Maintaining your Agilent GC and GC/MS Systems Maximize your efficiency. Minimize your downtime. Get the results you need.

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1 Operate your lab at peak performance Troubleshoot difficult problems Select the right Agilent supplies Plan preventative maintenance Maintaining your Agilent GC and GC/MS Systems Maximize your efficiency. Minimize your downtime. Get the results you need.

2 Our GC and GC/MS Maintenance Guide puts nearly 40 years of Agilent knowledge at your fingertips. At Agilent Technologies, we understand that many of today s labs face the challenge of operating with a reduced staff. That s why we re committed to bringing you the world s best GC and GC/MS systems plus the critical information you need to keep them running properly. In this newly updated Maintenance Guide, we share everything from essential service schedules to invaluable troubleshooting tips and problem-solving methods. We ve even included easy guides to help you order Agilent parts and supplies which have 40 years of high quality and technical experience built right in. So you can keep your downtime to a minimum, and get the results you need. Maintaining Your Agilent GC and GC/MS Systems Maximize your efficiency. Minimize your downtime. Get the results you need. TIPS AND TOOLS This icon denotes a helpful hint that provides useful information you can find throughout this guide and online at VIDEO This icon denotes a video that is available to view on our website. Just visit to view how-to videos and obtain more information. 2 Gas Management 3 Gas Types 4 Contaminants & Purities 4 Gas Purification Systems 12 Regulators 13 Tubing 14 Leak Detection 15 Flow Rates 18 Sample Introduction Consumables & GC Inlets Sample Introduction 19 Vials 21 Syringes Inlet Types 26 Packed-Column 28 Split/Splitless 31 Cool On-Column 34 Programmed Temperature Vaporizer PTV Inlet Accessories 36 Septa 42 Ferrules 47 Liners 52 Flip Top Inlet Sealing System 54 Parts & Supplies 56 Columns 57 Column Maintenance 57 Column Selection 58 Column Installation/Setup & Conditioning 59 Column Performance 63 Columns Types and Characteristics 68 Detectors 69 Flame Ionization Detector (FID) Thermal Conductivity Detector (TCD) 72 Electron-Capture Detector (ECD) 74 Thermal Conductivity Detector (TCD) 76 Flame Photometric Detector (FPD) 78 Nitrogen-Phosphorus Detector (NPD) 82 GC/MS Systems 83 Maintaining Mass Selective Detectors (MSDs) 87 Mass Spectrometer Symptoms 88 Ion Source 93 Vacuum Systems & Pumps 96 Electron Multipliers & Replacement Horn 97 Maintaining the MS Engine 99 Ion Source Parts & Supplies 100 General GC/MS Supplies 101 Test & Performance Samples 104 Services & Support 105 Expert Service, Training & Support Don t Miss GC Maintenance Schedule (inside back cover)

3 Gas Management The use of quality carrier gases is essential for consistent and accurate GC analyses. Proper gas management is key to achieving this goal. Agilent provides a diverse line of high quality gas management products gas purifiers, regulators, leak detectors and flowmeters all designed to prevent column damage, improve detector life, and improve the quality and consistency of your GC separations. This section explains how common contaminants like oxygen, moisture and hydrocarbons can damage your GC column, and helps you understand how to prevent it. Also, look for practical information about regulators, the importance of clean GC-tubing, and minimizing the likelihood of GC system contamination. Gas management is more than just selecting the highest quality carrier gas available. It s about selecting the appropriate carrier gas for your needs, and taking steps to prevent system contamination. Agilent understands this and provides products that make gas management easy to implement in your lab. Kenji Yamaguchi Applications Support Manager CATALOG For a complete selection of gas management supplies, see Agilent s Essential Chromatography Catalog. Or, visit our online catalog at

4 GAS MANAGEMENT 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. Carrier gas purity is also critical to prevent degradation of chromatographic hardware. Contaminants in carrier gases can have a significant effect on column life and subsequent analyte detection. Harmful effects of impure gases include contaminant peaks and elevated column bleed, along with column and/or detector damage. The following sections describe the gases and purities that are necessary for gas chromatography carrier gases, as well as other support gases. Support Gases Support gases may be specific for detectors or for applications. These gases include fuels, oxidants, coolants, detector gases, and pneumatic gases. The degree of purity required for support gases is dependent on how that gas is being used, and whether or not it will make contact with the sample. Coolant gases (carbon dioxide) and pneumatic gases (air or nitrogen) generally do not come in contact with the sample or detector. Therefore, these non-contact gases do not have to be the highest purity available. Fuels, oxidants and detector gases, in most cases, do come in contact with the sample and detector, and require higher purity gases. Unfortunately, gas nomenclature as it relates to purity is not consistent across specialty gas suppliers. It is important to recognize the impurities in your gas supplier s products, and to utilize the appropriate Agilent gas purification products (see next section). Carrier and Support Gases Sample Gas Type Function Contact Purity Required* Air Pneumatics No Low Grade Nitrogen Pneumatics No Low Grade Limit of Detection required: Trace (0-1 ppm) ppm 1000 ppm-1% 1%-100% Hydrogen Carrier or fuel gas for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero Hydrogen/Helium Mix Fuel gas for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero Methane/Argon Carrier or make-up or Nitrogen for ECD Yes Research Research Research N/A Air Oxidant for detector No Ultra-Pure Ultra-Pure UHP/Zero UHP/Zero Nitrogen, Helium, Carrier or or Argon make-up gas Yes Research Ultra-Pure Ultra-Pure UHP/Zero *Purities of gases depend upon the type of detector that is used. Use this table as a general guide only and refer to your detector manual for specific gas purities that are needed. Low Grade = Specialty or industrial gases ( %) UHP/Zero Grade (99.999%) Ultra-Pure Grade ( %) Research Grade ( %)

