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June 2000 - Scientific Instrument Services, Inc.
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1. FEATU RES Vacuum Pump Exhaust Filters The first of three articles reporting on the effectiveness of filters designed for use on the exhaust of vacuum pumps Replacing a DeTech Electron Multiplier in the Agilent 5973 MSD Replacing an electron multiplier can be successfully accomplished in just 15 minutes after the instrument is cooled down to the touch All that is required are a pair of clean room gloves and the DeTech Model 2300 Electron Multiplier NEW SIS Monthly E mail Newsletter Beginning in July SIS will be distributing a monthly e mail newsletter on SIS products services promotions news and other mass spectrometer related information To receive this free newsletter fill in the attached form pg 15 with your e mail address and return it to SIS by mail or drop it off at the ASMS meeting CONTENTS SIS Hospitality Suite e ee 1 ASMS Seminar Abstracts 2 Terms and Conditions 2 AutoDesorb TD4 vs Transfer Line 3 Vacuum Pump Exhaust Filters De lech Multipliers poet eaa i SGE MS noVent 13 Oin l Screwdriver gi ee ae eee 14 The Mass Spec Source Summer 2000 Vol XXII NO 1 Spring 2000 For Mass Spectrometry and Chromatography The Tradition Continues at ASMS nce again SIS will be attending the annual ASMS meeting in Long Beach California on June 12 15 SIS will be providing our traditional ice cream treats in our ASMS suite The SIS ho
2. O Mass Spec Source Newsletter O S I S monthly e mail newsletter O CD O A Software DEMO CD for NIST 98 SIMION 3D and ProLab 2 Please check technique s you use J EI Cl T APCI New J Electrospray T CF FAB J Thermospray T CE MS 1 LC MS O TOF 1 Direct Probe O ICP MS T FAB 3 What Mass Spectrometer s do you have in your lab Finnigan MAT m 4500 4600 MAT90 Incos 50 500XL O Trace AQA TSQ 70 700 7000 Agilent Technologies 1 5970 5971 5972 1 5973 VG Fisons MicroMass 70 70 ZAB O Platform LC MS MD800 Varian O Saturn Il I Other Manufacturers JEOL Sciex O Hitachi Nermag Perkin Elmer QMass Waters Integrity O PE Bio Mariner O LECO SIS Monthly E mail Newsletter T GCQ T LCQ J lon Trap ICP MS J Other 5985 5988 5989 J 5990 1 GCD m 1100LC MSD J Autospec m TRIO 1000 2000 J Quattro O Other O Saturn 2000 O Extrel O Shimadzu O Vestec O Balzers O Nicolet Bruker J Leybold Inficon Other Monthly Specials News from SIS New Products New Services Links to MS Resources To Get on This New E mail List Fill in Your E mail Address Above and Check the Appropriate Box in Section 1 a a The Mass Spec Source Summer 2000 15 Explore The World of Mass Spec SES Invites you to explore our web site hup www sisweb com tinuall
3. Abstract The combination of high performance liquid chromatography and mass spectrometry LC MS has had a significant impact on industrial applications over the past decade Continual improvements in LC MS interface technologies combined with powerful features for structure analysis qualitative and quantitative have resulted in a widened scope of application An iterative cycle of what is it and how much is there continues to fuel the tremendous growth of LC MS This talk will review the fundamentals of LC MS and provide perspective on strategies for method development Current applications of LC MS technologies and emerging industry trends will also be discussed Warranty S LS does not warranty that the items described herein are usable or fit for a particular purpose Our company makes no representation as to condition or character of the merchan dise S I S will not be responsible for consequential or special damages The Mass Spec Source Editorial Board amp Newsletter Staff John J Manura Christopher W Baker Dr Steve Colby Eric Butrym J Philip Tielmann Production Scientific Instrument Services Inc 1027 Old York Road Ringoes NJ 08551 1039 Phone 908 788 5550 FAX 908 806 6631 Web http www sisweb com E mail http www sisweb com contact Copyright 1999 by Scientific Instrument Services Ringoes NJ 08551 2 The Mass Spec Source Summer 2000 Mass Spec Desk Reference by O David Sparkman
4. e MSLinks expanded listings and reference materials Books expanded listings of scientific related books Application Notes on thermal desorption GC and GC MS Scientific Instrument Services 1027 Old York Rd Ringoes NJ 08551 Bulk Rate US Postage PAID Permit No 388 Somerville NJ
