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Maintaining your Agilent GC and GC/MS Systems
Maximize your efficiency. Minimize your downtime. Get the results you need.
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.
2 3 4 4 12 13 14 15 Gas Management Gas Types Contaminants & Purities Gas Purification Systems Regulators Tubing Leak Detection Flow Rates 56 57 57 58 Columns Column Maintenance Column Selection 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) 1
18 Sample Introduction Consumables & GC Inlets Sample Introduction 19 Vials 21 Syringes
TIPS AND TOOLS
This icon denotes a helpful hint that provides useful information you can find throughout this guide and online at www.agilent.com/chem.
26 28 31 34
Inlet Types Packed-Column Split/Splitless Cool On-Column Programmed Temperature Vaporizer PTV Inlet Accessories Septa Ferrules Liners Flip Top Inlet Sealing System Parts & Supplies
This icon denotes a video that is available to view on our website. Just visit www.agilent.com/chem/techsupport to view how-to videos and obtain more information.
36 42 47 52 54
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
For a complete selection of gas management supplies, see Agilent’s 2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
Harmful effects of impure gases include contaminant peaks and elevated column bleed.9995%) Research Grade (99. along with column and/or detector damage. coolants. These gases include fuels. 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. these non-contact gases do not have to be the highest purity available. The degree of purity required for support gases is dependent on how that gas is being used.9999%) 3 www.GAS MANAGEMENT Gas Types Carrier Gases The most frequently used carrier gases are helium and hydrogen. Unfortunately. detector gases. and whether or not it will make contact with the sample.999%) Ultra-Pure Grade (99. gas nomenclature as it relates to purity is not consistent across specialty gas suppliers. Support Gases Support gases may be specific for detectors or for applications. Low Grade = Specialty or industrial gases (≤99. although nitrogen and argon can be used. and pneumatic gases. as well as other support gases. oxidants and detector gases. do come in contact with the sample and detector. Use this table as a general guide only and refer to your detector manual for specific gas purities that are needed. Coolant gases (carbon Carrier and Support Gases Gas Type Function Sample Contact Purity Required* Air Nitrogen Pneumatics Pneumatics No No Low Grade Low Grade Limit of Detection required: Trace (0-1 ppm) 1-1000 ppm 1000 ppm-1% 1%-100% Hydrogen Hydrogen/Helium Mix Methane/Argon or Nitrogen Air Nitrogen. Therefore. Fuels.agilent. Contaminants in carrier gases can have a significant effect on column life and subsequent analyte detection. oxidants. dioxide) and pneumatic gases (air or nitrogen) generally do not come in contact with the sample or detector. The following sections describe the gases and purities that are necessary for gas chromatography carrier gases. Carrier gas purity is also critical to prevent degradation of chromatographic hardware. and require higher purity gases. It is important to recognize the impurities in your gas supplier’s products.998%) UHP/Zero Grade (99. in most cases.com/chem . and to utilize the appropriate Agilent gas purification products (see next section). or Argon Carrier or fuel gas for detector Fuel gas for detector Carrier or make-up for ECD Oxidant for detector Carrier or make-up gas Yes Yes Yes No Yes Research Research Research Ultra-Pure Research Ultra-Pure Ultra-Pure Research Ultra-Pure Ultra-Pure Ultra-Pure Ultra-Pure Research UHP/Zero Ultra-Pure UHP/Zero UHP/Zero N/A UHP/Zero UHP/Zero *Purities of gases depend upon the type of detector that is used. Helium.
proper installation and maintenance is required to achieve optimal performance from the purification system(s). moisture. the next step is to choose a gas purity level that comes closest to these requirements. A purifier that is not maintained will eventually expire and become ineffective. The greatest cost savings can be achieved by using the lowest purity gas which will neither interfere with the analysis nor damage your equipment. Regardless of which purification system is employed. including refillable. a source of contamination. indicating. 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 www. the higher the cost. Analytical gases are available in many grades of quality. from high purity (99. and can interfere with chromatographic results.com/chem 4 .GAS MANAGEMENT Contaminants & Purities Contaminants in gases are major contributors to capillary column degradation and detector noise. Moisture • can be introduced by improper handling and/or installation of plumbing • a common cause of column stationary phase degradation • can damage instrument 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. • can also cause baseline drift or wander. Purifiers are available in a variety of sizes and configurations to remove common contaminants like oxygen. Using the proper gas purification equipment to remove common contaminants and achieve the desired purity level is essential. Concentration of these contaminants vary by the grade of gas. a call to your gas supplier may be helpful. These systems provide the ability to design the right combination of filters needed for your application to achieve the proper gas purity. Agilent also offers gas purification systems with removable cartridges. contaminant peaks. S-shaped.agilent. and hydrocarbons.995%) to chromatography grade purity (99. Keep in mind that higher grades of gas generally cost more. or worse. and noisy or high offsets of baselines In some cases it may be difficult to determine which contaminant presents the biggest problem in a given analysis. are made to remove specific contaminants. If unsure. Gas Purification Systems Agilent brings the highest performance and largest variety of gas purifiers (traps) to gas chromatographers.9995+%). Common contaminants are: Hydrocarbons and Halocarbons • decrease detector sensitivity by increasing detector background noise 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. Once the problem contaminants have been identified and a general contaminant level is determined. In-line gas purifiers. The higher the purity. and metal body types. The illustration on the next page shows the most common gas purification configurations used in gas chromatography.
in-house line. See pages 104-115 for more information about our services and support.GAS MANAGEMENT Carrier Gas Purification Key: In-Line Gas Purifiers 1 = Moisture Trap 2 = Hydrocarbon Trap 3 = Oxygen Trap 4 = Indicating Oxygen Trap 5 = Gas Purification System 6 = Combination Trap for moisture. Any moisture or oxygen introduced into the gas stream due to the leak will be removed by the trap until it expires. results in rapid and severe column damage. and H2 -ORGas supply Gas Purification System -ORCombination Trap Gas supply Vent ECD make-up ELCD reaction gas Gas supply = cylinder. Little enhancement by traps to the GC system is obtained by traps when using very high purity gases (e. especially at high temperatures. A few combination traps are available which remove moisture. in the classroom. air. The use of oxygen and moisture traps for the carrier gas may extend column life and protect the instrument. TIPS AND TOOLS Tap Agilent’s GC knowledge over the phone. oxygen and/or organics with a single trap. This creates an opportunity to detect and fix the leak before column or instrument damage occurs.g.com/chem . Moisture (water). oxygen.agilent. oxygen and hydrocarbon traps are the most common traps used with GC systems. even at your site. Traps may provide some protection if there is a leak at or around the gas cylinder. ultra-high purity or similar grades) while obvious improvement is obtained with lower grades of gas. 5 www. or gas generator Regulator = Brass dual stage regulator MS carrier gas Gas Traps The purpose of gas traps is to remove detrimental impurities from the carrier and detector gases. online. and hydrocarbon removal Detector Gas Purification FID make-up. The effectiveness of the traps depends on the initial quality of the gas. Constant exposure of capillary columns to oxygen and moisture..
Refillable Glass Moisture Trap Moisture Removal Traps Size (cc) H2O Removal Capacity (g) Maximum Effluent H2O Concentration (ppb) 1/8 in.com/chem 6 .agilent. Part No. 1/4 in. Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap making refilling a more economical (and less wasteful) option. see Agilent catalog) Refillable Moisture Trap Adsorbent Refill (1 pint) for MT Series 200 36 18 MT200-2 MSR-1 MT200-4 MSR-1 Glass Indicating Moisture Traps (larger size is available. Indicating moisture traps are available in plastic and glass bodies. Part No. plastic shrink wrap or a high impact plastic shield (outer trap body).3 6 GMT-2-HP GMSR GMT-4-HP GMSR Moisture Removal S-Trap – can be reconditioned in the GC oven Moisture S-Trap – preconditioned Big Moisture Traps – for the Ultimate Moisture Capacity 5060-9084 Big Moisture Trap Refill for BMT Series (2 refills) 750 BMT-2 BMSR-1 BMT-4 BMSR-1 Refillable Moisture Trap Moisture S-Trap Big Moisture Trap www. Glass traps are normally encased in a protective.GAS MANAGEMENT Moisture (Water) Traps There are several different adsorbents and indicating materials used in moisture traps. Moisture traps can be easily refilled. with plastic Lexan body (other packings available. Description Molecular Sieve 13X and Indicating 4Å – Economy. thus they are safe for use at the typical pressures required by the GC. see Agilent catalog) Glass Indicating Moisture Traps Molecular Sieve Refill for GMT Series 100 250 16. Glass and plastic bodied traps are usually pressure tested at 150 psi. Glass body traps are used when potential contaminants from plastic trap bodies are a concern.
com/chem . Indicating oxygen traps change color when oxygen is present in the gas at harmful levels. Most oxygen traps reduce the oxygen concentration to below 15-20 ppb. Hydrocarbon traps remove organics. Part No. 2 refills) 200 HT200-2 ACR HT200-4 ACR Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity Big Hydrocarbon Trap Refill for Big Hydrocarbon Trap (2 refills) 750 BHT-2 BACR BHT-4 BACR Hydrocarbon Removal S-Trap – can be reconditioned in the GC oven Hydrocarbon S-Trap 5060-9096 Capillary Grade Hydrocarbon Traps – for crucial capillary applications Capillary Grade Hydrocarbon Trap Adsorbent Refill (1 pint. see Agilent catalog) Big Oxygen Trap 750 BOT-2 BOT-4 Hydrocarbon Traps Description Hydrocarbon Traps – General Purpose Hydrocarbon Traps Size (cc) 1/8 in. Metal (usually aluminum) trap bodies are recommended for GC analyses. from the gas stream. Indicating Oxygen Traps – glass body with plastic safety shield Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP Big Oxygen Traps – non-indicating. 1/4 in. In addition. 3 refills) 100 HT3-2 ACR HT3-4 ACR Hydrocarbon Trap 7 www. Some oxygen traps also remove moisture from the gas stream without affecting the oxygen removal capability. 1/4 in. but this is not their primary application. Indicating Oxygen Trap Big Oxygen Trap Oxygen Traps Description Size (cc) 1/8 in. Part No. Indicating traps are not intended to be the primary oxygen removal trap. The adsorbent is usually activated carbon or an impregnated carbon filter media. in addition to failing to remove oxygen. The capacity of a standard oxygen trap is approximately 30mg of oxygen per 100cc of trap volume. such as hydrocarbons and halocarbons. for the Ultimate Oxygen Capacity (smaller size available. many of the metal bodied oxygen traps can withstand high pressures (up to 2000 psi). Some plastics are permeable to air and contain contaminants that can degrade gas quality. Part No.GAS MANAGEMENT Oxygen Traps Oxygen traps usually include a metalcontaining inert support reagent. 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. including the typical solvents used in nearly every lab. Hydrocarbon-moisture combination traps are also available which remove water in Refillable Hydrocarbon Trap Adsorbent Refill (1 pint. Part No. but should be used in conjunction with a high capacity non-indicating oxygen trap. Oxygen traps can also remove some small organic and sulfur compounds from gas streams. Carbon removes organic solvents from the gas stream. Expired oxygen traps need to be immediately changed since they can contaminate the gas.agilent.
CO.agilent. one-piece design to eliminate potential leaks from using multiple traps 1/8 in. Capillary grade hydrocarbon traps are purged with ultra-high purity helium and packed with a very efficient activated carbon material. Part No. • Efficient design which prevents channeling and promotes efficient scrubbing • The ultimate in purification with a single trap (Big Universal Trap) Description Oxygen/Moisture Traps Size (cc) Agilent OT3 Trap Hydrocarbon/Moisture Traps 100 OT3-2 OT3-4 Agilent OT3 Trap Refillable Hydro-Moisture Trap Refill for Hydrocarbon/ Moisture Trap (1 pint. Big Hydrocarbon Trap Hydrocarbon S-Trap Combination Traps Agilent carries several Combination Traps that provide multiple contaminant removal in a single trap. 1/4 in. 2 refills) 200 HMT200-2 HCRMS HMT200-4 HCRMS Big Universal Trap Big Universal Traps – for the Ultimate in Gas Purification.GAS MANAGEMENT Hydrocarbon Traps continued addition to organics as described in the next section. hydrocarbons. moisture. Part No. removes oxygen. Most hydrocarbon traps can be refilled by the end user. and CO2 Big Universal Trap – Helium purged (also recommended for GC Mass Spec) Big Universal Trap – Hydrogen purged Big Universal Trap – Nitrogen purged Big Mounting Clip for mounting Big Traps 2/pk 750 750 750 RMSH-2 RMSHY-2 RMSN-2 UMC-5-2 RMSH-4 RMSHY-4 RMSN-4 UMC-5-2 Hydrocarbon Moisture Trap www. These traps offer: • Optimized adsorbents for maximum surface area and capacity • Leak-free.com/chem 8 . Metal trap bodies are used to prevent any contaminants in plastic trap bodies from contaminating the carbon adsorbent.
fittings Triple combination replacement cartridge for single cartridge system 5183-4598 5183-4599 5183-4600 5183-1907 5182-9776 5182-9780 Part No. High Capacity Gas Purification System Description Three Cartridge System–Includes manifold for wall or bench mount and 3 cartridges (H2O/hydrocarbon. • Agilent’s highest capacity and most economical gas purification system.com/chem . • Suitable for bench or wall mounting. fittings With 1/4 in. 9 www. one oxygen cartridge. fittings With 1/4 in. fittings Replacement Cartridge Kit– Includes all three cartridges for above system Single Cartridge System–Includes single cartridge manifold brackets for wall or bench mount. and a triple combination cartridge (H2O/hydrocarbon.agilent. and indicating O2) With 1/8 in. and one oxygen indicating cartridge. • Other cartridges are also available for detector gas supplies and as individual filters for specialized requirements. • Provides low-cost gas contaminant removal for up to 18 cylinders of carrier gas.GAS MANAGEMENT High Capacity Gas Purification System Three Cartridge System Three Cartridge High Capacity Gas Purification System 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. oxygen. • Includes a manifold with cartridge mounts and three replaceable cartridges: one moisture/hydrocarbon cartridge. • Consists of a permanent all-welded stainless steel manifold to minimize the potential for leaks. and O2 ) With 1/8 in.
com/chem . O2.agilent. Cartridges are quickly installed via a simple knurled retaining nut.agilent. and because there is low dead volume. Filter cartridges are of all metal or glass construction. Just visit www. As many as four cartridges can be replaced in a matter of seconds.com/chem/4ecatalog 10 www. drastically minimizing costly instrument downtime. you can find all your gas management supplies … all in one place. indicating O2. RQC-P Quick Change Plus (QC+) – Point of Operation Panels Description 4-Head Fitting (in. HC. GC-1 GC-2 GC-2-I GC-3 GC-4 EASY ONLINE ORDERING From oxygen traps to purification systems.GAS MANAGEMENT Quick Change Plus (QC+) Point of Operation Panel The QC+ Point of Operation Panel contains purifier cartridges that can be quickly changed. a minimal amount of gas system purge is required after installation. The cartridges are removed from the panel without interruption of gas flow to the system. H2O 1/8 RQC-P Replacement Cartridges Description High capacity oxygen High capacity moisture Indicating moisture Hydrocarbon Indicating oxygen Part No. eliminating infusion and resultant signal noise associated with filters constructed from plastics.) Part No. with no wrenches needed.
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 Carrier Gas Purification System: Single position system perfect for GC/MS, ECD and NPD detectors. Includes the triple filter cartridge. 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.
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. Filter cartridge bundle of 4 (oxygen, moisture, and 2 hydrocarbon)
Universal/External Split Vent Trap
Description Universal/external split vent trap with 3 cartridges (1/8 in. Swagelok fitting) Replacement cartridges (3/pk) Part No. 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.
Split Vent Trap and Cartridges
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. 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.
Brass Body Regulator
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
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.
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.
Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*
CGA 346, 125 psig max (8.6 bar), Air CGA 350, 125 psig max (8.6 bar), H2, Ar/Me CGA 540, 125 psig max (8.6 bar), O2 CGA 580, 125 psig max (8.6 bar), He, Ar, N2 CGA 590, 125 psig max (8.6 bar), Air
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below Regulator Outlet Adapters – Female NPT to Swagelok-style
5183-4641 5183-4642 5183-4643 5183-4644 5183-4645
TIPS AND TOOLS
1/4 in. to 1/8 in. brass (included with brass regulators) 1/4 in. to 1/4 in. brass**
** Required for plumbing 1/4 in. tubing to regulators above
Always depressurize a regulator before closing by adjusting knob and removing the regulator from the cylinder.
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 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.
Spectra-Link Tubing Connecting System on a two-stage regulator
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.
Determining Tubing Length
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig
Tubing Type Diameter (inches) Recommended Max. Length (feet) Pressure Drop (psig)
*Recommended when multiple instruments are connected to the same source
Description Copper tubing, 1/8 in., 50 ft. Copper tubing, 1/8 in., 12 ft. Part No. 5180-4196 5021-7107
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.
Agilent’s Gas Leak Detector enables quick and easy detection and measurement of gas leaks for 12 common gases. cable. 220 V 5182-9646 5182-9648 Gas Leak Detector www.com/chem 14 .agilent. Therefore.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 Spectra-Link with 1/8 in. 115 V Gas leak detector. battery. 35 cm) Part No. user manual. probe clip and template. extended flexible probe. and carrying case (available in 115 V or 220 V).. AC power adapter/battery charger. SS tubing Part No. this unit provides very high sensitivity and eliminates contamination caused by soap solution methods. 5183-1941 Cylinder Wall Bracket Leak Detection Leaks allow oxygen and other contaminants to enter the gas stream. SL-8 SL-4 Cylinder Bracket Description Cylinder wall bracket with strap and chain (cylinder size up to 14 in. fittings and 36 in. Gas Leak Detector Kit Description Part No. fittings and 36 in. Gas leak detector. Based on a dual cell micro volume thermal conductivity system. range extension nozzle. Leak detector includes probe. GC instrument maintenance should include checking fittings and connections with a gas leak detector. SS tubing Spectra-Link with 1/4 in. cleaning wipe.
and flow rate range. ease of use.. calibrating air pumps and flow controllers. multimode flowmeters Description Part No. -70 to 135ºC for the tubing ADM 1000 ADM 2000 In addition to the features of the ADM 1000.com/chem . injection port split ratios) ADM 2000 15 www. During maintenance.5 to 1000 mL/min • Split ratios–compare the ratio from one gas measurement to another (i. Selecting a Flowmeter Agilent manufactures the largest selection of volumetric and mass flowmeters for chromatography. FlowTracker Flowmeters – volumetric. FlowTracker 1000 Flowmeter FlowTracker 2000 5183-4779 5183-4780 5183-4781 FlowTracker 2000 Flowmeter and Leak Detector FlowTracker Universal AC Adapter (optional. verify carrier and support gas flows with the proper flowmeter.e. not supplied with FlowTracker units) ADM 1000 features include: • Accuracy ± 3% • Operating temperature range– 0 to 45ºC for the instrument. All flowmeters are calibrated to NIST-traceable standards. Choosing a flowmeter for your application depends upon measurement speed. independent of atmospheric pressure and temperature (calculated) • Data output through RS-232 port • 9V battery and AC power adapter (120 or 220 VAC) • Calibration–traceable to NIST primary standards • Real time.GAS MANAGEMENT Flow Rates Setting and maintaining GC flow rates greatly affect the instrument accuracy and sensitivity. accuracy. split ratio measurement • CE mark certified • Measures flow rates from 0. We have developed flowmeters for measuring capillary column flows.agilent. and verifying instrument gas flows. the ADM 2000 includes: • Mass flow measurements–measure flow rate.
com/chem 16 . Air ±3 ±3 Rechargeable Battery or 110 VAC Rechargeable Battery or 220 VAC Yes Yes HVF-500 HVF-500-2 Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters** Optiflow 420 Optiflow 570 Optiflow 650 0.5 0.5 0. H2.0 500 500 He. online.000 All All All +/. Air He.GAS MANAGEMENT Flowmeters Description Flow Rate (mL/min) Low High Gases Measured Accuracy (%) Power Supply RS-232 Data Output Part No. Ar/CH4 N2.5 1000 1000 1000 All All All ±3 ±3 ±3 9V Battery Battery or 120 VAC Battery or 220 VAC None Yes Yes 220-1170 220-1171-U 220-1171-E Electronic Mass Flowmeter – dedicated mass flowmeter. very accurate for specific gases* Veri-Flow 500 (110 V) Veri-Flow 500 (220 V) 5.0 5. Ar/CH4 N2. See pages 104-115 for more information about our services and support. measures all gases* ADM1000 ADM2000 ADM2000E 0.2 9V Battery 9V Battery 9V Battery None None None HFM-420 HFM-570 HFM-650 *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.5 5. H2. in the classroom.1 0. even at your site.3 +/. ADM Flowmeters – volumetric. www.agilent.0 50 700 5.3 +/.
and consumables that keep your instruments running in top condition. quotes. • Direct links – to the services.com/chem. order status. . and local sales information. • An expanded navigation – that includes links to product literature. • A newly designed online store – with fast access to pricing. events. The new site features: • A coherent page design – that automatically detects screen resolution and optimizes the page size for less scrolling. parts. go to www. and news. education. technical support. Based on customer feedback.You asked … we listened! Announcing the launch of our new Life Sciences and Chemical Analysis website. To experience these exciting new changes for yourself.agilent. we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.
agilent.agilent. syringes. Proper gas management is key high-quality Agilent offers a wide range of to achieving this goal. moisture infofrom proper syringe use and cleaning and hydrocarbons can damage your GC techniques to a detailed discussion on column. leak detectors our applications. syringes. Ph. look for useful common contaminants like oxygen. www. regulators. prevent it. Agilent provides a diverse line of sample vials. reliable results. and minimizing the likelihood of GC system contamination. Also. improve detector life.Sample Introduction Gas Management The use of quality carrier gases is essential for consistent and accurate GC analyses. and accurate sample delivery. optimal peak shape. This section explains how critical components. septa. This section reviews of your GC separations. visit our online catalog at www. and inlets. look for practical information about regulators. Just as you depend on and flowmeters – all designed to prevent meticulously engineered GC and GC/MS column damage. Time after time.” Bryan Bente.com/chem/4ecatalog. Also. liners and high quality broad range of gas-phase – gas inlets for a gas management products purifiers. see Agilent’s 2005-2006 Essential Chromatography Catalog. Technology Development Manager CATALOG For a complete selection of vials. Or. you can count on Agilent improve the quality and consistency these consumables. the importance of clean GC-tubing.com/chem 18 . and instruments. and helps you understand how to optimized inlet settings. Agilent’s commitment to offering the highest quality supplies means accurate.D. Consumables & GC Inlets “Good sample introduction helps ensure good reproducibility.
