www.vwr.com for the latest news, special offers and details of your local VWR distribution partner. W hen using SPME the fibre is very likely to bend and have problems penetrating the septa. In order to make penetration easier, we first reduced the crimp cap septa’s thickness from 3.0 mm (which is a standard in 20 mm Headspace Crimp Caps) to approximately half that thickness. However, in order to compensate this considerable decrease in septa thickness, the crimp neck of the vial had to be changed to ensure effective crimping. Whilst this change solved the SPME penetration problems, it meant using customised vials for SPME with additional cost and inconvenience for the user. With the Precision Thread Headspace Vials an improvement for Headspace as well as for SPME was introduced that could universally be used for both applications. The septa used in the Magnetic Screw Caps of these vials only had a thickness of 1.3 mm up to 1.6 mm which helped to protect the SPME fibre. Furthermore the risk of incorrectly crimped vials has been eliminated and reproducible analysis results are guaranteed. The special precision thread forces the septa firmly against the glass rim to seal the vial and ensure gas-tightness. With the pre-cut septa technology additional protection is offered to the SPME fibre. Here the Silicone layer is cut through in a star shape, without affecting the PTFE-lamination which remains intact. As the Silicone part of the septa represents the major share of the complete septa thickness, the needle can now easily penetrate through the star shape for most of the septa’s thickness. The intact PTFE-lamination will give 100 per cent sample integrity avoiding any contamination by Silicone material. Besides the ease of penetration with a pre-cut septa, there is also very low fragmentation of the fibre during the penetration process (very important for SPME). The star shape of the pre-cut was used to give the needle a large target area and to give the septa enough movement to spread apart for penetration. VWR Collection Vials with PRE-CUT septa for SPME applications Description Pack Cat. No. Vial screw neck 10 ml, 46 x 22,5 mm, clear 100 548-0247 Vial screw neck 20 ml, 75,5 x 22,5 mm, clear 100 548-0248 Vial screw neck 10 ml, 46 x 22,5 mm, amber 100 548-0552 Vial screw neck 20 ml, 75,5 x 22,5 mm, amber 100 548-0553 New precision thread headspace vials

New VWR Collection Vialses.vwr-cmd.com/ex/downloads/magazine/chromjournal_8/chromJournal8... · 2 VWR ChromJournal Issue 8 Spring 2010 Dear Chromatographer, The 25th anniversary of

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IJ-VTD 03/2010

Your European Distribution Partner

AustriaVWR International GmbHGraumanngasse 71150 WienTel.: 01 97 002 0Fax: 01 97 002 600E-mail: [email protected]

BelgiumVWR International bvbaResearchpark Haasrode 2020Geldenaaksebaan 4643001 LeuvenTel.: 016 385 011Fax: 016 385 385E-mail: [email protected]

DenmarkVWR - Bie & BerntsenTransformervej 82730 HerlevTel.: 43 86 87 88Fax: 43 86 87 90E-mail: [email protected]

FinlandVWR International OyPihatörmä 1 C 102240 EspooTel.: 09 80 45 51Fax: 09 80 45 52 00E-mail: [email protected]

FranceVWR International S.A.S.Le Périgares – Bâtiment B201, rue Carnot94126 Fontenay-sous-Bois cedexTel.: 0 825 02 30 30 (0,15 EUR TTC/min)

Fax: 0 825 02 30 35 (0,15 EUR TTC/min)

E-mail: [email protected]

GermanyVWR International GmbHHilpertstraße 20aD - 64295 DarmstadtTel.: 0180 570 20 00*Fax: 0180 570 22 22*E-Mail: [email protected](*0,14 €/Min. aus d. dt. Festnetz,Mobilfunk max. 0,42 €/Min.)

HungarySpektrum-3D LtdA VWR International CompanySimon László u. 4.4034 DebrecenTel.: (52) 521 131Fax: (52) 470 069E-mail: [email protected]

IrelandVWR International Ltd Orion Business CampusNorthwest Business ParkBallycoolinDublin 15Tel.: 01 88 22 222Fax: 01 88 22 333E-mail: [email protected]

Northern IrelandVWR International Ltd A10 Harbour Court, 7 Heron RdSydenham Business ParkBelfast BT3 9HBTel.: 028 9058 5800Fax: 028 9080 7812E-mail: [email protected]

ItalyVWR International s.r.l.Via Stephenson 9420157 Milano (MI)Tel.: 02 332 03 11Fax: 800 152 999E-mail: [email protected]

The NetherlandsVWR International B.V.Postbus 81981005 AD AmsterdamTel.: 020 4808 400Fax: 020 4808 480E-mail: [email protected]

NorwayVWR International ASHaavard Martinsensvei 300978 OsloTel.: 0 2290Fax: 815 00 940E-mail: [email protected]

PortugalVWR International - Material de Laboratório, LdaEdifício NeoparkRua Tomás Ribeiro, 43- 3 D2790-221 CarnaxideTel.: 21 3600 770Fax: 21 3600 798/9E-mail: [email protected]

