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Maintaining your Agilent
GC and GC/MS Systems
Our measure is your success.

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Summary of Contents for Agilent Technologies gc/ms series

  • Page 1 Maintaining your Agilent GC and GC/MS Systems Our measure is your success.
  • Page 2: Table Of Contents

    Table of Contents Gas Management..................1 Gas Types ....................................2 Gas Purification Systems................................4 Gas Traps.....................................6 Renewable Gas Purification System ............................12 Universal/External Split Vent Trap.............................13 Regulators ....................................14 Tubing......................................15 Flowmeters ....................................16 Gas Leak Detector..................................18 Sample Introduction ..................19 Vials......................................20 Electronic Crimpers and Decappers............................25 Gold Standard Autosampler Syringes ............................26 Headspace Sampler..................................34 CTC Autosampler Supplies................................37 Purge and Trap Supplies ................................41...
  • Page 3: Gas Management

    Gas Management Avoid column damage, improve detector life, and achieve reliable, consistent results. Gas management means more than just selecting the appropriate carrier gas for your needs. It also means taking steps to prevent contaminants like oxygen, moisture, and hydrocarbons from damaging your GC column. As you read through the following pages, you will find…...
  • Page 4: Gas Types

    Gas Types Carrier Gases The most frequently used carrier gases are helium and hydrogen, although nitrogen and argon can be used. Purity is essential for these gases since they sweep the sample through the column where it is separated into its component parts and then through the detector for component quantification.
  • Page 5 Gas Management Gas Purity and Selection Agilent recommends that carrier and detector gases be 99.9995% pure. Air needs to be zero grade or better. Agilent also recommends using traps to remove hydrocarbons, water and oxygen. When used with capillary columns, GC detectors require a separate makeup gas for optimum sensitivity.
  • Page 6: Gas Purification Systems

    Contaminants & Purities Contaminants in gases are major contributors to capillary column degradation and detector noise, and can interfere with chromatographic results. Concentration of these contaminants vary by the grade of gas. Hydrocarbons and Halocarbons • Decrease detector sensitivity by increasing detector background noise. •...
  • Page 7 Gas Management Carrier Gas Purification In-Line Gas Purifiers The Carrier Gas Purification illustration shows the most common gas purification configurations used in gas chromatography. Regardless of which purification system is employed, proper installation -OR- and maintenance is required to achieve optimal performance from Gas supply Gas Purification System the purification system(s).
  • Page 8: Gas Traps

    Gas Traps The purpose of gas traps is to remove detrimental impurities from the carrier and detector gases. Combination traps are available which remove moisture, oxygen and/or organics with a single trap. The effectiveness of the traps depends on the initial quality of the gas. Constant exposure of capillary columns to oxygen and moisture, especially at high temperatures, results in rapid and severe column damage.
  • Page 9 Gas Management Moisture (Water) Traps Indicating moisture traps are available in plastic and glass bodies. Glass body traps are used when potential contaminants from plastic trap bodies are a concern. Glass traps are normally encased in a Moisture trap protective, plastic shrink wrap or a high impact plastic shield (outer trap body).
  • Page 10 Moisture Traps Description Size Removal Max. 1/8 in. 1/4 in. (cc) Capacity (g) Effluent H Part No. Part No. Concentration (ppb) Silica Gel, Grade 40, and Indicating Silica Gel, Grade 48 (MT-S Series) Refillable 31.5 MT120-2-S MT120-4-S Moisture Trap Refillable 52.5 MT200-2-S MT200-4-S...
  • Page 11 Gas Management Hydrocarbon Traps Hydrocarbon traps remove organics, such as hydrocarbons and halocarbons, from the gas stream. The adsorbent is usually activated carbon or an impregnated carbon filter media. Carbon removes Hydrocarbon trap, HT200-2 organic solvents from the gas stream, including the typical solvents used in nearly every lab.
  • Page 12 Oxygen Traps Oxygen traps usually include a metal-containing inert support reagent. Most oxygen traps reduce the oxygen concentration to below 15-20 ppb. The capacity of a standard oxygen trap is approximately 30 mg of oxygen per 100 cc of trap volume. Oxygen traps can also remove some small organic and sulfur compounds from gas streams, but this is not their primary application.
  • Page 13 Gas Management Combination Traps Agilent carries several Combination Traps that provide multiple contaminant removal in a single trap. These traps offer: • Optimized adsorbents for maximum surface area and capacity. Agilent OT3 trap • Leak-free, one-piece design to eliminate potential leaks from using multiple traps. •...
  • Page 14: Renewable Gas Purification System

    Renewable Gas Purification System NEW! The Renewable Gas Purification System from Agilent not only traps large quantities of contaminants and lasts a long time, but it is also recyclable. With average use, you'll only have to purchase a replacement cartridge once per year or after approximately 20 cylinders worth of purification.
  • Page 15: Universal/External Split Vent Trap

    Gas Management Universal/External Split Vent Trap Split vent traps stop environmental pollution. The split vent trap was designed to protect the lab environment from the contaminants released by split injection systems, which can vent up to 500 times the amount of sample reaching the detector into the laboratory's air. A replaceable, impregnated carbon filter media traps and eliminates a broad range of contaminants.
  • Page 16: Regulators

    Regulators Agilent recommends using our economical brass body, dual stainless steel diaphragm regulators for most GC applications. These regulators, combined with the proper gas purification system, provide proper gas pressure control and purity for gas chromatography. Brass Body, Dual Stainless Steel Diaphragms, 1/8 in., U.S. Only* Description Part No.
  • Page 17: Tubing

    Gas Management Tubing Cleaning Tubing Agilent recommends using copper tubing for most applications, since it is easy to bend and plumb and is less expensive than stainless steel. Use stainless steel tubing only for Before any tubing is placed into service, crucial applications that require very high purity, or where building codes mandate its use.
  • Page 18: Flowmeters

    Flowmeters Setting and maintaining GC flow rates greatly affects the instrument accuracy and sensitivity. During maintenance, verify carrier and support gas flows with the proper flowmeter. NEW! Precision Gas Flow Meter Agilent's Precision Gas Flow Meter is the ultimate gas flowmeter for chromatography applications.
  • Page 19 Gas Management ADM 1000 • Accuracy ± 3%. • Operating temperature range – 0 to 45ºC for the instrument, -70 to 135ºC for the tubing. • Calibration – traceable to NIST primary standards. • Real time, split ratio measurement. • CE mark certified. •...
  • Page 20: Gas Leak Detector

