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- Application NotesNote 103: EPA Method 325B, Novel Thermal Desorption Instrument Modification to Improve Sensitivity Note 102: Identification of Contaminants in Powdered Beverages by Direct Extraction Thermal Desorption GC/MS Note 101: Identification of Contaminants in Powdered Foods by Direct Extraction Thermal Desorption GC/MS Note 100: Volatile and Semi-Volatile Profile Comparison of Whole Versus Cracked Versus Dry Homogenized Barley Grains by Direct Thermal Extraction Note 99: Volatile and Semi-Volatile Profile Comparison of Whole vs. Dry Homogenized Wheat, Rye and Barley Grains by Direct Thermal Extraction GC/MS Note 98: Flavor and Aroma Profiles of Truffle Oils by Thermal Desorption GC/MS Note 97: Flavor Profiles of Imported and Domestic Beers by Purge & Trap Thermal Desorption GC/MS Note 96: Reducing Warping in Mass Spectrometer Filaments, with SISAlloy® Yttria/Rhenium Filaments Note 95: Detection of Explosives on Clothing Material by Direct and AirSampling Thermal Desorption GC/MS Note 94: Detection of Nepetalactone in the Nepeta Cataria Plant by Thermal Desorption GC/MS Note 93: Detection of Benzene in Carbonated Beverages with Purge & Trap Thermal Desorption GC/MS Note 92: Yttria Coated Mass Spectrometer Filaments Note 91: AutoProbe DEP Probe Tip Temperatures Note 90: An Automated MS Direct Probe for use in an Open Access Environment Note 89: Quantitation of Organics via a Mass Spectrometer Automated Direct Probe Note 88: Analysis of Silicone Contaminants on Electronic Components by Thermal Desorption GC-MS Note 87: Design and Development of an Automated Direct Probe for a Mass Spectrometer Note 86: Simulation of a Unique Cylindrical Quadrupole Mass Analyzer Using SIMION 7.0. Note 85: Replacing an Electron Multiplier in the Agilent (HP) 5973 MSD Note 84: Vacuum Pump Exhaust Filters - Charcoal Exhaust Traps Note 83: Vacuum Pump Exhaust Filters - Oil Mist Eliminators Note 82: Vacuum Pump Exhaust Filters Note 81: Rapid Bacterial Chemotaxonomy By DirectProbe/MSD Note 80: Design, Development and Testing of a Microprocessor ControlledAutomated Short Path Thermal Desorption Apparatus Note 79: Volatile Organic Compounds From Electron Beam Cured and Partially Electron Beam Cured Packaging Using Automated Short Path Thermal Desorption Note 78: A New Solution to Eliminate MS Down-Time With No-Tool-Changing of Analytical GC Columns Note 77: The Determination of Volatile Organic Compounds in VacuumSystem Components Note 76: Determination of the Sensitivity of a CRIMS System Note 75: An Apparatus for Sampling Volatile Organics From LivePlant Material Using Short Path Thermal Desorption Note 74: Examination of Source Design in Electrospray-TOF Using SIMION 3D Note 73: The Analysis of Perfumes and their Effect on Indoor Air Pollution Note 72: 1998 Version of the NIST/EPA/NIH Mass Spectral Library, NIST98 Note 71: Flavor Profile Determination of Rice Samples Using Shor tPath Thermal Desorption GC Methods Note 70: Application of SIMION 6.0 To a Study of the Finkelstein Ion Source: Part II Note 69: Application of SIMION 6.0 To a Study of the Finkelstein Ion Source: Part 1 Note 68: Use of a PC Plug-In UV-Vis Spectrometer To Monitor the Plasma Conditions In GC-CRIMS Note 67: Using Chemical Reaction Interface Mass Spectrometry (CRIMS) To Monitor Bacterial Transport In In Situ Bioremediation Note 66: Probe Tip Design For the Optimization of Direct Insertion Probe Performance Note 65: Determination of Ethylene by Adsorbent Trapping and Thermal Desorption - Gas Chromatography Note 64: Comparison of Various GC/MS Techniques For the Analysis of Black Pepper (Piper Nigrum) Note 63: Determination of Volatile and Semi-Volatile Organics in Printer Toners Using Thermal Desorption GC Techniques Note 62: Analysis of Polymer Samples Using a Direct Insertion Probe and