SpainVWR International Eurolab S.L.Ronda Can Fatjó, nº 11 Edifici Tecnopark, III Parc Tecnològic del Vallès08290 Cerdanyola del VallèsBarcelonaTel.: 902 222 897Fax: 902 430 657E-mail: [email protected]

SwedenVWR International ABFagerstagatan 18a163 94 StockholmTel.: 08 621 34 00Fax: 08 621 34 66E-mail: [email protected]

SwitzerlandVWR International AGLerzenstrasse 16/188953 DietikonTel.: 044 745 13 13Fax: 044 745 13 10E-mail: [email protected]

UKVWR International LtdCustomer Service CentreHunter BoulevardMagna ParkLutterworthLeicestershireLE17 4XNTel.: 0800 22 33 44Fax: 01455 55 85 86E-mail: [email protected]

Go to www.vwr.com for the latest news, special offers and details of your local VWR distribution partner.

When using SPME the fibre is very likely to bend and have problems penetrating the septa. In order to

make penetration easier, we first reduced the crimp cap septa’s thickness from 3.0 mm (which is a standard in 20 mm Headspace Crimp Caps) to approximately half that thickness. However, in order to compensate this considerable decrease in septa thickness, the crimp neck of the vial had to be changed to ensure effective crimping. Whilst this change solved the SPME penetration problems, it meant using customised vials for SPME with additional cost and inconvenience for the user.

With the Precision Thread Headspace Vials an improvement for Headspace as well as for SPME was introduced that could universally be used for both applications. The septa used in the Magnetic Screw Caps of these vials only had a thickness of 1.3 mm up to 1.6 mm which helped to protect the SPME fibre. Furthermore the risk of incorrectly crimped vials has been eliminated and

reproducible analysis results are guaranteed. The special precision thread forces the septa firmly against the glass rim to seal the vial and ensure gas-tightness. With the pre-cut septa technology additional protection is offered to the SPME fibre. Here the Silicone layer is cut through in a star shape, without affecting the PTFE-lamination which remains intact. As the Silicone part of the septa represents the major share of the complete septa thickness, the needle can now easily penetrate through the star shape for most of the septa’s thickness. The intact PTFE-lamination will give 100 per cent sample integrity avoiding any contamination by Silicone material. Besides the ease of penetration with a pre-cut septa, there is also very low fragmentation of the fibre during the penetration process (very important for SPME). The star shape of the pre-cut was used to give the needle a large target area and to give the septa enough movement to spread apart for penetration.

VWR Collection Vials with PRE-CUT septa for SPME applications

Description Pack Cat. No.Vial screw neck 10 ml, 46 x 22,5 mm, clear

100 548-0247

Vial screw neck 20 ml, 75,5 x 22,5 mm, clear

100 548-0248

Vial screw neck 10 ml, 46 x 22,5 mm, amber

100 548-0552

Vial screw neck 20 ml, 75,5 x 22,5 mm, amber

100 548-0553

New precision threadheadspace vials

ChromJournalIssue 8 Spring 2010

ChromJournal

VWR ChromJournal Issue 8 Spring 20102

Dear Chromatographer,

The 25th anniversary of the VWR-Hitachi cooperation in development and distribution of HPLC systems is an opportunity to look back – but also to have a look in the future. I had the chance to meet three of the initiators of this business for an interview which gave interesting information about why and how this cooperation was started. The VWR-Hitachi cooperation has been established with the 5th generation of HPLC systems. Hitachi has become one of the most important suppliers of VWR and our customers. In the last years the VWR-Hitachi cooperation has been extended to the distribution of Hitachi HPLC columns, amino acid analysers, spectrophotometers and benchtop centrifuges. We’re looking forward to new Hitachi developments and new scientific instrument lines to be integrated into the VWR product range soon.

See the other interesting contributions of this ChromJournal issue for products and applications which make your life as an analyst easier and safer and which can reduce cost and improve the quality of your results.

The VWR Chromatography team wishes you well in your chromatographic tasks!

Kind regards

Wolf-Dieter Beinert

Product specialist at VWR International, Darmstadt, GermanyScientific Instruments & Applications

Merck/VWR-Hitachi Systems for Analytical HPLC . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3-5

SCAT: Keep your HPLC retention time constant and save expensive solvents! . . . . . . . . . . . . . . . . . 6-7

LaChrom Elite® Application: Drastically simplified sample preparation by application of Chromolith® columns . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-10

The new VWR Chromatography Catalogue available now!. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Prepare HPLC / UHPLC samples three times faster using Whatman Mini-UniPrep syringeless filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

VWR Collection HPLC Syringes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Speed up separations 10 times with Purospher® STAR UHPLC columns . . . . . . . . . . . . . . . . . . . . . . 13

SCAT Europe SafetyFunnels for collecting waste fluids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

New Headspace plunger from Hamilton for CTC PAL System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

VWR Collection PRE-CUT septa for SPME applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

editorial

EditorVWR International Europe bvbaHaasrode Researchpark Zone 3Geldenaaksebaan 4643001 LeuvenBelgium

CopywritingVWR International Europe bvba

Layout and typesettingMarketing Services VWR

PrintingStork, Bruchsal, Germany

No part of this publication may be reproduced or copied without prior permission by writing of VWR International Europe.