    Gas Leak Detector NEW! Gas leaks can cause detector noise and baseline instability, shorten column life and waste expensive carrier gas. Liquid leak detectors, although inexpensive, can contaminate your system. Agilent's G3388A electronic leak detector is an easy way to quickly identify leaks in your system.
  • Page 21: Sample Introduction

    Sample Introduction Ensure optimal peak shape and reproducibility through accurate sample delivery. They may be small, but sample introduction supplies can have a profound impact on your results. That is why Agilent vials, septa, and syringes are meticulously engineered to work seamlessly with your GC and GC/MS instruments. They can help you achieve reliable, repeatable results even for your most complex runs.
  • Page 22: Vials

    Vials Agilent's wide opening vials are designed specifically for analyzing samples with your GC. They have specially designed vial neck angles, bottom design, and height to ensure compatibility with Agilent autosamplers with rotating or robotic arm trays. Agilent offers a large variety of autosampler vials in different closures, cap colors, septa choices, and package options.
  • Page 23 Sample Introduction Vial Filling When filling sample vials, keep in mind: • If you need to test a large amount of sample over repeated injections, divide the sample among several vials to obtain reliable results. • When sample volume in the vial is low, contaminants from the previous sample injection or solvent washes may have a greater impact on the sample.
  • Page 24 Selecting Vial Septa Materials Vial cap septa are critically important to optimal analysis. Each septum complements the overall system and enhances chemical performance. Agilent's vial cap septa are specifically formulated and constructed for optimum system performance, with minimal coring and superior chemical inertness. Type Uses Red Rubber/PTFE...
  • Page 25 Sample Introduction Convenience Vial and Cap Packs Vials Caps Unit Part No. Certified Screw Top Vial Convenience Packs Clear Blue screw caps, PTFE/red 500/pk 5182-0732 rubber septa Clear with write-on spot Blue screw caps, PTFE/red 500/pk 5182-0867 Convenience vial and cap pack rubber septa Amber with write-on spot Green screw caps, PTFE/red...
  • Page 26 Convenience Vial and Cap Packs Certified Crimp Top Vial Convenience Packs Clear Silver aluminum crimp caps, 500/pk 5181-3400 PTFE/red rubber septa Amber with write-on spot Silver aluminum crimp caps, 500/pk 5181-8801 PTFE/red rubber septa Snap Top Vial Convenience Packs Clear Clear polypropylene snap caps, 500/pk 5182-0547 PTFE/red rubber septa...
  • Page 27: Electronic Crimpers And Decappers

    Sample Introduction Electronic Crimpers and Decappers Whenever large amounts of crimp vials need to be crimped or decapped, the electronic crimper or decapper is the right tool. It reduces stress and repetitive motion injury associated with manual plier-style crimpers and decappers. Agilent's newly-designed crimper offers easy, hand-held pushbutton operation and provides the following advantages: •...
  • Page 28: Gold Standard Autosampler Syringes

    Gold Standard Autosampler Syringes With a broad selection of syringes for auto injection, Agilent has what you need for accurate and effective sampling. Agilent delivers even more value in every autosampler syringe with the introduction of many new features in our line of Gold Standard GC Autosampler Syringes.
  • Page 29 Sample Introduction Needle Gauge Selection • Syringe needles compatible with Agilent Automatic Liquid Samplers are 42 mm long and have an HP style or cone shaped tip. • The Merlin Microseal requires 23 gauge needles. • The smaller the gauge, the larger the needle diameter. Needle Gauge Selection Inlet Needle Gauge...
  • Page 30 Syringe Characteristics and Recommended Uses Syringe Advantage Limitations Recommended Use 10 µL, PTFE-tipped • • • Less plunger binding than fitted More expensive than fitted plunger High sample throughput • • plunger PTFE-tipped syringes not available Samples in polar solvents •...
  • Page 31 Sample Introduction Syringe Troubleshooting Guide Proper care, cleaning, and handling of each syringe will help ensure correct performance and long life. When cleaning your syringe, it is best to use solvents that effectively dissolve the sample you are working with. Try to avoid cleaning agents that are alkaline, contain phosphates, or are strongly acidic.
  • Page 32 Problem Possible Cause(s) Suggested Action(s) Blocked needles • Remove the plunger and use a second syringe to fill Sample material or contaminants may be trapped the blocked syringe with solvent. Then, insert the inside the needle. • plunger and gently push solvent through needle. The needle may not have been properly cleaned.
  • Page 33 Sample Introduction Cleaning Syringes During an Autosampler Sequence To ensure the syringe is properly cleaned between injections, rinse and fill each solvent bottle with 4 mL of fresh solvent. The liquid level will be near the shoulder of the bottle. Good laboratory practice dictates using no more than 2 mL of the 4 mL solvent for syringe 4 mL fill volume washes.
  • Page 34 Straight Needle, 23 and 26s Gauge Autosampler Syringes Volume Description Unit Needle Part No. (µL) Cone-tipped, 23 gauge 23/42/HP 5188-5246 Cone-tipped, 23 gauge 23/42/HP 5188-5247 Straight, fixed, 26 gauge 26s/42/HP 9301-0891 Straight, fixed, 26 gauge 6/pk 26s/42/HP 5183-4728 Straight, fixed, 23 gauge 23/42/HP 9301-0892 Straight, fixed, 23 gauge...
  • Page 35 Sample Introduction GC Automatic Liquid Sampler Supplies Description Unit Part No. 4 mL Clear screw top wash vials with screw caps (no septa) 144/pk 9301-0723 Septa for 4 mL vial 144/pk 9301-1031 Diffusion inserts for 4 mL vials 12/pk 07673-40180 4 mL wash vials with fill markings and caps 25/pk 5182-0551...
  • Page 36: Headspace Sampler

    Headspace Sampler The appropriate maintenance frequency for the Headspace Sampler varies significantly depending on the sample matrix, solvents, temperatures, and sample throughput. Recommended Maintenance Schedule Maintenance Low Boiling Solvents High Boiling Solvents Activity (water, food, flavor analyses) (OVI, blood alcohol analysis) ≤...
  • Page 37 Sample Introduction Headspace Vials Description Unit Part No. Certified Flat Bottom Headspace Crimp Top Glass Vials 20 mL, clear, 23 x 75 mm 100/pk 5182-0837 10 mL, clear, 23 x 46 mm 100/pk 5182-0838 Certified Rounded Bottom Headspace Crimp Top Glass Vials 20 mL, clear, 23 x 75 mm 100/pk 5183-4474 10 mL, clear, 23 x 46 mm...
  • Page 38 Headspace Supplies Description Part No. Stainless Steel Sample Loops Sample loop, 1 mL, deactivated 2321700003 Sample loop, 3 mL, deactivated 2321700004 Probes and Unions Sample probe, deactivated 2322700011 M6 union, brass 2302533140 Union, zero dead volume, deactivated 2307230001 Union 2307232901 Transfer Line Needles and Unions Needle, headspace transfer line, deactivated 0.5 mm OD 2322590004...
  • Page 39: Ctc Autosampler Supplies

