TurboMatrix Headspace Sampler And HS 40/110 Trap User's Guide
TurboMatrixHeadspace Sampler andHS 40/110 TrapUser’s Guide
Release HistoryM0413401FFebruary 2008User AssistancePerkinElmer, Inc.710 Bridgeport AvenueShelton CT 06484-4794email: info@perkinelmer.comNoticesThe information contained in this document is subject to changewithout notice. PerkinElmer makes no warranty of any kind withregard to the material, including, but not limited to, the impliedwarranties of merchantability and fitness for a particular purpose.PerkinElmer shall not be liable for errors contained herein forincidental consequential damages in connection with furnishing,performance or use of this material.Copyright InformationThis document contains proprietary information that is protected bycopyright. All rights are reserved. No part of this publication may bereproduced in any form whatsoever or translated into any languagewithout the prior, written permission of PerkinElmer, Inc.Copyright 2008 PerkinElmer, Inc.Produced in the UK.TrademarksRegistered names, trademarks, etc. used in this document, evenwhen not specifically marked as such, are protected by law.PerkinElmer is a registered trademark and TurboMatrix andPPC are trademarks of PerkinElmer, Inc. HP is a registeredtrademark of Hewlett-Packard Corporation. Swagelok is a registeredtrademark of the Crawford Fitting Company. Teflon , Tefzel ,Viton and Vespel are registered trademarks of E.I. duPont deNemours and Company, Inc.
ContentsContentsIntroduction .11Introduction.13TurboMatrix Headspace.13HS 40/110 Trap .14About this Manual .15Unpacking the Instrument.16Symbols Used on the Instrument .20Safety Information .20Electrical Safety .22Electromagnetic Compatibility (EMC) .25Mechanical Hazard.25Chemicals.26Compressed Gases .27Extreme Temperatures .29Waste Disposal.30WEEE Instructions for PerkinElmer Products.31Sample Vials .32Cleaning and Decontamination.33Decontamination .33Cleaning the Instrument .34Installation .35Introduction.37Pre-Installation Checklist.38Laboratory Requirements .40Operating Environment .40Space Requirements for the Instrument .41Electrical Connections .43AC Line Connections.43Electrical Surge .45Connecting the HS to a Gas Chromatograph.46Gas Supply System .46Gas Supply Specifications.47Electrical Connections .49The HS Input/Output Port .49HS Output Signals.51HS Input Signals .53Timed Event Relays .54Connecting the HS to the AutoSystem XL orClarus 500 GC .553
ContentsConnecting the HS to other GCs except the HP 5890,HP 6890 and HP 7890 . 56Connecting the HS to the HP 5890 and HP 6890. 57Installing the Heated Transfer Line. 58Installing the Heated Transfer Line at the HSNeedle Unit (TurboMatrix Headspace Only)62Installing the Heated Transfer Line at the HSNeedle Unit (HS 40/110 Trap Only) . 65Installing the Heated Transfer Line at the GC Injectorfor Split Operation (TurboMatrix Headspace Only)68Liner Recommendations. 68Installing the Heated Transfer Line at the GC forDirect Connection . 71Recommended for the HS 40/110 trap . 71On-Column Connection. 72Recommended for the HS 40/110 trap . 72Composite Zero-Dilution Split Injector Liner forHeadspace Interfacing. 74Installation Instructions . 74Operation . 74Connecting to a Packed Column System. 75Gas Connections . 75Carrier Gas. 75HS 40/110 Trap Connections. 79Installing the Trap in the HS 40/110 Trap . 81Checking the Needle Purge Gas Flow . 85TurboMatrix Headspace and HS 40/110 Trap 85Leak Testing the Headspace. 86Leak Test the HS 40/110 Trap. 89Operation. 95Introduction . 97TurboMatrix Headspace and the HS 40/110 Trap. 97Powering up the Headspace Sampler . 98Setting the Carrier Gas Pressure. 100The Touch Screen Display . 103The Run Tab. 104Single Method Operation. 105Creating a Sequence . 106Status Tab (Headspace and HS 40/110 Trap). 108Temperature Screen (Headspace and HS 40/110 Trap)1094
ContentsTiming Tab (Headspace and HS 40/110 Trap) .112The Status Tab Option Tab (Headspace) .115HS 40/110 Trap.119Status Tab Temp .119Status Tab Timing Tab for the HS 40/110 Trap .121Gas Leaks Detected by ''Monitor Vial Integrity''- Dynamic Leak Test . 123Status Screen PPC Tab for the HS 40/110 Trap .128The Log Tab.129Tools .133Method Editor .133Test .135Log Out (Headspace and HS 40/110 Trap).135Calculator .135Reset.136Preferences Tab (Headspace and HS 40/110 Trap)136Run Tab .137Config Tab .138Setup Tab .141HS 40/110 Trap Setup Tab.145Connect Tab .145Starting a Run (TurboMatrix Headspace and HS 40/110Trap).147Preparing Samples.147Loading the Magazine.148Single Method Operation on the HS .149Multiple Method (Sequence) Operation.150Using the Tray Rotation Feature While Running AVial Sequence.151Creating a Sequence .153Editing a Sequence .155Logic Flow Diagram - A Description(HS 40/110 Trap Only) .155High Pressure Sampling (Headspace Only).159HS 40/110 Trap .160Shutdown (Headspace and HS 40/110 Trap).160Accessories .161Options Board .163Timed Events .163BCD Interface .165The Vial Shaker Accessory.166PPC .1675