EI Ionization Note 61: Analysis of Sugars Via a New DEP Probe Tip For Use With theDirect Probe On the HP5973 MSD Note 60: Programmable Temperature Ramping of Samples Analyzed ViaDirect Thermal Extraction GC/MS Note 59: Computer Modeling of a TOF Reflectron With Gridless Reflector Using SIMION 3D Note 58: Direct Probe Analysis and Identification of Multicomponent Pharmaceutical Samples via Electron Impact MS Note 57: Aroma Profiles of Lavandula species Note 56: Mass Spec Maintenance & Cleaning Utilizing Micro-Mesh® Abrasive Sheets Note 55: Seasonal Variation in Flower Volatiles Note 54: Identification of Volatile Organic Compounds in Office Products Note 53: SIMION 3D v6.0 Ion Optics Simulation Software Note 52: Computer Modeling of Ion Optics in Time-of-Flight mass Spectrometry Using SIMION 3D Note 51: Development and Characterization of a New Chemical Reaction Interface for the Detection of Nonradioisotopically Labeled Analytes Using Mass Spectrometry (CRIMS) Note 50: The Analysis of Multiple Component Drug Samples Using a Direct Probe Interfaced to the HP 5973 MSD Note 49: Analysis of Cocaine Utilizing a New Direct Insertion Probe on a Hewlett Packard 5973 MSD Note 48: Demonstration of Sensitivity Levels For the Detection of Caffeine Using a New Direct Probe and Inlet for the HP 5973 MSD Note 47: The Application Of SIMION 6.0 To Problems In Time-of-Flight Mass Spectrometry Note 46: Delayed Extraction and Laser Desorption: Time-lag Focusing and Beyond Note 45: Application of SIMION 6.0 to Filament Design for Mass Spectrometer Ionization Sources Note 44: The Design Of a New Direct Probe Inlet For a Mass Spectrometer Note 43: Volatile Organic Composition In Blueberries Note 42: The Influence of Pump Oil Purity on Roughing Pumps Note 41: Hydrocarbon Production in Pine by Direct Thermal Extraction Note 40: Comparison of Septa by Direct Thermal Extraction Note 39: Comparison of Sensitivity Of Headspace GC, Purge and Trap Thermal Desorption and Direct Thermal Extraction Techniques For Volatile Organics Note 38: A New Micro Cryo-Trap For Trapping Of Volatiles At the Front Of a GC Capillary Column Note 37: Volatile Organic Emissions from Automobile Tires Note 36: Identification Of Volatile Organic Compounds In a New Automobile Note 35: Volatile Organics Composition of Cranberries Note 34: Selection Of Thermal Desorption and Cryo-Trap Parameters In the Analysis Of Teas Note 33: Changes in Volatile Organic Composition in Milk Over Time Note 32: Selection and Use of Adsorbent Resins for Purge and Trap Thermal Desorption Applications Note 31: Volatile Organic Composition in Several Cultivars of Peaches Note 30: Comparison Of Cooking Oils By Direct Thermal Extraction and Purge and Trap GC/MS Note 29: Analysis Of Volatile Organics In Oil Base Paints By Automated Headspace Sampling and GC Cryo-Focusing Note 28: Analysis Of Volatile Organics In Latex Paints By Automated Headspace Sampling and GC Cryo-Focusing Note 27: Analysis of Volatile Organics In Soils By Automated Headspace GC Note 26: Volatile Organics Present in Recycled Air Aboard a Commercial Airliner Note 25: Flavor and Aroma in Natural Bee Honey Note 24: Selection of GC Guard Columns For Use With the GC Cryo-Trap Note 23: Frangrance Qualities in Colognes Note 22: Comparison Of Volatile Compounds In Latex Paints Note 21: Detection and Identification Of Volatile and Semi-Volatile Organics In Synthetic Polymers Used In Food and Pharmaceutical Packaging Note 20: Using Direct Thermal Desorption to Assess the Potential Pool of Styrene and 4-Phenylcyclohexene In Latex-Backed Carpets Note 19: A New Programmable Cryo-Cooling/Heating Trap for the Cryo-Focusing of Volatiles and Semi-Volatiles at the Head of GC Capillary Columns Note 18: Determination of Volatile Organic Compounds In Mushrooms Note 17: Identification of Volatile Organics in Wines Over Time Note 