    Sample Introduction CTC Autosampler Supplies Agilent now offers a portfolio of CTC-recommended supplies for your GC PAL and CombiPAL autosamplers. CombiPAL and GC PAL CombiPAL and GC PAL Liquid Injection Vials and Caps Liquid Injection Description Unit Part No. Vials and Caps 2 mL vials These micro and 2 mL vials and caps Crimp top vial, wide opening, clear...
  • Page 40 CombiPAL and GC PAL Liquid Injection Syringes A key feature of CTC's GC PAL and CombiPAL systems is the ability to inject a wide range of sample volumes – up to 500 µL for LVI applications. To help you take full advantage of this flexibility, Agilent offers a wide range of C-type syringes –...
  • Page 41 Sample Introduction CombiPAL Headspace Supplies Our fixed-needle headspace syringes CTC syringe, G6500-80109 feature a sideport needle for gas flushing, in conformance with strict CTC standards. Use with Agilent’s Merlin Microseal to CombiPAL Headspace Syringes minimize instrument downtime – and to prevent lost or compromised data caused Volume (µL) Description Gauge...
  • Page 42 CTC recommends screw-top vials CombiPAL Headspace Supplies and caps for the tightest seal and the most reproducible headspace results, Description Part No. and the precision-thread vials and caps 10 mL, screw top clear vial, 100/pk 5188-5392 listed are an excellent choice for dependability and ease of use.
  • Page 43: Purge And Trap Supplies

    Sample Introduction Purge and Trap Supplies Sparger Compared to a frit sparger, the fritless sparger may be the better choice when a water sample has a tendency to foam. This sparger is not appropriate for soil samples, which tend to clog the capillary tube. Available in 1/2 and 3/4 in. mount sizes. Glassware for Teledyne Tekmar Purge and Trap Concentrators, 1/2 in.
  • Page 44 Traps for Teledyne Tekmar Stratum Purge and Trap Concentrator Description Part No. Trap, BTEX + MTBE 5188-8813 Trap (#5),OV-1/Tenax/Silica Gel/Charcoal 5188-8814 Trap (#8), Carbopak B/Carbosieve S-III 5188-8815 Trap (#9), Proprietory 5188-8816 Trap, Tenax/Silica Gel/Carbosieve S-III 5188-8817 Strat-Trap, Tenax/Silica Gel, #2 5188-8818 Strat-Trap,Tenax/Silica Gel/Charcoal, #3 5188-8819...
  • Page 45: Markes Thermal Desorption

    Sample Introduction Markes Thermal Desorption Agilent now offers a comprehensive line of supplies for Markes Thermal Desorption (TD) instrumentation. Thermal desorption allows the introduction of volatile and semi-volatile compounds from a wide range of sample matrices, directly into a GC or GC/MS. Markes Thermal Desorption Supplies Description Unit...
  • Page 46 Markes Thermal Desorption Supplies Description Unit Part No. Tenex stainless steel tubes, preconditioned/capped 10/pk C-TBP1TC Empty glass TD tubes 10/pk C-GT010 PTFE inserts 10/pk C-PL010 Long term TD tube storage caps 10/pk C-CF020 Cap-LOK Tool for long term storage caps C-CPLOK Diffusive sampling caps 10/pk C-DF010...
  • Page 47: Inlets

    Inlets Be certain that you are accurately and predictably introducing samples into your GC and GC/MS Systems. Proper inlet selection and maintenance can significantly enhance the performance of your chromatography system and, ultimately, your analytical method. It can also prevent problems such as decomposition, flashback, and leaks that can compromise the integrity of your results.
  • Page 48: Premium Non-Stick Septa

    Premium Non-Stick Septa Agilent premium non-stick inlet septa are designed and manufactured to provide a reliable non-contaminating seal. Our tri-fold blister pack ensures that each septum remains clean and ready to use. • Proprietary plasma treatment prevents sticking and unnecessary inlet cleaning. •...
  • Page 49 Inlets Bleed and Temperature Optimized Septa (BTO) • Extended temperature range, lowest bleed. • Maximum injection port temperature 400°C. • Plasma coating eliminates sticking in the injection port. • Pre-conditioned; ready to use. • Blister packaging for cleanliness and convenience. •...
  • Page 50 Advanced Green Septa • True long-life, high temperature green septum. • More injections per septum. • Plasma coating eliminates sticking in the injection port. • Maximum injection port temperature 350°C. • High-performance alternative to competitors' "Green" septa. • Blister packaging for cleanliness and convenience. Advanced Green Septa Description Unit...
  • Page 51 Inlets Septa Troubleshooting Symptom Possible Causes Remedy Extra Peaks/Humps Septum bleed Turn off injector heater. If extra peaks disappear, use septum specified for higher temperature or analyze at lower inlet temperature. Baseline Change After Large Large leak at septum during Replace septum and use smaller Peak injection and for a short time...
  • Page 52: Ferrules

    Ferrules Using the wrong ferrule or a worn-out ferrule to seal your column connection can result in inconsistent and unreliable chromatography. An improper ferrule can cause leaks which allow air and other contaminants to enter the instrument through the column seal, causing major interference with column and detector performance.
  • Page 53 Inlets Ferrule Selection Recommendations Ferrule/ Seal Type Upper Temp. Usages Advantages Limitations Limit Graphite (100%) 450°C • • • General purpose for Easy to use stable seal. Not for MS or oxygen • capillary columns. Higher temperature limit. sensitive detectors. •...
  • Page 54 Capillary Column Ferrules Ferrule ID (mm) Column ID (mm) Unit Part No. General Purpose Graphite Ferrules (Short) 0.1, 0.2, 0.25, 0.32 10/pk 5080-8853 0.05, 0.25 10/pk 500-2114 0.45, 0.53 10/pk 500-2118 0.53 10/pk 5080-8773 85% Vespel, 15% Graphite Ferrules (Short) 0.1, 0.2, 0.25 10/pk 5181-3323 0.32...
  • Page 55 Inlets SilTite Metal Ferrules Description Unit Part No. For use with 0.25 mm ID capillary columns 10/pk 5188-5361 For use with 0.32 mm ID capillary columns 10/pk 5188-5362 For use with 1/16 in. OD stainless steel tubing 10/pk 5184-3571 Includes 2 column nuts For use with 0.53 mm ID capillary columns 10/pk 5188-5363 Column Nuts...
  • Page 56: Capillary Flow Technology Supplies