5. 11 Deplech _ Detech Detector Technology Inc Manu fa ctures a Complete Line of Committed to Excellence Quality and Affordable Electron Multipliers he DeTech family of multipliers is engineered for high performance and maximum reliability in applications ranging from low gain analog amplification to high gain pulse counting requirements DeTech s Committed to Excellence philosophy is not just a fancy slogan its the way they do business Defech is committed to the manufacturing of a quality product as well as providing total customer support All DeTech multipliers are comprehensively 100 tested before being shipped DISCOUNT on all DeTech Mass Spec Detectors Limit of 5 Offer Good Through July 2000 Photocopy this coupon and mail it in with your next order 12 The Mass Spec Source Summer 2000 SAVE 6 12 HOURS ELIMINATES MS VENTING CONNECTS SIMPLY TO MS INLET AND GAS LINES PREVENTS MS AIR CONTAMINATION IMMEDIATE AIR WATER CONFORMANCE 5 minute GC MS Column Changeover Peak 3 4 chlorophenol Peak 4 Decylamine Peak 5 Undecanol 113400 Ms NoVent Interface 650 00 585 00 113405 HP5970 2 x Restrictor 50 00 45 00 113407 HP5971 5972 2 x Restrictor 50 00 45 00 113409 HP5973 2 x Restrictor 50 00 45 00 113424 HP5988A 2 x Restrictor 50 00 45 00 113422 HP5989 Engine 2 x Restrictor 56 00 50 40 1138419 GCQ 2 x Restrictor 1 x Adapter 8
6. Elinginaber Stage A Lange elie i A 2 m ee ee E E Len I int E E EJI n a oa Fihan Sampl after H Mia Elmar Stage 1 Figure 4 Efficiency of the Oil Mist Eliminator at Removing Hydrocarbons chromatogram in Figure 4 A large number of straight and branched hydrocarbons were detected with carbon chains over 20 carbons in length The bottom total ion chromatogram in Figure 4 shows the air sampled after the oil mist eliminator When the oil mist eliminator is used these high molecular weight organics are trapped by the filter and returned to the pump They do not exhaust out of the oil mist eliminator and are not present in the chromatogram This study demonstrates that the oil mist eliminators are quite effective at performing the job for which they have been designed that is trapping the high molecular weight vacuum pump oils and returning them to the vacuum pump Silage Pump Exhaust Stage 1 ter CH Mit Elina Figure 5 Trapping Efficiency of Filter Stages 1 0ul of gasoline injected into pump However the oil mist eliminators with their paper filters are not effective at trapping the lighter hydrocarbons and organics in the vacuum pump exhaust as shown in the chromatograms of the second study Figure 5 In this study 1 0 ul of gasoline was injected directly into the vacuum pump and the exhaust air subsequently collected at the exhaust port of the vacuum pump and after the oil mist eliminator
7. a call Thanks for your continued support Tuesday Lunch How AMDIS Could Have Saved My Sister s Marriage by O David Sparkman AMDIS attempts to reconstruct original mass spectra for individual components in arbitrarily complex GC MS and LC MS reconstructed total ion current RTIC chromatograms and if a target library is provided AMDIS can directly identify target compounds AMDIS is especially useful when an RTIC chromatographic peak represents multiple components Regardless of each component s concentration pure mass spectra are deconvoluted for analysis AMDIS has been designed to reconstruct pure component spectra from complex RTIC chromatograms even when components are present at trace levels For this purpose observed chromatographic behavior is used along with a range of noise reduction methods AMDIS is distributed with specialized libraries environmental flavor and fragrance and drugs and toxins that were derived from the NIST98 Library AMDIS has a range of other features including the ability to search the entire NIST98 Library with any of the spectra extracted from the original data file It can also employ retention index windows when identifying target compounds and can make use of internal and external standards maintained in separate libraries A history list of selected performance standards is also maintained Wednesday Lunch LC MS Fundamentals and Applications by Mike Lee Milestone Development Services