ContentsComposite Zero-Dilution Split Injector Liner. 168Description. 168Installing the Zero Dilution Liner. 170Operation of the Zero Dilution Liner. 171Cryofocusing Accessory. 172Principle of Operation. 172Cryofocusing with the Water Adsorption Trap . 174Sample Vials. 175Using the Vial Gauge to Check Sample Vials. 175Crimped Top Sample Vials . 176Hand Crimper for Crimped Top Vials . 176Sealing the Hand Crimped Vials . 177Screw Top Sample Vials . 178Accessories (Screw and Crimp Cap Vials) . 178Seals. 179Headspace Control Software . 180HS 40/110 Trap Accessories . 182Method Development . 183Introduction . 185Principles of Headspace andHeadspace Trap Analysis . 185The HS Sampling Technique . 186HS 40/110 Trap Sampling Technique . 187Creating a New Method . 189Temperature Tab (Headspace and HS 40/110 Trap). 191Needle and Transfer Line Temperatures . 191Temperature Mode. 191Thermostatting Temperature (Headspace andHS 40/110 Trap) . 192HS 40/110 Trap Temperatures. 193Cryofocusing Temperature (Headspace Only) . 193Timing Tab . 194Pressurization Time(Headspace and HS 40/110 Trap). 194Vial Pressurization-Carrier Pressure(Headspace Only) . 194Injection Time (Headspace Only). 195Thermostatting Time(Headspace and HS 40/110 Trap). 196Injection Volume (Headspace Only) . 197Withdrawal Time (Headspace Only) . 198Setup (HS 40/110 Trap Only). 1986
ContentsDecay Time. 198Cycles . 201Pressurization Time . 202Trap Hold (HS 40/110 Trap Only).203Dry Purge Time (HS 40/110 Trap Only) .203Desorb Time (HS 40/110 Trap Only) .204Pre/Post-Cryofocusing Time (Headspace Only) .204The Option Tab .206Injection Mode (Headspace Only) .207Principles of High Pressure Sampling(Headspace Only) .208Setting the Withdrawal Time .211For High Pressure Sampling. 211Water Trap .212Operating Modes (Headspace Only) .212Number of Injections.214Shaker.215PPC Tab .216Split Sampling (Headspace Only).218Splitless Sampling .223Splitless Sampling with theHS 40/110 Trap.225HS 40/110 Trap Theory .225Headspace Sampling .226With Wide-Bore Capillary Columns . 226Headspace Sampling .227Using a Packed Column and aPacked Column Injector . 227MHE Theory and Calculations(Headspace Only) .229Routine Maintenance .233Introduction.235General Laboratory Cleanliness.236Cleaning and Decontamination .236Cleaning. 236Decontamination. 237Carrier Gas .237Tubing .237Sample Vials and Seals .238Important! Carrier Gas Shut Off .238Reproducibility Test (Headspace) .2397
ContentsChanging the Fuse . 241The Sampling Needle . 243Types of HS Needles . 243Removing and Replacing the Needle(Headspace Only) . 243Removing and Replacing the Needle(HS 40/110 Trap Only). 245Cleaning the Jet Needle . 246Changing the Upper Needle Seal Assembly. 247Changing the Lower Seal Assembly. 249Changing the O-Rings . 252Changing the O-Ring in the HS 40/110 Trap . 253Converting the HS 40/110 Trap to a TurboMatrixHeadspace Mode. 261Leak Testing the Sample Injection System . 261Leak Testing the HS 40/110 Trap. 263HS 40/110 Trap: Valve Leak Test . 267Magazine Maintenance. 269Removing and Replacing the Magazine . 269Cleaning the Magazine . 270Adjusting the Hand Crimper . 271Adjusting the Stop Pin . 271Adjusting the Crimp Plunger . 272Decapping the Vials . 274Installing the Transfer Line Cap. 275Zeroing the Carrier Gas PPC Module . 275HS 40/110 Trap Maintenance. 276Removing and Replacing the Trap . 276Trap Breaks Inside the Trap Assembly . 280Replacing the Dry Purge Assembly. 280Trap Maintenance . 282Introduction for Conditioning the Trap . 282Cleaning the Trap . 282Trap Test. 284System Maintenance. 288Troubleshooting . 293Status Messages. 295TurboMatrix Headspace and the HS 40/110 TrapInstrument Fault Conditions . 297ATTENTION: Carrier Gas Shut Off. 306Troubleshooting Procedures. 307Peak Broadening or Splitting . 3098