Vial Filling When filling sample vials.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Sample Introduction Vials Agilent’s wide opening vials are designed specifically for analyzing samples with your GC. divide the sample among several vials to obtain reliable results • when sample volume in the vial is low. cap colors. Agilent offers a large variety of autosampler vials in different closures. For small sample sizes. 19 www.agilent. septa choices and package options. TIPS AND TOOLS Do not inject air into the vials to prevent the vacuum.com/chem . for added convenience. and for trace analyses Polypropylene –for use with alcohols and aqueous solvents Amber Vials–for use with light-sensitive samples Microvolume Inserts–for High Recovery Vials– use with very small sample for use with limited sample volumes volumes Recommended fill volumes for sample vials 1 mL 3. Vial Options Glass–for general purpose use and for use with acids Silanized–for use with samples that bind to glass. Agilent also offers convenience packs with 500 vials and caps in a reusable blue storage box. contaminants from the previous sample injection or solvent washes may have a greater impact on the sample. This often damages the cap seal. They have specially designed vial neck angles. bottom design and height to ensure compatibility with Agilent autosamplers with rotating or robotic arm trays. use vials with small volume capacity. Agilent offers a variety of options. keep in mind: • if you need to test a large amount of sample over repeated injections. This could affect reproducibility. The airspace in the vial is necessary to avoid forming a vacuum when sample is withdrawn. You can use microvolume inserts with the wide opening vials or.6 mm* 50 µL 100 µL vial *Needle position based on standard sampling depth.
agilent. Each septum complements the overall system and enhances chemical performance. Teflon Disc • Good for MS and ECD analysis • Good for large-volume injections • Chemically inert • No resealing • Single injection • No long-term sampling storage 500/pk 5181-3400 500/pk 5182-0732 Viton • Chlorinated solvents • Organic acids • Limited resealing • Not suitable for 32 gauge syringe 500/pk 100/pk 500/pk 100/pk 100/pk 100/pk 5182-0547 5181-1270 5183-2087 9301-0977 5184-3551 5182-3454 TIPS AND TOOLS • if samples are run in small or large batches Unattended autosampler runs require a precise fit for uninterrupted operation.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Selecting Vial Septa Materials Vial cap septa are critically important to optimal analysis. unattended Teflon/Silicone/Teflon • Used in trace analysis applications • Above average resealing • Most resistant to coring • Least evaporation • Use with large diameter. clear crimp top 30 µL reservoir volume.com/chem 20 . Agilent’s vial cap septa are specifically formulated and constructed for optimum system performance. consider: • the number of samples run during a day/week Silicone/Teflon • Excellent resealing • Resists coring • Good for multiple injections • if samples are run manually or with an autosampler • if samples are run overnight. Typically. Micro-V vial. www. blunt tip syringe needles Vials Description Vials 2 mL Crimp top vial convenience pack with silver AI caps with Teflon/Red rubber septa 2 mL Screw top vial convenience pack with blue screw caps and Teflon/Red rubber septa 2 mL Snap top vial convenience pack with clear polypropylene snap caps and Teflon/Red rubber septa 100 µL Insert for wide opening vials 250 µL Polypropylene flat bottom inserts 100 µL Glass lined polypropylene vials Less than 5 µL dead volume. automated sample runs use a higher quality and quantity of vials. crimp top Quantity Part No. 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 Determining Your Quantity Needs To determine potential septa ordering quantities. High recovery vial.
3. Agilent syringes are designed: • for reproducible sample volume delivery • specifically for the Agilent inlet or autosampler • to maximize inlet septum lifetime Selecting Syringes 1. Sharp-tipped needles tend to tear the inlet septum and cause leaks. split or splitless (including PTV) Cool on-column Cool on-column Cool on-column 23 gauge or 23/26 gauge tapered 23/26 gauge tapered or 26 gauge 26/32 gauge tapered 26/32 gauge tapered any 530 µm 320 µm 250 µm Needle Tip Needle Shape Needle tips Sharp tip Cone tip Tapered needle Use syringe needles with an Agilent dualtaper needle or a conical tip. Refer to your automatic liquid sampler operating documentation for available syringe sizes and corresponding injection volumes. Select the syringe type based on the inlet (injection port) you are using and the volume of sample you want to inject. The Agilent line of syringes include a variety of plunger and needle choices to use with your autosamplers. page 38.agilent. Needle Gauge Selection Inlet Needle Gauge Column Type Packed. resulting in a large solvent tail on the chromatogram. Select the appropriate syringe needle gauge. 2.com/chem . use the Agilent Cone Tip (HP Point Style) with Agilent’s Centerguide Septa.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringes Syringe type and design are important for chromatography to ensure reproducible sample injections for consistent results. Also. TIPS AND TOOLS For best results. Select a syringe. a sharp-tipped needle tends to leave residual amounts of sample on the septum as it exits. 21 www.
www.5 µL injection • Plunger not replaceable 10 µL. To insert a needle into a syringe barrel: 1. 5. 4.agilent. 3. • 1 µL injections syringe for 1µL can bend • Clean samples injection more easily • Routine analysis • No hardware • Not ideal for higher modification needed viscosity samples for 0. syringe and column. use the instructions in the syringe box to wrap the needle yourself. Slide the spring and the cap down over the needle.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringe Characteristics and Recommended Uses Syringe Advantage Limitations Recommended Use 5 µL. Insert the needle into the syringe barrel. fitted plunger • Most accurate • Thinnest plunger. Make sure the needle has the Teflon disk. TIPS AND TOOLS Failure to use an on-column syringe when injecting into an on-column inlet could damage the injector. fitted plunger • Most economical • Most reliable fitted plunger syringe • Less bending • Better for high viscosity samples • Most accurate only • General purpose for 1 µL and larger syringe injections • Clean samples • Plunger not • Routine analysis replaceable 10 µL. Screw the cap back on the syringe barrel.com/chem 22 . Select the correct size needle for the column you plan to use. Unscrew the syringe barrel cap and remove the spring. 2. If the syringe barrel does not have the Teflon disk. gas-tight • Replaceable plunger • More expensive • Dirty samples 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.
the more likely it is to contain water. always use the proper septum nut and stainless steel insert for the column dimension you are using. Even better. NEW! Agilent Gold Standard GC Autosampler Syringes see page 25 VIDEO To view a video on syringe installation. can accelerate syringe wear dramatically. With these types of samples. use a Teflon tipped syringe plunger.25mm columns. especially when combined with water-extractable materials from samples.53mm id column. • Remove a gas-tight plunger from the syringe for long-term storage to keep the Teflon tip leak-free. • For on-column injections. as specified in the syringe cleaning procedure included with each syringe. • To maximize the lifetime of standard plungers.com/chem . and for maximum reproducibility and accuracy. • The more polar the solvent. Use a septum with a molded through-hole with injections onto 0. Trace amounts of water. • A 26-gauge syringe can be used for on-column injections into a 0. rinse the syringe and wipe the plunger with solvent (isopropanol or acetone) and a lint-free wipe. hard surface and let cool to room temperature. proactively replace syringes. 23 www. • Pump sample in and out of the syringe at least 5 times to remove any air bubbles.com/chem/techsupport. • Rinse syringes and clean their plungers before use to maximize syringe lifetime. Always check that on-column syringe needles fit inside the capillary column before installing the column and syringe in the GC. • Rinse the syringe 5-8 times between injections to minimize sample carryover. The plunger should reseal correctly to provide 10-25% more injections. since plunger bends may be inevitable.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. visit www.agilent.agilent. 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.32mm and 0.
• The syringe is nearing the end of its useful life. Blocked needles • Sample material or contaminants may be trapped inside the needle. This gradually wears away the rust-resistant metal on the shaft’s surface. and wipe it dry with a lintfree cloth. “Ring around the neck” (A dark ring between the top of the barrel and the end of the volume scale. it is best to use solvents that effectively dissolve the sample you are working with. Note: Plungers normally feel “loose” when non-polar solvents (like hexane and toluene) are used.agilent. metal. • Never touch the plunger shaft with your fingers. • To slow this process. • Rusting happens most rapidly when using water or solvents that may contain (or absorb) water. Loose plungers – accompanied by syringe leaks and area count reproducibility problems. When cleaning your syringe. • Use 23 to 26-gauge tapered needles to get the combined benefits of greater septa life and fewer bent needles. 1.” • 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. Problem Bent plungers or stuck syringes Possible Cause(s) • Particles such as dust. and handling of each syringe will help ensure correct performance and long life. • During normal use. • Narrow-gauge needles (26 gauge) bend more easily than larger (23 gauge) needles. • The needle may not have been properly cleaned. • Never cycle the plunger in a dry syringe. Bent needles • Improper needle alignment. Let syringe and plunger air dry. Then. and wipe the plunger dry with a lint-free cloth 3. • If build-up appears when water is the solvent: rinse syringe with acetone and wipe the plunger clean at the end of each day. Then. • Use only Agilent autosamplers. Remove the syringe from the autosampler. • Needles tend to bend when inserted into the sample vial – not the inlet port. • Remove the plunger and use a second syringe to fill the blocked syringe with solvent. • Only use Agilent vials and septa. and cycle the plunger to pull the solvent into and out of the barrel. Common choices are methanol. methylene chloride. They are precision-designed to ensure proper alignment with the syringe needle. cleaning.com/chem 24 . or are strongly acidic. flush the shaft with solvent. Rust Note: even minor rust can cause the plunger to become stuck in the barrel. Important: Try to use a cleaning agent that is appropriate for the contaminant. contain phosphates. Finally. 2. remove the water from the syringe at the end of each day. the plunger may bend if used further. insert the plunger and gently push solvent through needle. Rinse the syringe several times with a “dry” solvent. salts. such as acetone. Suggested Action(s) • If the plunger’s movement feels “gritty.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Syringe Troubleshooting Guide Proper care. Try to avoid cleaning agents that are alkaline. the shaft rubs against the glass walls of the barrel.” remove the plunger from the barrel. • Do not “mix & match” plungers and barrels.) • Skin oils and other organic material. Once this happens. or glass can fill the narrow gap between the plunger shaft and the inside wall of the barrel. • Always clean syringes after use. and acetone. acetonitrile. www. • Replace the syringe. This can be caused by septa that are too “tough. submerge the tip of the needle into a container of solvent. • Fine metal and glass particles from the syringe plunger and barrel may be rubbing together. carefully insert the plunger back into the barrel. leftover samples.
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 07673-60840 25 www.agilent.53 mm id columns) 10 µL 5 µL Straight Needle Syringes (use with Merlin Microseal) 10 µL 5 µL Straight Straight Fixed Needle Fixed Needle 23/42 23/42 6/pk 6/pk 9301-0725 5182-0875 Tapered Tapered Fixed Needle Fixed Needle 23-26s/42 23-26s/42 6/pk 6/pk 5181-3360 5181-8810 Gauge/Length Quantity Part No. 23/26 gauge needles.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Gold Standard GC Autosampler Syringes Description Tapered Needle Syringes (use for split/splitless or on-column injections with 0. GC septa (25/pk). GC Automatic Liquid Sampler Supplies Description Miscellaneous Autosampler Supplies 4 mL Clear screw top wash vials with screw caps (no Septa) Septa for 4 mL vial Diffusion caps for 4 mL vials 4 mL wash vial with fill marking.com/chem . caps Screw for mounting syringe Quadrant kit (4 tray sections) 7673/83 Basic Supply Kit contains: 10 mL syringes (6/ea). 2 mL automatic sampler vials with screw caps (1.000/pk). 4 mL vials with diffusion caps (144/pk). Vial racks (5/pk) 144/pk 144/pk 12/pk 25/pk 9301 0723 9301-1031 07673-40180 5182-0551 07673-20570 18596-40015 Black ink and gold illuminating backdrop for easier viewing of the volume scale Individually sealed packaging for contaminant-free use Unit Part No.
Packed-column inlets are simple in both design and use.com/chem 26 . and remove any column packing in the inlet zone. Change the septum on a regular basis and check column connections at the first stage of problems. Packed-column analysis is frequently done when high efficiency separations are not needed or when gases are analyzed by gas-solid chromatography. The inherent activity of packed-column inlets is somewhat mediated by the fact that they usually have low internal volume. Sample can be lost through the leak holes. make sure that the oven and inlet are at room temperature when not in use and when changing the septum. septum and column leaks will have a direct impact on retention times and peak areas. 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. This can cause several maladies. To prevent stationary phase decomposition. Decomposition Since packed-column inlets are active. especially if glass liners are not used. splitless inlets). Flashback The negative side of low inlet volume. Use to lower activity (replaceable) Sharpens peaks and reduces run time Will not break Better for polar or labile compounds Use with N2 carrier gas Use with He or H2 carrier gas Liner Initial column temperature Column type Carrier gas flow Troubleshooting Most problems with packed-column inlets involve sample decomposition. When inlet-caused decomposition is suspected. sample losses. and air can diffuse back into the inlet to cause column degradation. When this is coupled with the relatively fast flow rates used with packed columns. Sample decomposition caused by the inlet is easily diagnosed. including ghost peaks. and all carrier gas flow flushes through the inlet into the column in the standard configuration.agilent. flashback. or lower inlet temperatures. polar sample components will often tail or degrade in the inlet. try intracolumn direct injection. www. Leaks Since packed-column inlets are usually flow-controlled. or leaks. 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. irreproducible peak areas.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Packed-Column Inlets Packed-column direct inlets are very popular. the decomposition products will have peaks at the same retention times as standards for the decomposition product. Packed-Column Inlet Procedures/Practices Parameter Selection/Setting Rationale Inlet temperature Insert type BP of solvent +50˚C BP of major solute(s) 1/8-inch stainless steel 1/4-inch stainless steel Glass temperature programming 1/8-inch packed stainless 1/4-inch packed glass 20-40 mL/min 30-60 mL/min Ensures flash vaporization Use for neat samples Use for ss column only Inserts permit connection of columns up to 1/4-inch od. deactivated glass liners. Few parameters need to be set. and decomposition. however.
disposable Glass liner. Vespel/ graphiteferrule graphite ferrule 1/4 in. optimized. nonpurging Brass nut. nut 1/4 in. id Tubing nut. brass 12/pk 25/pk 5/pk 10/pk 10/pk 50/pk Unit Part No. even at your site. see the 6890 Series GC Instrument User and/or Service Manuals.in. column adapter 9 10 11 Upper insulation Nut warmer cup with insulation Column nut for 0. Vespel/ 1/4 in. online. 10/pk 19243-605050 5180-4105 27 www. 1/4 in. 1 18740-60835 5183-4757 19243-80570 5080-8898 5080-8732 5181-3382 5080-8774 5180-4105 2 3 4 Adapters with glass liners 8 0. disposable/deactivated 6 7 Vespel/graphite ferrules.com/chem .53 mm column adapter 1/8 in. See pages 104-115 for more information about our services and support. or 1/4 in. column adapter 1/4 in.53 mm column 2/pk 19244-80540 19243-80530 19243-80540 6 5 Liner 19243-00067 19234-60720 5181-8830 7 8 1/4 in. 11 mm Top insert weldment Viton O-rings Glass liner. 1/4 in. Universal Packed-Column Inlet (non-purged) Septum retainer nut for headspace sampling. or 1/4 1/8 in. stainless steel liner stainless steel liner Inside of Insideof Oven Oven 9 10 For a complete parts breakdown. in the classroom. 1/4 in.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 6890/6850 Series GC Packed Port Supplies* Item 1 2 3 4 5 Description Septum nut Septa Bleed temperature. nut 1/8 in. column adapter 19243-80510 19243-80520 Unit Part No. column adapter Tap Agilent’s GC knowledge over the phone. not EPC Adapters without glass liners 1/8 in. 19243-60570 TIPS AND TOOLS 1/4 in. * For Model 6890/6850 only 11 5890 Packed-Column Inlet Supplies Description Nonpurging septum nut assembly for manual flow control only.agilent.
and column ID Narrow initial peaks Minimizes ghosting Injection volume 0. www. or that have long injection times (valve injections) • have important minor peaks eluting directly before the solvent peak (as in solvent analysis) Split injection is also good for screening samples of which little is known or for those that have widely differing concentrations. Split Mode Split injection is an effective way to introduce small amounts of sample without overloading the column. Repeat if results are positive until no further improvement is seen. increase it by 50˚C and compare the results to the lower temperature analysis. Because it can be used in either split or splitless mode. check out Agilent’s new Flip Top Inlet Sealing System on page 52. Split inlets are also a good choice for dirty samples. Practices. Troubleshooting Split inlets are spared from most bandbroadening phenomena.agilent. since the split ratio can be adjusted easily. Therefore. low split flow. Both analytical accuracy and reproducibility decrease with the increases in discrimination and decomposition. since narrow peaks are generated as part of the splitting process. A majority of the problems encountered with split inlets are related to discrimination and decomposition.com/chem 28 . If you suspect that the inlet temperature may be too low. it provides a very effective combination that can cover most analysis requirements. (<20 mL/min on 6890) or low inlet temperature. deactivated Silanized glass wool Glass beads or frit None Ensures flash vaporization Minimizes inlet discrimination Minimizes flashback Minimizes degradation Retains non-volatiles Minimizes inlet discrimination Less active than wool Least active Split easily adjusted Split adjusted accordingly Less needle discrimination Reproducible discrimination Depends on sample and injection volume. Split Mode Variables. Split injection is required for samples that: • cannot be diluted for analysis (for example.5-3 µL liquid 0. solvents) • are gases that cannot be focused. and Rationales Parameter Selection/Setting Rationale Inlet temperature Inlet liner Inlet packing Try 250˚C or BP of last eluting compound Large volume. Split inlets suffer from both needle discrimination and inlet discrimination. any peak broadening or tailing observed with split injection is usually due to improper column installation.10-10 mL gas Injection technique Fast autoinjection Hot-needle fast manual injection Split ratio Initial column temperatures Septum purge 50:1 to 500:1 Not critical 2-3 mL/min TIPS AND TOOLS For fast and easy liner changes.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Split/Splitless Inlets The combined “split/splitless” inlet is the most popular inlet for capillary column gas chromatography.
samples with trace quantities of important solutes that elute on the solvent tail may be focused by the solvent to yield more sensitive analyses. sample preparation requirements are significant. & conditions Splitless Mode For splitless injection. Also. Additionally. visit www. Inlet liner Inlet packing Injection technique Fast autoinjection Most reproducible Less needle discrimination Hot-needle slow manual Inject 1-2µL.com/chem/techsupport. a conventional split injector is operated in a nonsplitting mode by closing the split valve during injection. use a solvent that is similar in polarity to the column stationary phase. 29 www.agilent. The most important benefit of splitless injection is that a majority of the injected sample is introduced into the column. The sample is flash-vaporized in the liner. and avoid mixed solvents. After most of the sample has been transferred into the column.agilent.8mL Small volume <0. Breaking these rules may result in split peaks. and gas injections Use only with slow injection Decreases degradation Use for fast autoinjection & dirty samples Depends on solvent. and Rationales Parameter Inlet temperature Selection/Setting Just above highest boiling point of solutes (+20˚C) Large volume >0. Purge flow Purge delay time 20-50 mL/min 20-80 sec Oven temperature Column flow 10-25˚C below solvent BP Necessary for solvent focusing >2mL/min when possible Clears inlet fast Reduces backflash and decomposition 2-3mL/min Internal standard Standard addition 1-3m.com/chem . liner. So column protection becomes as important as sensitivity. Practices.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Split Mode Variables.sec if narrow liner is used and >1µL injection Hot-needle fast manual Use for <1µL injections Higher if using constant flow Adjust according to column flow rate/liner type & sample conditions Solvent Effect One requirement of splitless injections is that the initial column temperature should be kept at least 10˚C below the boiling point of the sample solvent. Splitless injection is routinely used in areas such as: • environmental analysis • pesticide monitoring of foods • drug screening In these applications.5-2 µL liquid Rationale Ensures flash vaporization Reduce if degradation occurs Use higher for dirty samples and higher-boiling solutes Use with autoinjector Use only for slow manual injections. and sample vapors are carried into the column by the carrier gas where they are recondensed at temperatures below the boiling point of the solvent.2mL None Silanized glass wool Injection volume 0. This allows the sample solvent to condense at the front of the column trapping the solvent molecules into a tight. narrow band. and it is not always possible or economically justifiable to clean up a sample extensively. vapors remaining in the liner are cleared by opening the split vent which remains open for the duration of the run. deactivated (1-2m per µL injected) Reduces ghosting Maximizes reproducibility Use only with constant injection volume Reduces peak distortion Promotes solvent and stationary phase focusing Septum purge Quantification Retention gap VIDEO To view a video on liner and gold seal replacement. This results in much higher sensitivity than that achieved using split injection.