8. adsorbs and traps the volatile and semi volatile organics from the pump exhaust and prevents these organ ics from entering the laboratory environment It is recommended that both filters be used The oil mist eliminator traps the large vol ume of heavy oils which would otherwise quickly saturate the charcoal trap during initial pump down or when using the gas bal last valve to purge the pump oil When both filters are used in series on a vacuum pump exhaust port the exhaust from the final stage of filtering has been shown to be cleaner than the normal lab oratory air References 1 Vacuum Pump Exhaust Filters Part I Two Stage Vacuum Pump Exhaust Filter System by John J Manura April 2000 SIS Application Note 82 http www sisweb com referenc appInote app 82 htm 2 Vacuum Pump Exhaust Filters Part II Oil Mist Eliminators by John J Manura April 2000 SIS Application Note 83 http www sisweb com referenc appInote app 83 htm 3 Vacuum Pump Exhaust Filters Part III Charcoal Exhaust Traps by John J Manura April 2000 SIS Application Note 84 http www sisweb com referenc applnote app 84 htm 4 Design Development and Testing of a Microprocessor Controlled Automated Short Path Thermal Desorption Apparatus by John J Manura Vinod T Das Christopher Baker Daniel Lieske John C Miller John Manos Roland Roadenbaugh Thomas G Hartman SIS Application Note 80 http www sisweb com referenc appInote app 8
9. of the vacuum pump and the Oil Mist Eliminator was clamped to this fitting using a centering ring and clamp The Stage 2 charcoal trap used for this study is the Koby charcoal exhaust filter Scientific Instrument Services Part KA 1 which is fitted with an adaptor to mate it to the NW fitting on top of the oil mist eliminator The two filters are clamped together using a centering ring and clamp All studies were performed on a BOC Edwards model E2M1 5 rotary vacuum pump which is the standard model used on the Agilent mass spectrometers The old oil in the pump was drained and the pump was charged with a volume of Inland 45 pump oil Scientific Instrument Services Inland 45 pump oil is the vacuum pump oil of choice because it is a highly refined oil 4 The Mass Spec Source Summer 2000 comprised of aliphatic hydrocarbons with chain lengths of between 20 and 40 carbon units The pump was run for two hours and the oil drained The pump was again filled with a full charge of Inland 45 pump oil and run for 2 hours with the gas ballast valve open and then for an additional 2 hours with the gas ballast valve closed before any testing was done This cleaning and flushing procedure assured that the pump was free of contaminants from the previous use of the vacuum pump For this study a micro needle valve was attached to the intake port of the vacuum pump to permit a calibrated flow of air into the vacuum pump The flow through the needle valve
10. this series 3 demonstrat ed that each charcoal trap could be saturated with 70 ml of gaso line with no volatile emissions being eluted from the filter In addi tion to trapping volatile and semi volatile organics these charcoal traps will adsorb water oil mist dirt to 0 5 microns and bacteria to 0 5 microns The Koby charcoal traps produce minimal back pressure to the vacuum pump and can therefore operate safely on the exhaust port of the vacuum pump Pump Exhaunsi Stage 2 After Koby Charcoal Trap Figure 6 Trapping Efficiency of Two Filter Stages 1 0ul of gasoline injected into pump 6 The Mass Spec Source Summer 2000 In the next study 10 ul of gasoline was injected directly into the vacuum pump and the exhaust air from all three locations or stages of the pump filters was collected and analyzed as described above Figure 6 At the exhaust directly from the vacuum pump top chromatogram stage A as well as the exhaust after the oil mist eliminator middle chromatogram Stage 1 high concentra tions of the aromatics and hydrocarbons from the gasoline were detected However the charcoal trap was extremely efficient at removing all the volatile organics from the vacuum pump exhaust The exhaust from the top of the charcoal trap bottom chro matogram Stage 2 contained no peaks of any volatile or semi volatile organics As shown above none of the light hydrocarbons including hexane and pentane were eviden
11. 0 htm 5 Two Stage Vacuum Pump Exhaust Filter Systems Scientific Instrument Services 1027 Old York Road Ringoes NJ 08551 Phone 908 788 5550 http www sisweb com vacuum sis exfilter htm The Mass Spec Source Summer 2000 7 COMPLETE TWO STAGE VAQUUM PUMP EXHAUST FILTER KITS The charcoal trap Stage 2 adsorbs and traps the volatile and semi volatile organics from the Featu res pump exhaust and prevents these i a organics from entering the i laboratory environment Each trap Two Stage Vacuum Pump Exhaust System rie Mi onene chor SO ona ol e Purifies Vacuum Pump Exhaust Gases ee carbon with a surface area of about 1500 sq meters per gram e Provides for a Safe Laboratory Environment and has a high adsorption i A aaa capacity for adsorbing organic Stage 1 Oil Mist Eliminator contaminants The charcoal traps e Eliminates Pump Oil Fumes also adsorb waiter oil mist dirt and bacteria to 0 5 mi e Returns Used Oil to Vacuum Pump acteria to 0 5 microns Stage 2 Charcoal Filter 3 During initial pump down or when e Traps Organic Chemicals ae Eana e ee ae vapors exhaust from the vacuum e Traps Particles amp Bacteria to 0 5 microns pump The oil mist eliminator Stage 1 traps the hydrocarbons in this exhaust The paper wick inside the oil mist eliminator exposes the oil mist to a large surface area to adsorb the oil vapor and return it to the vacuum pump Pump Exhaust aft