16: Analysis of Indoor Air and Sources of Indoor Air Contamination by Thermal Desorption Note 14: Identification of Volatiles and Semi-Volatiles In Carbonated Colas Note 13: Identification and Quantification of Semi-Volatiles In Soil Using Direct Thermal Desorption Note 12: Identification of the Volatile and Semi-Volatile Organics In Chewing Gums By Direct Thermal Desorption Note 11: Flavor/Fragrance Profiles of Instant and Ground Coffees By Short Path Thermal Desorption Note 10: Quantification of Naphthalene In a Contaminated Pharmaceutical Product By Short Path Thermal Desorption Note 9: Methodologies For the Quantification Of Purge and Trap Thermal Desorption and Direct Thermal Desorption Analyses Note 8: Detection of Volatile Organic Compounds In Liquids Utilizing the Short Path Thermal Desorption System Note 7: Chemical Residue Analysis of Pharmaceuticals Using The Short Path Thermal Desorption System Note 6: Direct Thermal Analysis of Plastic Food Wraps Using the Short Path Thermal Desorption System Note 5: Direct Thermal Analysis Using the Short Path Thermal Desorption System Note 4: Direct Analysis of Spices and Coffee Note 3: Indoor Air Pollution Note 2: Detection of Arson Accelerants Using Dynamic Headspace with Tenax® Cartridges Thermal Desorption and Cryofocusing Note 1: Determination of Off-Odors and Other Volatile Organics In Food Packaging Films By Direct Thermal Analysis-GC-MS Tech No. "A" Note 14: Elimination of "Memory" Peaks in Thermal Desorption Improving Sensitivity in the H.P. 5971 MSD and Other Mass Spectrometers - Part I of II Improving Sensitivity in the H.P. 5971 MSD and Other Mass Spectrometers- Part II of II Adsorbent Resins Guide Development and Field Tests of an Automated Pyrolysis Insert for Gas Chromatography. Hydrocarbon Production in Pine by Direct Thermal Extraction A New Micro Cryo-Trap for the Trapping of Volatiles at the Front of a GC Capillary (019P) - Comparison of Septa by Direct Thermal Extraction Volatile Organic Composition in Blueberry Identification of Volatile Organic Compounds in Office Products Detection and Indentification of Volatiles in Oil Base Paintsby Headspace GC with On Column Cryo-Trapping Evaluation of Septa Using a Direct Thermal Extraction Technique INFLUENCE OF STORAGE ON BLUEBERRY VOLATILES Selection of Thermal Desorption and Cryo-Trap Parameters in the Analysis of Teas Redesign and Performance of a Diffusion Based Solvent Removal Interface for LC/MS The Design of a New Direct Probe Inlet for a Mass Spectrometer Analytes Using Mass Spectrometry (CRIMS) Application of SIMION 6.0 to Filament Design for Mass Spectrometer Ionization Sources A Student Guide for SIMION Modeling Software Application of SIMION 6.0 to Problems in Time-of-flight Mass Spectrometry Comparison of Sensitivity of Headspace GC, Purge and TrapThermal Desorption and Direct Thermal Extraction Techniques forVolatile Organics The Influence of Pump Oil Purity on Roughing Pumps Analysis of Motor Oils Using Thermal Desorption-Gas Chromatography-Mass Spectrometry IDENTIFICATION OF VOLATILE ORGANIC COMPOUNDS IN PAPER PRODUCTS Computer Modeling of Ion Optics in Time-of-Flight mass Spectrometry using SIMION 3D Seasonal Variation in Flower Volatiles Development of and Automated Microprocessor Controlled Gas chromatograph Fraction Collector / Olfactometer Delayed Extraction and Laser Desorption: Time-lag Focusing and Beyond A New Micro Cryo-Trap for the Trapping of Volatiles at the Front of a GC Column Design of a Microprocessor Controlled Short Path Thermal Desorption Autosampler Computer Modeling of Ion Optics in Time-of-Flight Mass Spectrometry Using SIMION 3D Thermal Desorption Instrumentation for Characterization of Odors and Flavors