(See page 61).SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Troubleshooting Most problems encountered with splitless injection are related to incorrect purge time. degradation.com/chem 30 . 18740-60835 See page 36 G1544-60575 See page 52 See page 47 G1544-20590 19251-20620 18740-20880 18740-20885 5 6 7 8 9 10 11 12 13 14 Split vent trap assembly (6890/6850 only) G1544-80550 Retaining nut (6890/6850 only) Retaining nut (5890 only) SS seal Gold-plated seal Washer. Removing or reducing the amount of liner packing can also decrease inlet activity. www. 6890/6850 Split/Splitless Inlet Supplies* Item 1 2 3 4 1 2 3 4 6 5 Description Septum retainer nut Septa Insert Weldment Liner O-ring Liner Unit Part No. TIPS AND TOOLS 11 12 13 14 A guard column or retention gap is often beneficial for splitless injections. Match inlet temperature. and flashback. od Reducing nut Insulation (requires 3) Lower insulation cover Ferrule Column nut (6890/5890 only) Column nut (6850 only) Angled wrench for split/splitless inlet 2/pk 2/pk 5181-8830 5183-4732 19251-00100 12/pk 5061-5869 18740-20800 19243-00067 19243-00070 7 8 9 10 * For a complete parts breakdown. Decomposition Loss of peak area or generation of new peaks. 0. leading to irreproducibility and nonlinearity of peak areas.375 in. improving peak shape and extending column life when analyzing dirty samples. Appropriate initial column temperature is critical. liner volume. Sample vapors can be lost through the septum purge line if the insert is overfilled with sample vapor (either too large injection volume or too small liner volume). improper focusing.agilent. see the 6890/6850 Series GC Instrument User and/or Service Manuals. can sometimes be dramatically reduced by changing liner type or by deactivating the liner and inlet with silanizing reagents. and injection volume carefully to avoid backflash.
and it becomes apparent that cool on-column injection should be considered whenever high precision and accurate results are required. and injection rate must often be optimized Advantages: • elimination of sample discrimination • elimination of sample alteration • solvent focusing of early eluting solutes • high analytical precision Cool On-Column Inlet Procedures/Practices Parameter Selection/Setting Rationale Initial inlet temperature Initial inlet temperature ramp Injection volume Injection technique Oven temperature Column flow Septum purge Quantification Retention gap requirements = or 3˚C above column oven temperature Same as oven (oven track) Faster than oven 0. deactivated Ensures sample focusing in solvent front Simple and effective Narrows initial peak width Use smaller injections for small id columns.5 µL to 2.1-2. Limitations: • maximum sample volumes are smaller compared with other inlets (0. Add to this the elimination of thermal decomposition and rearrangement reactions. cool on-column injection provides the most accurate and precise results of the available inlets. since the liquid is introduced directly into the column. inlet-related discrimination does not occur. solvent nature. nonvolatile sample components can accumulate at the head of the column and will degrade efficiency and/or interact with subsequent injections. 31 www.agilent. Moreover.0 µL liquid Fast autoinjection Fused silica needle Inlet temperature or slightly lower 50-80cm/sec 30-50cm/sec 12-15mL/min All methods 1-3m. If done properly.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Cool On-Column Inlets Cool on-column injection is superior in many ways to other sample introduction techniques. Automated oncolumn injection provides even higher analytical precision. Syringe discrimination is completely eliminated. Depends on column capacity Projects droplets away from syringe tip Use for manual injection into small id columns Prevents backflash Use for H2 carrier gas Use for He carrier gas Use if installed to prevent ghosting Inherently reproducible technique Lack of discrimination Corrects peak distortion Protects column from non-volatile components Permits autoinjection with narrow-bore columns TIPS AND TOOLS Since the sample is directly deposited into the column.0 µL) • solute peaks eluting just before the solvent cannot be focused and are difficult to determine • capillary columns (especially those with a large phase ratio or small inner diameter) can be easily overloaded with sample • parameters such as initial column temperature.com/chem .
Only columns with an immobilized stationary phase should be used with cool on-column injection to prevent displacement of the stationary phase by solvents. visit www.com/chem 32 .53 mm 5/pk Unit 2/pk 10/pk 10/pk Part No. VIDEO To view a video on cool on-column installation and septum replacement. • the incompatibility of some solvents with the stationary phase. Troubleshooting The major problems found with cool oncolumn injection are associated with column overload. solvent/stationary phase incompatibility. Loss of column efficiency with on-column injection usually is caused by contamination or degradation of the stationary phase at the head of the column. the column must be replaced and a retention gap should be used for all further injections of dirty samples.18-0. Many of the problems associated with these variables can be resolved by using a retention gap ahead of the analytical column.agilent. poor wettability). If that does not return column performance. Immobilized stationary phases can be washed to remove contaminants and renew performance.com/chem/techsupport.agilent. column contamination. www.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Sample Considerations Sample preparation is important for on-column injection because of: • the potential for column overload. and column contamination. Column/Retention Gap Installation Consumables Description Column nut 250 µm graphite/Vespel ferrule 320 µm 0. If column performance does not improve after washing.5m off the inlet side of the column. • dependence of the initial column temperature on the boiling point of the solvent. peaks will be broad or split. cut 0. A retention gap usually will resolve this problem. Use only well-deactivated retention gaps and high quality capillary columns from Agilent. If the flooded zone after injection is too long (large injections. 5181-8830 5181-3323 5062-3514 160-2255-5 160-2325-5 160-2535-5 5181-3396 TIPS AND TOOLS Sample degradation can occur with cool on-column injection if column or retention gap activity is high.5 mm graphite/Vespel ferrule 250 µm retention gap (one 5 m piece) 320 µm retention gap (one 5 m piece) 530 µm retention gap (one 5 m piece) Quartz deactivated column connector fits 0.
33 www. see the 6890 Series GC Instrument User and/or Service Manuals.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 6890 Series Cool On-Column Inlet Supplies* Item Description Manual injection 1c 1d Cooling tower assembly Duckbill septum Fused silica syringe needles Syringe barrel for use with fused-silica needles.agilent.com/chem . 1a 1b 1c 1d 19320-80625 10/pk 6/pk 19245-40050 19091-63000 9301-0658 2 3 4 19245-60760 6890 Series GC Cool On-Column Inlet Supplies Automatic Injection 1a 1b 2 Septum nut base for 320 mm assembly Septum nut base for 530 mm assembly Advanced green 5 mm through hole septa BTO 5 mm through hole septa 50/pk 50/pk 19245-80521 G1545-80520 5183-4760 5183-4758 5890 Series Cool On-Column Inlet Supplies Automatic Injection 1a 1b Septum nut (5890 Series II GC) Needle guide (for 7673A only) 19245-80520 19245-20670 * For a complete parts breakdown.10 µL Common Supplies 3 4 Spring Inserts for capillary columns For 200 µm columns (one ring) For 250 µm columns (six rings) For 320 µm columns (five rings) For 530 µm columns (no rings) For 530 µm Al clad columns (four rings) 5 6 Ferrule Column nut 2/pk 19245-20510 19245-20515 19245-20525 19245-20580 19245-207804 5080-8853 5181-8830 5 6 Unit Part No.
fast or slow 10-25˚C below solvent BP Sample dependent Column flow Septum purge Quantification 30-50 cm/sec 1-5mL/min Any method Retention gap 1-3m. Cryogenic cooling of the inlet can reduce inlet temperature enough to thermally focus gas injections from other sampling devices in the liner.5µL only in solventelimination mode Not critical for cold split & splitless modes For proper solvent effect in splitless mode For split mode Clears inlet faster Less backflash Minimizes ghosting Inherently reproducible Low discrimination in cold injection modes Compensates for extended flooded zone and solventcolumn incompatibility Advantages • no syringe-needle discrimination • minimal inlet discrimination • no special syringe needed • use of large injection volumes • removal of solvent and low boiling components • trapping of nonvolatile components in liner • split or splitless operation • retention time and area reproducibility approaching cool on-column injection PTV inlets are actively cooled before and during injection by Peltier devices or by forced gases (air.1-1. This is a distinct advantage of using PTV inlets in comparison to conventional inlets for coupling auxiliary sampling devices to capillary columns. Then the inlet temperature is increased to vaporize the sample. or liquid CO2).agilent. splitless and on-column inlets. The sample is usually injected into a cool liner. Post-injection. www. less expensive instrumentation For general use For labile samples For focusing gaseous injections from auxiliary sampling devices Use lower volumes for volatile solvents and fast ramp rates Use volumes larger than 1. 2˚C/sec to 12˚C/sec) Rationale For general use and sample screening For trace analysis Use slower ramp rates for labile. liner installation and silver seal replacement.e. visit www. The user programs vent times and temperature to achieve the equivalent of split or splitless transfer of sample vapors to the column. inlet temperature ramps are either ballistic (i.com/chem 34 . PTV Inlet Procedures/Practices (cold split/splitless modes) Parameter Injection mode Selection/Setting Cold split Cold splitless Inlet temperature ramp rate Adjustable (i.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Programmed Temperature Vaporizer (PTV) Inlets PTV inlets combine the benefits of split. PTV inlets are heated using electrical heaters or preheated compressed air. or large volume samples Use faster ramp rates for most samples Use faster ramp rates to shorten splitless purge delay time Simpler.agilent. PTV injection is considered the most universal sample introduction system because of its flexibility. complex. deactivated VIDEO To view a video on PTV column installation. ramped to the maximum temperature at an uncontrolled maximum rate) or programmable.5µL Sample Injection technique Oven temperature Autosampler or manual.. Injection volume Inlet liner Straight with silanized wool Baffled Packed with an adsorbent Ballistic 0. liquid N2.com/chem/techsupport. Depending on design.. so syringe needle discrimination does not occur.e.
2 mm id 180 µL volume.25-0. deactivated PTV Liner Fritted Glass.25 mm 0.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 6890 PTV Inlet Item 1 2 3 4 5 6 7 8 Description Septumless head Septum head Septum nut PTV inlet assy PTV LCO2 cooling jacket PTV LN2 cooling jacket Silver seal Graphpak inlet adapter 0.20 mm 0.53 mm 10 11 Split nut for inlet adapters PTV insulation block PTV cryo insulator (not shown) Teflon ferrule (needle seal) Kalrez seal Valve body Pressure spring Viton seal Sealing element CO2 Cryo inline filter Service kit for septumless head contains Kalrez seal. 2 mm id 200 µL volume. deactivated PTV Liner Multi Baffle.20 mm 0. PTV liners require packing or a modified surface to hold the liquid sample in place before and during the vaporizing process. 6 7 8 9 10 11 There are few choices in liner design for PTV inlets. PTV Liners Description PTV Liner Single Baffle. 5183-2038 5183-2036 5183-2037 5183-2041 35 www. deactivated.5 mm id 150 µL volume. 1.53 mm 9 Ferrules for Graphpak inlet 0. liner volume and activity are still key issues to be considered when selecting among the few available PTV liners. valve body.com/chem TIPS AND TOOLS . glasswool PTV Liner Single Baffle.5 mm id 150 µL volume. and pressure spring Graphpak 3D ferrules Installation tool for 3D ferrules 10/pk 10/pk 10/pk 10/pk 5/pk Column ID Unit Part No. G2617-60507 G2618-80500 18740-60835 G2617-60506 G2617-60508 G2619-60501 5182-9763 5182-9754 5182-9761 5182-9762 5182-9756 5182-9768 5182-9769 5182-9770 5062-3525 G2617-20510 G2617-60510 5182-9748 5182-9759 5182-9757 5182-9758 5182-9775 5182-9760 3150-0602 5182-9747 5/pk 5182-9749 G2617-80540 1 3 2 4 5. deactivated Part No.agilent. However. 1.33 mm 0.32 mm 0.
and consistency for our complete line of 11 mm and 9. Septa maintain the leak-free seal and exclude air from the inlet. No longer do you need to reach into a jar and wonder how clean the septa are or if you are contaminating other septa. the new packaging delivers the following features and added value: • No more clumping or sticking: Septa don’t stick to each or the jar • Easy to see exactly how many are left: Know exactly when to reorder • Compact storage size: Fits easily into drawers • Convenient quantities: All septa are packaged in either 50 or 100 packs • High quality PET packaging: Tested by GC-FID. and GC-ECD to ensure the absence of interfering background peaks www. decreased column life and ghosting. and can withstand more punctures (injections) than their high-temperature counterparts. How to Minimize Problems Avoid problems by: • using within the recommended temperature range • changing regularly • installing “hand tight” • using septum purge when available • using autoinjectors • using sharp syringe needles Your 50th Septum will be as Clean as Your 1st! The primary benefit behind the new packaging is that each septum is individually packaged for the ultimate cleanliness. they can leak or decompose. GC/MS. This new packaging is a tri-fold blister pack that provides cleanliness. Each septum is easily dispensed one at a time by pushing it through the back foil.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Septa One of the key components of sample introduction is the inlet septum. Lower temperature septa are usually softer. In addition. however. lower column flow. This causes sample losses. What is the Function The septum isolates the sample flow path from the outside world.agilent. as is commonly done with pharmaceutical capsules and tablets.5 mm septa. They are generally made of special high-temperature. convenience. All columns must have carrier gas head pressure to establish flow through the column.com/chem 36 . It must provide a barrier that is readily penetrated by the injector needle while maintaining internal pressure without contaminating the analysis. They come in many different sizes and are made from many different types of material specific to inlet type and analysis needs. low-bleed silicone rubber formulations. If used above their recommended temperatures. Septa are usually available according to their recommended upper temperature limits. seal better. Why Replace Septa should be replaced regularly to avoid: • leaks • decomposition • sample loss • reduced column or split vent flow • ghost peaks • column degradation Agilent Introduces Innovative Packaging for Inlet Septa Agilent has recently introduced a new and innovative packaging design for inlet septa.
If extra peaks disappear. To maintain system integrity. Replace septum and use smaller diameter needles. Important: always use the septum specified for higher temperature or analyze at lower inlet temperature. septa can become prone to leakage.com/chem . Remedy Turn off injector heater. Replace septum or tighten connections if necessary. change septa regularly. Check for leaks. clean the inlet and change the liner. Normal Problem Problem MAINTENANCE MINDER After repeated injections. Normal Problem Baseline Change After Large Peak Large leak at septum during injection and for a short time thereafter (common with large diameter needles).SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Septa Troubleshooting Symptom Extra Peaks/Humps Possible Cause Septum bleed. If cored septa particles are present. 37 www. use a centerguide septa and a 23-26 gauge tapered syringe. Normal Problem (flow increase) Problem (flow decrease) Retention Times Prolonged Carrier gas leaks at septum or column connection.agilent.
agilent. Available in Bleed Optimized. So your GC system will maintain its integrity. Agilent’s plasma-treated non-stick septa But Agilent’s new non-stick septa are plasma coated. • Proprietary plasma treatment ensures non-stick septa without the use of potentially damaging talcum powder • Center point guides the needle for easy penetration and less coring • Reduce needle bending • Precision molding assures accurate fit in the inlet • Each batch tested on an Agilent 6890 GC-FID for bleed Introducing Agilent Premium Non-Stick Septa – featuring a proprietary plasma coating that won’t stick or clump. this coating can accumulate inside split vent lines and interfere with the analysis of active analytes. Long-Life.com/chem 38 . stay cleaner and require less maintenance. Other suppliers coat their septa with powder to prevent sticking. and Advance Green. Competitor “non-stick” septa www. However.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Premium Non-Stick Septa Our premium non-stick septa have a recess on the injection side. to guide the syringe needle to the same point with every injection. which eliminates chemical bleed and contamination from foreign substances.
1 autoinjection 100 autoinjections 700 autoinjections Figure 1.agilent. creating variations in geometry. • Less chance that a cone of material will be punched out of the bottom during the first few injections • Virtually no septa material falling into the inlet liner.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Because bleed from septa can be a major contributor to the overall signal. With and Without CenterGuide (30x magnification) High-Temperature Septa Without CenterGuide: Major Coring Before 1 00 Autoinjections Agilent BTO Septa With CenterGuide: Very Little Coring Even After 700 Autoinjections Summary of Inlet Septum Characteristics SEPTUM TYPE BTO (Bleed and Temperature Optimized) Long Life Advanced Green ✔✔✔ = best BLEED ✔✔✔ (optimized for high temperature) LIFETIME ✔ TEMPERATURE LIMIT to 400ºC ✔ ✔✔ ✔✔ = very good ✔✔✔ ✔✔ ✔ = good to 350ºC to 350ºC 39 www. high-temperature tested silicone rubber. improving chromatographic quality • Up to 1. each Agilent premium septum is molded to a perfectly uniform size and shape. the septum. Agilent septa are made of highly durable. Individual molding lets us put a dimple in the center of each septum to guide the syringe needle into the inlet. Agilent’s premium GC inlet septa are not garden-variety septa stamped out in large sheets. Rather. the syringe needle enters the septum at precisely the same spot each time. not cutting.000 autoinjections under optimal conditions before failure with HP Point syringes. The result: minimal coring (see Figure 1). Comparison of Coring. Each lot is tested to ensure low bleed at high temperatures. a high-quality septum is an absolute necessity for analyses demanding increased sensitivity.com/chem . The HP Point syringe yields optimal performance and reliability and reduces coring by parting. With the dimpled CenterGuide.