12. 2 00 73 80 113426 SSQ7000 2 x Restrictor 1 x Adapter 80 00 72 00 113410 MS 5000 5050 2 x Restrictor 1 x Adapter 82 00 73 80 113412 Saturn 2000 2 x Restrictor 1 x Adapter 82 00 73 80 113414 Saturn 1 2 amp 3 2 x Restrictor 1 x Adapter 82 00 73 80 6 3 4 5 6 7 8 9 min WITHOUT ms NoVent The Mass Spec Source Summer 2000 13 The SIS Tradition Continues at ASMS Get Your FREE 10 in 1 Screwdriver At Our Annual Ice Cream Hospitality Suite Date Monday June 12 Tuesday June 13 Wednesday June 14 Time 7 30 10 30pm Hospitality Suite 12 00 1 00pm Lunchtime Lectures Place Hyatt Hotel r Hyatt Seaview C First Floor Lunchtime Lecture Presentations at the SIS Hospitality Suite Monday Applications of the AutoDesorb System Stuart Batterman University of Michigan Tuesday How AMDIS Could Have Saved my Sister s Marriage Dave Sparkman NIST Wednesday LC MS Fundamentals and Applications Mike S Lee Milestone Development Services Scientific Instrument Services Inc Phone 908 788 5550 Web Site http www sisweb com 14 The Mass Spec Source Summer 2000 To Receive Your FREE 10 in 1 Screwdriver Ay Just Fill in this survey and bring i ae to our booth at ASMS Name Mass Spec User Survey Company Address FAX Phone e mail 1 Would you like oO S I S GC MS Supplies Catalog O Printed
13. The Mass Spec Survival Guide You will be able to e Communicate more effectively through written and oral presentations e Verify that you are utilizing the correct terminologies e Submit higher quality proposals e Understand and utilize the appropriate formats and conventions ass OC a fm You will have at your fingertips e A complete list of correct and incorrect terminology e Important formulas and equations e A thorough overview of modern instrumentation and techniques e A comprehensive bibliography of mass spectral publications e Where to find information on any topic in mass spectrometry Whether you are a newcomer teacher manager or experienced practitioner engaged in mass spectrometry you will find this handy desk reference and invaluable tool for improving your results Part No Description Price 0 9660813 2 3 Mass Spec Desk Reference 29 95 The Mass Spec Source Summer 2000 3 Vacuum Pump Exhaust Filters Part A Two Stage Vacuum Pump Exhaust Filter System By John J Manura Scientific Instrument Services Inc 1027 Old York Road Ringoes NJ 08551 INTRODUCTION The quality of indoor air is affected by many factors including construction materials heating and ventilation systems and emissions of volatile organic compounds VOC s from building furnishings equipment and maintenance supplies In the laboratory chemicals and instrumentation are additional contribu
14. and analyzed as described above The exhaust at the top of the vacuum pump top chromatogram Stage A as well as the exhaust after the oil mist eliminator second chromatogram Stage 1 exhibit high concentrations of the volatile aromatics and hydrocarbons from the gasoline Additional studies described in the second article of this series 2 demonstrates that these volatiles are not purged out of the vac uum pump oil very quickly but are in fact purged out over many hours or days of continuous pumping Therefore venting the vac uum pumps for a short period of time when hazardous materials are analyzed will not be effective in preventing these materials from entering the laboratory environment The vacuum pumps must be externally vented continuously or a better system such as the addition of a charcoal trap is needed to trap these more volatile organics Charcoal Traps Charcoal traps are ideally suited for the trapping of volatile and semi volatile organics in air The Koby charcoal trap used for this study has been designed for the trapping of volatile and semi volatile organics from the vacuum pump exhausts Each trap con tains about 100 grams of carbon with a surface area of about 1500 sq meters per gram This high surface area provides for very effi cient air purification These charcoal filters have a high adsorption capacity and affinity for adsorbing organic contaminants Further testing described in the third article of