Run68.000 copiesPublication date: March 2010

Due to the high sales volume of promoted articles some items may be temporarily out of stock - VWR Terms and Conditions of Sale apply.

table of contents

VWR ChromJournal Issue 8 Spring 2010 3

Analytical HPLC

The cooperation contract with Hitachi was finalised on the 4th of November 1983, and Merck began marketing Merck-Hitachi HPLC

systems in 1984. These first-generation systems can still be found in some laboratories – and are still going strong! The Merck-, later VWR-Hitachi HPLC Systems, were successful in capturing a considerable market share within a very short time. Today, the VWR-Hitachi Systems are known throughout the world and highly valued in laboratories for their robustness, sophisticated technology and their ability to provide reliable analytical results of the highest precision and sensitivity year in and year out.

On the occasion of this 25-year jubilee of the cooperation between Merck and VWR with Hitachi, ChromJournal interviewed three of the men who had primarily been involved right from the beginning: Dr. Friedhelm Eisenbeiß (former Head of Chromatography Research at Merck), Dr. Edgar Schättle (former Head of Product Management for HPLC Systems at Merck) and Dr. Reinhold Spatz (former Head of the Development Laboratory for Chromatographic Systems at Merck).

ChromJournal:Dr. Eisenbeiß, looking back, what were the motives for Merck to look for a manufacturer and supplier of HPLC systems?

Dr. Eisenbeiß:At that time, analytics was becoming more and more complex and increasingly instrument-oriented. This resulted in customers expressing the wish to have the chemistries, i.e. Reagents, instruments, methods, support and service from one single source. For Merck, as one of the leading suppliers of chemicals and other products for analytics, the question was raised as to what we should do to meet customer requirements, but not to become too dependent on the manufacturers of analytical systems. In the area of laboratory analytics, Merck had already successfully introduced a series of rapid tests along with simple instruments. Not only that, but in its diagnostics division, Merck was able to develop a very successful business in marketing systems. This involved providing the customer with a complete solution for the determination of clinical parameters – the chemistry (diagnostic kits), the instrument and the method.

At this point, Merck had already been very successful in the development of chromatographic products and had a broad portfolio of chromatography consumables

such as sorbents, columns, thin-layer plates, solvents, reagents and, importantly, considerable application know-how. It was thus logical for Merck to round off its chromatography range with HPLC instruments, hence giving impetus to its overall business in chromatography. An excellent example of this was the successful cooperation with CAMAG in the area of thin-layer chromatography.

ChromJournal:How did the cooperation with Hitachi come about?

Dr. Eisenbeiß:Initially, we considered cooperation with LKB, Kontron, Knauer or Waters. However, at visits to exhibitions around the world, our contacts to Hitachi became stronger and more concrete. At our first discussion in Japan in February 1983, I had the opportunity to visit their development and production departments and was very impressed by the quality and range of scientific instruments in their programme.

ChromJournal:What convinced Hitachi to cooperate with Merck?

Dr. Eisenbeiß: By 1962, Hitachi had already developed an amino acid analyser based on liquid chromatography; this was followed by a compact HPLC system. At the time of our visit, Hitachi had just introduced its Series 655A Modular HPLC System and was looking for a competent partner in the area of chromatography to market its HPLC systems throughout the world outside of its own East-Asian home territory.Hitachi was highly interested in the chromatography products and know-how of Merck and indicated that it would be willing to develop further analytical systems in partnership with Merck.This was followed up by several discussions in Germany and Japan and finally resulted in the cooperation contract being signed at the end of 1983.

ChromJournal:Dr. Schättle, Merck started marketing the Merck-Hitachi HPLC Systems in 1984. What sort of preparation was necessary?

Dr. Schättle:At that time, the technical and economic aspects of marketing scientific instruments were new to us; up

Merck/VWR-Hitachi Systems for Analytical HPLC

The early days of the cooperation with Hitachi

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 20104

until then, we had focussed entirely on chemical, diagnostic and pharmaceutical products. When I joined Merck in 1982 as a chromatography specialist, I had already considerable experience in the marketing of HPLC products, including instruments. In preparation for the cooperation with Hitachi I was assigned the task of writing a business plan that would include everything necessary for establishing the Merck-Hitachi HPLC System in the market (build-up of a sales organisation, service, application labs, warehouse, spare parts etc). Of course, to implement this, considerable preparatory work, investments and additional personnel were necessary. But, with respect to the product itself, it was no easy task to convince Hitachi to change the original Hitachi orange of the 655A system to the traditional blue of Merck for corporate design and marketing reasons. The first instruments delivered for evaluation purposes, however, were in the original orange design. These may still be somewhere within the Merck organisation.

ChromJournal:How was the Merck-Hitachi instrumentation introduced to Europe?