5 GAS MANAGEMENT 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. Analytical gases are available in many grades of quality, from high purity (99.995%) to chromatography grade purity ( %). The higher the purity, the higher the cost. Identifying Contaminants To make a proper purity choice it is helpful to understand the contaminants most common in GC gases and how they can affect your analysis. Common contaminants are: Hydrocarbons and Halocarbons decrease detector sensitivity by increasing detector background noise can also cause baseline drift or wander, contaminant peaks, and noisy or high offsets of baselines Moisture can be introduced by improper handling and/or installation of plumbing a common cause of column stationary phase degradation can damage instrument Oxygen most common contaminant a common cause of column stationary phase and inlet liner degradation can cause decomposition of labile analytes opportunity for introduction at every fitting present in the gas line or during use of gas permeable tubing. In some cases it may be difficult to determine which contaminant presents the biggest problem in a given analysis. If unsure, a call to your gas supplier may be helpful. Once the problem contaminants have been identified and a general contaminant level is determined, the next step is to choose a gas purity level that comes closest to these requirements. Keep in mind that higher grades of gas generally cost more. The greatest cost savings can be achieved by using the lowest purity gas which will neither interfere with the analysis nor damage your equipment. Using the proper gas purification equipment to remove common contaminants and achieve the desired purity level is essential. Gas Purification Systems Agilent brings the highest performance and largest variety of gas purifiers (traps) to gas chromatographers. Purifiers are available in a variety of sizes and configurations to remove common contaminants like oxygen, moisture, and hydrocarbons. In-line gas purifiers, including refillable, indicating, S-shaped, and metal body types, are made to remove specific contaminants. Agilent also offers gas purification systems with removable cartridges. These systems provide the ability to design the right combination of filters needed for your application to achieve the proper gas purity. The illustration on the next page shows the most common gas purification configurations used in gas chromatography. Regardless of which purification system is employed, proper installation and maintenance is required to achieve optimal performance from the purification system(s). A purifier that is not maintained will eventually expire and become ineffective, or worse, a source of contamination. Other Considerations determine desired purity level keep number of fittings in gas line to a minimum install purifiers in a convenient location close to the GC purifier log books are useful for determining maintenance schedule use indicating traps closest to the GC so you can determine when to change the traps that are upstream

6 GAS MANAGEMENT Carrier Gas Purification Gas supply -OR- In-Line Gas Purifiers Gas Purification System Key: 1 = Moisture Trap 2 = Hydrocarbon Trap 3 = Oxygen Trap 4 = Indicating Oxygen Trap 5 = Gas Purification System 6 = Combination Trap for moisture, oxygen, and hydrocarbon removal Detector Gas Purification FID make-up, air, and H 2 Gas supply -OR- Vent Combination Trap ECD make-up ELCD reaction gas Gas supply = cylinder, in-house line, or gas generator MS carrier gas Regulator = Brass dual stage regulator Gas Traps The purpose of gas traps is to remove detrimental impurities from the carrier and detector gases. Moisture (water), oxygen and hydrocarbon traps are the most common traps used with GC systems. A few 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. Little enhancement by traps to the GC system is obtained by traps when using very high purity gases (e.g., ultra-high purity or similar grades) while obvious improvement is obtained with lower grades of gas. Constant exposure of capillary columns to oxygen and moisture, especially at high temperatures, results in rapid and severe column damage. The use of oxygen and moisture traps for the carrier gas may extend column life and protect the instrument. Traps may provide some protection if there is a leak at or around the gas cylinder. Any moisture or oxygen introduced into the gas stream due to the leak will be removed by the trap until it expires. This creates an opportunity to detect and fix the leak before column or instrument damage occurs. TIPS AND TOOLS Tap Agilent s GC knowledge over the phone, online, in the classroom, even at your site. See pages for more information about our services and support

7 GAS MANAGEMENT Moisture (Water) Traps There are several different adsorbents and indicating materials used in moisture traps. Moisture traps can be easily refilled. Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap making refilling a more economical (and less wasteful) option. 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 protective, plastic shrink wrap or a high impact plastic shield (outer trap body). Glass and plastic bodied traps are usually pressure tested at 150 psi, thus they are safe for use at the typical pressures required by the GC. Refillable Glass Moisture Trap Moisture Removal Traps Size H 2 O Removal Maximum Effluent H 2 O 1/8 in. 1/4 in. Description (cc) Capacity (g) Concentration (ppb) Part No. Part No. Price Molecular Sieve 13X and Indicating 4Å Economy, with plastic Lexan body (other packings available, see Agilent catalog) Refillable Moisture Trap MT200-2 MT200-4 $104 Adsorbent Refill (1 pint) for MT Series MSR-1 MSR-1 $ 55 Glass Indicating Moisture Traps (larger size is available, see Agilent catalog) Glass Indicating Moisture Traps GMT-2-HP GMT-4-HP $119 Molecular Sieve Refill for GMT Series 250 GMSR GMSR $ 63 Moisture Removal S-Trap can be reconditioned in the GC oven Moisture S-Trap preconditioned $226 Big Moisture Traps for the Ultimate Moisture Capacity Big Moisture Trap 750 BMT-2 BMT-4 $235 Refill for BMT Series (2 refills) BMSR-1 BMSR-1 $ 58 Refillable Moisture Trap Moisture S-Trap Big Moisture Trap