    Capillary Flow Technology Supplies Agilent offers a family of GC accessories based on our proprietary Capillary Flow technology. These accessories increase system productivity and performance: • QuickSwap MSD interface provides vent-free removal of columns. • Deans Switch device simplifies the analysis of complex samples. •...
  • Page 57: Split/Splitless Liners

    Inlets Split/Splitless Liners Injection port liners have a variety of features to help vaporize the sample so that a true representation of the sample enters the column. Additionally, Agilent liners are individually packaged to maintain cleanliness until used. The part number and lot are silk screened on the liner for quality control and user convenience, and lot tracking is available for quality assurance.
  • Page 58 Tapers None Bottom Tapers Dual Tapers Straight tubes used in split • • Directs sample onto head Contain sample within glass injection with autosamplers. of column and limits analyte liner limiting contact with exposure to bottom of inlet. metal inlet surface. •...
  • Page 59 Inlets Agilent MS Certified Liners NEW! Agilent MS Certified Split and Splitless Liners are manufactured and tested to our highest level of scrutiny to assure reproducibility. We have built years of experience into the MS Certified Liners to provide the quality and consistency needed for critical applications, especially those using esterification agents for trace level analysis such as toxicology or drugs of abuse applications.
  • Page 60 Agilent Split Liners Description 1/pk 5/pk 25/pk Single Taper Split Liners Single taper, glass wool, deactivated, low pressure 5183-4647 5183-4701 5183-4702 drop Single taper, MS certified liner with restriction to hold 5188-6576 glass wool Single taper, glass wool, deactivated 5183-4711 5183-4712 5183-4713 Straight Split Liners Straight, glass wool, non-deactivated...
  • Page 61: Direct Connect Liners

    Inlets Direct Connect Liners Agilent's Direct Connect Liners provide maximum recovery and minimal decomposition of active compounds for methods requiring splitless injection, such as EPA 8270. They are best for relatively clean samples containing active analytes, such as water extracts. The liners directly connect with the column, similar to press-fit connectors, to aid complete transfer of sample onto the column, eliminating the problem of inlet discrimination and further increasing sensitivity.
  • Page 62: Split/Splitless Inlets

    Split/Splitless Inlets The combined split/splitless inlet is the most popular inlet for capillary column gas chromatography. Because it can be used in either split or splitless mode, it provides a very effective combination that can cover most analysis requirements. Split Inlet Troubleshooting Split inlets are spared from most band-broadening phenomena, since the splitting process generates narrow peaks.
  • Page 63 Inlets Splitless Inlet Troubleshooting Most problems encountered with a splitless injection are related to: • Incorrect purge time • Degradation • Improper focusing • Inappropriate column temperature • Flashback You can also improve the reproducibility and linearity of peak areas and avoid backflash by matching: •...
  • Page 64 Split Mode Variables, Practices and Rationales Parameter Selection/Setting Rationale Inlet temperature Try 250°C or BP of last eluting Ensures flash vaporization compound Minimizes inlet discrimination Inlet liner Large volume, deactivated Minimizes flashback Minimizes degradation Inlet packing Silanized glass wool Retains non-volatiles Minimizes inlet discrimination Glass beads or frit Less active than wool...
  • Page 65 Inlets Splitless Mode Variables, Practices and Rationales Parameter Selection/Setting Rationale Inlet temperature Just above highest boiling point Ensures flash vaporization of solutes (+20°C) Reduce if degradation occurs Use higher for dirty samples and higher-boiling solutes Inlet liner Large volume > 0.8 mL Use with autoinjector Small volume <...
  • Page 66 Flip Top Inlet Sealing System Agilent's Flip Top Inlet Sealing System is the faster, smarter way to change inlet liners on Agilent GC's. • Cuts liner replacement time to as little as 30 seconds. • Eliminates frustrating searches for special wrenches or tools. •...
  • Page 67 Inlets 7890 Turn Top Inlet System Convenient new turn top design is built into each 7890 split/splitless inlet, allowing you to change liners in less than 30 seconds without special tools or training. 7890 Turn Top Inlet System Description Part No. Turn top G3430-40035 Split ring...
  • Page 68 Changing the Split Vent Trap* 1. Remove the retaining clip. 2. Remove the old filter cartridge and two O-rings. 3. Verify the new O-rings are seated properly on the new filter cartridge. 4. Install the new filter cartridge then reassemble the trap. Do not fully tighten yet. 5.
  • Page 69 Inlets 7890/6890/6850 Split/Splitless Inlet Supplies Item Description Unit Part No. QuickPick Split Vent and Inlet PM Kit 5188-6496 QuickPick Splitless Vent and Inlet PM Kit 5188-6497 Headspace septum retainer nut 18740-60830 Septum retainer nut 18740-60835 11 mm non-stick BTO septa 50/pk 5183-4757 For complete offering of liners, see pages 58-59...
  • Page 70 7890/6890/6850 Split/Splitless Inlet Supplies Item Description Unit Part No. Split vent trap kit G1544-60610 Replacement cartridge for P/N G1544-60610 G1544-80530 Split vent trap assembly G1544-80550 Retaining nut G1544-20590 Stainless steel seal 18740-20880 Certified gold plated seal kit, includes washer 5188-5367 Replacement for 18740-20885 Gold-plated seal with cross 5182-9652...
  • Page 71: Cool On-Column Inlets

    Inlets Cool On-Column Inlets Cool on-column injection is superior in many ways to other sample introduction techniques. Advantages include: • Elimination of sample discrimination. • Elimination of sample alteration. • Solvent focusing of early eluting solutes. • High analytical precision. Sample Considerations Sample preparation is important for on-column injection because of: •...
  • Page 72 Cool On-Column Inlet Practices and Rationales Parameter Selection/Setting Rationale Initial inlet temperature Equal to or 3°C above column Ensures sample focusing in oven temperture solvent front Initial inlet temperature ramp Same as oven (oven track) Simple and effective Faster than oven Narrows initial peak width Injection volume 0.1 - 2.0 µL liquid...
  • Page 73 Inlets Installing a Capillary Column into a Cool On-Column Inlet Syringe Insert 1. Gently insert the column into the inlet until it bottoms. Column 2. Insert the column nut into the inlet fitting and finger tighten. 3. Tighten the column nut an additional 1/4 turn with a wrench or until the column does not move.
  • Page 74 Changing the Septum on the Cool On-Column Inlet 1. Replace the septum. If you are using a septum nut, grasp the knurling and unscrew. Remove the old septum with tweezers. Use tweezers to install a new septum. Push the septum into the septum nut until properly seated.
  • Page 75 Inlets 7890/6890 Cool On-Column Inlet Supplies Item Description Unit Part No. Automatic Injection Septum nut base for 320 mm assembly 19245-80521 Septum nut base for 530 mm assembly G1545-80520 Advanced Green Inlet Septa, 5 mm 50/pk 5183-4760 BTO Inlet Septa , 5 mm 50/pk 5183-4758 Manual Injection Cooling tower assembly...
  • Page 76 Column/Retention Gap Installation Supplies Description Unit Part No. Ultimate union kit, deactivated G3182-61580 Ultimate union kit, non-deactivated G3182-61581 Universal column nut 2/pk 5181-8830 SilTite metal ferrules, 0.10-0.25 mm ID capillary columns 10/pk 5188-5361 SilTite metal ferrules, 0.32 mm ID capillary columns 10/pk 5188-5362 SilTite metal ferrules, 0.53 mm ID capillary columns 10/pk 5188-5363...
  • Page 77: Purged Packed Inlets