15. aphy is a versatile method for identifying and quantifying trace levels of volatile organic compounds VOCs Points to be discussed include the appropriate choices of sorbents and method parameters in order to accommodate a wide range of compounds and high humidity The advantages of an automated short path system for minimizing artifacts losses and carry over effects are illustrated As examples results will be presented that demonstrate the performance of a thermal desorption method for 77 VOCs using laboratory and field tests and a dual sorbent system Tenax GR Carbosieve SIII Laboratory tests showed that the method requirements for ambient air sampling were easily achieved for most compounds e g using the average and standard deviation across target compounds blank emissions were lt 0 3 ng sorbent tube for all target compounds except benzene toluene and phenol the method detection limit was 0 05 0 08 ppb reproducibility was 12 6 linearity as the relative standard deviation of relative response factors was 16 9 desorption efficiency was 99 28 samples stored for 1 to 6 weeks had recoveries of 86 9 and high humidity samples had recoveries of 102 11 Due to sorbent column and MSD characteristics performance was somewhat poorer for phenol groups ketones and nitrogen containing compounds The laboratory results were confirmed in an analysis of replicate samples collected in two field studies that sampled ambient air along r
16. e studies of the ability of the filters to trap volatiles 10 ul of gasoline was injected directly into the vacuum pump Gasoline was selected because it contains a wide range of volatile and semi volatile organics and would accurately simulate the wide range of chemicals that might be injected into a mass spectrometer DISCUSSION Oil Mist Eliminator Oil mist eliminators are designed to trap the heavy oil vapors or mists which escape from the vacuum pump during initial pump down during extended operation or when using the gas ballast valve to purge or outgas the vacuum pump oil The oil mist elim inator contains a replaceable paper cartridge inside the filter hous ing The paper wick exposes the oil mist to a large surface area to adsorb the oil vapor and return it to the vacuum pump When a vacuum pump is first turned on this oil mist is easily seen as a fine mist which enters the laboratory environment See the second article in this series for a more thorough description of the oil mist eliminator 2 The effectiveness of the oil mist eliminator is demonstrated in Figure 4 For this study the purge leak valve on the vacuum pump inlet was opened and the leak flow was adjusted to 300 ml minute At the vacuum pump exhaust port stage A of the pump a high concentration of high molecular weight hydrocar bons is exhausted from the pump as shown in the top total ion The Mass Spec Source Summer 2000 9 Eshmat Sampled Before C4 Mist
17. er Charcoal Trap HHE Eibyl Bansane Avice viene 1 Eibyl I Methy Beneene 1 3 Tribeca l Bs tie Lhe ae ti W H E H H i Hydrocarbon Cui 1 1 ai M re z ee 4 E 1h Ue Viens d it Ww tt tt Hh P Pump Exhaust with No Filtering 8 The Mass Spec Source Summer 2000 COMPLETE TWO STAGE VAQUUM PUMP EXHAUST FILTER KITS Alcatel Pump Filter Kit Kit Part FK101 For all Models of Alcatel Vacuum Pumps with NW25 flange Alcatel Vacuum Pump Kit Kit FK101 contains the Alcatel Oil Mist Eliminator Koby Filter and the fittings shown below This kit is all you need to install the complete two stage exhaust filter to your Alcatel vacuum pump It can also be used with any other manufacturers pumps that have an NW25 flange type fitting on the exhaust port Part No Description Price FK101 Alcatel Pump Filter Kit 223 20 Edwards Large Filter Kit For Edwards Models E1M5 8 E2M3 5 8 and RV3 5 8 pumps The Pump Filter Kit for the Edwards Pump includes the Edwards EMF10 Oil Mist Eliminator Koby Charcoal Trap and all fittings needed to attach this two filter system on the larger Edwards vacuum pumps This kit is to be used with Edwards models E1MS5 8 E2M2 3 5 8 and the RV3 5 8 vacuum pumps It can also be used with any other manufacturers pumps that have an NW25 flange type fitting on the exhaust port Part No Description Price FK201 Edwards Large Filter Kit 234 70 Edwards Small Fil