Dr. Schättle:In Germany, we employed six sales representatives in 1984. Practically in parallel we started marketing in France, Austria and Switzerland. About a year later we tackled Scandinavia, Italy, Spain and Portugal. Marketing in the then Eastern Bloc countries, especially Poland, was carried out from Austria, “The door to the East”.

ChromJournal:Dr. Spatz, you headed the HPLC System Development Laboratory at Merck that had been established to provide support for the

Merck-Hitachi business. What were the main tasks of the lab?

Dr. Spatz:The initial task was to develop suitable HPLC system packages, i.e. To provide complete solutions for certain HPLC analyses involving a Merck-Hitachi instrument, Merck columns and reagents and appropriate methods. Typical applications for such packages were e.g. Amino acid analyses, ion chromatography and the determination of clinical parameters such as catecholamines. However, the lab quickly progressed to contributing directly to technical development in line with to customer wishes and the competitive situation on the market. In this way, our lab very quickly exerted a strong influence on the further development of the Merck-Hitachi HPLC System. The aspects primarily involved here were the operation of the instrument, the user interface, the improvement of specifications and, from 1987 onwards, the development of the user interface for the Diode Array Detector Software and subsequently the HPLC System Software. All new prototypes were comprehensively tested in our labs, particularly for applications and overall performance. Today, these activities are carried out by the HPLC application laboratory at VWR.

ChromJournal:Development of the D-2000 Integrator from 1984 onwards was, as it were, your masterpiece. This was in fact the first milestone in Merck exerting influence on Hitachi regarding HPLC instrument development. How did this come about?

Dr. Spatz:The integrator provided by Hitachi at the time was not developed enough for western markets due to a lack of performance and user interface. My own extensive knowledge of chromatography data systems and integrators gained during my time as Head of the Application Laboratory at Spectra Physics made it relatively easy to convince Hitachi of the benefits of the project. I was able to propose specifications (unique selling points) that would render Hitachi far superior to its main competitors. This proposal turned out to be a winner: Hitachi spontaneously made resources available so that my “dream integrator” could be realised within the shortest possible time (1 year). The resulting D-2000 Integrator was unbeatable with respect to storage capacity for chromatograms, the insertion of calculated baselines and, especially, price-benefit ratio. At the Pittsburg Conference in

Hitachi brochure on the 655A HPLC system.

Analytical HPLC

VWR ChromJournal Issue 8 Spring 2010 5

1985, the D-2000 was a real surprise for the integrator specialists from the competition. Technically, its performance was only reached by competitive models about 4 years later. For Hitachi and Merck, the new integrator was a huge success and this continued for many years; it was also the basis for the development of follow-up models and ultimately of the Data System Software.

ChromJournal:Merck-Hitachi has in the meantime become VWR-Hitachi HPLC systems. How did this come about?

Dr. Spatz:In the year 2000, Merck acquired the company VWR International, one of the largest trading companies in the world for laboratory equipment. Subsequently, the entire Merck marketing organisation for laboratory products was integrated into VWR, including the Hitachi HPLC System. When Merck divested VWR International in 2004, the then Merck-Hitachi systems became today’s VWR-Hitachi systems. Numerous previous Merck employees followed their products to VWR, many of them with careers going back to the initial cooperation with Hitachi.

ChromJournal:Thank you very much for this interview.

The interview was carried out by: Dr. Wolf-Dieter Beinert, Specialist in the VWR Chromatography Team

The Merck-Hitachi HPLC system 655A

(high-pressure gradient configuration) with

the Merck Auto-Fix II loading device for

column cartridges (from a Merck brochure 1984).

The Merck-Hitachi Integrator D-2000

(reprint of a GIT article from 1985).

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 20106

500

520

540

560

580

600

620

640

660

680

0 5 10 15 20

Mas

se (g

)

Day

Bottle A (g) Bottle B (g)

Keep your HPLC retention time constant and save expensive solvents!

A simple test was carried out to compare the use of ‘open to atmosphere’ eluent caps versus SCAT Europe SafetyCaps. A test mixture of 3 PAHs (Polycyclic Aromatic Hydrocarbons) was used for a 20 day comparison of the chromatograms. Water and acetonitrile at low flow rate (to reduce solvent consumption) was selected as the mobile phase.The test revealed clearly that without using a closed solvent delivery system such SCAT Europe SafetyCaps, unreliable retentions times may be encountered even after a relative short time. Also volatile expensive solvents may be wasted!

Test conditionsBottle A: This bottle was closed with a SCAT SafetyCap (590-0506), precisely fitting the standard GL45 glass

bottle thread.Bottle B: This bottle was closed with a cap with a 10 mm hole in the plastic material, giving an ‘open to

atmosphere´ area of ~0.785 cm2 .