ContentsSystem Contamination for theHeadspace and HS 40/110 Trap.312Poor Sample Recovery orReduced Sensitivity .315HS 40/110 Trap Only Troubleshooting .320Monitor Vial Integrity .321Troubleshooting the Leaks .324Log Error Messages .324Fast pressure decay:. 324Slow pressure decay: . 325Extended therm: Trap . 325GC not ready:. 326Status Messages .327Appendices.333Appendix A.335Customer Service .335Appendix B .336Warranty Exclusions and Limitations .336Appendix C .337Supplies, Accessories and Replacement Parts .337Sample Vials and Seals .337Tools for Sample Preparation.338Replacement Parts .338Adapter Kits for Gas Chromatographs.340Appendix D.341Reference Material .341Headspace Gas Chromatography .341Laboratory Safety Practice .342Multiple Headspace Extraction .342Bibliography.3439
Contents10
Introduction1
IntroductionIntroductionIn headspace sampling the sample (either a gas, a liquid, or a solid)is placed into the headspace vial, which is closed immediately andequilibrated and pressurized. An aliquot is then withdrawn from theclosed vial and transferred directly to the gas chromatographicsystem or pre concentrated on a trap for focusing (in headspace traponly).The HS is an automatic sampler for headspace analysis. Threemodels of the HS are available, as are various accessories thatenhance the operation of your system.TurboMatrix HeadspaceThe HS-16 provides automated headspace analysis of up to 16 vials(not available in the trap functionality). Standard PerkinElmer vialscan be loaded into the vial magazine. A single vial oven allows youto thermostat your sample before injection onto the GC via theheated transfer line. You can upgrade the HS-16 to an HS-40 or anHS-110.Up to 40 vials can be loaded into the magazine of the HS-40. Theoven can accommodate up to 12 vials and overlappingthermostatting allows the instrument to obtain maximum samplethroughput. An optional shaker device is available to reduceequilibration time. You can upgrade the HS-40 to an HS-110.NOTE: The HS-40 and HS-110 have exactly the same functionexcept for the number of vials.The HS-110 can accommodate up to 110 vials. The 12-vial oven isstandard and overlapping thermostatting allows the instrument toobtain maximum sample throughput. The advanced automationsystem can be programmed to run series of vials according to presetmethods. The HS-110 also comes standard with BCD outputcapability, which is optional on the other models.NOTE: The 12-vial oven is in reality a 15-vial oven but the softwareonly allows up to 12-vial simultaneous loading andoverlapping thermostatting.Programmed pneumatic control (PPC) provides the electroniccontrol of pressures and flows for inlet, and auxiliary gases. Thisoption can be installed on any one of the above models to automate13
Introductiongas handling and delivery in the HS. PPC comes standard on the HS40/110 trap. High pressure sampling is supplied as part of the PPCoption.HS 40/110 TrapNOTE: The Trap model is offered with two vial options for either40 or 110 but for the purposes of this Users Guide it will bereferred to as the HS 40/110 Trap.The HS 40/110 Trap includes the ability to prioritize sample vialscontaining rush samples during an active sequence and a timesaving, pre-programmed shut-down and wake-up mode that allowsfor complete unattended operation.The HS 40/110 trap improves headspace detection limits. It allowsfor the extraction of the full vapor content of the sample vial into thetrap to the GC and subsequent transfer.European Union Industrial Environment230V / 50Hz. TurboMatrix headspace instruments manufactured foruse in the European Union are intended for the industrialenvironment. The instrument is to be connected to a mains powernetwork supplied from a high or medium-voltage transformerdedicated for the supply of an installation feeding a manufacturingor similar plant.Industrial environments are characterized by the existence of one ormore of the following conditions: industrial, scientific and medical (ISM) apparatus arepresent heavy inductive or capacitive loads are frequently switched currents and associated magnetic fields are highThese are the major contributors to the industrial electromagneticenvironment and as such distinguish the industrial from otherenvironments. The instrument is not intended for connection to apublic mains network supplying residential, commercial and lightindustrial locations.14