    Inlets Purged Packed Inlets Packed column analysis is frequently done when high efficiency separations are not needed or when gases are analyzed by gas-solid chromatography. Purged packed inlets are simple in both design and use. Few parameters need to be set, and all carrier gas flow flushes through the inlet into the column in the standard configuration.
  • Page 78 Purged Packed Inlet Troubleshooting Purged packed inlets are active, have low volume and are generally flow controlled. This means that most packed column inlet problems involve sample decomposition, flashback, or leaks. Decomposition Diagnose inlet sample decomposition by comparing retention times for decomposition products to their standard retention times.
  • Page 79 Inlets 7890/6890/6850 Purged Packed Inlet Supplies Septum nut Merlin cap Description Unit Part No. Merlin Microseal Septum QuickPick Purged Packed Inlet PM Kit 5188-6498 Top insert weldment Includes 5 non-stick BTO septa, 1 O-ring, 1 ferrule, and 1 disposable glass liner O-ring Merlin Microseal 5182-3444...
  • Page 80: Programmed Temperature Vaporizer (Ptv) Inlets

    Programmed Temperature Vaporizer (PTV) Inlets PTV inlets combine the benefits of split, splitless and on-column inlets. The sample is usually injected into a cool liner, so syringe needle discrimination does not occur. Then the inlet temperature is increased to vaporize the sample. The user programs vent times and temperature to achieve the equivalent of split or splitless transfer of sample vapors to the column.
  • Page 81 Inlets PTV Inlet Practices and Rationales (cold split/splitless modes) Parameter Selection/Setting Rationale Injection mode Cold split For general use and sample Cold splitless screening Cold solvent vent For trace analysis Inlet temperature ramp rate Adjustable (i.e., 2°C/sec to Use slower ramp rates for labile, 720°C/sec max) complex, or large volume samples...
  • Page 82 7890/6890 PTV Inlet Supplies Description Column ID (mm) Unit Part No. Microseal high pressure nut 5182-3445 Merlin Microseal 5182-3444 Septumless head G2617-60507 Septum head G2618-80500 Septum retainer nut 18740-60835 PTV inlet assembly G2617-60506 PTV LC0 cooling jacket G2617-60508 PTV LN cooling jacket G2619-60501 Silver seal...
  • Page 83 Inlets Guide cap Septum nut Merlin cap PTFE ferrule Merlin Microseal Septum Kalrez seal Septumless head assembly Valve body Pressure spring Septum head Viton seal Sealing element Carrier gas tube Graphpak 3D ferrule Liner PTV inlet assembly Silver seal Graphpak inlet adapter Ferrule for Graphpak adapter Column nut Programmable Temperatue Vaporizing (PTV) Inlet assembly...
  • Page 84 Programmable Temperature Vaporizing (PTV) Liners Description ID (mm) Volume Part No. (µL) PTV liner, single baffle, glass wool, deactivated 5183-2038 PTV liner, single baffle, deactivated 5183-2036 PTV liner, multi baffled, deactivated 5183-2037 PTV liner, high temperature, quartz 5188-5313 PTV liner, high temperature, borosilicate 5188-5356 PTV liner, sintered glass, deactivated 5190-1426...
  • Page 85: Detectors

    Detectors Make sure damaging contaminants do not compromise your GC detector’s operation. At Agilent, we understand that sensitive GC detectors require regular maintenance and decontamination to ensure peak performance and minimize the risk of costly downtime. That is why we have devoted this section to… •...
  • Page 86: Flame Ionization Detector (Fid)

    Flame Ionization Detector (FID) The FID requires routine maintenance to ensure optimum performance. Maintenance requirements are application dependent, but Agilent recommends periodically cleaning or replacing the following items: FID Routine Maintenance Item Comments FID Jet A plugged jet results in longer retention times as the column exit/detector pressure increases.
  • Page 87 Detectors Flame Ignition If the flame goes out or will not light: • Measure the hydrogen/air and makeup flow rates – Low H or makeup flows indicated a plugged jet, or a leak at the column fitting. Measure each gas flow independently. •...
  • Page 88 Installing a Capillary Column in the FID 1. Gather the required supplies and tools. 2. Load the GC maintenance method and wait for the GC to become ready. 3. If using the adaptable detector, verify that the adapter is installed. 4.
  • Page 89 Detectors FID Jet Identification and Selection FID Jets Description Jet Tip ID Length (mm) Part No. Before ordering parts for FID maintenance, Jets for capillary optimized fittings determine which type of FID is installed on your GC. The FID is available in Capillary 0.29 mm (0.011 in.) G1531-80560...
  • Page 90 Jet Cleaning Procedure Use Agilent cleaning kit, part number 9301-0985 1. Run a cleaning wire through the top of the jet. Run it back and forth a few times until it runs smoothly. Be careful not to scratch the jet. (Do not force too large a wire or probe into the jet opening or the opening will become distorted.
  • Page 91 Detectors Flame Ionization Detector (FID) Supplies Item Description Unit Part No. PTFE chimney (optional) 19231-21050 Collector nut 19231-20940 Spring washer 10/pk 5181-3311 Ignitor castle 19231-20910 Hastelloy ignitor castle (optional) 19231-21060 Ignitor glow plug assembly 19231-60680 Collector insulator G1531-20700 Collector body G1531-20690 Hastelloy Collector Body G1531-21090...
  • Page 92 Flame Ionization Detector (FID) Supplies Item Description Unit Part No. FID MDL test sample for 7890 only 5188-5372 3 x 0.5 mL ampoules. Contains 2.36 mg/L n-Tridecane, 2.36 mg/L n-Tetradecane, 23.6 mg/mL n-Penta-decane, 23.6 mg/mL n-Hexadecane in iso-octane O-rings 12/pk 5080-4978 FID/NPD adapter for capillary column 19244-80610...
  • Page 93: Electron Capture Detector (Ecd)