ProcedureBoth bottles were filled at the start of the test with an identical mixture of water : acetonitrile (20:80 w/w).•Using Bottle A as the reference, a chromatogram of a mixture of three PAHs (Polycyclic Aromatic •Hydrocarbons) - Benzo(a)pyrene, Benzo(ghi)perylene, and Indeno(1,2,3,c,d) pyrene, was acquired for comparison.After the reference chromatogram was obtained, both bottles were stored at room temperature in a fume •hood, this provided a gentle air flow over the top of the bottles.The analysis of the test mixture was repeated after 9 and 20 days.•

HPLC system A VWR Hitachi LaChrom Elite® HPLC system with Diode Array Detector, and under the control of EZChrom EliteTM Software was used. Isocratic pump conditions with the premixed mobile phase were set.HPLC Column: Merck Superspher® 100, RP-18e (5 µm), 125 x 2 mm Flow rate = 500 µl/ min

ResultsAs expected, bottle A did not show any significant change in weight, concluding that no solvent vapours escaped from this bottle, see Tab. 1. Bottle B showed significant and varied loss of liquid by vaporization. The composition of water and acetonitrile in the vapour may have varied over the time due to the fact that mixtures of water and acetonitrile form azeotropes.

Tab. 1: Weight-loss of bottles over a period of 20 days

Day Bottle A (g) Bottle B (g)0 666.44 673.599 666.22 650.8520 665.26 609.12

Fig. 1: graphical representation

Analytical HPLC

VWR ChromJournal Issue 8 Spring 2010 7

Minutes0,5 1,0 1,5 2,0 2,5 3,0 3,5 4,0 4,5 5,0 5,5 6,0 6,5 7,0 7,5 8,0

mA

U

0

200

400

600

800

1000

1200

1400

1600

1800

2000

2200

2400

1,07

2,29

3,45

4,77

1,07

2,32

3,51

4,86

1,15

DAD-CH1 265 - 390 nm10 µl PAH-Mix

Retention Time

DAD-CH1 265 - 390 nm2009 05 29 Bottle B Reps

Retention Time

DAD-CH1 265 - 390 nm2009 06 18 PAH Mix Bottle B

Retention Time

Benzo(ghi)perylene

Indeno(1,2,3,c,d) pyrene

Day 0

Day 9

Day 20 2,88

4,52

6,39

Benzo(a)pyrene

The significant loss of more acetonitrile than water from the ‘open to atmosphere’ bottle was revealed by the chromatographic results; see Fig. 2.

As a result of storing the solvent bottle with a premixed mobile phase ‘open to atmosphere’, a significant shift in retention time of the test compounds was observed.This would make a retention time based compound identification completely impossible.If one suggests roughly the same “linear behaviour” of the vaporization of volatile HPLC solvents out of a eluent mixture, it becomes obvious, that even after one day of using non-sealed mobile phase bottles the user may expect changes of retentions times.

Conclusion:Without using tightly sealed solvent bottles as containers for premixed HPLC eluents there is clear risk of uncontrolled vaporization of solvents, resulting possibly in wrong retention time assignment for eluting compounds. The use of SCAT SafetyCaps definitely prevents such uncontrolled evaporation, and in addition preserves your laboratory environment from contamination of toxic compounds!

Tab. 2: Retention time shift over 9 and 20 daysDay 0 Day 9 Days 20

Compound 1 2.29 2.32 2.88Compound 2 3.45 3.51 4.52Compound 3 4.77 4.86 6.39

Fig. 2: Chromatograms after 9 and 20 days of storage of Bottle B

Much better!

Fig. 1: graphical representation

Not this way!

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 20108

LaChrom Elite® application

Drastically simplified sample preparation by application of Chromolith® columns

Example: Determination of beer bitterness at 80% reduced total analysis time

“Beer is a fermented aqueous drink based on starch and flavoured by hops. It is brewed by using water, barley malt and hops. The most important asset of hops is the bitter taste conferred to particularly, blond beers. Furthermore, hops are necessary for the stabilization of beer foam, while, on the other hand the most precarious off-flavour in beer, called lightstruck flavour, involves degradation of hop-derived components. Reduced iso-α-acids hop extracts (rho-, tetrahydro-, and hexahydro-iso-α-acids) are in widespread use in breweries around the world for the purpose of achieving light-stable products with foam and cling enhancement. Brewers can take advantage of blending these reduced iso-α-acids to produce beers with different flavour profiles. The HPLC method is currently the only analytical tool for controlling hop dosing and bitterness in beers brewed with reduced iso-α-acids.

Beer decomposes on exposure to light, thereby generating an offending ‘skunky’ flavour. Thus, beer must be stored in green or brown bottles, in order to prevent light from being transmitted through the glass. The cause for this phenomenon is the vulnerability of the iso-alpha-acids to light. The resulting decomposition leads to formation of the so-called ‘lightstruck flavour’. The mechanism for the formation of the lightstruck flavour was confirmed by the unambiguous identification of 3-methylbut-2-ene-1-thiol in illuminated beers. The flavour threshold of the thiol is so low that even concentrations of few ppb spoil irreversibly the beer quality.” (1)

Fig. 1: LaChrom Elite® system

Fig. 2: Decomposition of Iso-α-acidsActivation of, for example, the isohumulones with UV light causes bond cleavage by a Norrish Type I reaction, leading to a ketylacyl radical pair. Subsequent loss of carbon monoxide from the acyl radical and recombination of the resulting fragment with a thiol radical furnish 3-methylbut-2-ene-1-thiol, also known as ‘skunky thiol’