8 GAS MANAGEMENT Oxygen Traps Indicating Oxygen Trap Big Oxygen Trap Oxygen Traps Oxygen traps usually include a metalcontaining inert support reagent. Most oxygen traps reduce the oxygen concentration to below ppb. The capacity of a standard oxygen trap is approximately 30mg of oxygen per 100cc of trap volume. Oxygen traps can also remove some small organic and sulfur compounds from gas streams, but this is not their primary application. Metal (usually aluminum) trap bodies are recommended for GC analyses. Some 1/8 in. 1/4 in. Description Size (cc) Part No. Part No. Price Indicating Oxygen Traps glass body with plastic safety shield Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP $143 Big Oxygen Traps non-indicating, for the Ultimate Oxygen Capacity (smaller size available, see Agilent catalog) plastics are permeable to air and contain contaminants that can degrade gas quality. In addition, many of the metal bodied oxygen traps can withstand high pressures (up to 2000 psi). Some oxygen traps also remove moisture from the gas stream without affecting the oxygen removal capability. Indicating oxygen traps change color when oxygen is present in the gas at harmful levels. Indicating traps are not intended to be the primary oxygen removal trap, but should be used in conjunction with a high capacity non-indicating oxygen trap. They are installed after the high capacity oxygen trap in the gas line to indicate when the high capacity trap has expired and needs to be changed. Expired oxygen traps need to be immediately changed since they can contaminate the gas, in addition to failing to remove oxygen. Big Oxygen Trap 750 BOT-2 BOT-4 $235 Hydrocarbon Traps 1/8 in. 1/4 in. Description Size (cc) Part No. Part No. Price Hydrocarbon Traps General Purpose Refillable Hydrocarbon Trap 200 HT200-2 HT200-4 $106 Adsorbent Refill (1 pint, 2 refills) ACR ACR $ 63 Big Hydrocarbon Traps for the Ultimate Hydrocarbon Capacity 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 organic solvents from the gas stream, including the typical solvents used in nearly every lab. Hydrocarbon-moisture combination traps are also available which remove water in Big Hydrocarbon Trap 750 BHT-2 BHT-4 $235 Refill for Big Hydrocarbon Trap (2 refills) BACR BACR $ 52 Hydrocarbon Removal S-Trap can be reconditioned in the GC oven Hydrocarbon S-Trap $232 Capillary Grade Hydrocarbon Traps for crucial capillary applications Capillary Grade Hydrocarbon Trap 100 HT3-2 HT3-4 $ 98 Adsorbent Refill (1 pint, 3 refills) ACR ACR $ 63 Hydrocarbon Trap

9 GAS MANAGEMENT Hydrocarbon Traps continued addition to organics as described in the next section. Capillary grade hydrocarbon traps are purged with ultra-high purity helium and packed with a very efficient activated carbon material. Metal trap bodies are used to prevent any contaminants in plastic trap bodies from contaminating the carbon adsorbent. Most hydrocarbon traps can be refilled by the end user. Big Hydrocarbon Trap Hydrocarbon S-Trap 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 Leak-free, one-piece design to eliminate potential leaks from using multiple traps Efficient design which prevents channeling and promotes efficient scrubbing The ultimate in purification with a single trap (Big Universal Trap) 1/8 in. 1/4 in. Description Size (cc) Part No. Part No. Price Oxygen/Moisture Traps Agilent OT3 Trap 100 OT3-2 OT3-4 $104 Hydrocarbon/Moisture Traps Agilent OT3 Trap Refillable Hydro-Moisture Trap 200 HMT200-2 HMT200-4 $ 98 Refill for Hydrocarbon/ Moisture Trap (1 pint, 2 refills) HCRMS HCRMS $ 63 Big Universal Traps for the Ultimate in Gas Purification, removes oxygen, moisture, hydrocarbons, CO, and CO 2 Big Universal Trap Big Universal Trap Helium purged (also recommended for GC Mass Spec) 750 RMSH-2 RMSH-4 $261 Big Universal Trap Hydrogen purged 750 RMSHY-2 RMSHY-4 $261 Big Universal Trap Nitrogen purged 750 RMSN-2 RMSN-4 $261 Big Mounting Clip for mounting Big Traps 2/pk UMC-5-2 UMC-5-2 $ 21 Hydrocarbon Moisture Trap

10 GAS MANAGEMENT Three Cartridge High Capacity Gas Purification System High Capacity Gas Purification System Three Cartridge System Agilent s highest capacity and most economical gas purification system. Provides low-cost gas contaminant removal for up to 18 cylinders of carrier gas. Includes a manifold with cartridge mounts and three replaceable cartridges: one moisture/hydrocarbon cartridge; one oxygen cartridge; and one oxygen indicating cartridge. Consists of a permanent all-welded stainless steel manifold to minimize the potential for leaks. Suitable for bench or wall mounting. Single-Cartridge System Contains a triple-combination cartridge that offers the same highly efficient contaminant removal properties from eight cylinders of carrier gas but without the visual indicator. Other cartridges are also available for detector gas supplies and as individual filters for specialized requirements. High Capacity Gas Purification System Description Part No. Price Three Cartridge System Includes manifold for wall or bench mount and 3 cartridges (H 2 O/hydrocarbon, oxygen, and indicating O 2 ) With 1/8 in. fittings $612 With 1/4 in. fittings $567 Replacement Cartridge Kit Includes all three cartridges for $393 above system Single Cartridge System Includes single cartridge manifold brackets for wall or bench mount, and a triple combination cartridge (H 2 O/hydrocarbon, and O 2 ) With 1/8 in. fittings $239 With 1/4 in. fittings $255 Triple combination replacement cartridge for single cartridge system $