18. ess of a two Stage vacuum pump filtering system The first stage filter consists of an oil mist eliminator to trap the heavy oils from the pump oil mist and return them to the vacuum pump The second stage is a charcoal trap for the containment of volatile organics in the vacuum pump exhaust The second article in this series 2 describes the design of the oil mist eliminator and includes additional studies of the effectiveness of the oil mist eliminator The third article in this series 3 describes the efficiency of the charcoal trap in greater detail The combination of the two vacuum pump exhaust filters described in this article can provide for efficient and safe trapping of emissions from laboratory vacuum pumps and can improve the quality of air in the instrumentation laboratory EXPERIMENTAL at Stage 2 Filter i Carbon Filter Trap Variable Gas Leak 0 to 1000 ml min ka i Clamp Stage 1 Filter Oil Mist Eliminator Vacuum Pump Intake Port Clamp Vacuum Pump Exhaust Port Figure 1 Vacuum Pump Exhaust Filtering System Mounted on a Vacuum Pump The two stage vacuum pump exhaust filtering system is shown above Figure 1 The two filters attach in series to the exhaust port of a vacuum pump For these studies an Alcatel oil mist eliminator was used Scientific Instrument Services part 66827 as the stage 1 filter An NW25 vacuum pump exhaust fitting was first attached to the exhaust port
19. manufacturer s mount Typical Autotune for DeTech Model 2300 Step 6 Take the DeTech Model 2300 and install it into the existing manufac turer s mount Close the clips Scan 10 00 700 00 Samples 8 Thresh 100 176 Peaks Base 69 00 Abundance 492672 100 Ion Pol POS MassGain 90 MassOffs Emission 75 4 AmuGain 80 EleEnergy 69 9 AmuOffs Filament 2 Wid219 70 DC Pol Repeller 25 26 60 TonFocus 90 2 HED EntLens 28 0 EMVolts When installing the new 50 EntOffs 18 07 DeTech Model 2300 make sure of the following 10 1 The Anode Pin 0 output 1s making good contact with the output plate on the mounting 300 400 500 600 Samples 40 PFTBA OPEN Averages StepSize 30 Zones MS Source 250 TurboSpd 20 MS Quad 150 frame Abund Rel Abund IsoMass Iso Abund Iso Ratio 492672 100 00 70 00 5556 1 13 a 459392 93 24 220 00 20312 2 The back arm of the spring clip is making contact with the electron i a 2 e i multiplier s steel frame Palmer Industrial Park 9 Third Street Palmer MA 01069 Close the Mass Spectrometer s door Reconnect both the power and Tel 413 284 9975 Fax 413 284 9979 computer cables Close the vent valve and replace the top cover E Mail dticorp aol com www detechinc com Your installation is now complete Turn on the vacuum pumps Refer to your user s manual for pump time information De plech Detector Technology Inc The Mass Spec Source Summer 2000
20. o the AutoDesorb system and first purged with 30 ml of helium The desorption tubes were then desorbed from 100 to 250 C at a rate of 60 per minute and held at 250 for a total desorption time of 6 minutes The desorbed analytes were trapped on a GC Cryo Trap Scientific Instrument Services which was pre cooled to 65 C using liquid CO gt al a AutoDesorb Tower SIS AutoDesorb System Automated Short Path Thermal Desorption 12 Tube Carousel PC Controls the AutoDesorb n LLY EPLL EMT AutoDesorb h Ep Electronics EZT Console E 1 p z Tha B Er Wid MS Source HP 5973 MSD Capillary Column Figure 3 Schematic of the SIS AutoDesorb System on a GC MS System The AutoDesorb system was attached to an Agilent Technologies 6890 GC for the separation of the analytes and the Agilent 5973 MSD to detect and identify the analytes The GC column for these studies was an Agilent DB5 MS 0 25 u film thickness x 0 25 mm I D x 30 meters long A 6 long DB 5 1 5 u film thickness x 0 53 mm I D guard column was used at the front of the GC column and inside the Cryo Trap When the desorption was complete the Cryo Trap was rapidly heated to 250 C The GC column was held at 40 C for 5 minutes and then temperature programmed to 280 C at 10 per minute The total GC run time was 29 minutes The Agilent MSD was operated in the EI mode and scanned from 35 to 450 daltons For th
21. oadways and indoor air in a large office building Replicates collected under field conditions demonstrat ed good agreement except at very low concentrations or for large gt 4 1 volume samples of high humidity air Overall the method provides excellent performance and satisfactory throughput for many applications Terms and Conditions Scientific Instrument Services S I S continues to supply The Mass Spec Source newsletter as a service to our customers Printed four times a year it includes articles and notes on new products and procedures of interest to mass spec and GC users Papers from all fields of scientific inquiry in which mass spectrometry and gas chromatography can play a role will be considered and subject to review However S I S reserves the right to reject any article that is in direct competition with S I S products Articles and Application Notes Editorials and reviews on new instrumentation and techniques for GC MS will be con sidered for publication These articles may be any length and our Graphics Department will aid you in any way you may need Mass Spec Tips Any new ideas or tips that could benefit other mass spectroscopists can be submitted for inclusion in this section For More Information Anyone interested in writing in any of the areas above should contact the editor of the Mass Spec Source at 908 788 5550 We are always trying to improve this newsletter if you have any suggestions please give us