Analytical HPLC

VWR ChromJournal Issue 8 Spring 2010 9

This application is based on the original publication from Alexis Bolívar and Mónica Gasparri (2). It describes a rapid and fully validated HPLC method for routine analysis of reduced Iso-α-acids in beer within six minutes run time and drastically simplified sample preparation procedure by application of a 4.6 mm i.d. Chromolith® column instead of a particulate column. In the original application the IAA’s (Iso-α-acids) and HHIAA’s (Hexa-hydro-iso-α-acids) are coeluting. The Polar brewery (Caracas, Venezuela) uses only white glass bottles and no IAA (Iso-α-acids) for their blendings, therefore they don’t need a perfect separation of the critical peak pairs H3/I1 and H5/I2 (please refer to Fig. 6a and 6b).

In many parts of the world the breweries use green or brown glass to bottle their beers. Therefore for a more general approach it was necessary to achieve a full separation between the reduced iso-α-acids isomers (RIAA‘s) beside the iso-α-acids isomers (IAA‘s). In order to reduce the flow rate from originally 3 ml to 1.5 ml and to save solvent a 3 mm i.d. Chromolith® column was applied instead of a 4.6 mm i.d. Chromolith® column.

Separation of Iso-α-acids and reduced Iso-α-acids in brewing using the Merck Chromolith® column

Fig. 3: Chromolith® column

Fig.4a: Complex sample preparation procedure using solid phase extraction when particulate columns are used. Particulate columns can be blocked easily by the matrix of natural samples.

Fig. 4b: When the Chromolith® columns are used only filtration is necessary as sample preparation. The pore structure of the Chromolith® with its 130 Å mesopores and 2 µm macropores explains the high robustness which allows the direct injection of natural samples with a high content of matrix.

Fig. 5: Scanning Electron Microscope (SEM) pictures of the pore structure of a Chromolith®. This unique pore structure allows to inject natural samples like beer e.g. directly on the column without any sample preparation.

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 201010

Fig. 7a: Injection of 50 µl Heineken beerThe Heineken beer contains Iso-α-acids (IAA’s) and small amounts of Tetrahydro-Iso-α-acids (THIAA’s)Column: Merck Chromolith® Performance RP-18e, 100-3 mmColumn temperature: 25°CEluent A: Tetrabutyl-ammonium hydroxide buffer, pH 6.8Eluent B: 80 % Acetonitrile/ 20 % THF premixedIsocratic elution: 65 % A/ 35 % B, mixed by the pump, Flow rate: 1.5 ml/minWavelength: 254 nm with reference at 350 nm

SummaryIn this application a baseline separation of the Iso-α−acids(IAA’s)andthereducedIso-α-acids (RIAA’s) in eleven minutes run time was achieved. Using the Chromolith® column from Merck it is possible to inject 50 µl of wort and beer samples directly onto the column without any sample preparation. With conventional particulate columns in contrast a complicated and time consuming sample preparation has to be done prior to the normal HPLC analysis. Using the Chromolith® columns the breweries can save about 60 % costs and 86 % time for the complete procedure to measure their beer bitterness.

References: 1) Fundamentals of beer and hop chemistry, Denis De

Keukeleire, University of Gent - Faculty of Pharmaceutical Sciences - Laboratory of Pharmacognosy and Phytochemistry, Gent (Belgium), Quimica Nova, 23(1): 108-112, 2000

2) Alexis Bolívar, Mónica Gasparri and Carsten Zufall, Corporative Quality, Innovation and Development Department, Cervecería Polar C. A., Caracas, Venezuela; J. Am. Soc. Brew. Chem. 64(1):39-46, 2006

Fig. 6a: Sample: Calibration standard containing Iso‑α‑acids and reduced Iso‑α‑acidsThe conditions from the original application (1) was transferred to the Merck Chromolith® Performance RP-18e, 100-3 mm columnEluent A: Tetrabutyl-ammonium hydroxide buffer, pH 6.8 Eluent B: Acetonitrile Isocratic elution: 59 % A / 41 % B, mixed by the pumpFlow rate: 1.5 ml/minRun time: 6 min

Fig. 6b: Sample: Calibration standard containing Iso‑α‑acids and reduced Iso‑α‑acidsWhen 20 % of Tetrahydrofurane (THF) is added to the acetonitrile it is even possible to separate the two critical peak pairs H3/I1 and H5/I2.Eluent A: Tetrabutyl-ammonium hydroxide buffer, pH 6.8 Eluent B: 80 % Acetonitrile/ 20 % THF, premixedIsocratic elution: 65 % A/ 35 % B, mixed by the pump, Flow rate: 1.5 ml/minRun Time: 11 min

Fig. 7b:Overlay of 50 µl Heineken beer with the calibration standard

The new VWR Chromatography Catalogue available now!Outstanding chromatography solutions to support your analytical or preparative requirements. Featuring a wide range of market leading brands for chromatography consumables, instruments and accessories.