11 GAS MANAGEMENT Quick Change Plus (QC+) Point of Operation Panel The QC+ Point of Operation Panel contains purifier cartridges that can be quickly changed. The cartridges are removed from the panel without interruption of gas flow to the system, drastically minimizing costly instrument downtime. Filter cartridges are of all metal or glass construction, eliminating infusion and resultant signal noise associated with filters constructed from plastics. Cartridges are quickly installed via a simple knurled retaining nut, with no wrenches needed. As many as four cartridges can be replaced in a matter of seconds, and because there is low dead volume, a minimal amount of gas system purge is required after installation. RQC-P Quick Change Plus (QC+) Point of Operation Panels Description Fitting (in.) Part No. Price 4-Head O 2, indicating O 2, HC, H 2 O 1/8 RQC-P $1604 Replacement Cartridges Description Part No. Price High capacity oxygen GC-1 $ 64 High capacity moisture GC-2 $ 64 Indicating moisture GC-2-I $106 Hydrocarbon GC-3 $ 64 Indicating oxygen GC-4 $155 EASY ONLINE ORDERING From oxygen traps to purification systems, you can find all your gas management supplies all in one place. Just visit

12 GAS MANAGEMENT Super-Clean Gas Filter System Super-Clean gas filter systems are designed to provide the utmost in convenience and contamination reduction. The system is tested for leak-tightness and the glass and metal construction of the cartridges eliminates diffusion of contaminants into the gas stream. During cartridge replacement, check valves and close off the system to the atmosphere, further minimizing the entry of contaminants. Super-Clean Gas Purification Systems Available with 1/8" fittings only Description Part No. Price Carrier Gas Purification System: Single position system perfect for GC/MS, ECD and NPD detectors. Includes the triple filter cartridge $ 398 Super-Clean Gas Purification System: For your most demanding GC application, includes four position baseplate manifold with four filter cartridges: oxygen, moisture (both with indicator), and two hydrocarbon cartridges $1291 Replacement Filter Cartridges Triple Filter Cartridge: A single carrier gas filter now with hydrocarbon, moisture, and oxygen trapping capability. Includes moisture and oxygen indicator so you know exactly when to replace the cartridge $ 186 Filter cartridge bundle of 4 (oxygen, moisture, and 2 hydrocarbon) $ 530 Description Part No. Price Universal/external split vent trap with 3 cartridges (1/8 in. Swagelok fitting) RDT-1020 $ 94 Replacement cartridges (3/pk) RDT-1023 $ 45 Split Vent Trap and Cartridges 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. The traps are also easy to change and come with three packs of replacement cartridges each. Replace approximately every six months

13 GAS MANAGEMENT Regulators Pressure regulators are an integral component in any gas handling system. Their function is to reduce the pressure from a high pressure source, such as a cylinder, to a suitable use pressure. Although regulators are very good at controlling pressure, they do not control flow. They have a maximum flow rate which is dictated by the design. Basically, the flow is determined by the pressure drop across the regulator. Types of Regulators There are primarily two types of regulators: single stage and dual (or two) stage. The difference is that a dual stage regulator is actually two regulators connected in a series. Dual stage regulators provide more precise and consistent pressure control than single stage regulators. The reason is that in a single stage regulator, as the gas cylinder empties and the inlet pressure to the regulator decreases (inlet decay), the pressure on the diaphragm is reduced. Without proper adjustment, the outlet pressure might slowly rise. A dual stage regulator overcomes this problem by connecting two regulators together. The first stage regulates the pressure to the second stage, thus creating a constant pressure and allowing minimal inlet decay. Agilent recommends using two-stage regulators with our GC Systems to provide the proper pressure control for optimal use. Regulator Materials Regulators are usually constructed of brass or stainless steel. The choice of material follows the same guidelines as the choice of tubing. Generally, it is not recommended that the materials be interchanged. If stainless steel tubing were chosen due to purity considerations, then a stainless steel regulator should be chosen for the same reasons. Steel regulators are more expensive, which is why Agilent offers brass regulators for less demanding applications. No matter which material is chosen for the regulator body, be sure to specify one with stainless steel diaphragms for critical applications such as use on carrier, fuel or detector gases. Agilent recommends using our economical brass body, dual stainless Brass Body Regulator 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. When ordering a regulator, be sure to specify the proper connections. In the US, most gas manufacturers follow CGA connection guidelines. In Europe, there are a number of organizations designating cylinder connections that are specific to individual countries. It is best to contact your local supplier for the proper connection designation. Description Part No. Price Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)* CGA 346, 125 psig max (8.6 bar), Air $275 CGA 350, 125 psig max (8.6 bar), H 2, Ar/Me $275 CGA 540, 125 psig max (8.6 bar), O $275 CGA 580, 125 psig max (8.6 bar), He, Ar, N $275 CGA 590, 125 psig max (8.6 bar), Air $275 *For 1/4 in. tubing, purchase a 1/4 in. adapter listed below Regulator Outlet Adapters Female NPT to Swagelok-style 1/4 in. to 1/8 in. brass (included with brass regulators) $ 14 1/4 in. to 1/4 in. brass** $ 15 ** Required for plumbing 1/4 in. tubing to regulators above TIPS AND TOOLS Always depressurize a regulator before closing by adjusting knob and removing the regulator from the cylinder