45 Durometer. they are made of durable material to minimize the risk of contamination and the need for reconditioning • Convenient blister packs of 50 or 100 septa minimize risk of contamination and need for reconditioning www. is specified to withstand over 200 automatic injections at an injection port temperature of 350ºC.agilent. low-bleed • Maximum Injection Port Temperature 400ºC • Virtually eliminates injection-port sticking • Pre-conditioned. packaged in glass to prevent contamination • Ideal for use with low-bleed. Agilent’s General Purpose red/gray septa are cost-effective choices which provide: • Low bleed for reduced instrument maintenance downtime and increased laboratory productivity • Less frequent replacement for long lifetime and the ability to withstand more than 200 autosampler injections at maximum injection port temperatures • While general purpose septa do not have the centerguide of premium septa. You can have confidence in your chromatographic results knowing that each lot of septa is placed through a demanding QC test to ensure that only the highest quality product is delivered to your laboratory. Easy On Autosampler Needles Agilent Advance Green Non-Stick Septa • True Long-Life. High Temperature Green Septum • More Injections per Septum • Reduced Injection Port Sticking • Maximum Injection Port Temperature 350ºC • Packaged in glass vials for high purity • Economical alternative to competitor’s “Green” Septa General Purpose Septa Agilent’s General Purpose Septa are made from an enhanced injection-molded silicone rubber material. The septa material. dark red or gray in color. “Mass Spec” capillary columns Agilent Long-Life Non-Stick Septa • Pre-pierced for extended life and reduced coring • The preferred Septum for Autosamplers • Ideal for Overnight Runs • Up to 400 Injections Per Septum injection • Maximum Injection Port Temperature 350ºC • Soft.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS p/n 5183-4757 p/n 5183-4761 p/n 5183-4759 Agilent Bleed and Temperature Optimized Non-Stick Septa (BTO) • Extended temperature range.com/chem 40 .
5890.5 mm (3/8 in. 6850 and 6890 GCs (50/pk) 11 mm septa for 4890.agilent. 6850 and 6890 GCs (100/pk) 5 mm septa through-hole for on-column in glass jar (50/pk) Agilent Advanced Green Non-Stick Septa 5183-4757 5183-4757-100 5183-4758 11 mm septa for 4890. 6850 and 6890 GCs (50/pk) 11 mm septa for 4890. 5890. Just visit www. 5890.) for 5700 series and 5830/40 GCs (50/pk) 9.com/chem . 6850 and 6890 GCs (100 pk) 11 mm with partial through-hole for 5880. 5890.) for 5700 series and 5830/40 GCs (50/pk) 9. 6850 and 6890 GCs (100/pk) 5 mm septa through-hole for on-column in glass jar (50/pk) Agilent Long-Life Non-Stick Septa 5183-4759 5183-4759-100 5183-4760 11 mm septa for 4890.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) Red Septa 5080-8896-50 5080-8894-100 5080-8728-50 5080-8728-100 11 mm solid for 5880. 5890. (100/pk) 6850 and 6890 GCs 9. 6850 and 6890 GCs (50/pk) 11 mm solid for 5880.agilent.com/chem/4ecatalog 41 www.5 mm (3/8 in. 6850 and 6890 GCs (100/pk) 9. (50/pk) 6850 and 6890 GCs 11 mm with partial through-hole for 5880. 5890. 5890. 6850 and 6890 GCs (50/pk) 11 mm septa for 4890.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Septa Ordering Information Part No. 6850 and 6890 GCs (100/pk) 5 mm septa through-hole for on-column in glass jar (50/pk) General Purpose Septa Gray Septa 5183-4761 5183-4761-100 5183-4762 11 mm for 5880. Premium Non-Stick Septa Agilent Bleed and Temperature Optimized Non-Stick Septa 11 mm septa for 4890. on-column inlets* (25/pk) * 5 mm septa are packaged in glass jars 5181-1263-50 5181-1263-100 5181-3383-50 5181-3383-100 5181-1283-50 5181-1283-100 5181-1260 5181-1261 EASY ONLINE ORDERING Our online store offers every GC inlet and consumable that your system might need – including pieces that are hard to find. 5890. 5890. 5890. 5890. (25/pk) automatic or manual injections* 5 mm solid for high column backpressure.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5 mm through-hole for on-column inlets. 6850 and 6890 GCs (50/pk) 11 mm for 5880. 5890.
Column Ferrule Types Advantages Graphite Easy-to-use. easily deformed or destroyed • possible system contamination • not for use with GC/MS transfer-lines What is the Function Ferrules seal the connection of the column or liner to the system.agilent. Three main types of ferrules are used with capillary GC columns: graphite. Vespel and Vespel-graphite composites. stable seal Higher temperature limit Limitations Soft. An improper ferrule can cause leaks which allow air and other contaminants to enter the instrument through the column seal. and will tolerate temperature cycling. Graphite ferrules can withstand temperatures as high as 450ºC. seals with minimum torque. or other damage before reusing them • change ferrules when new columns or injector/detector parts are installed www. Agilent offers a comprehensive selection of ferrules made of different materials and configurations for a leak-free connection between the column and injector. respectively. and Vespel and Vespelgraphite ferrules are rated to 280ºC and 350ºC. The ideal ferrule provides a leak-free seal. accommodates various column outer diameters. ferrules should be replaced every time the column is replaced and when performing column maintenance. For optimum performance.com/chem 42 . Vespel or Vespel-graphite Mechanically robust Long lifetime Flows at elevated temperature • must retighten frequently • prone to leakage Polymer bleed problematic with some detectors (NPD and ECD) Why Replace Signals that a ferrule is damaged include: • background noise from oxygen diffusing into the system • column bleed catalyzed by oxygen • sample degradation • loss of sample • increase in detector signal/noise • poor retention time reproducibility How to Minimize Problems General technique for installing ferrules: • don’t overtighten – finger-tighten column nut. will not stick to the column or fittings. causing major interference with column and detector performance. chips.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Ferrules Using the wrong ferrule or a worn-out ferrule to seal your column connection can result in inconsistent and unreliable chromatography. then use wrench to tighten • maintain cleanliness • bake out ferrules prior to use (Vespel and Vespel/Graphite only) • avoid contamination – such as fingerprint oils • inspect used ferrules with magnifier for cracks.
verify 4-6mm installation distance) 100% Graphite Ferrules Reusing a ferrule – or using off-brand ferrules – may be a costly mistake.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Ferrule Troubleshooting Problems possible after changing ferrules Normal Peaks Tailing Solvent Peaks Wrong Peak Ratios Normal Peaks Tailing Solvent Peaks Wrong Peak Ratios Correct column positioning in both injection port and FID Column positioned incorrectly in the injection port. TIPS AND TOOLS Do not use 100% graphite ferrules in GC/MS transfer lines. always use new Agilent ferrules. or possible ferrule or septum particle in the carrier gas flow path Column positioned incorrectly in the inlet (either too far or not far enough. Two different types of Agilent column nuts can be used with these ferrules: • The universal column nut (p/n 51818830) has a hexagonal head requiring the use of a wrench to tighten it completely. which feature the highest quality design. That’s because you’ll increase the likelihood of dangerous leaks that can damage the GC column and sensitive detector parts. and are supported by decades of technical expertise. It can only be used with the 100% graphite ferrules.com/chem . They will deform and leak over time. For best results. • The finger-tight column nut (p/n 50208293 for 530um columns and p/n 50208292 for columns 320µm or less) does not require a wrench to tighten. 43 www.agilent. due to the softness of the graphite.
like the ECD.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Vespel/Graphite (85%/15%) Ferrules The combination of graphite and Vespel results in a ferrule having low oxygen diffusion rates which does not shrink to the same extent as pure Vespel. The ferrule hole must match the column OD exactly to ensure a leak-free seal. Vespel/Graphite Nut & Ferrule Combinations Standard ferrule and standard nut Universal Column Nut 5181-8830 + Vespel/Graphite Ferrules 5181-3323 (0. The larger ferrule can also be used to make column connections to inlets and other detectors but requires a specially designed column nut (p/n 05988-20066) to accommodate the longer ferrule. In addition. If left unchecked. and 0.53 mm) www. The standard sized ferrule is compatible with the universal column nut.25 mm ID columns) 5062-3506 (0. When using Vespel/graphite ferrules.1.agilent.25 mm ID columns) 5062-3514 (0.45 and 0. then an additional 1/4 – 1/2 turn with a wrench. an improper seal at the injector will result in high column bleed and a shortened column lifetime. but are also compatible with other detectors like FID and NPDs.2. An improper seal at the detector can result in increased detector signal/noise.com/chem 44 . 0. Proper installation requires a finger-tight turn on the nut.53 mm) Longer ferrule with MS interface nut MS Interface Column Nut 05988-20066 + Vespel/Graphite Ferrules 5062-3508 (0.32 mm) 5062-3538 (0. there is a specific ferrule for each column diameter. Choosing a ferrule with a larger hole than is specified for a given column dimension can result in a large leak. 0. In the case of the MSD it can also contribute to oxidation of the ion source which can increase the frequency of detector maintenance. These ferrules are very hard and cannot be deformed sufficiently to seal multiple column diameters. For capillary column applications. 0.2. the Vespel/graphite ferrules provide added confidence of leak-free connections when installed correctly.1. Agilent recommends tightening the column nut to a 1/4 turn after the first temperature program runs. The second ferrule size is slightly longer and is specifically designed to fit with the MS interface nut used for the GC/MS transfer line connection. Two different lengths of Vespel/graphite ferrules are available for capillary column use.32 mm) 5062-3512 (0. These ferrules are recommended for use with GC/MS or other oxygen sensitive detectors. Even preconditioned ferrules can exhibit some shrinkage after a temperature programmed run.45 and 0.
Most reliable leak-free connection. visit www. VIDEO To view a video on ferrules. So.agilent.com/chem/techsupport. These ferrules do not deform easily. Recommended for MS or oxygen sensitive detectors. Recommended for high temperature and cool on-column applications. oxygen sensitive Suitable for FID and NPD. -----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel 280ºC Isothermal operation. Agilent Ferrule Selection Recommendations Ferrule/Seal Type Upper Temperature Limit Usages Limitations -----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Graphite 450ºC General purpose Not for MS or (100%) for capillary columns.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS 100% Vespel Ferrules Vespel is a high-temperature polyimide based material which is very hard. Can be removed easily. making it an excellent sealing material when making metal or glass connections. The main disadvantage of 100% Vespel ferrules is the shrinkage of the material when exposed to temperature cycling conditions. 100% Vespel ferrules should only be used for isothermal applications. -----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------SilTite N/A Use only with SilTite Nut Kits Not Reusable (100% metal) 45 www.com/chem . it is important to match the ferrule hole size to the proper column diameter. Leaks after (100%) temperature cycle. (85%/15%) capillary columns. detectors. This material has the lowest permeability to oxygen.agilent. -----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel/Graphite 350ºC General purpose for Not reusable.
1 ea 1 ea 1 ea 05988-20066 05921-21170 8710-0510 www.32 0.45.80.32 0.5 0.5 0.2.20-0.8 Preconditioned 85% Vespel.1.8 10/pk Universal column nut. 85% Vespel.com/chema 46 . Always match short nuts with short ferrules and long nuts with long ferrules. hex Finger-tight column nut for 0.4 0.5 1.32 mm columns* and smaller Blanking plug.53 mm columns* Finger-tight column nut for 0. 0.5 10/pk 10/pk 10/pk 5184-3569 5184-3570 5184-3571 5188-2789 0. 1 /4 in. 0.45.1.32 0.25 0. 0. 15% Graphite Ferrules (Short Ferrules) 0. Includes 2 nuts Column Nuts Short Nuts 0.80.25 mm ID capillary columns.53 10/pk 10/pk 10/pk 10/pk 5062-3516 5181-3323 5062-3514 5062-3512 0.3 0. 0. 0.25 0.80. 0.25 0.4 ID holes 0. 0. finger-tight style 6850 Column Nut Long Nuts 2/pk 1 ea 1 ea 1 ea 2/pk 5181-8830 5020-8293 5020-8292 5020-8294 5183-4732 MS interface column nut Column nut for GC/MS ferrules Column nut wrench.53 10/pk 10/pk 10/pk 5181-3322 5062-3513 5062-3511 Specialty Ferrules.1.4 0. 0. 15% Graphite Two Hole No Hole SilTite Metal Ferrules 0. 0.4 0.80. 0.53 0. and 5 /16 in.25 0.25 0.32 10/pk 10/pk 10/pk 5062-3580 5062-3581 5181-3308 For use with 0.2 0.5 0. 0.53 10/pk 10/pk 10/pk 10/pk 5080-8853 5080-8773 500-2114 500-2118 0. 0.2. Includes 2 column nuts For use with 0.05-0. 15% Graphite Ferrules (Long Ferrules) 0.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Ferrule Ordering Information Ferrule Id (mm) General Purpose Graphite Ferrules (Short Ferrules) Column Id (mm) Quantity Part No.1 0. 0.3 0. 0. * For use with graphite ferrules only.4 0.agilent.32 mm ID capillary columns.1. Includes 2 column nuts For use with 1/16 in.5 ID holes 0. 0.1. 1/16 in.8 These ferrules are recommended for use in isothermal analysis only.8 These ferrules are recommended for use with GC/MS. 0.2.53 mm ID capillary columns.4 0. od SS tubing.1.25.8 85% Vespel.2. 0.2.0 0.32 0. Includes 2 column nuts For use with 0.45.53 10/pk 10/pk 10/pk 10/pk 5062-3507 5062-3508 5062-3506 5062-3538 100% Vespel High-Performance Ferrules (Short Ferrules) 0. 0.
47 www. The three liner characteristics that must be considered for each application are: • Liner volume • Liner treatments or deactivation • Any liner design features that might affect carrier gas flow through the inlet or sample vaporization What is the Function Liners are the centerpiece of the inlet system in which the sample is evaporated and brought into the gas phase. visit www.com/chem . So you can get consistent results.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Liners Agilent offers a complete selection of GC split and splitless inlet liners that deliver consistent quality. Why Replace These problems will occur if the liner is not changed on a regular basis or if the correct liner is not used: • peak shape degradation • solute discrimination • poor reproducibility • sample decomposition • ghost peaks • reduced column life How to Minimize Problems Change liners on a regular basis determined by: • previous use pattern • sample cleanliness • chromatographic abnormalities such as: – peak shape changes – peak discrimination – poor reproducibility – sample pyrolysis – active analyte response loss or decomposition VIDEO To view a video on Liners.com/chem/techsupport. Agilent liners are built to Agilent’s precise inlet tolerances which helps ensure optimal dimensional accuracy and inertness toward demanding compounds.agilent. And unlike other manufacturer’s liners. Choosing the proper liner for a specific application can be a difficult and challenging task.agilent.
even deactivated liners can begin to exhibit activity. the liner should be replaced.agilent. and tools might scratch the glass surface of the liner.” then. The elevated temperatures used in the inlet vaporize the liquid sample to a gas for transfer to the head of the column. should be injected without chemical change. click “GC Pressure/Flow Calculator.com/chem/techsupport. with long lifetimes.” www. Liners can be cleaned to remove particulate material or solvent rinsed to remove less volatile components. Agilent liners are deactivated using deactivation procedures that produce reproducible and inert liners. gas samples. TIPS AND TOOLS Agilent offers a free software tool that calculates the vapor volume of an extended list of common solvents. Deactivation agents are used to cover or react with active sites on the glass surface of the liner. Some solvents may remove the deactivation layer. When this occurs. For splitless applications or when even slightly polar compounds must be analyzed. Both can compromise reproducibility and sensitivity. The vaporized sample should be a true representation of the liquid sample and.agilent. choosing the proper liner cleaning procedure can be difficult. it could result in backflash. Click “User Contributed Software. resulting in the generation of unwanted active sites. Liner Deactivation Active sites on inlet liners can adsorb sample components and cause peak tailing. go to www.com/chem 48 . or sample loss caused by expansion into the septum purge or split vent lines. unless specifically desired. With use. To download. The small volume liners have a smaller ID and are usually used with small injection sizes (< 1 µL). and potential loss of sensitivity and reproducibility. or when using external sampling devices like headspace and purge and trap. a deactivated liner should be used. If the volume is too great for the liner.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Discussion of Liner Characteristics Liner Volume The purpose of the injection port is to allow the introduction of a sample into the gas chromatograph in an accurate. fast 100 µm ID columns. reproducible manner. Larger volume liners (> 800 µL) are characterized by larger inside diameters (ID) and are typically used with injection sizes of 1 µL or more. This phase transition is accompanied by a very significant volume change. Backflash also frequently results in sample carryover. The volume of the resulting vapor must be small enough to fit within the volume of the liner. based on your choice of inlet temperatures and pressures for a given Agilent inlet liner. However. A new liner almost always outperforms a cleaned and re-deactivated one – especially for trace analysis.
Glass cup liners are also available with additional glass wool and inert packing to increase reproducibility and limit sample discrimination. The glass wool is positioned or held in place near the center of the liner to: • Provide additional surface area for complete volatilization of the sample to minimize thermal discrimination • Trap non-volatile components and septum particles before they reach the column • Wipe any sample from the syringe needle. Glass wool is generally not recommended for the following analytes: • phenols • organic acids • pesticides • amines • drugs of abuse • reactive polar compounds • thermally labile compounds Glass Cups Another design feature used to help volatilize the sample and provide good mixing is the incorporation of a glass cup inside the liner.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Liner Design Features Dimensions • The outside diameter (OD) of the liner determines if the liner is more effectively used in split or splitless mode • Larger OD liners are designed for splitless operation. Figure 1. Reproducible positioning is important for repeatable quantitative results. its main purpose is simply to trap non-volatile components. Therefore. If glass wool is positioned at the bottom of the liner. 5183-4647 and 5183-4711. you should check the instrument manual for proper installation distances and determine which distance is appropriate for your application. or about 4-6 mm from the column tip to the top of the ferrule (See Figure 1). thereby increasing reproducibility and preventing sample residue build-up at the septum Glass wool liners that have glass wool near the center of the liner.com/chem . fit tightly and limit sample contact with metal parts of the inlet • Larger OD liners improve analyte recovery by retaining more sample inside the liner • Agilent splitless liners are all designed with exacting dimensional tolerances to fit tightly in the inlet and minimize sample contact with metal surfaces • Smaller OD liners are designed for split injection because they produce less resistance to carrier and split flow through the inlet • Large volume liners are used for split injections with enforced dimensional stability for a wide range of split ratios Packing Glass Wool Many liner designs use deactivated glass wool packing. the column must be installed correctly in the injection port with the tip of the column ideally located about halfway into the taper. are recommended for automatic injections. Some applications will work better with different column installation depths. Not recommended for use with Electronic Pressure Control Inlets on 6890 or 6850 GCs. 49 www.agilent. such as Agilent Part Nos. Tapers Tapering or narrowing the liner internal diameter (ID) is done for a number of purposes: • Bottom taper focuses sample onto the head of the column • Bottom taper minimizes contact with metal parts of the inlet • Center taper positions glass wool correctly • Top taper minimizes sample backflash To operate properly.
