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...
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…...
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.
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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.
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. •...
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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).
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.
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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).
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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...
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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.
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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.
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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. •...
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.
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.
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.
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.
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.
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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. •...
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.
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.
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.
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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.
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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...
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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...
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: •...
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.
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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...
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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 •...
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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.
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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.
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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.
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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...
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...
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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 –...
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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...
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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.
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.
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...
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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...
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.
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. •...
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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. •...
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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...
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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...
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.
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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. •...
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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...
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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...
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. •...
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.
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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. •...
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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.
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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...
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.
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.
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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: •...
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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...
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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 <...
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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. •...
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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...
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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.
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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...
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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...
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: •...
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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...
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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.
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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.
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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...
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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...
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.
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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.
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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...
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.
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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...
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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...
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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...
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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...
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… •...
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.
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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. •...
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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.
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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...
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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.
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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...
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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...
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.
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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.
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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...
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.
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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.
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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.
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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.
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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.
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.
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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.
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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.
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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.
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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 •...
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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.
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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...
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.
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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.
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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.
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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.
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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.
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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...
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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...
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.
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: •...
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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...
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.
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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.
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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 •...
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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.
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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.
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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...
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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.
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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.
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.
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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. •...
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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.
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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...
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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.
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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...
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.
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.
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.
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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. •...
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.
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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 •...
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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.
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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.
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: •...
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...
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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.
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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.
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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.