Order your free copy online today at:

http://eu.vwr.com/chrom

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Analytical HPLC

VWR ChromJournal Issue 8 Spring 2010 11

Prepare HPLC / UHPLC samples three times faster using Whatman Mini-UniPrep syringeless filters

Whatman Mini-UniPrep™ Syringeless Filters provide a faster, easier way to remove particulates from samples

and will provide a visual confirmation that all samples analysed are filtered.Instead of using a syringe, syringe filter, vial, and septum, just use one Mini-UniPrep and perform the same manipulation in just a few seconds.

Because of the specific demands for sample preparation in chromatography applications, sample preparation can become a bottleneck in the daily activity of the laboratory. Protection of columns for HPLC applications has always been advised and with the latest developments of instruments moving towards Ultra HPLC, this has become increasingly important. Using smaller particle sizes and higher pressures, columns can achieve increased resolution of separated components. However, the cleanliness of the sample preparation is critical.

Continuously striving to improve and innovate, Whatman has listened to these new needs and created a whole family of Mini-UniPrep filters.

You will see the huge benefits for your laboratory with the time and money saved by

3 times faster sample preparation

removing the need for multiple consumables from the sample preparation process.

For customers using slit septa, Whatman offers Slit Septa Mini-UniPrep.

For customers who need to protect samples from light damage, there is Amber Mini-Uniprep. To maximise the sample preparation throughput, Whatman developed the 6 Place Compressor. This will allow you to process 6 Mini-UniPrep at the same time and will reduce the risk of hand stress.

The filter membrane is housed at one end of a plunger, with a cap/septum at the other. By pressing the plunger through the sample placed into the chamber, positive pressure forces the filtrate into the reservoir of the plunger. Air escapes through the vent holes until the

SimplePlace unfiltered sample in chamber.

InnovativeCompress filter plunger into sample chamber. Clean filtrate fills reservoir from bottom up.

ConvenientThe Mini-UniPrep vial shape fits easily in autosamplers.

evaporation seal is engaged, providing an airtight seal. Within seconds the Mini-UniPrep can be placed into your autosampler for injection into your instrument.

Six position compressor makes your job even easier

Please contact your local VWR customer support for availability of amber coloured housing or slit septum.

Mini-UniPrep benefits:

Reduces sample prep time and improves efficiency•Reduces costs•Reduces laboratory waste•Protects columns – as filtration is in vial•Gives visual conformation sample has been filtered•Flexible: designed to fit in autosamplers that take •standard 2 ml vialsFlexible: available with a choice of membranes•

Technical specificationDimensions Equivalent in size to 12 mm x 32 mm vialsMaterials of construction Housing and cap: Polypropylene

Filter media: As specifiedSepta: PTFE membrane and silicone rubber

Filtering capacity 0.4 mlNominal force needed to compress Approximately 8 psi (0.6 bar)Max operating temperature 120° F (50 °C)

Choose the right Mini-UniPrep filtering mediaSample media Suitable Mini-UniPrep mediaParticulate laden liquids Glass Microfibre (GMF) Aqueous/organic samples in 3 to10 pH range Nylon (NYL)General filtration media/solvent based samples Polypropylene (PP)Chemically aggressive solutions Polytetrafluoroethylene (PTFE)Biological samples requiring low protein binding media Polyethersulphone (PES)Aqueous/organic solvents – low nonspecific protein binding media Polyvinylidinefluoride (PVDF)Aqueous/organic solvents – high flow and loading capacity Polypropylene Depth (dp PP)Aqueous/organic solvents – low nonspecific protein binding media Regenerated Cellulose (RC)

Sample preparation

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 201012

VWR is proud to present the new VWR Collection Chromatography Syringes. This new line from VWR is the optimum addition to your laboratory providing easy liquid transfer.VWR introduce a broad range of different syringes for manual or automated sample preparation, or sample injection into HPLC or GC systems. The syringes give optimum precision and accuracy together with excellent price-performance ratio.

Chromatography accessories

VWR Collection HPLC syringes

One of the new VWR Collection Chromatography Syringe product lines is:

Super Elastic Plunger modelsThe Super Elastic Plunger models are a new age of syringes with a special Titanium-Nickel alloy plunger which have stronger resistance to chemicals and bending.

Super Elastic Plunger features:

Description Cat. No.Syringemicro10μlSTDfixed needle

549-0199

Syringemicro100μlGasTight luer lock

549-0539

Syringemicro10μl 23 Gauge, Agilent 7673A

549-0567

New syringe product

line!

Superior flexibility of a special Ti-Ni alloy which will bend but won’t kink. It simply springs back (ref. Fig. 1)

- Plunger can be wound into a 16 mm diameter coil- Caution: Super-elasticity is weakened below -10°C and

disappears over 200 °C

Superior chemical resistance•- The robust Ti-Ni alloy is more resistant to acid, alkalis

and salt solutions than standard stainless steel (ref. Fig. 2)

• Accuracy and reproducibility- Accuracy and reproducibility of injection is within ± 1 %

Compatible with Agilent and Rheodyne HPLC valves.