Remove inlet liner and check cleanliness. See also”Septum Troubleshooting. Column/sample residues could also be the problem. Use new. Remove inlet liner and check cleanliness. adjust if necessary. Use a guard column to prolong column life. Trim the front end of the column a minimum of 6 inches.com/chem 50 . square cut using a reliable capillary fused silica cutting tool (such as a ceramic wafer or the Agilent Column Cutter). Make sure total flow in inlet is above 40 mL/min. Normal Problem Problem Baseline Change After Large Peak Column and inlet liner misaligned. Remove column. then reinstall column. inlet liner or contaminated gold inlet seal. Remedy Use new. Broken or chipped inlet liner. Partially remove packing from liner or use without packing. Needle hitting and breaking packing in inlet liner. Normal Problem Problem www.agilent. Use new. Normal Problem Problem Unresolved Peaks Column or inlet liner contaminated or column deteriorating. deactivated liner or clean old liner and replace glass wool. Make a clean. Normal Problem Column end poorly cut (sample absorption). Baseline Rise Before or After Peak Sample decomposing. Inlet flow too low. deactivated liner or replace glass wool and packing.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Liner Troubleshooting Symptom Tailing Peaks Possible Cause Sample components adsorbed by column.” page 37 Check installation of column end and inlet liner. deactivated liner or replace glass wool and packing.
and wipes any residual sample from the sample needle – reproducibility is the result. Direct Connect liners also eliminate sample exposure to metal parts. The Focus Liner traps a precisely controlled amount of glass wool in the ideal position in the injection port liner. Direct Connect Direct Connect liners are ideal for customers running highly sensitive compounds. These liners are: Direct injection: Straight liner without glass wool. 5183-4647 (with extraordinarily tight dimensional control for optimum split performance). glass bead for easy positioning. 5181-8818 (use only for gas samples. drilled hole in the side of the liner whose size and placement was optimized by Agilent R&D engineers to allow them to work with EPC. 51834647. The liners are deactivated. 5181-3316EN and 5181-3315EN. and deactivated. headspace. or purge and trap applications). come in either a single or double taper. Note: For pesticide analysis – especially DDT and Endrin. deactivated. Intensive liner development and testing have resulted in a set of liners that we recommend whenever new methods are being developed.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Agilent Liners Our engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Agilent Part No. Focus Liner Improve reproducibility. Agilent Part No. where breakdown is a problem – we recommend Agilent Part Nos. there is a small. minimizing inlet-related degradation. In addition to these liners we offer a broad selection of liners for your specific application needs. The graphite seals should be used when inlet temperatures exceed 350ºC. 51 www. or for users who require maximum inertness performance and minimal inlet discrimination for trace GC and GC/MS applications. Liner O-Rings Liners are sealed in the inlet with O-rings or graphite seals.agilent. 5183-4711. and utilize a press fit connection to the column. bottom taper. Agilent Part No. 5181-3316EN. improve results. deactivated. or when problems with existing methods are encountered. These liners are included in our new 8270 EPA Applications kit designed specifically for optimizing a 6890/5973 GC/MSD to this method. O-ring seals are easier to remove and to replace than graphite that deforms and flakes apart. when methods are being optimized. the glass wool provides extra surface area for vaporization. Splitless injection: Single tapered liner without glass wool. but with an outer diameter that compromises for both split and splitless injections. Agilent Part No.com/chem . In addition. traps nonvolatile sample residue. General purpose split/ splitless injection: Similar design to Agilent Part No. At the point of injection. Split injection: Agilent low-pressure-drop split liner with glass wool.
visit www.com/chem/fliptop2 . and into the heated source resulting in multiple problems for the operator including shortened column life and air background in the MS. VIDEO Description Flip Top Inlet Sealing System Liner O-rings (10/pk) www. Once the dirty liner is replaced. or simply awkward to use. Do you want to increase your productivity and column life? 4. the inlet nut must be replaced on the injection port and occasionally the wrench slips off the nut leading to scrapes. The Easiet Way to Change Inlet Liners! Agilent’s new Flip Top Inlet Sealing System is a device designed to allow the user to safely and reliably change an inlet liner in as little as 30 seconds without tools in a consistent leakfree manner. the Flip Top has a levered arm that attaches to any 6890/6850/5890 insert weldment and locks to the injection port using an adapter ring screwed onto the inlet. By the time the operator finishes the procedure and re-equilibrates. no more burns or scrape • Decreased downtime = increased productivity • Minimizes exposure to ambient air extending column life • Installs easily in 15 minutes (customer installable) Questions to ask yourself: 1. smarter way to change inlet liners on Agilent GC’s • Cuts liner replacement time to as little as 30 seconds • No more frustrating searches for special wrenches or tools • Improved inlet ergonomics – no more handling of heated parts. No longer will you have to contend with frustrating searches for wrenches or burning your fingers on hot inlets. It can take at least 5 minutes of wrestling with this hot injection port nut and wrench combination just to take out the old liner and put in a new one. How long does it take you to change a liner (total downtime)? 3. the inlet nut is usually too hot to handle so it must be turned several times with the wrench before it will release the top assembly of the injection port. Do you change liners more than 2-3 times per week? 2. the user simply lifts the arm of the Flip Top which releases the insert weldment from the injection port. and allows instant access to the liner. Once installed.com/chem Part No. too thin. In addition. bent at an odd angle.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Flip Top Inlet Sealing System Agilent’s NEW Flip Top Inlet Sealing System is the faster. Have you ever burned your fingers or scraped your knuckles trying to open a hot inlet? One of the most frequent maintenance tasks customers face when running a GC or GC/MS system is changing the inlet liners.agilent. Available exclusively from Agilent. doing this with a GC/MS causes even more problems as ambient air is drawn into the capillary column. and cuts. The process is simply reversed to re-seal the weldment to the port. The special wrench used for this operation is often misplaced.agilent. burns. 5188-2717 5188-2741 52 To view videos on the Flip Top Inlet Sealing System. A hot inlet may have to be opened on each system every 24 to 48 hours to change a dirty inlet liner. through the hot MS interface. it can result in 15 minutes of downtime! Of course.
agilent. or purge and trap applications) For split/splitless injection 250 5181-8818 5183-4703 5183-4704 Liner. straight. 4 mm ID. splitless 4.0 mm ID Split Inlet Liner Liner.0 mm 4. headspace. direct.5 mm 6. deactivated Liner. low press. split. non-deactivated. split. glass wool. deactivated NEW! Liner. deactivated 870 5183-4711 5183-4712 5183-4713 Splitless Inlet Liners Liner.3 mm X 78. glass wool. deactivated Dual taper direct connect liner. 5180-4182 5180-4173 5180-4168 5188-2741 Dimensions 6.0 mm Wool Yes Yes 250 140 18740-80220 18740-80200 5183-4707 5183-4709 5183-4708 5183-4710 990 990 800 800 19251-60540 18740-80190 18740-60840 210-3003 5183-4691 5183-4699 5183-4697 210-3003-5 5183-4692 5183-4700 5183-4698 Part No. splitless. deactivated Focus Liners Focus liner Focus liner ID 4.5 mm Liner O-Rings Fluorocarbon O-ring (12/pk) Graphite O-ring for splitless liner (10/pk) Graphite O-ring for split liner (10/pk) Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk) 53 www.com/chem .SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Liner Ordering Information Application Agilent Choice Liners Liner. for manual injection Direct Connect Liners Single taper direct connect liner. 4 mm ID. taper. headspace. with cup. glass wool. double-taper. with cup. no glass wool. non-deactivated [use for gas samples. direct. non-deactivated Split Inlet Liners For Manual Injection Liner. Single-taper. deactivated NEW! Liner.3 mm X 78. no glass wool. taper. Splitless. drop. Splitless. single-taper. quartz Liner. polymerically deactivated Liner. deactivated Liner Volume(µl) 870 Single Liner 5183-4647 5/pk 25/pk For split injection 5183-4701 5183-4702 For splitless injection For trace pesticide analysis 900 900 5181-3316 5181-3316EN 5183-4695 5183-4696 For direct injection (use for gas samples. glass wool. polymerically deactivated For trace pesticide analysis 900 800 800 5062-3587 5181-3315 5181-3315EN 5183-4693 5183-4705 5183-4694 5183-4706 Direct Inlet Liners Liner. double-taper. 1. 2 mm ID. splitless. general purpose split/splitless. no glass wool Liner. direct. or purge and trap applications] Liner. splitless. split. deactivated Liner. glass wool. 2 mm ID. no glass wool. single-taper. G1544-80730 G1544-80700 Part No.5 mm ID. 210-4004-5 210-4022-5 Part No. no glass wool. split. and packing [not recommended for use with electronic pressure control (EPC)].
D. 10/pk – Part No.50 mm I. for 6890 GC with EPC Viton O-Ring Part No. 5062-3516. Our inlets are backed by the same 40 years of design experience that you’ve come to expect from our instruments. 12/pk Reducing Nut Part No. for 320 µm Columns.D. Agilent supplies every replacement part that your system might need – not just a few select pieces. 2/pk www. 12/pk Liners See page 47 Heater-Sensor Assembly Part No.D.com/chem. 0. G1544-61140 TIPS AND TOOLS For a complete parts breakdown. all in one place. Gold-Plated Seal (Splitless) See page 55 Retaining Nut Part No. G1544-20590 Washer Part No. don’t settle for imitations. 0. 18740-20800. for 250 µm Columns.. see the 5890.40 mm I. 5061-5869.. choose only genuine Agilent parts.agilent. 18740-60835 Septum See page 36 Split/Splitless Inlet Weldment Part No. 15% Graphite) – Part No. 10/pk – Part No.D. or visit www.74 mm I. for 100-200 µm Columns. 6890.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Instrument Inlet Parts and Supplies When it comes to inlet replacement parts for your Agilent GCs. 0. 10/pk – Part No. So you can get all your consumables.37 mm I.agilent. 0. 5180-4182. G1544-60575. 5181-8830. 5181-3323. 5062-3512. plus the reproducible results that your lab demands..com/chem 54 . So you get optimal performance. 1 each Ferrules (85% Vespel.. for 530 µm Columns. What’s more. 5062-3514. and 6850 series GC Instrument User and/or Service Manuals. Septum Nut Part No. 10/pk Column Nut for 6890 GC Part No.
Similar to G1544-60575 except carrier lines separated for interface to valved systems of a G1540A instrument. see the 5890. Top Bottom Gold-plated seal with cross p/n 5182-9652 Use when inlet flow exceeds 400 ml/min. Liner Seals and Washers Stainless steel Gold-plated seal Gold-plated seal with cross Washers (12 pk) 18740-20880 18740-20885 5182-9652 5061-5869 Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity.com/chem . Used with large charcoal canister type filter for 6890/6850. 19251-60575 G1544-60575 G1544-80580 G1544-60585 G1580-60575 G1580-60585 5890 Split/Splitless Multimode Inlet Supplies Septum retainer nut 18740-60835 Retainer nut for headspace sampling 18740-60830 Retaining nut 19251-20620 Reducing nut 18740-20800 For a complete parts breakdown. This insert assembly uses the large charcoal canister split vent filter for 6890/6850. Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to clean carrier gas for ECD operation.agilent. Gold-plated seal p/n 18740-20885 55 www.SAMPLE INTRODUCTION CONSUMABLES & GC INLETS Part No. 6890/6850 Split/Splitless Insert Assemblies Standard manual pneumatics Original standard EPC using 1/4" split vent filter. S/SL insert weldment. 6890 and 6850 series GC Instrument User and/or Service Manuals. and may compromise your results. Other manufacturers’ seals are not machined. S/SL insert assembly for G1540A with valved system option.
agilent.” Phil Stremple.000 different columns.Columns Choosing the right GC column and following Agilent’s simple column care recommendations will maximize GC column performance and lifetime. as well as appropriate recovery measures. plus give helpful hints about avoiding thermal and oxygen degradation.agilent. for nearly 40 years.com/chem 56 . www. Because GC column contamination is the primary cause of shortened column lifetime. It’s no wonder that. install and store your GC column. customers have built products – and entire businesses – around the results they get from our DB.and HPcapillary GC columns. GC Columns Program Manager CATALOG For a complete selection of GC columns and parts. “Agilent lets you choose from over 1. see Agilent’s 20052006 Essential Chromatography Catalog. we’ve also included a detailed discussion about the prevention of non-volatile and semi-volatile contamination. visit our online catalog at www. Or.com/chem/4ecatalog. In this section our experts offer practical advice on how to select.
Column bleed is the natural degradation of the stationary phase that occurs at higher temperatures.d.agilent. and avoiding the primary factors that cause column performance degradation (breakage. but there are some dimensional considerations. and most stationary phases can be used with a GC/MS system. the main focus should be how to obtain the highest performance and lifetime from a capillary column. chemical damage and contamination). the frequency and type of column maintenance that is required varies due to many system and sample factors. There are a few simple rules for choosing columns with lower bleed levels: • Choose a low-bleed phase for your application – Agilent has developed several low-bleed versions of the most popular phases. 57 www. These are chemically designed to possess minimal levels of column bleed possible and often have the benefit of an increased uppertemperature limit. Instead of simply following a predefined timetable of maintenance items. Many types of GC column phases can be used with the MSD. • If a low-bleed column is not available. Column bleed will deposit in the MSD ion source. which can decrease MSD performance.COLUMNS Column Maintenance While GC column maintenance is simple. This depends on choosing the right column.25mm i. it is a good idea to choose a phase for your application that has the lowest amount of column bleed as possible. oxygen damage. but try to make it the least polar column that will do the job) Primary “Quantion” is hidden Primary “Quantion” is enhanced Dimensions All dimensions can be used with conventional GC systems. The amount of bleed will rise with increases in polarity. the column flow should be 1mL/min (2mL/min for Performance Turbo Pumps). and length. film thickness. However. column length and internal diameter combinations are restricted to provide the appropriate flow to the GC/MS. you will help reduce the frequency of required ion source maintenance. By minimizing the amount of column bleed. The maximum allowable flow rate and optimal sensitivity flow rates will vary depending upon the type of pump. thermal damage. In general. and smaller) can be installed directly into the GC interface. Selection of Capillary Columns for GC and GC/MS Phases All phases can be used with conventional GC systems. (Choose a more polar phase when you must. • Narrow-bore columns (0. correct installation/system setup. which appears as an elevated baseline as the temperature rises to the column’s upper thermal limit. • Use more polar phases when difficult isomer separations are required.com/chem . choose a low-polarity column with a moderate film thickness. Therefore.
If using a wide-bore column with a shorter length. an effluent splitter or jet separator should be utilized.25µm DB-35ms. & Conditioning The first step in obtaining optimal column performance and lifetime is proper installation: • Choose the appropriate size and material ferrule for the column. injector and detector type.25mm i. 0. When the column and inlet are first heated. See pages 104-115 for more information about our services and support.25µm Part No. Conditioning the column briefly prior to installation into the MSD will minimize the contamination brought into the ion source.25µm HP-5ms. For these columns. • Briefly conditioning a column before installing it into the GC/MS interface is recommended.25µm HP-INNOWax.25mm i. 0. Setup. 0. even at your site.25µm DB-XLB. 30m. an effluent splitter or jet separator should be installed. • Verify that all fittings are leak-free and the carrier gas is oxygen-free before heating the oven. • Avoid re-using ferrules.d.32mm should not be directly interfaced into the GC interface.d. • The column should be placed on a column hanger and no portion of the capillary tubing should touch the oven walls. These materials are then carried by the carrier gas into the MSD and can deposit in the MSD ion source. 30m. TIPS AND TOOLS Tap Agilent’s GC knowledge over the phone..COLUMNS Popular Column Choices • Wide-bore columns (0. • Use an appropriate column cutting tool such as a ceramic wafer or diamond tipped scribe. 0. 0. www. This can decrease MSD performance. • Columns with internal diameters greater than 0..) that are 30m or longer can be installed directly into the 5973 GC interface (other MSDs may require 50m or longer). 0.d.. 30m. 0.25mm i.25mm i. 0..32mm i. in the classroom.agilent.com/chem 58 . 30m. • Install the column the appropriate distance into the injector and detector as specified by the GC manufacturer. 0. 0. volatile materials within the flow-path and a small portion of the column stationary phase move into the gas phase. Description DB-1ms. • Make sure column ends are cleanly cut and free of particulate matter before installing into the injector and detector.d. online..25mm i. 30m.d.d. 122-0132 19091S-433 122-1232 122-3832 19091N-133 Column Installation.
While under these stresses. damage to the stationary phase is very likely. (0. 705-0905 5181-3396 500-1200 Recovery • If a broken column has been heated.5mm ID. Discard the back of the column (the column half without carrier gas). vibrations caused by the oven fan as well as being wound on a circular cage all place stress on the tubing. • Avoid winding or bending the column too tightly.53mm id) are more prone to breakage. • Condition the column as specified in the literature provided with each column. Continuous heating and cooling of the oven. NOTE: Larger diameter columns Description Fused Silica Union.agilent.32mm) 10/pk General Purpose Graphite ferrule (1. 5181-8836 430-1020 20x Magnifier General Purpose Graphite ferrule (0. • If the broken column has not been heated. metal edges in the GC oven.0mm ID. Trim 6 inches off the end of the column and reinstall.45-0. for column IDs ≤ 0. No more than 2-3 unions should be installed for one column. column cutters and other miscellaneous items on the lab bench. connect the two pieces with a low volume union. for 0.45.53mm ID columns) 10/pk Gas leak detector 115V Gas leak detector 220V 5080-8853 Good 5080-8773 5182-9646 5182-9648 Example of column cuts • Check the installation and set the linear velocity by injecting a non-retained compound. flaws will propagate until breakage occurs.com/chem .COLUMNS Column Installation & Setup continued Description Ceramic wafer (4/pk) Bad Part No. Universal 2-way (5/pk) Quartz deactivated column connector (5/pk) Polyimide Sealing resin (5 grams) Part No. 59 www. Prevention • Avoid scratches and abrasions by not exposing the column to sharp edges such as column hangers and tags. Causes of Performance Degradation Column Breakage Fused silica columns can break wherever there are small scratches or abrasions in the protective polyimide coating.0.
1/8" fitting) Big Universal Trap (Combination Trap) (750cc. 50/pk) Part No. the column is irreversibly damaged. Oxygen Damage Oxygen is an enemy to all capillary GC columns. The life of the column will be reduced after thermal damage. With two columns in the oven be sure to set the maximum temperature to the temperature limit of the column with the lowest value. The column usually does not return to its original performance. septa) is the most common source of oxygen exposure. In less severe cases. www. 5183-4780 BOT-2 BMT-2 RMSH-2 5183-4759 TIPS AND TOOLS Install a moisture trap upstream of the oxygen trap to increase the oxygen trap lifetime. This results in the premature onset of excessive column bleed. A leak in the carrier gas flow path (e. injector.. Description FlowTracker 2000 Flowmeter and Leak Detector Big Oxygen Trap (750 cc. very rapid degradation of the stationary phase occurs. however.agilent. peak tailing for active compounds and/or loss of efficiency (resolution). He) Advanced Green Septa (11mm. however. NOTE: Oxygen damage occurs very rapidly. gas lines.g. This results in the premature onset of excessive column bleed. severe damage occurs as the column temperature increases. Recovery Perform column “bakeout” as described under thermal damage recovery. NOTE: Momentary exposure to oxygen such as an injection of air or removing the septum nut for a short period of time is not a problem. column should only be held there for about 5-10 minutes • Set the GC maximum oven temperature function at or a few degrees above the temperature limit of the column.COLUMNS Thermal Damage Exceeding a column’s upper temperature limit results in accelerated degradation of the stationary phase and tubing surface. peak tailing for active compounds and/or loss of efficiency (resolution). 1/8" fitting.com/chem 60 . Prevention Maintain an oxygen and leak-free system by: • performing periodic leak checks • changing septa regularly • using high quality carrier gases • installing and maintaining oxygen traps • changing gas cylinders before they are completely empty Prevention • Do not exceed the columns specified upper temperature limits: – Isothermal limit: temperature that the column can be held at for an indefinite time – Programmed limit: maximum column temperature. Recovery • Disconnect column from detector • Heat the column 8-16 hours at the isothermal limit • Remove 10-15 cm from the column end • Reinstall into the detector and condition as usual NOTE: Thermal damage cannot be reversed. the column may still be functional but at a reduced performance level. In more severe cases. it is often still functional. fittings. Constant exposure to oxygen does not damage the column at or near ambient temperatures. 1/8" fitting) Big Moisture Trap (750 cc. As the column is heated.
This greatly reduces the interaction between the residues and the sample. Thus. The only organic compounds that have been reported to chemically damage stationary phases are perfluoroacids and these need to be present at high levels (e. GUARD COLUMN A guard column is a piece of fused silica tubing attached with a union to the front of the analytical column with the following characteristics: • Material should be deactivated fused silica tubing to minimize solute interactions.” then “GC Reference Library.agilent. Unfortunately. Guard columns with larger ids can be used for additional residue capacity.com/chem.” The procedure can be found under “General Information. but it may be rendered unusable.com/chem . DuraGuard columns offer the guard column built into the analytical column as a single piece of fused silica. Typical lengths of 5-10 meters allow substantial trimming before the entire guard column has to replaced. Most of these acids and bases have low volatility and accumulate at the front of the column. Guard columns are used to minimize the effect of non-volatile residues on the analysis. 1% or higher).agilent. • Internal diameter are generally the same as the column. The non-volatile residues deposit in the guard column and not in the analytical column. eliminating the need for unions. minimizing water retention will render these compounds relatively harmless to the column. • A low volume union should be used to attach the tubing to the column. Click on “Technical Support.” 61 www. peak tailing for active compounds and/or loss of efficiency (resolution).COLUMNS Chemical Damage Inorganic or mineral acids and bases are the primary sources of chemical damage to stationary phases. There are two basic types of contaminants: nonvolatile and semivolatile.5 to 1 meter from the front of the column • Severe cases may require the removal of 5 or more meters Guard Column Column Column Contamination Column contamination is the most common problem encountered in capillary GC. If allowed to remain. the acids or bases damage the stationary phase. The onset of peak shape problems is the usual indicator that the guard column needs trimming or changing.g. This results in the premature onset of excessive column bleed. it mimics most other chromatographic problems and is often misdiagnosed. • Length should be from 1-10 meters. A contaminated column is usually not damaged. Glass pressfit unions are inexpensive and easy to install. Prevention • Perform sample preparation to remove inorganic acids and bases from the sample • Install guard column and trim frequently • If acids or bases must be used choose an organic alternative or HCl or NH4OH Guard Column INJECTOR DETECTOR Recovery • Remove 0. NOTE: Hydrochloric acid and ammonium hydroxide are the least harmful of the group as both tend to follow any water that is present in the sample. Periodic cutting or trimming of the guard column is usually required upon a build-up of residues. Union Guard column installation instructions are available at www.. if HCl or NH4OH are present in a sample.