14 GAS MANAGEMENT Tubing Spectra-Link Tubing Connecting System on a two-stage regulator Determining Tubing Length Tubing Precleaned When constructing or maintaining a gas delivery system for GC, choosing the proper tubing material is very important and will help to eliminate potential problems and improve the overall quality of the gas system. Although there are many common tubing materials available, some pose safety or cleanliness problems. Non-metallic types of tubing such as polyethylene and Teflon are not recommended for GC applications due to their gas permeability and difficulty in cleaning. This type of tubing can be used for non-critical applications, such Parameters: 2000sccm (4.2 scfh); Temperature: 70 F; Pressure 30 psig Tubing Type Diameter Recommended Pressure Drop (inches) Max. Length (feet) (psig) Copper 1/8* 50 2 Copper 1/4* *Recommended when multiple instruments are connected to the same source Description Part No. Price as pressurizing pneumatic lines; however, be aware of its pressure limitations. In view of these problems, the list of appropriate tubing materials has been narrowed down to two: copper and stainless steel. 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 crucial applications that require very high purity, or where building codes mandate its use. Cleaning Tubing Before any tubing is placed into service, or if it becomes contaminated with use, it is essential that it be properly cleaned. Unclean or improperly cleaned tubing can lead to contamination of the system with disastrous results. Cleaning tubing requires the use of suitable detergents and solvents along with nitrogen and a purgeable oven for drying. This may be done easily for small lengths of tubing, but in larger systems the cleaning procedure sometimes becomes unwieldy, leaving behind a large quantity of solvent requiring proper disposal. Fortunately, Agilent provides clean, high quality GC grade tubing for large systems as an economical alternative. Copper tubing, 1/8 in., 50 ft $56 Copper tubing, 1/8 in., 12 ft $28 MAINTENANCE MINDER Always replace cylinders at around 500 psi, to reduce the risk of having a drastic pressure drop right in the middle of an important analysis

15 GAS MANAGEMENT Spectra-Link is No Ordinary Flexible Tubing! Stainless Steel: no outgassing or permeation through polymeric materials Quick Connection: prevents air from entering gas lines during tank changeover Tested: each system has leak rates lower than 1x10-5 cc/sec Description Part No. Price Spectra-Link with 1/8 in. fittings and 36 in. SS tubing SL-8 $496 Spectra-Link with 1/4 in. fittings and 36 in. SS tubing SL-4 $496 Cylinder Bracket Description Part No. Price Cylinder wall bracket with strap and chain $ 60 (cylinder size up to 14 in., 35 cm) Cylinder Wall Bracket Leak Detection Leaks allow oxygen and other contaminants to enter the gas stream. Therefore, GC instrument maintenance should include checking fittings and connections with a gas leak detector. Agilent s Gas Leak Detector enables quick and easy detection and measurement of gas leaks for 12 common gases. Based on a dual cell micro volume thermal conductivity system, this unit provides very high sensitivity and eliminates contamination caused by soap solution methods. Gas Leak Detector Kit Description Part No. Price Leak detector includes probe, extended flexible probe, range extension nozzle, probe clip and template, cable, AC power adapter/battery charger, battery, user manual, cleaning wipe, and carrying case (available in 115 V or 220 V). Gas leak detector, 115 V $1915 Gas leak detector, 220 V $1915 Gas Leak Detector

16 GAS MANAGEMENT Flow Rates Setting and maintaining GC flow rates greatly affect the instrument accuracy and sensitivity. During maintenance, verify carrier and support gas flows with the proper flowmeter. Choosing a flowmeter for your application depends upon measurement speed, ease of use, accuracy, and flow rate range. Selecting a Flowmeter Agilent manufactures the largest selection of volumetric and mass flowmeters for chromatography. We have developed flowmeters for measuring capillary column flows, calibrating air pumps and flow controllers, and verifying instrument gas flows. All flowmeters are calibrated to NIST-traceable standards. FlowTracker Flowmeters volumetric, multimode flowmeters Description Part No. Price FlowTracker 1000 Flowmeter $ 816 FlowTracker 2000 FlowTracker 2000 Flowmeter and Leak Detector $1143 FlowTracker Universal AC Adapter (optional, not supplied with FlowTracker units) $ 43 ADM 1000 ADM 2000 ADM 1000 features include: 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 Measures flow rates from 0.5 to 1000 ml/min Split ratios compare the ratio from one gas measurement to another (i.e., injection port split ratios) ADM 2000 In addition to the features of the ADM 1000, the ADM 2000 includes: Mass flow measurements measure flow rate, independent of atmospheric pressure and temperature (calculated) Data output through RS-232 port 9V battery and AC power adapter (120 or 220 VAC)