- MSAgilent Bruker Extrel JEOL Kratos Perkin Elmer SCIEX Shimadzu Thermo Varian Waters (Micromass/VG) FLIR/Griffin Inficon/Leybold/Balzers MKS/UTI Hiden Dupont/CEC Nermag Vestec Filaments Heaters/Sensors Wire Material Electron Multipliers Probe/Sample Vials Ion Transfer Tubes Calibration Compounds MALDI-TOF Supplies Ceramic Insulators Cleaning Supplies Other Filament Repair Source Cleaning Transfer Line Repair GC Injection Port Repair Vacuum Feedthru Repair Other Repair Services NIST MS Library Wiley MS Libraries SIMION® 8.1 Catalog Page A1 Catalog Page B1
- Probe/Sample Vials
- Reference Material on InstrumentationArticle - A High Temperature Direct Probe for a Mass Spectrometer Design of a Direct Exposure Probe and Controller for use ona Hewlett-Packard 5989 Mass Spectrometer SIS AP1000 AutoProbe™ SIS AP2000 AutoProbe™ - Description of System HPP7: Direct Probe Electronics Console HPP7: Direct Probe for the Agilent (HP) 5973/5975 MSD HPP7: HP Direct Probe Application Notes HPP7: Installation Directions for the Direct Probe HPP7: Side Cover for the HP 5973 MSD HPP7: Support HPP7: Probe Inlet System for the Agilent (HP) 5973 and 5975 MSD with Automatic Indexed Stops HPP7: Theory of Operation of the Direct Probe and Probe Inlet System Direct Thermal Extraction Thermal Desorption Application Notes Environmental Thermal Desorption Application Notes Food Science Thermal Desorption Application Notes Forensic Thermal Desorption Application Notes GC Cryo-Trap Application Notes Headspace Application Notes Purge & Trap Thermal Desorption Application Notes Theory of Operation of the AutoDesorb® System AutoDesorb Notes for SIS Dealers Adsorbent Resin Application Notes Installation of the Short Path Thermal Desorption System on Agilent (HP) and Other GCs Installation of the Short Path Thermal Desorption System on a Varian 3400 GC AutoDesorb® System Development Team Thermal Desorption Applications and Reference Materials Installation of the Short Path Thermal Desorption System - TD5 Part I - Design & Operation of the Short Path ThermalDesorption System Installation Instructions for the Model 951 GC Cryo-Trap on the HP 5890 Series GC Installation Instructions for the Model 961 GC Cryo-Trap on the HP 5890 Series GC Operation of the Model 951/961 GC Cryo-Trap SIS GC Cryo Traps - Theory of Operation NIST/EPA/NIH Mass Spectral Enhancements - 1998 version (NIST98) SIMION 3D Ion Optics Class Mass Spectrometer Source Cleaning Methods MS Tip: Mass Spectrometer Source Cleaning Procedures Mass Spec Source Cleaning Procedures Micro-Mesh® Abrasive Sheets Research Papers Using New Era Syringe Pump Systems EI Positive Ion Spectra for Perfluorokerosene (PFK) Cap Liner Information How do I convert between fluid oz and milliliters? Which bottle material should I choose? Which bottle mouth should I choose? The Bottle Selection Guide CGA Connections for Gas Tanks BenchTop/PBM Mass Spectrometry Library Search System Chemical Reaction Interface Mass Spectrometry (CRIMS)
- HPP7: HP Direct Probe Application NotesNo. 1 - Design of a Direct Exposure Probe and Controller for use on a Hewlett-Packard 5989 Mass Spectrometer No. 2 - A High Temperature Direct Probe for a Mass Spectrometer No. 44 - The Design of a New Direct Probe Inlet for a Mass Spectrometer No. 48 - Demonstration of Sensitivity Levels of Caffeine for a New Direct Probe and Inlet for the HP 5973 MSD No. 49 - Analysis of Cocaine Utilizing a New Direct Insertion Probe on a Hewlett Packard 5973 MSD No. 50 - The Analysis of Multiple Component Drug Samples Using a Direct Probe Interfaced to the HP 5973 MSD
- Note 44: The Design Of a New Direct Probe Inlet For a Mass Spectrometer (This Page)
Direct introduction of samples into a mass spectrometer continues to be a fast and convenient method to analyze many samples. Applications, as screening methods and molecular weight determination, in areas such as drug development are particularly suited to rapid analyses such as can be achieved using direct probe sample introduction.