Active solutes are those containing a hydroxyl (-OH) or amine (-NH) group. they may cause peak shape and size problems and. deactivated (5/pk) Quartz deactivated column connector (5/pk) Polyimide sealing resin (5 grams) Deactivated Fused silica. the column ends need to be trimmed by 2-4 cm to ensure that a small piece of septa is not lodged in the column. there should always be carrier gas flow through the column. detector and transfer lines are turned off (i. If you can see anything where the drop was. Place GC septa over the ends to prevent debris from entering the tubing. Capillary column rinse kit Part No. Also. NPD. 0. wander. If a column is left in a heated GC. Put the slide over the heated GC inlet for 20 minutes. drift.com/chem 62 . The carrier gas flow can be turned off only if the oven. 1. injector.e.d. Place 20-30 µL of the sample onto a microscope slide. 10m. not heated).53mm i. no glass wool. Recovery • Bakeout the column: limit 1-2 hours (excess baking may polymerize some contamination and reduce column lifetime) • Solvent rinse the column Semivolatile Contaminants Semivolatile contaminants or residues accumulate in the column.). Without carrier gas flow. in addition. Upon reinstallation of the column.25mm i. Hold the slide up to the light. 3. are usually responsible for many baseline problems (instability. but eventually elute. ghost peaks. Description Split/Splitless Inlet liner: glass wool. 0. deactivated (5/pk) Splitless Inlet liner: single-taper. www. Deactivated Fused silica. Hours to days may elapse before they completely leave the column. Like nonvolatile residues. taper. Does Your Sample Have Residues? Perform this simple test. 2.agilent.5 to 1 meter of the front of the column • Turn the column around (install detector end into injector).d. 5183-4712 5183-4695 5181-3396 500-1200 160-2535-10 160-2255-10 430-3000 Prevention • Perform sample cleanup to remove nonvolatile materials from the sample • Use injection port liners packed with glass wool (may not be feasible when analyzing active compounds) • Install a guard column and trim regularly Recovery • Do not bakeout the column • Front End Maintenance: – Clean or change the injection port liner – Clean out the injector – Cut off typically 0. • Solvent rinse the column • Cut the column in half and use the back half (detector side) Prevention • Perform sample cleanup to remove semi-volatile materials from the sample • Increase the final temperature of the GC run (not to exceed the temperature limit of the column) • Change septa regularly Column Storage Capillary columns should be stored in their original box when removed from the GC. and MS detectors. your sample has residues. and some thiols (-SH) and aldehydes.. 10m. The column becomes coated with these residues which interfere with the proper partitioning of solutes in and out of the stationary phase. Not recommended for sensitive ECD. etc. damage to the heated portion of the column occurs. the residues may interact with active solutes resulting in peak adsorption problems (evident as peak tailing or loss of peak size).COLUMNS Nonvolatile Contaminants Nonvolatile contaminants or residues do not elute and accumulate in the column (most often confined to the first few meters).
PCBs. 63 www.32 0.10 0.10 0.33 0.32 0.10 0.25 0.COLUMNS Column Types and Characteristics DB-1ms • 100% Dimethylpolysiloxane • Identical selectivity to DB-1 • Nonpolar • Very low bleed characteristics • Improved acid performance compared to standard 100% Dimethylpolysiloxane columns • Improved signal-to-noise ratio for better sensitivity and mass spectral integrity • Excellent general purpose column • Bonded and cross-linked • Solvent rinsable DB-1ms Order Guide Temperature Limits (-60 to 340/360°C) I.10 0.33 0. CP-Sil 5CB Applications General purpose: Amines.25 Part No.25 0.40 0. phenols. hydrocarbons.10 0.40 0.25 0. sulfur compounds. 0.com/chem .25 0.agilent.10 0.25 0. flavors and fragrances.20 0. Rtx-1ms.20 0. 127-0112 127-0113 127-0122 127-0123 128-0112 128-0122 122-0131 122-0132 122-0162 123-0131 123-0132 123-0162 Similar Phases HP-1ms.25 0.10 0.D.10 0.32 Length 10 10 20 20 12 25 30 30 60 30 30 60 Film 0. pesticides.
32 0.25 0.32 0. alkaloids.25 0.50 0. pesticides.25 0.32 0.agilent.25 0.25 1. CP-Sil 8CBms.32 0. FAMEs.33 0.32 0.20 0.18 0.18 0.25 0.18 0.25 0.00 0. BPX-5 Semivolatiles.25 0.10 0.com/chem 64 .25 0.25 0.25 0. HP-5ms. DB-5ms.25 0.10 0. Rtx-5 Amine Applications Semivolatiles.25 0.32 0.D. Length Film Part No. 0.25 0.33 0.25 0.25 Applications 121-5522 121-5542 128-5522 128-5552 122-5522 122-552A 122-5531 122-5532 122-5536 122-5552 122-5561 122-5562 123-5531 123-5532 123-5536 123-5552 123-5561 123-5562 Rtx-5ms. Length Film Part No. halogenated compounds. PTE-5. www.33 0. 0.00 0. drugs. FAMEs.25 19091S-101 19091S-102 19091S-105 19091S-331 19091S-431 19091S-231 19091S-333 19091S-433* 19091S-133 19091S-336 19091S-436 19091S-211 19091S-112 19091S-313 19091S-413 19091S-113 19091S-316 19091S-416 Similar Phases Rtx-5ms.50 0.52 0.20 0. drugs.32 0.50 0. BPX-5. PTE-5.10 0. herbicides HP-5ms • (5%-Phenyl)-methylpolysiloxane • Nonpolar • Very low bleed characteristics • Excellent inertness for active compounds • Improved signal-to-noise ratio for better sensitivity and mass spectral integrity • Bonded and cross-linked • Solvent rinsable • Certified for MS • Equivalent to USP Phase G27 HP-5ms Order Guide Temperature Limits (-60 to 325/350°C) I.32 12 25 50 15 15 15 30 30 30 60 60 15 25 30 30 30 60 60 0.25 0.50 0.25 1.32 0.25 0.25 0.32 0.32 0.25 0.40 0.COLUMNS DB-5ms • Phenyl Arylene polymer equivalent to a (5%-Phenyl)-methylpolysiloxane • Nonpolar • Very low bleed characteristics • Excellent inertness for active compounds • Improved signal-to-noise ratio for better sensitivity and mass spectral integrity • Bonded and cross-linked • Solvent rinsable • Certified for MS • Exact replacement of HP-5TA • Close equivalent to USP Phase G27 DB-5ms Order Guide Temperature Limits (-60 to 325/360°C) I.33 0.20 0.10 0.25 0.33 0.25 0.10 0.25 0.25 0. CP-Sil 8CBms. alkaloids.20 0.18 0.25 0.20 0. halogenated compounds.32 0.10 0.D.10 0. herbicides * This column is shipped with the 5973 MSD. pesticides.32 Similar Phases 20 40 25 50 25 25 30 30 30 50 60 60 30 30 30 50 60 60 0.10 0.25 0.10 0.
20 0.18 0.50 1.10 0.D.25 0. drugs of abuse 65 www.25 1.25 0.20 0.20 0.25 0. phenoxy acid methyl esters.10 0.25 0. 0.32 0.32 Similar Phases Rtx-35.com/chem . haloacetic acids DB-35ms • Equivalent to a (35%-Phenyl)methylpolysiloxane • Midpolarity • Very low bleed characteristics • Extended temperature limit of 360°C • Excellent inertness for active compounds • Certified for MS • Ideal for confirmational analyses • Bonded and cross-linked • Solvent rinsable • Replaces HP-35ms • Close equivalent to USP Phase G42 DB-35ms Order Guide Temperature Limits (50 to 340/360°C) I.COLUMNS DB-XLB • Exceptionally low bleed • Low polarity • Extended temperature limit of 360°C • Unique selectivity • Excellent inertness for active compounds • Ideal for confirmational analyses • Excellent for pesticides. PCBs. herbicides. pesticides.50 0.25 0.25 0.33 0.25 0. PCBs and PAHs • Certified for MS • Bonded and cross-linked • Solvent rinsable DB-XLB Order Guide Temperature Limits (30 to 340/360°C) I. chlorinated herbicides.18 0.25 0.32 Similar Phase MDN-12 20 30 12 25 15 15 15 30 30 30 30 60 30 30 30 60 0.32 0.25 Applications 121-1222 121-1232 128-1212 128-1222 122-1211 122-1212 122-1213 122-1231 122-1232 122-1236 122-1233 122-1262 123-1231 123-1232 123-1236 123-1262 PCB congeners. pharmaceuticals. Sup-Herb 15 25 15 30 30 60 30 60 0.25 0. 0.15 0.00 0. haloacetic acids.25 0. Length Film Part No.32 0.25 0.25 Applications 128-3812 128-3822 122-3812 122-3831 122-3832 122-3862 123-3832 123-3862 Aroclors. AT-35.D.10 0.25 0. Length Film Part No.00 0.25 0. SPB-35. pesticides.25 0.18 0.25 0.20 0.18 0.33 0.25 0.25 0.25 0.32 0. amines.33 0.agilent.33 0.25 0. chlorinated herbicides.
25 0. CP-Sil 43CB.32 Similar Phases 20 15 15 30 30 60 30 30 0.agilent.com/chem/4ecatalog www.25 Applications 122-2912 122-2932 122-2962 123-2932 HP-225. HP-50+.32 0.18 0.COLUMNS DB-17ms • Equivalent to (50%-Phenyl)methylpolysiloxane • 320/340°C Upper temperature limit • Very low bleed midpolarity column • Excellent inertness for active compounds • Enhanced mass spectral integrity • Bonded and cross-linked • Solvent rinsable • Best column for CLP pesticides DB-17ms Order Guide Temperature Limits (40 to 320/340°C) I.25 0.18 0. SP-2330. neutral sterols EASY ONLINE ORDERING Need a column that’s custom-designed for your lab? Just visit www.25 0.25 0. glycols. 0.com/chem 66 .25 0. BP-225. 007-225 Alditol acetates.25 0.25 0. BPX-50. SPB-50. Length Film Part No.25 0. FAMEs.25 0. Rtx-50.15 0. SPB-17 Drugs.15 0.25 0.15 0. Rtx-225. pesticides. CB-225. steroids DB-225ms • Equivalent to (50%-Cyanopropylphenyl)methylpolysiloxane • Mid/high polarity • Excellent for separations of cis.25 0.25 0. OV-225.25 0.D.and trans-fatty acid methyl esters (FAMEs) • Low bleed • Bonded and cross-linked • Solvent rinsable • Close equivalent to USP Phase G7 DB-225ms Order Guide Temperature Limits (40 to 240°C) I.25 Applications 121-4722 122-4711 122-4712 122-4731 122-4732 122-4762 123-4731 123-4732 DB-17. 0.32 Similar Phases 15 30 60 30 0. Length Film Part No. 007-17.agilent.D. SP-2250. RSL-500.25 0.
D. trace-level sulfurs.25 0.32 0.32 0. 0. DB-WAXetr Applications Alcohols.25 0. CO2. solvents GS-GasPro • Unique bonded PLOT column technology • Excellent choice for light hydrocarbons and sulfur gases • Retention stability not affected by water • Separates CO and CO2 on a single column • Ideal PLOT column for GC/MS – no particles GS-GasPro Order Guide Temperature Limits (-80 to 260/300°C) I.40 0.50 0.50 0. SF6.COLUMNS HP-INNOWax • Polyethylene glycol (PEG) • High polarity • Highest upper-temperature limits of the bonded PEG phases • Column-to-column repeatability • Bonded and cross-linked • Solvent rinsable • Close equivalent to USP Phase G16 HP-INNOWax Order Guide Temperature Limits (40 to 260/270°C) I. Stabilwax. 007-CW.15 0.15 0.20 0.agilent.25 0.32 25 25 50 50 30 30 30 60 60 60 30 30 30 60 60 60 0. CB-WAX. BP-20.50 0.32 0.32 Length 30 60 Part No. inorganic gases.20 0. Length Film Part No.com/chem .50 19091N-102 19091N-202 19091N-105 19091N-205 19091N-033 19091N-133 19091N-233 19091N-036 19091N-136 19091N-236 19091N-013 19091N-113 19091N-213 19091N-016 19091N-116 19091N-216 Similar Phases HP-20M. CP-WAX 52CB.25 0.15 0. SUPEROX II. 0.25 0.15 0.20 0. halocarbons.25 0. Carbowax. essential oils.32 0.20 0.25 0. aromatics. hydride gases.25 0. 67 www.40 0.D.25 0.32 0.20 0.20 0.32 0. SUPELCOWAX 10. 113-4332 113-4362 Similar Phase CP-Silica PLOT Applications C1 to C12 hydrocarbons.25 0. oxygen/nitrogen separation at -80°C.
agilent. including FID. maintain and replace common detectors. “GC detectors are highly sensitive systems that are often compromised by various types of contamination.com/chem/4ecatalog. learn how to resolve flame ignition problems associated with your flame photometric detector and test electron capture detectors for radioactivity leaks. GC system performance will deteriorate and can cause detector failure. visit our online catalog at www. you can minimize instrument downtime and keep your GC system working at peak efficiency. see Agilent’s 2005-2006 Essential Chromatography Catalog. By implementing some recommended detector maintenance routines. Or. ECD.” Bernhard Rothweiler Applications Chemist CATALOG For a complete selection of Detector supplies. www. Without routine detector maintenance.Detectors Most detectors require simple but periodic cleaning to maintain peak performance. For example.agilent. TCD. NPD.com/chem 68 . Also included are special handling techniques and specific recommendations to maximize specific detector operations. Detailed procedures on how to clean. This is especially true for highly sensitive GC detectors. and FPD are summarized in this section.
Flame Ionization Detector (FID)
Flame Ionization Detectors require little maintenance to keep them performing at satisfactory levels. The primary task is to occasionally measure hydrogen, air and makeup gas flows. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be independently measured to obtain the most accurate values.
Igniter Glow Plug Assembly
Since the FID combustion process results in water formation, the detector temperature must be kept above 100˚C to prevent condensation. Such condensation, especially when combined with chlorinated solvents or samples, causes corrosion and sensitivity loss.
If the flame goes out or will not light: • Check the column flow rate. It may be too high. Decrease the flow rate or pressure. Switch to a more restrictive column (longer or with a smaller id). If you must use a large id column, first cool the GC oven to below 50˚C, then turn off the carrier flow long enough to allow the FID to light. Check for partially or completely plugged jet. • Check that the right type of jet is installed for the column you are using. • Injecting large volumes of aromatic solvent or water can cause the flame to go out. Switch to a nonaromatic solvent or inject less solvent. • The lit offset value may be too low or too high. Adjust the value.
Cleaning & Replacement
Even with normal use, deposits develop in the jet and detector (usually white silica from column bleed or black carbonaceous soot). These deposits reduce sensitivity and cause chromatographic noise and spikes. Although you can clean the jet, it is usually more practical to replace dirty jets with new ones. If you do clean the jet, be careful not to scratch the jet internally; scratches will ruin the jet
FID Cleaning Kit, P/N 9301-0985
To view a video on FID column installation, jet replacement, collector maintenance, or ignitor replacement, visit www.agilent.com/chem/techsupport.
Jet Cleaning Procedure
(using Agilent’s FID Cleaning Kit #9301-0985)
6890/6850 Ionization Detector (FID) Supplies
Item Description 1 2 3 4 5 6 7 9 PTFE chimney (optional)** Collector nut Spring washer Ignitor castle Optional Hastelloy Ignitor Castle* Ignitor glow plug assembly Collector insulator Collector body Hastelloy Collector Body FID collector assembly 1 Detector insulation assembly FID collector cleaning brush Collector Housing FID retainer nut wrench (5880, 5890, 6890) 1/4 in. Nut Driver for FID jet-drilled shaft FID supplies kit-Includes: Jet, packed standard FID performance evaluation sample kit Ignitor glow plug assembly Jet, cap. series 530 µm FID flow measuring insert Cleaning wires for 0.03 in. ID jet Cleaning wires: 0.018 in. ID/530 µm jet Wire, jet cleaning, Capillary inlet cleaning wires Detector cleaning kit 3 each 2 each 2 each 3 each 2 each 1/pk 5 each 2/pk 10/pk Unit Part No. 19231-21050 19231-20940 5181-3311 19231-20910 19231-21060 19231-60680 G1531-20700 G1531-20690 61531-21090 G1531-60690 G1531-20700 8710-1346 G1531-20740 19301-00150 8710-1561 5182-3450 18710-20119 18710-60170 19231-60680 19244-80560 19301-60660 5180-4150 5180-4152 19301-20720 5180-4153 9301-0985
1. Run a cleaning wire through the top of the jet. Run it back and forth a few times until it moves 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. A loss of sensitivity, poor peak shape and/or lighting difficulties may result if the opening is deformed.) 2. Fill an ultrasonic cleaning bath with aqueous detergent, and place the jet in the bath. Sonicate for five minutes. 3. Use a jet reamer to clean the inside of the jet. 4. Sonicate again for five minutes.
NOTE: From this point on, handle the parts
only with forceps! 5. Remove the jet from the bath and rinse it thoroughly, first with hot tap water and then with a small amount of GC-grade methanol. 6. Blow the jet dry with a burst of compressed air or nitrogen, and then place the jet on a paper towel and allow it to air dry.
**Not included in assembly. *Hastelloy components may be used when analyzing highly corrosive materials. 1 Does not include Hastelloy component.
Plugged FID jet
EASY ONLINE ORDERING
Here’s another time-saving reason to place your order through our website: you can instantly view and edit the items in your shopping cart – while keeping track of your total order price. Just visit www.agilent.com/chem/4ecatalog
Jets for capillary dedicated FID
Length(mm) 48 48
Part No. G1531-80560 G1531-80620
Capillary jet (0.011 in./0.29 mm ID tip) High-temperature jet (SimDIS 0.018 in. ID tip)
Capillary 0.53 mm jet (0.011 in. ID tip) Packed (0.018 in. ID tip) Packed (0.030 in. ID tip) 0.53 mm high temp (0.018 in. ID tip) for SimDIS
61.5 63.5 63.5 61.5
19244-80560 18710-20119 18789-80070 19244-80620
Agilent FID Jets (from top to bottom): Dedicated capillary, Adaptable capillary, Adaptable packed
Description FID flow measuring insert FID ignitor cable FID Performance evaluation sample kit, 0.03% C14, C15, and C16 normal alkanes in hexane O-rings Cleaning wire Jet cleaning wire for 0.03 in. ID jet Jet cleaning wire for Series 530 mm and 0.018 in. ID jet
Part No. 19301-60660 G1531-60680 18710-60170
8 6 7
12/pk 5/pk 5/pk
5080-4978 19301-20720 5180-4150 5180-4152
6890 Series GC FID Detector
TIPS AND TOOLS
Different size jets are available to optimize flame shape for capillary columns, or reduce contamination build-up for high molecular weight eluents. Usually, small bore jets produce the greatest signal, but can plug up or contaminate more easily relative to large jets, so compromise may be necessary.