IntroductionAbout this ManualThis manual is an integral part of your automatic headspace samplerproduct. It begins with unpacking and general safety information inChapter 1. Installation and setup are described in Chapter 2.Operation of the instrument is covered in Chapter 3. Optionalaccessories are described in Chapter 4 and method development isoffered in Chapter 5. A routine maintenance schedule and the relatedprocedures are discussed in Chapter 6. Chapter 7 contains lists ofpossible fault and error messages and some basic troubleshootingprocedures.If you find an error in this manual or have any comments orsuggestions, please let us know so that we can correct the mistake orimprove the manual. Contact information is provided in theAppendix A.Conventions in this Manual—In the text you will also find variouswarnings and notes.Warnings, other cautionary information and notes are denoted in thetext as follows:WARNINGCAUTIONThis indicates a warning. We use the term warning to informyou about situations that could result in personal injury toyourself or other persons.This indicates a caution note. We use the term caution toinform you about situations that could result in seriousdamage to the instrument or other equipment.NOTE: The term Note indicates any significant information thatcan help you avoid false analytical results or deteriorationin instrument performance.Other Manuals and Reference Material—Before you install oruse your automatic headspace sampler, and in order to get the bestresults, you should be familiar with all the instruments in the systemand know how to operate them. You must also be aware of the safetyprocedures that are in effect in your laboratory.15
IntroductionDetails of gas chromatography are not covered in this manual, but aworking knowledge of your gas chromatograph and the theory of gaschromatography are required to operate this instrument. Refer to thedocumentation supplied with your GC.Some accessories are supplied with separate installation guides anduser manuals. If you have any of these accessories installed, pleaserefer to the associated manual for detailed information on operation,troubleshooting and maintenance of the accessory.For information on the TurboMatrix Control Software refer to theTurboMatrix HS Control Software User’s Guide.A list of reference materials covering the theory of headspacechromatography and various applications is provided in this manual.Refer to Appendix C.Unpacking the InstrumentKeep the original packing materials for possible future storage orreshipment.Observe the following information when unpacking the instrument:1. Open the carton at the top, folding the flaps outward. Ontop of the instrument is a foam insert containing variousaccessories.2. Lift out the insert and accessories using the hand grips atthe side.3. Lift out the instrument.4. Check that all ordered parts have been receivedundamaged (see Tables 1 and 2).16
IntroductionThe following items should be included with your HS instrument:Part No.DescriptionQty.00090652Septum Kit, Fairprene (50/Pkg.)109903157Nut 1/16"1L1003026Graphite Vespel Ferrule, 1.6 mm ID304966624Wrench Open End104972433Graphite Ferrule, 0.5 mm ID3B0131410Tool O-Ring Assembly1B0147449O-Ring Extractor Tool1B0151737Vial Gauge1B0500843Spigot Key1B0503956Glass Lined Tube Adapter1B0505266HS Injector Adapter1B0510403Transfer Line Cover109907233Wrench Open End (1/4 in x 5/16 in)1M0415330Top Seal Changing Tool1M0417030Terminal Block Plug, 14 Poles1N1011206HS Start/Ready Cable2N9301357Fused Silica Transfer Line, 0.32 ID1N9301376Wafer-Ceramic Cutter (10/Pkg)109904956Rheodyne Nut, 1/16 in1M0417002Fuse 5 x 20 MM 10A 250V, TD2M0417038Fuse 5 x 20 MM 5@ 250V, TD2M0413401Users Manual1Table 1 TurboMatrix 16, 40, 110 Headspace Shipping Kit(Part No. M041-3403)17
IntroductionThe following items should be included with TurboMatrix Trap.18Part No.DescriptionQty.00090652Septum Kit104966624Double Ended Wrench2L1003026Graphite Vespel Ferrule, 1.6 mm ID3M0413628Air Monitor Trap109903392Nut Union 1/16109900105Graphite Vesp Ferrules 1/16 x 0.5 mm309926067O-Ring 0.0145 ID x 0.070 WD5B0131410O-Ring Tool Assembly1N6701077Trap Removal Tool, TygonB014-7449O-ring Extract Tool1B1511737Vial Gauge1B0500843Spigot Key for All Systems1B0505266HS Adapter Injector1B0510403HS 40/110 Transfer Line Cover1L4271302Ferrule Trap Tube, PTFE5M0413401Users Manual1M0415010Locking Nut1M0415330Top Seal Changing Tool1M0417002Fuse 5 x 20mm 10.0A 250V, TD2M0417030Terminal Block Plug1M0417038Fuse 5 x 20mm 5.0A 250V, T2N1011206Cable Assembly for All Systems2N6701053Washer, non-trap109200061Wrench, 5/8 in1