17 GAS MANAGEMENT Flowmeters Flow Rate (ml/min) Gases Accuracy Power RS-232 Data Description Low High Measured (%) Supply Output Part No. Price ADM Flowmeters volumetric, measures all gases* ADM All ± 3 9V Battery None $620 ADM All ± 3 Battery or 120 VAC Yes U $725 ADM2000E All ± 3 Battery or 220 VAC Yes E $725 Electronic Mass Flowmeter dedicated mass flowmeter, very accurate for specific gases* Veri-Flow 500 He, H 2, Ar/CH 4 Rechargeable Battery (110 V) N 2, Air ± 3 or 110 VAC Yes HVF-500 $681 Veri-Flow 500 He, H 2, Ar/CH 4 Rechargeable Battery (220 V) N 2, Air ± 3 or 220 VAC Yes HVF $681 Optiflow Flowmeters Gas Flowmeters versatile volumetric flowmeters** Optiflow All +/- 3 9V Battery None HFM-420 $573 Optiflow All +/- 3 9V Battery None HFM-570 $573 Optiflow ,000 All +/- 2 9V Battery None HFM-650 $677 *non-corrosive gases only **non-corrosive and mildly corrosive gases only Veri-Flow 500 Optiflow 420 TIPS AND TOOLS Tap Agilent s GC knowledge over the phone, online, in the classroom, even at your site. See pages for more information about our services and support

18 You asked we listened! Announcing the launch of our new Life Sciences and Chemical Analysis website. Based on customer feedback, we ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services. The new site features: A coherent page design that automatically detects screen resolution and optimizes the page size for less scrolling. An expanded navigation that includes links to product literature, technical support, education, events, and news. A newly designed online store with fast access to pricing, order status, quotes, and local sales information. Direct links to the services, parts, and consumables that keep your instruments running in top condition. To experience these exciting new changes for yourself, go to

19 Gas Sample Management Introduction Consumables & GC Inlets The use of quality carrier gases is essential for consistent and accurate GC analyses. Proper Agilent gas offers management a wide range is key of high-quality to achieving this sample goal. vials, Agilent septa, provides syringes, a diverse liners line and of high inlets quality for a broad gas management range of gas-phase products gas purifiers, applications. regulators, Just as leak you detectors depend on our and meticulously flowmeters engineered all designed GC and to prevent GC/MS column instruments, damage, you improve can count detector on Agilent life, and improve consumables. the quality This and section consistency reviews these of your GC critical separations. components. This section Also, look explains for useful how common infofrom contaminants proper syringe like use oxygen, and cleaning moisture and techniques hydrocarbons to a detailed can damage discussion your GC on column, optimized and inlet helps settings. you understand how to prevent it. Also, look for practical information about regulators, the importance of clean GC-tubing, and minimizing the likelihood of GC system contamination. Good sample introduction helps ensure good reproducibility, optimal peak shape, and accurate sample delivery. Agilent s commitment to offering the highest quality supplies means accurate, reliable results. Time after time. Bryan Bente, Ph.D. Technology Development Manager CATALOG For a complete selection of vials, syringes, and inlets, see Agilent s Essential Chromatography Catalog. Or, visit our online catalog at

20 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Sample Introduction 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. Agilent also offers convenience packs with 500 vials and caps in a reusable blue storage box. For small sample sizes, Agilent offers a variety of options. You can use microvolume inserts with the wide opening vials or, for added convenience, use vials with small volume capacity. 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. The airspace in the vial is necessary to avoid forming a vacuum when sample is withdrawn. This could affect reproducibility. Vial Options Glass for general purpose use and for use with acids Silanized for use with samples that bind to glass, and for trace analyses Polypropylene for use with alcohols and aqueous solvents Amber Vials for use with light-sensitive samples Microvolume Inserts for use with very small sample volumes High Recovery Vials for use with limited sample volumes Recommended fill volumes for sample vials 1 ml 50 µl 3.6 mm* *Needle position based on standard sampling depth. 100 µl vial TIPS AND TOOLS Do not inject air into the vials to prevent the vacuum. This often damages the cap seal

21 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 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. Red Rubber/Teflon Routine analysis Moderate resealing Excellent chemical inertness Not recommended for multiple injections or storage of samples Least expensive Silicone/Teflon Excellent resealing Resists coring Good for multiple injections Teflon/Silicone/Teflon Used in trace analysis applications Above average resealing Most resistant to coring Least evaporation Use with large diameter, blunt tip syringe needles Teflon Disc Good for MS and ECD analysis Good for large-volume injections Chemically inert No resealing Single injection No long-term sampling storage Viton Chlorinated solvents Organic acids Limited resealing Not suitable for 32 gauge syringe Determining Your Quantity Needs To determine potential septa ordering quantities, consider: the number of samples run during a day/week if samples are run in small or large batches if samples are run manually or with an autosampler if samples are run overnight, unattended Vials Description Quantity Part No. Price Vials Unattended autosampler runs require a precise fit for uninterrupted operation. Typically, automated sample runs use a higher quality and quantity of vials. 2 ml Crimp top vial convenience pack with silver AI caps with Teflon/Red rubber septa 500/pk $115 2 ml Screw top vial convenience pack with blue screw caps and Teflon/Red rubber septa 500/pk $183 2 ml Snap top vial convenience pack with clear polypropylene snap caps and Teflon/Red rubber septa 500/pk $ µl Insert for wide opening vials 100/pk $ µl Polypropylene flat bottom inserts 500/pk $ µl Glass lined polypropylene vials 100/pk $158 TIPS AND TOOLS Less than 5 µl dead volume, Micro-V vial, clear crimp top 100/pk $ µl reservoir volume, High recovery vial, crimp top 100/pk $