Collector Body, P/N G1531-20690
ECD Warnings Although beta particles at this energy level have little penetrating power – the surface layer of the skin or a few sheets of paper will stop most of them – they may be hazardous if the isotope is ingested or inhaled.” A wipe test kit is supplied with each new detector. Records of tests and results must be maintained for possible inspection by the Nuclear Regulatory Commission and/or the responsible local agency. corrosive chemicals must not be introduced into the detector. To remove contamination. The procedure used is a “wipe test. For this reason the cell must be handled with care. Thermal Cleaning If your baseline is noisy or the output value is abnormally high and you have determined that these problems are not being caused by leaks in the GC system. causing possible hazardous exposure to ß and x-radiation. Radioactivity Leak Test Electron capture detectors must be tested for radioactive leakage at least every six months. More frequent tests may be conducted when necessary. you should perform a thermal cleaning (bakeout) of the detector.DETECTORS Electron-Capture Detector (ECD) Agilent provides two types of electron capture detectors. but at a cost of linear range. Warning: Detector disassembly and/or cleaning procedures other than thermal should be performed only by personnel trained and licensed appropriately to handle radioactive materials. www. or other contaminants can improve sensitivity.agilent. oxygen. and the effluent from the detector must be vented outside the laboratory environment. Gas Purity For successful EC detection. Refer to the information card supplied in the Wipe Test Kit for instructions on performing the test. the inlet and outlet fittings must be capped when the detector is not in use. Trace amounts of radioactive 63Ni may be removed during other procedures. These two types can be distinguished by the top cover of the detector – the ECD has a solid cover and the µ-ECD has a perforated cover.com/chem 72 . The regular detector (ECD) has a larger internal volume (approximately 10 times) than the microcell detector (µ-ECD). Radioactive leak tests must be performed at the required intervals. Always precondition the column before connection to the detector. it’s important that the carrier and purge gases are very clean and dry (99. Moisture. you may have contamination in the detector from column bleed and sample residues.9995%).
fused silica ECD end cap ECD chemical sample kit. 73 www. 3 ampoules solution of 33 pg/mL (0.DETECTORS Electron-Capture Detector (ECD) Supplies Item Description 1 ECD makeup gas adapter* Part No. See pages 104-115 for more information about our services and support. G1533-80565 19234-60720 19233-20625 19233-20755 18713-60040 2. online. Records of tests and results must be maintained for possible inspection by the NRC (Nuclear Regulatory Commission) and/or responsible state agency. TIPS AND TOOLS Tap Agilent’s GC knowledge over the phone. in the classroom.033 ppm) each of lindane and aldrin in isooctane ECD wipe test kit 18713-60050 *Includes one each of P/N 19233-20625 and P/N 19233-20755 1 2 3 6890 Series GC ECD Detector ECD Wipe Test: A wipe test kit (P/N 18713-60050) is supplied with each new ECD. 3 Nut warmer cup with insulation ECD adapter replacement liner.agilent.com/chem . even at your site. The kit includes an information card with instructions for performing the test.
and C16. The most common source of oxygen is a leak(s) near the detector – or in the carrier or makeup gas line fittings. 0. 1.0 mm id Graphite ferrules. 18711-60060 www. Chemically active sample components such as acids and halogenated compounds may attack and damage the filaments. C15. then increase the filament current in several increments to the desired value.agilent. Turn on the filaments at the lowest possible current setting. If the cell becomes contaminated. for 6850 TCD packed column adapter (6890/6850 only) TCD chemical sample kit.3% C14. 2. Cell Contamination Cell contamination is a problem when a lower detector temperature is used to improve sensitivity.DETECTORS 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). a solvent flush of the detector may help to remove the condensed material. Purge the detector with carrier and makeup gas for 10-15 minutes before turning on the filaments.5 mm id Capillary column nut. 0. Increasing Filament Lifetime Increased filament lifetime will result if the following startup process is used: 1. This reduces the power surge upon current introduction and prolongs filament lifetime.com/chem 74 .5 mL. Most procedures involve improving filament life or keeping the filament from becoming damaged or contaminated. 1/8 to 1/4 in. normal alkanes in hexane 5890 TCD Supplies Makeup gas adapter. Turning off or substantially reducing the filament current when the TCD is not in use also prolongs filament life. 3 ampoules. The damage caused by oxygen is more severe at high filament currents. Also. This prevents oxidation of the filaments due to the presence of oxygen that has diffused into the cell under no flow conditions. 5 solution of 0. Proper column installation techniques and regular leak checks (especially after column installation) help to keep leak problems to a minimum. glass TCD replacement cartridge 19232-80550 19302-80020 19232-60676 10/pk 10/pk 2/pk 2/pk 10/pk G1532-60675 18740-20950 18740-20960 5080-8773 5080-8853 5181-8830 5183-4732 G1532-20710 Unit Part No. Thermal Conductivity Detector (TCD) Supplies Description 6890/6850/5890 Common TCD Supplies TCD replacement cell (6890/6850 only) TCD cap column adapter seal TCD cap column adapter Graphite ferrules. low filament currents promote contamination since the filament is maintained at a lower temperature at lower currents. A constant presence of oxygen can permanently damage filaments through oxidative processes. Oxygen traps are recommended for the carrier and makeup gases to reduce oxygen levels. TCD TCD column adapter. Filament Maintenance The primary maintenance for a TCD involves the filament. Avoiding these compounds when possible increases filament life. for 6890 Capillary column nut.
Also. or bakeout (heating the detector block to evaporate the contaminant). leaks in plumbing. Do not inject halogenated solvents such as methylene chloride and chloroform into the detector.agilent. Place a septum in a nut or fitting assembly that fits onto the detector entrance. A wandering baseline. 3. 6. in non-modulated designs. Samples with active components. decrease the temperature to the normal value and install the column as usual.com/chem . Thermal cleaning. wandering baselines due to temperature variation can be corrected by making sure the detector temperature remains constant. 4. Some types of contaminants can be removed by temperature bakeout. such as acids and halogenated compounds can chemically attack the filament as well. Watch out for decreased sensitivity caused by samples that react with the filament. or changes in response on a checkout chromatogram all indicate contamination. After the final injection.DETECTORS Solvent Flush Procedure 1. Also. originating from oxygen-contaminated carrier gas. allow makeup gas to flow for 10 minutes or more. Cool the cell to room temperature and remove the column. Inject 20-100 µL volumes of toluene or benzene into the detector through the septum. Inject a total volume of at least 1mL of solvent. sample condensation will contaminate the detector cell if the temperature is too low. 75 www. After 30 minutes. Place the nut or assembly on the detector fitting and tighten. Thermal Cleaning The TCD can become contaminated with deposits from such things as column bleed or dirty samples. increased noise level. Slowly raise the temperature of the cell to 20-30˚C above the normal operating temperature. Verify the presence of makeup gas flow. 2. should be performed only after you have confirmed that the carrier gas and the flow system components are leak-free and contaminant-free. or column bleeding. 5.
Thoroughly leak check the whole system. • If the flame still won’t light. High detector temperatures reduce the PMT life.agilent. Contamination anywhere along the light path between flame and PMT can reduce detector sensitivity. Ignition is best confirmed by holding a mirror or shiny surface near the aluminum exhaust tube. the GC will not know that the flame is lit and will shut down the detector. fingerprints. turn off the PMT to maximize its usable lifetime. When not in use. thus reducing response. The Photo Multiplier Tube (PMT) needs periodic replacement. If it is too large. selectivity) the FPD jet should be inspected for deposits and. Occasionally. Cleaning & Parts Replacement The FPD requires periodic cleaning. which will momentarily go to greater than 65500 counts when the flame lights. The filter or any of the window parts should be handled gently. check the pin connections at the printed circuit board. causing non-ideal ignition conditions. A fine wire is used to clean the jet opening of particulates. Dust. They can drift over time or be changed unintentionally without knowledge of it occurring. • The flame is easier to light at higher detector temperatures. and atmospheric contaminants can dirty both quartz windows. Gas flows are also critical for optimized selectivity and sensitivity. the detector module should be removed from the instrument. The filter and related parts should be clean and free from fingerprints. A loss of sensitivity. www. Agilent provides brushes and wires that simplify the cleaning of all detector parts (see FPD Supplies on page 77). which effects flame temperature. and the total gas flow. If the display doesn’t change. Since the detection zone is above the flame. This results in measured flow rates being different from actual flow rates. and/or the photomultiplier tube window. • Under some operating conditions. Do not force too large a wire or probe into the jet opening or the opening may become distorted. • If the flame doesn’t light at all. the lead connection on the glow plug and the appropriate 5A fuse on the GC main circuit board. if necessary. Some PMTs may have a shelf life and should not be stored for prolonged periods before use. and observe condensation if the flame is lit. the filter. air and makeup gas flows should be measured occasionally. and followed by appropriate service (see jet cleaning procedure on page 70). Flame Ignition Problems If the FPD flame won’t light or stay lit: • Be sure there is a problem. reinstall the drip tube. the transfer line fused silica liner between the column and FPD module must be inspected. • Check Lit Offset. cleaned and/or replaced. and less frequently. After lighting the flame. the gas flows and jet diameter must be optimized so that components burned (activated) in the flame will emit in the detection zone. the filter. the flame may be more easily lit with the rubber drip tube removed. Observe the visual display. This makes the flame easier to light but does not affect the air flow rate setpoint. To properly service the jet. check the glow plug circuit. cleaned or replaced. there could be a large leak in the system. autoignition is turned off. The most critical parameters are the hydrogen/air or hydrogen/oxygen ratio. Column bleed and/or effluent can contaminate the first quartz window (heat shield) nearest the detector module. and/or lighting difficulties may result if the opening is deformed. this only involves the jet. If it is zero. The hydrogen. • Increase the air supply pressure to the pneumatics module. Scratches or other surface deformities reduce the amount of light passing through the filter. In most cases. The brushes are used to dislodge particulates clinging to the metal surfaces. noise. If a response problem is encountered (sensitivity. poor peak shape. with the rubber drip tube removed.DETECTORS Flame Photometric Detector (FPD) Maintenance Flame Photometric Detectors require minimal maintenance to keep them performing at satisfactory levels.com/chem 76 . The PMT is defective and needs to be rebuilt or replaced if: • high voltage is on and the flame is lit • low or no signal and/or noise not attributed to any other source such as bad cables are observed • light leaks occur • high temperatures are used • defective signal boards are present Flame Conditions & Gas Flows The flame conditions are critical to successful operation. Each gas flow should be measured independently to obtain the most accurate values.
com/chem MAINTENANCE MINDER Install the correct optical filter. 3 ampoules 19305-60580 77 www. 1. first heat shield Disk. 1/8 in. M3 x 12 (4 required) Clamp O-ring. SS Screw.926 in. depending on the choice of Sulfur or Phosphorus mode. . 1/4 in. columns Adapter weldment. brass. capillary Start-up kit (5890 only) FPD O-ring (5890 only) Liner/ferrule kit Sulfur filter Phosphorus filter Kalrez O-ring. use the 393 nanometer filter. ignitor. id Adapter weldment. 0. outer window Flange adapter Flange ring O-ring.239 in. inner window Window. second heat shield O-ring. id 12/pk 12/pk 12/pk 12/pk 12/pk 10/pk Unit Part No. size 2-011 Fluorocarbon Elastomer O-ring. For Phosphorus Mode. Kalrez Spacer. brown. use the 525 nanometer filter. Viton. heat shield Window. size 2-002 Kalrez O-ring. ignitor FPD Ignitor Replacement Kit Ignitor cable assembly (6890 only) Gasket. block O-ring. 19256-60700 1 5180-4105 3 2 19256-80560 0905-1610 19256-20590 19256-60800 G1535-60600 19256-80045 19256-80030 19256-20580 19256-20550 0515-0911 19256-00090 5061-5886 19256-80060 5061-5891 19256-20510 19256-00200 5061-5890 19256-80590 19256-80570 19256-60500 5061-5867 19256-60590 19256-80000 19256-80010 0905-1609 0905-1608 5061-5889 8 7 6 5 4 9 10 11 12 13 14 15 16 17 18 19 20 21 FPD Performance Evaluation Sample: Solution of 20 ng/mL (20 ppm) dodecanethiol and tributylphosphate in isooctane. For Sulfur Mode. Weldment. heat shield Coupling.agilent.DETECTORS 6890/5890 FPD Supplies Item Description 1 2 4 5 6 7 8 9 10 11 12 14 15 16 17 18 19 20 21 Exit tube assembly Nut.
com/chem 78 . and makeup gases. It has been observed that higher hydrogen flows and bead currents decrease bead life. Bead Life To extend the life of the bead: • Use the lowest practical adjust offset or bead voltage. but will shorten the bead life as well. They can drift over time or be changed unintentionally without knowledge of it occurring. air. We strongly recommend that moisture and hydrocarbon traps be used on the carrier gas and all detector gases. To evaporate this water. • Keep the detector temperature high (320 – 335˚C). The bead requires the most maintenance. If the NPD is not in use.agilent. including the detector hydrogen.DETECTORS Nitrogen-Phosphorus Detector (NPD) Bead Maintenance NPDs are temperamental and require frequent maintenance. The beads have to be kept dry which limits their storage life to about six months. water may accumulate in the detector. the NPD requires very pure gases (99. • If the NPD is off for an extended period of time in a high humidity environment. • Turn off the hydrogen flow during solvent peaks and between runs. Small changes in any of a number of parameters can significantly change the performance characteristics of an NPD. Each gas flow should be measured independently to obtain the most accurate values. the hydrogen flow and bead current should be reduced or turned off to increase bead life. Gas Purity Because of its high sensitivity. Rapid heating can crack or break the bead especially if it has been stored under humid conditions. air and makeup gas flows should be measured frequently. It needs to be changed frequently. slowly raise the detector temperature and bead current. NPDs are very sensitive to changes in the gas flows and consistent flows are necessary to maintain performance levels. set the detector temperature to 100˚C and maintain it for 30 minutes.999% or better). Make sure there is some type of gas flow in a heated detector or when there is current to the bead. Gas Flow The hydrogen. When a new bead is installed. • Turn off the bead when not in use. Dirty gases will not only give poor chromatographic performance. • Run clean samples and keep the inlet/liner clean to minimize contamination. www. Then set the detector temperature to 150˚C and maintain it for another 30 minutes. thus a spare is a necessity.
Agilent provides brushes and wires that simplify the cleaning of all detector parts (see NPD Supplies on page 79).53 mm jet (0.agilent. Eventually the jet needs to be replaced. Do not force too large a wire or probe into the jet opening or the opening will become distorted. so acid washing of glassware followed by distilled water and solvent rinsing is recommended. The brushes are used to dislodge particulates clinging to the metal surfaces. residue from the bead or sample can build up in the collector and cause baseline problems. polyimide-coated columns. id tip) 48 G1531-80560 61. id tip) Packed (0. it is usually more practical to simply replace dirty jets with new ones.5 63. Capillary jet (0. The various parts can be ultrasonicated after cleaning with a brush. so it is strongly recommended to have spare jets on hand. A ceramic insulator and seal kit is available. In most cases. You should clean the collector after you have changed the bead two or three times. this only involves the collector and the jet.DETECTORS Cleaning & Replacement The NPD requires periodic cleaning. the rings may not seal effectively. Chlorinated solvents and silanizing reagents can decrease the useful lifetime of the alkali source. excess reagent should be removed prior to injection. use the cleaning wire. The metal C-rings wear slightly with each assembly and disassembly. You can also use a sonicator bath to clean the jet. After several assemblies and disassemblies (five or more). A fine wire is used to clean the jet opening of particulates. Because there is no flame in the NPD. Over time./0.018 in.5 19244-80560 18710-20119 79 www. Because it is a trace detector. Solvents Solvents should be checked for purity. Always cool the detector to near-ambient when changing seals and insulators. be careful not to contaminate the analytical system.29 mm id tip) (6890 only. Other Contamination Sources Phosphate-containing leak detectors. Phosphate detergents should be avoided. If you do clean the jet. phosphoric acid-treated columns or glass wool. taking care not to damage the inside of the jet.011 in. causing an erratic baseline. Contaminants Some chemical problems can also arise when using the NPD.com/chem .011 in. dedicated) 6890/5890 Adaptable Capillary 0. A loss of sensitivity or poor peak shape may result if the opening is deformed. the jet does not collect silica and soot as does the FID jet. NPD Jets Description Length (mm) Part No. Glassware Glassware must be very clean. or nitrogen-containing liquid phases can add noise to the system and should be avoided. Although you can clean the jet. if possible.
com/chem 80 . 5. M4 x 10 mm NPD interconnect assembly Mounting pallet Jets (see page 79) Base weldment.DETECTORS Nitrogen-Phosphorous Detector (NPD) Supplies Item Description Part No. Quantity discounts available. M4 x 10 mm J-Clamp Screw. Capillary NPD Base Weldment.5 x 8 mm (Pozidriv) NPD white ceramic bead assembly* NPD black ceramic bead assembly** 3 4 5 6 7 8 9 10 11 12 13 14 15 Lid weldment Metal C-ring. top Alumina insulator. lower Metal C-ring bottom and top Screw. and 8 17 18 Column adapters for packed NPD Nut warmer cup with insulation 19234-60720 G1534-80500 G1534-80540 G1534-20590 5182-9722 17 15 16 0515-0655 G1534-60570 5183-2007 G1534-80510 0905-2580 G1534-40020 G1534-20530 G1534-40030 0905-1284 0515-2495 1400-0015 0515-2495 G1534-60610 G1531-40020 13 14 6 4 5 9 10 12 11 1 2 3 8 7 18 5890 NPD Supplies NPD collector (NPD bead) Recoating kit. Packed NPD 16 Lid stop NPD Ceramic Insulator Kit includes items 4. M3 x 0. but does not exhibit peak tailing and typically has a longer lifetime.agilent. 6890 NPD Supplies 1 2 Screws. sufficient for 10 collectors Detector Trap Replacement Kit 19234-60540 5080-8872 19231-60790 *This bead is more sensitive. 7. upper Collector funnel Alumina insulator. but exhibits some tailing for phosphorous compounds. **The black bead is potentially a little less sensitive. www.
We’ve streamlined our online store to complement the design and content of our 2005-2006 Essential Chromatography Catalog.com/chem/4ecatalog for one-click access to: • A time-saving “quick-buy” feature • Product pricing links (when available) • Local sales contact information • Online quote requests • Order status updates • Real-time customer support … and more .You asked … we listened! Our new e-Catalog makes online ordering easier than ever. Visit www.agilent.
agilent. we have devoted an entire section of this guide to MSDs. Or. Therefore. visit our online catalog at www.agilent.GC/MS Systems Your mass spectrometer is a sensitive. highly specialized device that offers more functionality – and requires more maintenance – than other GC detectors.com/chem 82 . “We offer intelligent.” Jim McCurry Senior Applications Chemist CATALOG For a complete selection of gas management supplies. see Agilent’s 2005-2006 Essential Chromatography Catalog. creative solutions to help our customers maximize the performance of their GC/MS systems.com/chem/4ecatalog. www.
*For more information on inlet maintenance. Every day Check. See page 52 for ordering information. Check the tightness of the column nuts. you don’t have to check or change liners. Check for leaks (inlet and column connections). Consult your hardware manual for specific instruction. This makes it easier to identify variations from normal performance and to take corrective action. Change the injection port liners and O-rings. Gas ballast the foreline pump. and if necessary. replace the septum. and maintenance operations performed. Monitor Record all tune values such as electron multiplier and ion source parameters in a log book to monitor instrument performance. Every week Check the foreline pump oil level and diffusion pump fluid.). Replace the carrier gas trap. Common maintenance tasks are listed in the table below. and if necessary. Autotune. see pages 26-34. EM. Replace the column. Subtle differences may exist between MSD models. So you save time and effort.com/chem . etc. Replace worn-out parts (filaments.agilent. Every three months Replace gas cylinders (when below 500 psig). It is advisable to keep a log book of system performance. In addition note the high vacuum and foreline vacuum pressures. Lubricate seals. Clean the ion source. refill the calibration vial. Check. Recondition or replace internal and external traps and chemical filters on the GC.GC/MS SYSTEMS Maintaining Mass Selective Detectors (MSDs) Some parts of the MSD require regularly scheduled maintenance. 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 Clean the ion source Change the carrier gas trap(s) and purifier Replace the worn out parts Lubricate seals (where appropriate) Replace column • •* • • • • • • • • • • • • Every year Replace the diffusion pump fluid. Every month Clean the split/splitless inlet vent line trap. TASK EVERY WEEK EVERY 6 MONTHS EVERY YEAR AS NEEDED Every six months Replace the foreline pump oil. Hint: With Agilent’s new Flip Top Inlet Sealing System. As needed Tune the MSD. 83 www. Check the injection port liners.