22. p The Koby filter comes with _ NPT male fit tings on both ends of the trap Therefore a NW flange to _ female adaptor must be first attached to the Koby filter before it is attached to the top of the oil mist eliminator using another center ing ring and quick clamp The oil mist eliminators Koby charcoal traps as well as all the fittings necessary for the assembly of the dual exhaust filter system are available from Scientific Instrument Services 5 In addition complete kits for the common pumps are also available 5 CONCLUSION This is Part I of a three part series of articles on the effective ness of the vacuum pump exhaust traps Part I describes the two stage vacuum pump exhaust filter system for the complete treat ment of vacuum pump exhaust 1 Part II describes the operation and the effectiveness of the oil mist eliminator 2 Part II of this series describes the charcoal trap and its effectiveness at removing volatiles and semi volatiles from vacuum pump exhaust 3 The Two Stage Vacuum Pump Exhaust Filter System has been shown to be an effective system for removing volatile and semi volatile organics from the exhaust of vacuum pumps and can help maintain an environmentally safe atmosphere in the instrumenta tion laboratory The oil mist eliminator Stage 1 has been shown to effectively trap the high molecular weight hydrocarbons from the pump oil and return these oils back into the vacuum pump The charcoal trap Stage 2
23. spitality suite hours will be Monday through Wednesday from 7 30 10 30 pm Stop by and receive our free 10 in one screwdriver after filling out the attached survey form See page 15 We have invited three other companies to share our suite These include DeTech the fastest growing man ufacturer of mass spectrometer detectors Prolab Resources a service company and manufacturer of replacement data sys tems and Mass Sensors a manufacturer of small mass spectrometers for process analytical and educational uses In addition SIS will be sponsor ing lunchtime presentations at our hospitality suite See next page SIS Posters at ASMS 1 Controlling Laboratory Air Contamination from Rotary Vacuum Pumps by Using a Two Stage Vacuum Pump Exhaust System by John Manura Poster 1270 2 Analysis of Silicone Contaminants on Electronic Components by Thermal Desorption GC MS by Eric Butrym Poster 1425 j Go A T SIS Topical Seminars at ASMS SIS is sponsoring three introductory seminars at this year s ASMS conference Each presentation is designed as an introduction to the selected topic These walk in sessions will be held from 12 15 1 00 on each day in our hospitality suite Hyatt Seaview C first floor Monday Lunch Applications of Thermal Desorption Volatile and Semi Volatile Analysis in Air by Stuart Batterman University of Michigan Air sampling using sorbents thermal desorption and gas chromatogr
24. t in the charcoal trap exhaust nor was acetone or any of the aromatics common in gaso line present in the charcoal trap exhaust Sora Alr Simpl a m pi he aaie E e ieee Fi T Yann Pump Erhan after ihe Roby Charcoal Fila dnd after LO ul getline iapertied Ineo Yocum Pomp Figure 7 Vacuum Pump Exhaust After the Koby Air Filter An additional study Figure 7 demonstrates that the air exhausted by the vacuum pump through the Koby charcoal traps was cleaner than the normal indoor air in our testing facilities Note that the results shown in this graph are shown at 50X scale expansion from the data shown in Figure 5 previously The small peaks shown in the graph are not from the gasoline but are silox anes from the GC septum aa Carbon Filter Trap aes Adaptor Clamp lt Centering Ring Variable Gas Leak 0 to 1000 ml min Oil Mist Eliminator E Clamp Centering Ring Pump Adaptor Figure 8 Assembly of the Two Stage Vacuum Pump Exhaust Filtering System ASSEMBLY OF SYSTEM The combination of the two exhaust filters are joined together and to the vacuum pump using standard NW or QF vacuum type connectors If the vacuum pump exhaust port is not equipped with an NW type fitting either NW10 16 or 25 then the appropriate adaptor for the pump must be first installed The oil mist elimina tor is then attached to this fitting using a centering ring and O ring using a quick clam