22 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringes Syringe type and design are important for chromatography to ensure reproducible sample injections for consistent results. The Agilent line of syringes include a variety of plunger and needle choices to use with your autosamplers. Agilent syringes are designed: for reproducible sample volume delivery specifically for the Agilent inlet or autosampler to maximize inlet septum lifetime Selecting Syringes 1. Select the syringe type based on the inlet (injection port) you are using and the volume of sample you want to inject. 2. Select a syringe. Refer to your automatic liquid sampler operating documentation for available syringe sizes and corresponding injection volumes. 3. Select the appropriate syringe needle gauge. Needle Gauge Selection Inlet Needle Gauge Column Type Packed, split or splitless (including PTV) 23 gauge or 23/26 gauge tapered any Cool on-column 23/26 gauge tapered or 26 gauge 530 µm Cool on-column 26/32 gauge tapered 320 µm Cool on-column 26/32 gauge tapered 250 µm Needle Tip Needle Shape Sharp tip Cone tip Needle tips Tapered needle TIPS AND TOOLS Use syringe needles with an Agilent dualtaper needle or a conical tip. Sharp-tipped needles tend to tear the inlet septum and cause leaks. Also, a sharp-tipped needle tends to leave residual amounts of sample on the septum as it exits, resulting in a large solvent tail on the chromatogram. For best results, use the Agilent Cone Tip (HP Point Style) with Agilent s Centerguide Septa, page

23 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringe Characteristics and Recommended Uses Syringe Advantage Limitations Recommended Use 5 µl, fitted Most accurate Thinnest plunger, 1 µl injections plunger syringe for 1µL can bend Clean samples injection more easily Routine analysis No hardware Not ideal for higher modification needed for 0.5 µl injection viscosity samples Plunger not replaceable 10 µl, fitted Most economical Most accurate only General purpose plunger Most reliable fitted for 1 µl and larger syringe plunger syringe injections Clean samples Less bending Plunger not Routine analysis Better for high replaceable viscosity samples 10 µl, Replaceable plunger More expensive Dirty samples gas-tight for reduced than fitted plunger Gases and volatile repair cost Not available in samples Less plunger binding 5 µl size Reactive samples than fitted plunger Tight seal between plunger and barrel Replacing On-column Syringe Needles The stainless steel needles used for 250-µm and 320-µm injections must be inserted into a glass syringe barrel. Select the correct size needle for the column you plan to use. To insert a needle into a syringe barrel: 1. Unscrew the syringe barrel cap and remove the spring. 2. Make sure the needle has the Teflon disk. If the syringe barrel does not have the Teflon disk, use the instructions in the syringe box to wrap the needle yourself. 3. Slide the spring and the cap down over the needle. 4. Insert the needle into the syringe barrel. 5. Screw the cap back on the syringe barrel. TIPS AND TOOLS Failure to use an on-column syringe when injecting into an on-column inlet could damage the injector, syringe and column

24 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringe Tips Make sure to input the proper syringe size when setting up the injection section of your data handling device. Rinse syringes and clean their plungers before use to maximize syringe lifetime. Rinse the syringe 5-8 times between injections to minimize sample carryover. Pump sample in and out of the syringe at least 5 times to remove any air bubbles, and for maximum reproducibility and accuracy. A 26-gauge syringe can be used for on-column injections into a 0.53mm id column. Always check that on-column syringe needles fit inside the capillary column before installing the column and syringe in the GC. For on-column injections, always use the proper septum nut and stainless steel insert for the column dimension you are using. Use a septum with a molded through-hole with injections onto 0.32mm and 0.25mm columns. The more polar the solvent, the more likely it is to contain water. Trace amounts of water, especially when combined with water-extractable materials from samples, can accelerate syringe wear dramatically. With these types of samples, use a Teflon tipped syringe plunger. Even better, proactively replace syringes, since plunger bends may be inevitable. Remove a gas-tight plunger from the syringe for long-term storage to keep the Teflon tip leak-free. If a gas-tight plunger does not fit properly, place it in hot water for about 10 minutes then press the tip uniformly on a clean, hard surface and let cool to room temperature. The plunger should reseal correctly to provide 10-25% more injections. To maximize the lifetime of standard plungers, rinse the syringe and wipe the plunger with solvent (isopropanol or acetone) and a lint-free wipe, as specified in the syringe cleaning procedure included with each syringe. NEW! Agilent Gold Standard GC Autosampler Syringes see page 25 VIDEO To view a video on syringe installation, visit