    Detectors Electron Capture Detector (ECD) Liner Selection The only assembly that requires routine maintenance is the glass liner in the makeup gas assembly, especially for the µECD. All sample passes through the indent in the mixing liner of the µECD. The mixing liner should be replaced if there is a significant loss of sensitivity or any time the column is removed/reinstalled in the detector.
  • Page 94 Thermal Cleaning If your baseline is noisy or the output value is abnormally high (> 1000 Hz), and you have determined that these problems are not being caused by leaks in the GC system, you may have contamination in the detector from column bleed and sample residues. To remove contamination, you should perform a thermal cleaning (bakeout) of the detector.
  • Page 95 Detectors Electron Capture Detector (ECD) Supplies Item Description Part No. Standard ECD makeup gas adapter* G1533-80565 Micro ECD makeup gas adapter G2397-80520 Micro ECD mixing liner, also compatible with standard ECD design G2397-20540 ECD makeup gas adapter, 7890A only G3433-67565 2, 3 Insulating cup 19234-60720...
  • Page 96: Thermal Conductivity Detector (Tcd)

    Thermal Conductivity Detector (TCD) The TCD compares the thermal conductivities of two gas flows – pure carrier gas (also called the reference gas) and carrier gas plus sample components (also called column effluent). Filament Maintenance The primary maintenance for a TCD involves the filament. Most procedures involve improving filament life or keeping the filament from becoming damaged or contaminated.
  • Page 97 Detectors Solvent Flush 1. Cool the cell to room temperature and remove the column. 2. Place a septum in a nut or fitting assembly that fits onto the detector entrance (7 mm septum in a 1/8 in. nut). 3. Place the nut or assembly on the detector fitting and tigthen. Verify the presence of makeup gas flow.
  • Page 98 Installing a Capillary Column in the TCD 1. Gather the required supplies and tools. 2. Assemble the ferrules and 1/8 in. brass Swagelok nut on the column. 3. Score the column using a glass scribing tool. The score must be square to ensure a clean break.
  • Page 99 Detectors Determining the TCD Electronic Pressure Control (EPC) If you have a 6890A or 6890A Plus GC, you may have an older design EPC Flow manifold for the TCD. The older design requires removal of sheet metal panels to attached the TCD reference flow gas supply inside the GC.
  • Page 100 Thermal Conductivity Detector (TCD) Supplies Item Description Unit Part No. For 1/8 in. SS Packed Column Installation Vespel/graphite ferrule, 1/8 in. 10/pk 0100-1332 1/8 in. nut, brass 10/pk 5180-4103 For 1/4 in. SS Packed Column Installation Vespel/graphite ferrule, 1/8 in. 10/pk 0100-1332 1/8 in.
  • Page 101: Flame Photometric Detector (Fpd)

    Detectors Flame Photometric Detector (FPD) In 2005, Agilent released an improved FPD with minimum detectable levels (MDL) of 3.6 pg/sec for sulfur and 60 fg/sec for phosphorus. This is more than a 5x improvement for sulfur. The updated design is based on a one-piece, deactivated transferline jet assembly and improved optics.
  • Page 102 Maintenance Managing gas purity; contamination from column bleed, sample residue, and corrosion; and air leaks can help keep your FPD at peak performance. Gas purity Sulfur contamination is a common problem and causes noise and/or a higher baseline offset in the FPD. To minimize sulfur contamination and achieve the lowest MDLs, use at least 99.9995% pure gases, clean tubing, and regulators with metal diagrams.
  • Page 103 Detectors Flame Ignition Problems You can tell if your FPD is lit by checking the detector "Output" and "Flame" on the display. The detector senses that the flame is on by comparing the output with the offset. An optimized FPD normally runs with an output in the range of 30 to 80 with the offset set point at 2.0.
  • Page 104 Installing a Capillary Column Adapter to the FPD 1. Gather the required supplies and tools. 2. Load the GC maintenance method and wait for the GC to become ready. 3. Insert the capillary adapter into the 1/8-inch nut as shown, then thread the nut onto the detector fitting.
  • Page 105 Detectors Attaching a Capillary Column to the FPD 1. Gather the required supplies and tools. What you need: 2. Load the GC maintenance method and wait for the GC to become ready. • Column measuring tool, 3. Assemble a septum, column nut, and ferrule on the end of the column. p/n 19256-80640 •...
  • Page 106 FPD Ignitor and Heat Shield Assembly Item Description Part No. FPD Exit Tube Assembly Aluminum 19256-60700 Stainless Steel 19256-20705 Ferrule, 1/4 in. Vespel, 10/pk 5080-8774 Emission chamber, single FPD single 19256-80560 FPD, dual 19256-80600 FPD igniter replacement kit 19256-60800 Includes items A, B, C A.
  • Page 107 Detectors FPD Lens Assembly Item Description Part No. Clamp 19256-00090 Screw, M3 x 25 (4 required) 0515-0683 Window O-ring, inner, 0.926 in. ID, orange 5061-5886 Convex lens 1000-1438 Lens housing 19256-20900 Flange ring 19256-00200 Fluorocarbon Elastomer O-ring, brown, 1.239 in. ID 5061-5890 FPD lens assembly FPD PMT and Bracket Assemblies...
  • Page 108: Nitrogen Phosphorus Detector (Npd)