One of the difficulties of using probes for the introduction of samples into the mass spectrometer has been the interface or probe inlet which allows the probe to be inserted into the mass spectrometer. These inlets must provide a sealed intermediate pumping, area where a partial vacuum can be pulled before a valve is opened to allow insertion of the probe into the source of the mass spectrometer. This requires that the seals that are used in these inlets are designed to withstand the wear due to repetitive insertion and removal of the probe and that there be some method of insuring that the valve is closed and opened at the proper time so that venting of the mass spectrometer does not occur. One or both of these potential problems exist on many of the probe inlets such as the inlet that is supplied with the Hewlett-Packard 5989 MS Engine.
We have designed a new probe inlet for use on the HP Engine which provides for much longer seal life and minimizes the chance of accidental venting of the mass spectrometer.
Probe Inlet Design
The new probe design consists of three basic parts. These are the probe seal assembly where the probe seals are located, the isolation valve which isolates the high vacuum of the mass spec source, and the probe guide bar and auto-stop assembly which protects against accidental venting of the mass spectrometer. These are shown in the schematic in Figure 1.
Figure 1 - Design Of HP Probe Inlet
The newly designed probe seals and the intermediate pumping area are part of the probe seal assembly. Our design consists of two PTFE vacuum seals which use Viton® o-rings. Previous designs, as those used on the engine, were manufactured from graphitized Vespel® which wear quickly with use. As these seals wear, small particles of graphite are released providing possible contamination of the inlet. The new PTFE seals provide for a clean, contamination free, long lasting seal. The small intermediate pumping region is located between these two seals. This area is small minimizing the additional vacuum pump requirements.
The isolation valve is the valve which isolates the intermediate pumping region from the high vacuum of the mass spec source. This valve is a precision designed ball valve specifically designed for vacuum applications.
Figure 2 - Probe Inserted into MS source
The guide bar and auto-stop assembly is an indexed probe slide which automatically stops at three locations. There is a load position and then stop positions at the first PTFE seal and then another stop at the second PTFE seal. This prevents pushing the probe in too far which could damage the probe tip, and also prevents pulling the probe out past the PTFE seal which would vent the mass spectrometer. A quick release push button must be activated by the user to allow movement of the probe past one of the auto-stops. Figure 1 shows the probe at the high vacuum auto-stop location. This stop is where the isolation valve would be activated. Figure 2 is a schematic drawing showing the probe inserted completely into the mass spec source.
Figure 3 - Probe Inlet System Attached To HP Engine Mass Spec
Figure 3 is a picture of the newly designed probe inlet installed on a Hewlett-Packard 5989 MS Engine. The probe inlet is attached to this mass spec using the standard HP o-ring fitting supplied with the mass spectrometer. The probe inlet could also be modified to mount on other mass spectrometers which use one half inch diameter probes.
Probe Inlet Seal Life Study
Figure 4 - Probe Seal Life Study
A study was done to compare the seal life on the Hewlett-Packard inlet system and the newly designed SIS inlet system. The results are shown in the chart in Figure 4.
The SIS probe inlet and the HP probe inlet systems were mounted onto an automatic probe injection system which was fitted to a vacuum chamber where the vacuum was measured with an ionization gauge tube. The vacuum in the chamber was measured after each injection of the probe through the inlet. This allowed us to monitor the vacuum levels as the probe seals began to wear from repeated injections. The probe inlet seals were considered to have failed when the ionization gauge would not remain on (i.e. the vacuum was greater than 1 x 10-4 torr).
The chart shows that the SIS probe inlet system provided satisfactory performance for over 2500 injections of the probe before it failed at injection number 2649. The HP probe inlet first failed the test at injection number 14. The inlet was removed and inspected. There were fine particles of graphite throughout the probe inlet. The inlet was cleaned and the same seals were installed again in the inlet and the test was continued. The probe inlet failed again at injection 29. The cleaning process was repeated and the test continued with the same seals. This cleaning process was repeated seven times before the probe inlet seals failed completely at injection number 290.
We have designed a new probe inlet system which greatly improves the seal life and reliability of previous probe inlets systems. The new design also greatly reduces the possibility of accidental venting of the mass spectrometer. The probe inlet mounts easily onto a Hewlett-Packard 5989 MS Engine but could be modified to work with other mass spectrometers.
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