IntroductionPart NoDescriptionQtyN6701079Valco Ferrule Removal Tool Kit1N9301357Empty Fused Silica Tubing 0.321N9301376Wafer Ceramic Cutter1Table 2 HS 40/110 Trap Shipping Kit(Part No. N670-0116)If any of these items are missing or are damaged, please contactPerkinElmer immediately. In the event of damage, file an immediateclaim with the carrier and report the matter to your PerkinElmeroffice.19
IntroductionSymbols Used on the InstrumentIndicates alternating current.Indicates the off position of the main power switchIndicates the on position of the main power switchIndicates the Protective Conductor TerminalIndicates Hot SurfaceIndicates Risk of Electric ShockIndicates an earth ground terminalCaution, risk of dangerDocumentation must be consulted to determine thenature of the potential hazard and any actions whichhave been taken.Safety InformationWARNINGDo not attempt to make adjustments, replacements or repairsto this instrument except as described in the accompanyinguser documentation.NOTE: This equipment requires no specified inspection orpreventive maintenance to ensure the continuousfunctioning of its safety features.20
IntroductionPlease read this section carefully before beginning operation of theHS and pay particular attention to any advice it contains concerningpotential hazards that may arise from the use of the instrument.This manual contains information and warnings that must befollowed by the user to ensure safe operation.Possible hazards that could harm the user or result in damage to theinstrument are clearly stated throughout this manual.The advice is intended to supplement, not supersede, the normalsafety code of behavior prevailing in your country.WARNINGWARNINGWARNINGWarning: Toxic Fumes-Fume Ventilation SystemWithout adequate ventilation, potential toxic vapors canbuild up in the laboratory. your laboratory must have areliable fume ventilation system before you use thisinstrument.Warning: Explosive AtmosphereThis instrument is not designed for operation in an explosiveatmosphere.This equipment must be used in a manner specified by thismanual. Otherwise the protection provided by the equipmentmay be impaired.21
IntroductionElectrical SafetyElectrical Protection—The following precautions have been takento provide electrical protection:PollutionDegreeThis equipment will operate safely inenvironments that contain nonconductive foreignmatter up to Pollution Degree 2 as defined inIEC 61010-1.Table 3 Electrical ProtectionIf you suspect for any reason that the instrument is not electricallysafe for use, do not operate it and secure it against any unauthorizedoperation. Have the equipment inspected by a PerkinElmer ServiceEngineer or similarly qualified person.The instrument is likely to be electrically unsafe when it:22 Has been subjected to severe transportation stresses. Shows visible damage. It has been subjected to prolonged storage underunfavorable conditions. pa
User Assistance PerkinElmer, Inc. 710 Bridgeport Avenue Shelton CT 06484-4794 email: info@perkinelmer.com Notices The information contained in this document is subject to change without notice. PerkinElmer makes no warranty of any kind with regard to the material, including, but not limited to, the implied
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Lot-tested, certified and approved septa deliver reproducible results NEW from PerkinElmer, headspace screw top vials and preassembled caps allow for samples to be taken in the field and directly analyzed on
7890A GC's backflush feature. Store all essential parameters in an Agilent ChemStation chromatographic method. Quickly and easily transfer methodsdirectly from your 6890 Series GC to the 7890A GC. Dramatically improve precision, sensitivity, and throughput by combining the G1888 Headspace Sampler with Agilent's flagship 7890A GC system.
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Winchester Model 70 measured 1.630" and brass from my .243 Browning BLR measured 1.631". My brilliant deduction is that new case handloads and factory cartridges see as much as .011" headspace in my firearms when initially fired, and that is substantial as headspace goes. Fired, pressure formed cases are well within the spec range defined by
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materials. Headspace gas chromatography (GC) or GC mass spectrometry instrumentation is used. A vial-in-vial method is used, in which the volatile agent is placed in a small inner vial, and the inner vial is capped with a layer of fabric or film to be tested. The agent permeates from the inner vial into an outer headspace vial.
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