25. ter Kit Kit Part FK251 For Edwards Models E2M0 7 E2M1 and E2M1 5 pumps The Pump Filter Kit for the Edwards Pump includes the Oil Mist Eliminator Koby Charcoal Trap and all the fittings needed to attach this two filter system on the Edwards series of vacuum pumps This kit is to be used with Edwards models E2M0 7 E2M1 and E2M1 5 vacuum pumps It can also be used with any other manufacturers pumps that have an NW 10 flange type fitting on the exhaust port Part No Description Price FK251 Edwards Small Filter Kit 205 70 The Mass Spec Source Summer 2000 9 Replacing an Electron Multiplier in the Agilent HP 5973 MSD Jay S Ray Detector Technology Inc Replacing an electron multiplier can be successfully accomplished in just 15 minutes after the instrument is cooled down to the touch All that is required are a pair of clean room gloves and the DeTech Model 2300 Electron Multiplier Vent the instrument Make sure that all volt ages applied to the mul tiplier and the conver sion dynode are turned off prior to venting the system Remove power and computer cables from the Mass Spectrometer 10 The Mass Spec Source Summer 2000 TECHNICAL APPLICATION NOTES Step 4 Put on a pair of clean room gloves To remove the old multiplier simply push together the mounting clips and allow them to open so you can gain access to the multiplier Then reach in and remove the existing multiplier from the
26. tors to the contamination of the indoor air Vacuum pumps are widely used for mass spectrometers electron microscopes lyophilizers and other vacuum equipment These pumps can be a major source of indoor air contamination It is normally recommended that these vacuum pumps be vented outside the room or to a laboratory exhaust hood However this is not always practical when the instrumentation is located within the interior of a building Indoor air contamination by vacuum pumps originates from the lubricating oils used in the pumps and also from chemicals that have contaminated the pump oil When the vacuum pumps are first turned on a large volume of air is pumped through the pump oil which causes a fine mist of oil fumes to be emitted from the pump exhaust and into the laboratory air When the vacuum pumps are used in instruments such as mass spectrometers all the residual organic chemicals analyzed by the mass spectrometer are trapped in the vacuum pump oil Eventually these organics are purged out of the oil and into the laboratory air via the vacuum pump exhaust Often the organic chemicals analyzed by these vacuum system instruments can be quite toxic or carcinogenic This can present a serious environmental health problem in the laboratory This is the first of three articles reporting on the effectiveness of filters designed for use on the exhaust ports of vacuum pumps 1 2 amp 3 This first article demonstrates the effectiven
27. was adjusted to 100 ml min or 300 ml min for some studies and calibrated with a Gilibrator Air Flow Calibration System Scientific Instrument Services Part 800844 2 Exhaust After Charcoal Trap Stage 2 Variable Gas Leak 0 to 1000 ml min Exhaust After Oil Mist Eliminator Stage 1 Pump Exhaust No Filtering Stage A Figure 2 Analysis of Vacuum Pump Exhaust in the Two Stage Exhaust Filtering System For these studies air samples were collected at three levels in the exhaust stream from the vacuum pump Figure 2 The first level Stage A is directly from the pump exhaust with no filtering Another air sample was collected after the oil mist eliminator Stage 1 and the final air samples were collected after the charcoal trap Stage 2 and right before the exhaust air would enter the laboratory air Thermal Desorption tubes were packed with 100 mg of Tenax TA and flow conditioned with pure nitrogen at 50 ml min at 300 C for 3 hours Air samples were collected from the three pump stages onto the Tenax adsorbent traps at a collection rate of 25 ml min for 20 minutes 500 ml total using a Gilian LFS 113 Air Sampling Pump Scientific Instrument Services The collected samples were analyzed using the SIS Automated Short Path Thermal Desorption System AutoDesorb Model 2000 Scientific Instrument Services which is described in previous articles 4 and shown below Figure 3 The desorption tubes were attached t
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