    Nitrogen Phosphorus Detector (NPD) Bead Maintenance NPDs are temperamental and require frequent maintenance. Small changes in any of a number of parameters can significantly change the performance characteristics of an NPD. The bead requires the most maintenance. It needs to be changed frequently, thus a spare is a necessity.
  • Page 109 Detectors Gas Flow The hydrogen, air and makeup gas flows should be measured frequently. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be measured independently to obtain the most accurate values. NPDs are very sensitive to changes in the gas flows and consistent flows are necessary to maintain performance levels.
  • Page 110 Cleaning and Replacement The NPD requires periodic cleaning. In most cases, this only involves the collector and the jet. Agilent provides brushes and wires that simplify the cleaning of all detector parts. The brushes are used to dislodge particulates clinging to the metal surfaces. A fine wire is used to clean the jet opening of particulates.
  • Page 111 Detectors Contaminants Some chemical problems can also arise when using the NPD. Because it is a trace detector, be careful not to contaminate the analytical system. Glassware Glassware must be very clean. Phosphate detergents should be avoided, so acid washing of glassware followed by distilled water and solvent rinsing is recommended.
  • Page 112 NPD Jet Identification and Selection Before ordering parts for NPD maintenance, determine which type of NPD is installed on your GC. The NPD is available in two versions: • Dedicated, Capillary Optimized: for capillary columns only • Adaptable: for packed or capillary columns Hint: Adaptable jets are longer than dedicated capillary jets.
  • Page 113 Detectors Nitrogen Phosphorus Detector (NPD) Supplies Item Description Part No. Screws, M3 x 0.5 x 8 mm (Pozidriv) 0515-0655 NPD bead assembly* G1534-60570 NPD black ceramic bead assembly** 5183-2007 Lid weldment G1534-80510 Metal C-ring, top 0905-2580 Alumina insulator, upper G1534-40020 Collector funnel G1534-20530 Alumina insulator, lower...
  • Page 114 Nitrogen Phosphorus Detector (NPD) Supplies Item Description Part No. Ferrule, 1/4 in. Vespel, 10/pk 5080-8774 530 µm, 1.0 mm ID graphite ferrule, 10/pk 5080-8773 320 µm, 0.5 mm ID graphite ferrule, 10/pk 5080-8853 1/4 in. nut, brass, 10/pk 5180-4105 Universal column nut, 2/pk 5181-8830 Nitrogen-Phosphorus Detector Sample 18789-60060...
  • Page 115: Nitrogen And Sulfur Chemiluminescence Detectors

    Detectors Nitrogen and Sulfur Chemiluminescence Detectors Nitrogen Chemiluminescence Detector (NCD) Supplies Description Part No. Dual plasma burner accessory kit G6600-60038 Includes ferrules, fittings and quartz tube PM Kit, dry piston pump G6600-67006 Includes dry piston seal, 6 Moleculite vacuum pump traps and 1 set of ceramic tubes PM Kit, DP RV5 oil pump G6600-67007...
  • Page 116 Sulfur Chemiluminescence Detector (SCD) Supplies Description Part No. PM Kit, dry piston pump G6600-67006 Includes dry piston seal, 6 Moleculite vacuum pump traps and 1 set of ceramic tubes PM Kit, dry piston pump G6600-67008 Includes 6 Chemical traps for Ozone destruction and 2 repair kits for pump 12-month maintenance kit G6600-67009 Includes 6 quarts oil, 12 chemical traps, 4 oil filter elements, 2 sets of ceramic...
  • Page 117: Gc/Ms Systems

    GC/MS Systems Prevent, detect, and correct problems now and promote a lifetime of reliability and low operating costs. Your mass spectrometer is a sensitive, specialized device that delivers a higher level of functionality than other GC detectors. However, it also requires more stringent adherence to a regular maintenance schedule.
  • Page 118: Maintaining Mass Selective Detectors (Msd)

    Maintaining Mass Selective Detectors (MSD) Your GC/MSD is highly sensitive. To continue achieving optimal results, it is critical to maintain your system properly by performing the essential tasks within this section. Some of the benefits of maintaining your GC/MSD include: •...
  • Page 119 GC/MS Systems Maintenance Schedule Task Every week Every 6 months Every year As needed Tune the MSD Change injection port liners Check the foreline pump oil level Gas ballast the foreline pump Check the calibration vial Replace the foreline pump oil Check the diffusion pump fluid Replace the diffusion pump fluid Replace the traps and filters...
  • Page 120: Msd Contamination

    MSD Contamination Contamination is usually identified by excessive background in the mass spectra. It can come from the GC or from the MSD. The source of the contamination can sometimes be determined by identifying the contaminants. Some contaminants are much more likely to originate in the GC, others are likely to originate in the MSD.
  • Page 121 GC/MS Systems Contamination Sources in the MSD • Air leaks • Cleaning solvents and materials • Fingerprints inside the manifold • Diffusion pump fluid • Foreline pump oil The action required to remove contamination depends on the type and level of contamination.
  • Page 122 Symptoms of leaks • Higher than normal vacuum manifold pressure or foreline pressure • Higher than normal background • Peaks characteristic of air (m/z 18, 28, 32, and 44 or m/z 14 and 16) • Poor sensitivity • Low relative abundance of m/z 502 (this varies with the tune program and MSD used) Remedy •...
  • Page 123 GC/MS Systems Cleaning Solvents It is common to see cleaning solvent peaks in the mass spectra shortly after the ion source is cleaned. Remedy • Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them. Refer to specific cleaning procedures in your MSD Hardware Manual or MSD The easiest way to insure that you Maintenance and Troubleshooting Manual.
  • Page 124 Diffusion Pump Fluid If the diffusion pump fluid is allowed to operate with no column (carrier gas) flow into the vacuum system, vapor from the diffusion pump fluid can drift up into the vacuum manifold. A more serious problem is when fluid is back streamed into the vacuum manifold by sudden or improper venting of the vacuum system.
  • Page 125 GC/MS Systems MSD Contamination Identification The following table lists some of the more common contaminants, the ion characteristics of those contaminants, and the likely sources of those contaminants. Common Contaminants Ions (m/z) Compound Possible Source 13, 14, 15, 16 Methane CI gas Even preconditioned ferrules 18, 28, 32, 44 or 14, 16...
  • Page 126 Mass Spectrometer Symptoms Mass spectrometer symptoms can typically be classified as either affecting system sensitivity or affecting the repeatability of a measurement. Most symptoms can be corrected by following the suggested corrective actions. Mass Spectrometer Symptoms Symptoms Remedy Sensitivity Wrong retention time Check GC, method, application and carrier gas velocity.
  • Page 127 GC/MS Systems Mass Spectrometer Symptoms Symptoms Remedy Repeatability Dirty syringe needle Clean or replace the syringe. Wrong syringe needle Replace syringe and septa. Leaking injection port Perform injection port maintenance. Replace the injection port liner, septa and liner O-ring. Injection is too large Check method and injection volume, split ratio and/or 5975 MSD splitless purge time.
  • Page 128: Cleaning And Maintenance Supplies

    Cleaning and Maintenance Supplies Description Part No. One Year Maintenance Kit (for diffusion pump systems) 5183-2096 Includes Big Universal Trap for He (1/8 in.), abrasive sheets (5/pk), lint-free cloths (15/pk), cotton swabs (100/pk), SantoVac Ultra, 18.5 mL (2 each), rough pump oil (1 liter), filament assembly, Octafluoronapthalene (OFN) Nylon gloves, lint-free, large, 1 pair 8650-0030 Nylon gloves, lint-free, small, 1 pair...
  • Page 129 GC/MS Systems Cleaning and Maintenance Supplies Description Part No. Tools Screwdriver, 3 in. Pozidriv shaft No. 1 pt, fits no. 2-4 screws 8710-0899 Screwdriver, 4 in. Pozidriv shaft No. 2 pt, Fits no. 5-10 screws 8710-0900 Open end wrench, 1/4 and 5/16 in. 8710-0510 MS Interface Column Installation Tool G1099-20030...
  • Page 130: Ion Source