The Super Elastic plunger provides extended syringe life time.

Figure 1

Figure 2

VWR ChromJournal Issue 8 Spring 2010 13

Hibar® HR Purospher® STAR RP-18 endcapped UHPLC columns from Merck, available with 2 µm and 3 µm particle sizes, are ideal for rapid applications such as high-throughput screening and analysis, process monitoring, QC analyses, method development, and LC/MS. Accelerating separations by up to 90%, these columns offer highest performance, resolution, and stability.

Speed up separations 10 times with Purospher® STAR UHPLC columns

Speed up separations, drop solvent consumptionWhen used with UHPLC instruments, all Hibar® HR Purospher® STAR RP-18 endcapped UHPLC columns from Merck accelerate applications by 10 times – and maintain excellent peak shape. Users will also see an up to 84.5% drop in solvent consumption. Not only are these columns incredibly efficient, they perform so well that one column type is enough for most applications.

High resolution keeps methods flexible

During ultra-fast applications, using e.g. 5 µm particle sizes can actually result in lower resolution of critical peaks. To offset this, Merck offers column material that accommodates 2 µm and 3 µm particulate silica. As the sorbent is highly pure, applications will consistently give optimum peak symmetry.

Outstanding pH and pressure stability – for an even wider range of applications

Hibar® HR Purospher® STAR RP-18 endcapped 2 µm UHPLC columns remain stable at pressures up to 600 bar and can be used with alkaline eluents up to pH 10.

Description Cat noHibar® HR 30-2.1 Purospher® STAR RP-18 endcapped 2 µm

1.50645.0001

Hibar® HR 50-2.1 Purospher® STAR RP-18 endcapped 2 µm

1.50646.0001

Hibar® HR 30-2.1 Purospher® STAR RP-18 endcapped 3 µm

1.50650.0001

Hibar® HR 50-2.1 Purospher® STAR RP-18 endcapped 3 µm

1.50651.0001

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom

VWR ChromJournal Issue 8 Spring 201014

In line with the SCAT Europe target to offer quality, safety and over all functionality SafetyFunnels are now available from VWR.

Not only used in the laboratory but also in production and storage areas; the SafetyFunnels with cover, stainless steel sieve and grounding connection is especially developed for use in tight spaces. There’s no safer way! Ignition sources are avoided by the electroconductive HDPE which offers perfect protection against electrostatic charges.

In combination with the electroconductive 10 litre waste container with mechanical level control the total height is just 39.5 cm including

the angled adapting connecting piece - used to keep the funnel upright. Available with different thread diameters; the SafetyFunnel can be used on every standard waste container. Also there’s a special connector available for barrels.

Simple to install and remove, the funnel has a diameter of 13.5 cm and in combination with the stainless steel sieve that acts as an additional splash guard the disposal of large quantities of liquid waste becomes easy. The cut-way drawing explains the functional details of the funnel. It’s clear to be see that SCAT Europe does what ever is possible to reduce dangerous vapours in the laboratory.

SCAT Europe products are distributed by our partner VWR. In addition to the SafetyFunnels VWR offers the complete range from SCAT Europe including; SafetyWasteCaps, SafetyCaps and fire resistant products. By using these products you protect yourself, your employees, save money and create added value to your operation.

SCAT Europe SafetyFunnels for collecting waste fluids

SeeChrom Shop for special

pricing

Chromatography accessories

VWR ChromJournal Issue 8 Spring 2010 15

A spring supported seal increases the performance in Headspace analysis.

The new sealing system allows the plunger to work with enhanced tightness over •the whole temperature range from 40-150 °C.

The lifetime is 3-5 times higher compared to today’s Headspace syringes on the •market.*

* lifetime may vary on conditions used on application.

New Headspace plunger from Hamilton for CTC PAL System

With this new plunger design Hamilton has set a new standard for Headspace syringes.The new patented plunger design has been optimised for higher throughput in Headspace analysis.

CTC Instrument are original equipped with HAMILTON syringes, ask VWR for the HAMILTON syringe catalogue

patent pending PAL is a registered trademark of CTC Analytics AG l Switzerland

Description Pack size Cat noModel 1001; Volume 1000 µL; Gauge 23; (23/51/5) CTC 1 pk 549-1324Model 1002; Volume 2500 µL; Gauge 23; (23/51/5) CTC 1 pk 549-1325Model 1005; Volume 5000 µL; Gauge 23; (23/51/5) CTC 1 pk 549-1326Model 1001; Volume 1000 µL; Gauge 26; (26/51/5) CTC 1 pk 549-1327Model 1002; Volume 2500 µL; Gauge 26; (26/51/5) CTC 1 pk 549-1328Model 1005; Volume 5000 µL; Gauge 26; (26/51/5) CTC 1 pk 549-1329

For more information on these products contact your local VWR sales office, send an e-mail to [email protected] or visit our website http://eu.vwr.com/chrom