25 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 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. Problem Possible Cause(s) Suggested Action(s) Bent plungers or stuck syringes Particles such as dust, leftover samples, salts, metal, or glass can fill the narrow gap between the plunger shaft and the inside wall of the barrel. If the plunger s movement feels gritty, remove the plunger from the barrel, flush the shaft with solvent, and wipe it dry with a lintfree cloth. Then, carefully insert the plunger back into the barrel. Finally, submerge the tip of the needle into a container of solvent, and cycle the plunger to pull the solvent into and out of the barrel. Never cycle the plunger in a dry syringe. Do not mix & match plungers and barrels. Always clean syringes after use. Bent needles Improper needle alignment. Narrow-gauge needles (26 gauge) bend more easily than larger (23 gauge) needles. Needles tend to bend when inserted into the sample vial not the inlet port. This can be caused by septa that are too tough. If the needle has been slightly bent when mounted in the autosampler or when the syringe is installed into the autosampler then it is more likely to bend further when it pushes through the septa on the sample vial caps. Use only Agilent autosamplers. They are precision-designed to ensure proper alignment with the syringe needle. Use 23 to 26-gauge tapered needles to get the combined benefits of greater septa life and fewer bent needles. Only use Agilent vials and septa. Blocked needles Sample material or contaminants may be trapped inside the needle. The needle may not have been properly cleaned. Remove the plunger and use a second syringe to fill the blocked syringe with solvent. Then, insert the plunger and gently push solvent through needle. Important: Try to use a cleaning agent that is appropriate for the contaminant. Common choices are methanol, methylene chloride, acetonitrile, and acetone. Rust Note: even minor rust can cause the plunger to become stuck in the barrel. During normal use, the shaft rubs against the glass walls of the barrel. This gradually wears away the rust-resistant metal on the shaft s surface. Rusting happens most rapidly when using water or solvents that may contain (or absorb) water. To slow this process, remove the water from the syringe at the end of each day. 1. Rinse the syringe several times with a dry solvent, such as acetone. 2. Remove the syringe from the autosampler, and wipe the plunger dry with a lint-free cloth 3. Let syringe and plunger air dry. Ring around the neck (A dark ring between the top of the barrel and the end of the volume scale.) Skin oils and other organic material. Fine metal and glass particles from the syringe plunger and barrel may be rubbing together. Once this happens, the plunger may bend if used further. Never touch the plunger shaft with your fingers. If build-up appears when water is the solvent: rinse syringe with acetone and wipe the plunger clean at the end of each day. Loose plungers accompanied by syringe leaks and area count reproducibility problems. The syringe is nearing the end of its useful life. Replace the syringe. Note: Plungers normally feel loose when non-polar solvents (like hexane and toluene) are used

26 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Gold Standard GC Autosampler Syringes Description Gauge/Length Quantity Part No. Price Tapered Needle Syringes (use for split/splitless or on-column injections with 0.53 mm id columns) 10 µl Tapered Fixed Needle 23-26s/42 6/pk $198 5 µl Tapered Fixed Needle 23-26s/42 6/pk $303 Straight Needle Syringes (use with Merlin Microseal) 10 µl Straight Fixed Needle 23/42 6/pk $191 5 µl Straight Fixed Needle 23/42 6/pk $292 GC Automatic Liquid Sampler Supplies Description Unit Part No. Price Miscellaneous Autosampler Supplies 4 ml Clear screw top wash vials with screw caps (no Septa) 144/pk $ 64 Septa for 4 ml vial 144/pk $ 21 Diffusion caps for 4 ml vials 12/pk $ 19 4 ml wash vial with fill marking, caps 25/pk $ 26 Screw for mounting syringe $ 13 Quadrant kit (4 tray sections) $ /83 Basic Supply Kit contains: 10 ml syringes (6/ea), 23/26 gauge needles, 4 ml vials with diffusion caps (144/pk), 2 ml automatic sampler vials with screw caps (1,000/pk), GC septa (25/pk), Vial racks (5/pk) $755 Gold Standard GC ALS Syringe Features Lot Numbers ensure certified performance to all specifications Gold protective cap prevents chipping of the glass syringe barrel as it contacts the septum retainer nut Black ink and gold illuminating backdrop for easier viewing of the volume scale Individually sealed packaging for contaminant-free use

27 SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Packed-Column Inlets Packed-column direct inlets are very popular. Packed-column analysis is frequently done when high efficiency separations are not needed or when gases are analyzed by gas-solid chromatography. Packed-column 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. Packed-Column Inlet Procedures/Practices Parameter Selection/Setting Rationale Inlet temperature BP of solvent +50 C Ensures flash vaporization BP of major solute(s) Use for neat samples Insert type 1/8-inch stainless steel Use for ss column only 1/4-inch stainless steel Inserts permit connection of columns up to 1/4-inch od. Liner Glass Use to lower activity (replaceable) Initial column temperature programming Sharpens peaks and temperature reduces run time Column type 1/8-inch packed stainless Will not break 1/4-inch packed glass Better for polar or labile compounds Carrier gas flow ml/min Use with N 2 carrier gas ml/min Use with He or H 2 carrier gas Troubleshooting Most problems with packed-column inlets involve sample decomposition, flashback, or leaks. Decomposition Since packed-column inlets are active, especially if glass liners are not used, polar sample components will often tail or degrade in the inlet. Sample decomposition caused by the inlet is easily diagnosed; the decomposition products will have peaks at the same retention times as standards for the decomposition product. When inlet-caused decomposition is suspected, try intracolumn direct injection, deactivated glass liners, or lower inlet temperatures, and remove any column packing in the inlet zone. The inherent activity of packed-column inlets is somewhat mediated by the fact that they usually have low internal volume. When this is coupled with the relatively fast flow rates used with packed columns, the residence time of sample in the inlet is short and decomposition is reduced in comparison to the decomposition that occurs with some capillary inlets (for example, splitless inlets). Flashback The negative side of low inlet volume, however, means that excessively large sample injections will easily exceed the capacity of the liner and will flash back into gas supply lines and onto the septum. This can cause several maladies, including ghost peaks, sample losses, irreproducible peak areas, and decomposition. Leaks Since packed-column inlets are usually flow-controlled, septum and column leaks will have a direct impact on retention times and peak areas. Sample can be lost through the leak holes, and air can diffuse back into the inlet to cause column degradation. Change the septum on a regular basis and check column connections at the first stage of problems. To prevent stationary phase decomposition, make sure that the oven and inlet are at room temperature when not in use and when changing the septum

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