    Ion Source The ion source operates by electron ionization (EI) or chemical ionization (CI). The sample enters the ion source from the GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting them.
  • Page 131 GC/MS Systems Preparing to Clean Prior to cleaning, the mass spectrometer must be vented and the ion source must be removed. Before venting the system, the following conditions must be met: • Heated zones are less than 100°C. • The diffusion pump is off and cool. •...
  • Page 132 Electron Impact (EI) Ion Source The recommended cleaning material for the EI ion source is abrasive powder, aluminum oxide powder. Abrasively clean the surfaces that contact the sample or ion beam. Use an abrasive slurry of alumina powder and reagent-grade methanol on a cotton swab. Use enough force to remove all discolorations.
  • Page 133 GC/MS Systems 5972/5971/GCD MSD Ion Source Parts (EI) Description Part No. Entrance lens 05971-20126 Lens insulator, 597X MSD G3170-20530 Ion focus lens 05971-20143 Drawout cylinder G1072-20008 Electron Impact (EI) Ion Source Drawout plate, 3 mm 05971-20134 Set screw 0515-1446 Repeller assembly 05971-60170 Screw for filament on the source 0515-1046...
  • Page 134 Chemical Ionization (CI) Ion Source Because the CI ion source operates at much higher pressures than the EI ion source, it will probably require more frequent cleaning than the EI ion source. The source should be cleaned whenever there are performance anomalies that are associated with a dirty ion source.
  • Page 135 GC/MS Systems 5975/5973 MSD Chemical Ionization Ion Source Parts (CI) Item Description Part No. Source body G1999-20430 Draw out plate G1999-20446 Draw out cylinder G1999-20444 Lens insulator G3170-20540 Ion focus lens G1999-20443 Entrance lens G3170-20126 Repeller insulator G1999-20433 Repeller G1999-20432 High temperature filament G1099-80053 Cap screw, gold plated...
  • Page 136: Installing A Capillary Column In The Gc/Msd Interface

    Installing a Capillary Column in the GC/MSD Interface 1. Condition the column. 2. Vent the MSD and open the analyzer chamber. Be sure you can see the end of the GC/MSD interface. 3. If the CI interface is installed, remove the spring-loaded tip seal from the MSD end of the interface.
  • Page 137: Quickswap Ms Interface Restrictors

    GC/MS Systems Installing a capillary column in the GC/MSD interface Analyzer chamber Interface column nut Column GC/MSD interface (MSD end) GC/MSD interface 1 to 2 mm (GC end) QuickSwap MS Interface Restrictors Agilent's QuickSwap capillary flow technology module and pre-swaged fused silica tubing restrictors can increase the productivity of your Agilent 5973N and 5975 inert MSD systems, allowing you to change columns without venting the MSD.
  • Page 138: Msd Filaments

    MSD Filaments Like the filaments in an incandescent light bulb, the ion source filaments will eventually burn out. Certain practices will reduce the chance of early failure. • When setting up data acquisition parameters, set the solvent delay so that the analyzer will not turn on while the solvent peak is eluting.
  • Page 139 GC/MS Systems Quadrupole Mass Filter The mass filter does not require periodic maintenance. It should not be removed from the radiator or distributed in any way. • Never put the quadrupole in an ultrasonic cleaner. • Never change the physical orientation of the quadrupole mass filter. •...
  • Page 140: Vacuum Systems And Pumps

    Vacuum Systems and Pumps The vacuum system creates the high vacuum (low pressure) required for the MSD to operate. Without this vacuum, the molecular mean free path is too short. Ions cannot travel from the ion source through the mass filter to the electron multiplier (detector) without colliding with other molecules.
  • Page 141 GC/MS Systems Pressure Symptoms This section describes unusual pressure Pressure Symptoms readings and their possible causes. The Symptoms Possible Causes symptoms in this section are based on typical pressures. At typical column flow Foreline pressure is too high. rates (0.5 - 2.0 mL/min), the foreline •...
  • Page 142 Diffusion Pump It is not necessary to change the diffusion pump fluid more than once a year, unless you observe symptoms that suggest a problem with the diffusion pump fluid. The MSD must be vented in order to check the diffusion pump fluid (except for the 5975/5973). Therefore, the best time to check the fluid is when the instrument is already vented for other maintenance.
  • Page 143 GC/MS Systems Foreline Pump The oil in the foreline or rough pump should be replaced on average once every six months, but can vary depending upon applications. After oil replacement, if a foreline trap is present, the molecular sieves should be replaced. Avoid contact with the pump oil.
  • Page 144: Msd Electron Multipliers And Replacement Horn

    MSD Electron Multipliers and Replacement Horn The lifetime of an electron multiplier is directly related to the current that flows through it and the extent of contamination or condensation that it experiences. Replace the electron multiplier or replacement horn when voltage is over 2500 volts. To maximize electron multiplier life: •...
  • Page 145: Ms Test And Performance Samples

    GC/MS Systems MS standards MS Test and Performance Samples Tuning Samples Performance Verification Samples Checkout Samples EI Tune CI Tune Negative Positive HighMass Semi-Volatile Volatile Mode CI Mode CI 5975 PFTBA PFDTD Benzophenone PFHT DFTPP 1 pg/µL 100 pg/µL 100 pg/µL 5973 PFTBA PFDTD...
  • Page 146 Calibration The calibration valve is an electromechanical valve with a vial for tuning compounds. Perfluorotributylamine (PFTBA) is the most commonly used tuning compound. It is required for automatic tuning of the MSD in EI mode. The tuning compound is usually a liquid but can be a volatile or semi-volatile solid.
  • Page 147 The Agilent J&W GC Column Selection Guide Your single source for the highest-performing GC columns, plus expert advice to help you achieve reliable results, faster. From low-bleed columns for MS… to premium polysiloxane columns… to specialty columns for pesticide, petroleum, or life science applications… our GC Column Selection Guide has everything you need to analyze your most challenging compounds.
  • Page 148 How to contact Agilent For the latest information on the complete line of Agilent Technologies columns and supplies: • Visit our Web site: www.agilent.com/chem • Contact your local Agilent sales office • Contact your local Agilent Authorized Distributor Information, descriptions, and specifications in this publication are subject to change without notice.

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