Contamination sources in the GC: • column or septum bleed • dirty injection port • injection port liner • contaminated syringe • poor quality carrier gas • dirty carrier gas tubing • fingerprints • air leaks • cleaning solvents and materials Contamination sources in the MSD: • air leak • cleaning solvents and materials • diffusion pump fluid • foreline pump oil • fingerprints inside the manifold The action required to remove the contamination depends on the type of contamination and the level of contamination. 32. diffusion pump fluid or fingerprints is much more difficult to remove. 28.agilent. The source of the contamination can sometimes be determined by identifying the contaminants. Serious contamination by rough pump oil.com/chem 84 . Leaks are generally caused by vacuum seals that are damaged or not fastened correctly. it may require extensive cleaning. 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) www.GC/MS SYSTEMS Contamination Contamination is usually identified by excessive background in the mass spectra. Some contaminants are much more likely to originate in the GC. It can come from the GC or from the MSD. Symptoms of leaks include: • higher than normal vacuum manifold pressure or foreline pressure • higher than normal background • peaks characteristic of air (m/z 18. Air Leaks Air leaks are a problem for any instrument that requires a vacuum to operate. Minor contamination by water or solvents can usually be removed by allowing the system to pump (with a flow of clean carrier gas) overnight. For further details contact your Agilent Customer Engineer (CE). others are more likely to originate in the MSD.
Fingerprints Fingerprints contain hydrocarbons that can appear in mass spectra. Corrective Action • Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them. Refer to specific cleaning procedures in your MSD Hardware Manual. nylon gloves and proper cleaning techniques. Replace if necessary. or from installing the column. Hydrocarbon contamination is characterized by a series of mass peaks 14 amu apart. This typically occurs after some maintenance or part replacement.GC/MS SYSTEMS Leaks can occur in many more places in the MSD: • GC/MSD interface column nut • side/top plate O-ring (all the way around) • vent valve O-ring • calibration valve • high vacuum gauge tube fitting • cracked ion gauge tube • front and rear end plate O-rings • GC/MSD interface O-ring (where the interface attaches to the vacuum manifold) • diffusion pump co-seal and/or baffle adapter O-ring • turbomolecular pump O-ring • new Vespel/graphite ferrules contract when heated Description MS interface column nut Column nut for GC/MS and two-hole ferrules Universal Column Nut (2/pk) Part No. 05988-20066 05921-21170 5181-8830 TIPS AND TOOLS The most likely point for an air leak is a seal you recently opened. 85 www. lint-free. Small Part No. • Use a temperature that’s just above the boiling point of the solvent. nylon gloves during ion source cleaning. Fingerprint contamination is usually caused by the failure to wear lint-free. Corrective Action • Check interface nut for tightness. Use special care to avoid recontamination of parts after you clean them. • Check leak/test the GC injection port. If a diffusion pump has back streamed. Corrective Action • If m/z 446 appears please call Agilent for assistance. lint-free.com/chem . Description Nylon gloves. GC inlet maintenance. A more serious problem is when fluid is back streamed into the vacuum manifold by sudden or improper venting of the vacuum system. The abundances of these peaks decrease as peak mass increases. Large Nylon gloves. Corrective Action • Reclean using clean. 8650-0030 8650-0029 Diffusion Pump Fluid If the diffusion pump 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 prominent peak will often be seen at m/z 446 and the spectral baseline will exhibit increased background noise.agilent. Cleaning Solvents It is common to see cleaning solvent peaks in the mass spectra shortly after the ion source is cleaned.
air leaks. Corrective Action • Call Agilent for assistance. 28. 181. 16 31. 119.14. 92 105. 106 151. 295. 207. 464. 264. foreline pump oil www. 262. 69. 376. 354. 169. 221.15. the ion characteristic of those contaminants. outgassing from Vespel™ ferrules PFTBA (tuning compound) Methanol Acetone Benzene Toluene or xylene Xylene Trichloroethane Foreline pump fluid or PFTBA Dimethylpolysiloxane Diffusion pump fluid Plasticizer (phthalates) Hydrocarbons Cleaning solvent Cleaning solvent Cleaning solvent Cleaning solvent Cleaning solvent Cleaning solvent Foreline pump oil vapor or calibration valve leak Septum bleed or methyl silicone column coating Diffusion pump fluid and related ions Vacuum seals (O-rings) damaged by high temperatures. Contamination Identification The following table lists some of the more common contaminants. 355. 44 or 14. 170. 100. 168. 131. 153 69 73. 58 78 91. use of vinyl or plastic gloves Fingerprints. 147.com/chem 86 .GC/MS SYSTEMS Foreline Pump Oil Foreline pump oil contamination is characterized by peaks spaced 14 amu apart (hydrocarbons). O PFTBA and related ions Possible Source CI gas Residual air and water. Common Contaminants Ions (m/z) 13. 51. 429 77. Contamination with foreline pump oil is less common than contamination with diffusion pump fluid. 446 149 Peaks spaced 14 amu apart Compound Methane H2O. 141. 32. 281. 502. 576. O2. 219.agilent. 115. CO2 or N. 614 31 43. 214. 94.16 18. and the likely sources of those contaminants. N2. 426. 414.
those that affect the system sensitivity. method. check flow rate and temperature stability Check time parameters. and temperature Ensure the MSD is located in an environment where the temperature is stable – Keep MSD out of drafts and direct sunlight – Check that the carrier gas is steady and well regulated – Service the foreline pump and/or diffusion pump Clean source Check internal and external analyzer wiring connections. coeluting peaks. Some symptoms can be corrected by following the suggested corrective actions. leak test GC injection port Do Autotune. column flow. septa. 2. Typically.GC/MS SYSTEMS Mass Spectrometer Symptoms Sensitivity This section describes some of the symptoms you might observe – either in the spectra of samples or in a tune report.com/chem . those that affect the repeatability of a measurement. column type Do Autotune and compare to background specifications Check time parameters Retune Check for contamination Check tune file.agilent. make sure all are secure Check main electrical lines Dirty ion source Loose connections in the analyzer Ground loops 87 www. application and carrier gas velocity Check GC. Others require the services of an Agilent Customer Engineer. Symptoms Wrong retention time Low signal Leaking injection port Air leak Peak widths Interfering peaks Excessive background Incorrect mass assignment Abnormal spectra – excessive background contamination Incorrect tuning Repeller voltage is too low Dirty ion source Corrective Action Check GC. tune vacuum system Clean the injection port Replace the injection port liner and septa Check and tighten interface nut. and liner o-ring Check method and injection volume. these symptoms fall into two broad classes: 1. check sample Raise voltage to test for response Clean source Repeatability Symptoms Dirty syringe needle Wrong syringe needle Leaking injection port Injection is too large Corrective Action Clean or replace the syringe Replace syringe and septa Perform injection port maintenance Replace the injection port liner. retune. split ratio and/or splitless purge time Loose column connections Tighten column nuts on injection port or transfer line Replace column nuts and ferrule Variations in pressure.
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. The positive voltage on the repeller pushes the positive ions into the lens stack, where they pass through several electrostatic lenses. These lenses concentrate the ions into a tight beam, which is directed into the mass filter.
5973 Ion Source Assembly (EI)
Maintaining the Ion Source
Cleaning procedures for MSDs vary. Refer to your MSD Hardware Manual for specific ion source cleaning procedures. Common measures of instrument performance: • abundance of certain ions (e.g. percentage of the 502 ion from the Autotune report) • shape of lens ramps and the chosen voltages, especially Repeller Ramp • sensitivity obtainable for a given analysis • ability to tune to a given reference compound (e.g. DFTPP) When to Clean: The ion source should be cleaned: • according to a customer’s predefined schedule • based on instrument performance (e.g. deteriorated performance over time) Frequency of Cleaning The cleaning frequency is determined by: • the number of samples run (throughput) • the type of samples • unique, established laboratory protocol Selecting a Cleaning Method The primary action of any cleaning procedure is to remove contamination from surfaces. Removing this contamination restores the electrostatic properties of the ion source lensing system. Numerous cleaning methods have been developed for restoring ion source performance. The cleaning methods include abrasive, sonic, and electropolish. Abrasive methods offer several advantages: • provide adequate energy to remove contamination from surfaces • require minimal equipment • pose minimal risks to the user A popular material used to abrasively clean stainless steel ion source parts is aluminum oxide. It is available in either powder form or an abrasive film. After the critical surfaces have been abrasively cleaned, the loose particles must be removed. One method of removing particles is swabbing with a cotton swab or a clean cloth dipped in acetone. A clean swab should be used for each element followed by a sonication. These cleaning supplies are listed on page 89. 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 • the turbo pump is off and not spinning • the rough pump is off Always allow the automatic venting routine to run its full course. Improper venting may cause diffusion pump fluid to be deposited into the analyzer (backstreaming). It can also reduce the life of the multiplier, or other sensitive MS parts.
TIPS AND TOOLS
Agilent’s new MS Inert Ion Source improves inertness – and maintains it over multiple cleanings. For more information see page 90.
Cleaning and Maintenance Supplies
Cleaning and Maintenance Nylon gloves, lint-free, Large Nylon gloves, lint-free, Small Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk) Generic ion source cleaning kit for all GC/MS types Includes: Cloths, lint-free (15/pk), Abrasive sheets (5/pk), Cotton swabs (100/pk), Nylon gloves, lint-free, Alumina powder, abrasive Cloths, lint-free (15/pk) Abrasive Sheets, aluminum oxide green lapping paper for ion source cleaning, 600 mesh (5 sheets) Alumina powder, abrasive PFTBA sample, certified (10 g) PFTBA sample kit, 1 mL Activated alumina, absorbent pellets for Edwards rough pump traps, non-LC/MS (1 lb can) PFTBA glass vial Cotton swabs (100/pk) Tools Screwdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws Wrench, open-end, 1/4 x 5/16 in. Screwdriver, TORX, T15 Screwdriver, TORX, T10 Ferrules and O-rings Teflon 1/4 in. ferrule (back) Teflon 1/4 in. ferrule (front) Retainer rings (10/pk) 5973 One Year Maintenance Kit (for diffusion pump systems) Includes: Big Universal Trap for He, Abrasive sheets (5/pk), Cloths, lint-free (15/pk), Cotton swabs (100/pk), SantoVac Ultra, 18.5 mL (2 ea.), Rough pump oil, 1 liter, Filament assembly, Octafluoronapthalene (OFN) MSD Tool Kit Includes: Small cleaning rod, Large cleaning rod, Source hold tool, Cotton swabs (100/pk), Nylon gloves, lint-free, Abrasive sheet, 30 mm (5/pk), Tool kit (wrenches, driving tools) 8650-0030 8650-0029 9310-4828 5181-8863
05980-60051 5061-5896 8660-0791 8500-0656 05971-60571 8500-1233 05980-20018 5080-5400 8710-0899 8710-0900 8710-0510 8710-1622 5182-3466 0100-0160 0100-0787 5181-1258 5183-2096
5973 MSD Ion Source Parts (EI) Description (A) Ion source body (B) Repeller (C) Interface socket (D) Drawout plate (E) (F) Drawout cylinder Ion focus lens 5973 Part No. G1099-20130 G1099-20132 G1099-20136 05971-20134 G1072-20008 05971-20143 05971-20126 G1099-20133 0515-1446 3050-0891 0535-0071 G1099-60104 05971-20130 G1099-60106 G1099-60177 G1099-60170 0515-1046
5973 Ion Source Parts (EI).
H M L
(G) Entrance lens (H) Repeller insulator (I) (J) (L) Set screw Washer, M3 (1/pk) Ion Source Sensor Ion source assembly Source heater assembly Repeller assembly Screw (for filament on the source)
F E D
(K) Nut, 5.5 mm (M) Lens insulator, (2/pk)
MS Inert Ion Source Parts Description Drawout plate – 3 mm Inert Drawout plate – 6 mm Inert** G2589-20045 EI High Temp Filament Repeller assembly, Inert source G1099-60170 Screws for filament High Temp 0515-1046 Source body, Inert Source Washer, Inert G1099-20130 G1099-60170 0515-1046 G1099-20130 G2589-20045 5973A 5973N 5973 inert**
G2589-20100 G2589-20045 G2590-60053 G2589-60102 G1999-20021 G2589-20043 G2589-20101
5973 Repeller Assembly (EI).
**used in G2860A and G2860B extended linearity kits
0 1.1 0.1 0. 05972-60226 Transfer line tip.0 2.0 91 www.0 1. (2/pk) (C) Ion focus lens (D) Drawout cylinder (E) Drawout plate (F) Ion source body (G) Set screw (H) Repeller assembly (I) Screw (for filament on the source) 5972/5971/GCD Part No. gold-plated 5972/5971 Part No. G1800-20305 MSD Flowrates (ml/min) Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates below for flow limitations.0 2.com/chem .1 Max Diff Pump 2.1 0. 05971-20126 05971-20130 05971-20143 G1072-20008 05971-20134 05971-20128 0515-1446 05971-60170 0515-1046 Ion source assembly 5972 Part No. Scratched source parts lead to poor performance. 05971-20305 GCD Part No.agilent.0 Max Turbo Pump 4. 5973 5972 5971 GCD Min 0.5 1.0 1. H F TIPS AND TOOLS B 5972/5971/GCD Ion Source (EI) 5972/5971/GCD MSD Ion Source Parts (EI) Description (A) Entrance lens (B) Lens insulator.0 NA NA NA Tuning Max 2.GC/MS SYSTEMS A B D C E I G It is good practice to replace scratched lenses and other ion source parts.
The active filament carries an adjustable ac emission current. www. the ion source filaments will eventually burn out. • To save time and effort. both filaments have an adjustable dc bias voltage. It should not be removed from the radiator or distributed in any way. 5971 (EI/CI) / GCD (EI) 2/pk Unit Part No. usually -70 eV. • The material in the cusps of the quadrupole is very hygroscopic. always select “No. always select MS Off before changing any of the filament parameters. • Never put the quadrupole in an ultrasonic cleaner.GC/MS SYSTEMS Filaments Two filaments are located on opposite sides outside of the ion source. TIPS AND TOOLS It is very useful to switch from one filament to the other every three months so that when one filament fails.agilent. If exposed to water. 5973 (CI) Filament. This will allow you to change both filaments at the same time. The emission current heats the filament. 5972 (EI/CI) Filament. Maintaining the Filaments Like the filament in an incandescent light bulb. The bias voltage determines the energy on the electrons. • If you are controlling your MSD from the Edit Parameters screen. 5973 (EI) Filament. Certain practices will reduce the chance of early failure: Tips to increase filament life • When setting up data acquisition parameters. • Never change the physical orientation of the quadrupole mass filter.” • Higher emission current will reduce filament life.com/chem 92 . causing it to emit electrons. • Cleaning techniques appropriate for other manufacturers’ instruments are not suitable for Agilent MSDs – and may actually harm the mass filter. Filament Assembly Description Filament. • When the software prompts Override solvent delay at the beginning of a run. • The fused-quartz quadrupole is fragile and will break if dropped or handled roughly. the quadrupole must be dried very slowly to prevent damage. contact a trained Agilent service representative to perform the mass filter cleaning. In addition. EI High Temperature for the 5973 inert Filament. use only Agilent MSD mass filters. you know the other will fail soon. which do not require periodic cleaning or maintenance. • In case of extreme contamination. set the solvent delay so that the analyzer will not turn on while the solvent peak is eluting. these electrons ionize the sample molecules. which helps to maximize your instrument uptime. 05972-60053 G1099-80053 G2590-60053 05972-60053 05971-60140 Quadrupole Mass Filter The mass filter does not require periodic maintenance. for the 5973 and 5972.
This is more likely if the vial is overfilled. This sometimes causes an “Excess source pressure” error message during the first tune after refilling.agilent. Without this vacuum. The tuning compound is usually a liquid but can be volatile or semi-volatile solid.GC/MS SYSTEMS Vacuum Systems and Pumps Vacuum System Operation The vacuum system creates the high vacuum (low pressure) required for the MSD to operate. Fill the vial to 0. How to Refill The calibration vial can be refilled without venting the system. It is required for automatic tuning of the MSD in EI mode. Ions cannot travel from the ion source through the mass filter to the electron multiplier (detector) without colliding with other molecules. certified (10 g) (EI) PFDTD sample (10 g) (CI) Part No.com/chem . 93 www. DO NOT overfill. Description PFTBA sample. the molecular mean free path is too short. use Perfluorodimethyltrioxadodecane (PFDTD) sample. Calibration The calibration valve is an electromechanical valve with a vial that contains a tuning compound. Be sure to purge the air upon refilling the vial. The major components of the vacuum system are: • Vacuum manifold • Foreline gauge • Calibration valve • Gauge controller (optional) • Vacuum seals • Foreline pump and/or trap • Diffusion/turbo pump and fan • High vacuum gauge tube A properly maintained vacuum system will: • Prevent premature filament failure • Provide better sensitivity • Require less frequent source cleaning • Extend quadrupole lifetime • Prevent premature EM Horn failure MAINTENANCE MINDER Keeping a pan under the vacuum pump helps to detect and identify the origin of oil leaks.5 cm from the top. Air is trapped in the vial when it is refilled. Perfluorotribuylamine (PFTBA) is the most commonly used tuning compound. 8500-0656 8500-8130 MAINTENANCE MINDER If using the 5973 with a CI source.
The symptoms in this section are based on typical pressures. At typical column flow rates (0. Vacuum manifold pressure is too low Symptom Possible Cause • Pressure is below 1. • Column (carrier gas) flow is too high • Wrong carrier gas • Air leak (normally at transferline interface) • Foreline pump oil level is low or oil is contaminated • Foreline hose is constricted • Foreline gauge is not working correctly • Foreline pump is not working correctly Vacuum manifold pressure is too high Symptom • Pressure is above 1.4 x 10-4 Torr. The foreline pressures listed can only be measured on diffusion pump-equipped systems.4 x 10-4 Torr.0 ml/minute). • Column (carrier gas) flow is too high • Wrong carrier gas • Air leak • Foreline pump is not working correctly • Diffusion pump fluid level is low or fluid is contaminated • Foreline pump is not working correctly • Defective gauge controller • Faulty ion gauge tube Possible Cause Possible Cause Foreline pressure is too low Symptom Possible Cause • Pressure is below 20 mTorr.agilent. • Column (carrier gas) flow is too low • Wrong carrier gas • Column plugged or crushed by an overtightened nut • Empty or insufficient carrier gas supply* • Bent or pinched carrier gas tubing* • Defective gauge controller • Faulty ion gauge tube * These could create a fault condition in the GC that would prevent the GC from operating. The vacuum manifold pressure will be approximately 1 x 10-6 to 1. Turbomolecular pumps are controlled according to their speed and do not have foreline pressure gauges.4 x 10-6 Torr.GC/MS SYSTEMS Pressure Symptoms This section describes unusual pressure readings and their possible causes. • Column (carrier gas) flow is too low • Wrong carrier gas • Column plugged or crushed by an overtightened nut • Empty or insufficient carrier gas supply* • Bent or pinched carrier gas tubing* • Foreline gauge is not working correctly * These could create a fault condition in the GC that would prevent the GC from operating. • Pressure for a given column flow has increased over time. The vacuum manifold pressures can only be measured if your system is equipped with the optional gauge controller. Foreline pressure is too high Symptom • Pressure is above 100 mTorr.com/chem 94 . These pressures can vary widely from instrument to instrument so it is important that you are familiar with the pressures that are typical for your instrument at a given carrier gas flow and oven temperature. the foreline pressure will be approximately 20 to 100 mTorr. • Pressure for a given column flow has increased over time.5 – 2. www.
1 liter Inland 45 (5973. 1 gal Inland 45 (5973. remove the stack parts. 3. 5972 or 5971/GCD) Rough pump oil. 18.GC/MS SYSTEMS Diffusion Pump It is not necessary to change the diffusion pump fluid more than once a year. The residue from some samples may be toxic. 6a. unless you observe symptoms that suggest a problem with the diffusion pump fluid. Description Diffusion pump fluid: SantoVac Ultra 5P. Too little fluid will cause the pump to run at a higher temperature because there is less fluid to carry away the heat resulting in fluid cracking or degradation and loss of high vacuum. if the foreline trap is present. Remove the pump and cover the top with aluminum foil. Use a metal ruler to determine the depth of the fluid. 4. After oil replacement. shut down and vent the MSD according to instrument manual. 6040-0809 59864B 0960-0376 0960-0897 Foreline Pump The oil in the foreline or rough pump should be replaced on average once every six months. Dispose of used oil properly. 5.5 ml (5973. the molecular sieves should be replaced. It is normal that up to 2 ml of oil may be in the rear portion of the vacuum manifold. 5972 or 5971/GCD) Ion gauge controller (5973/5972A) Ion gauge tube for measuring vacuum (5971/5972) Triode gauge tube for measuring vacuum (5972/5973) Part No. After heating the pump in a GC oven at 60°C for 15 minutes to make the fluid flow down into the reservoir at the bottom. A pump that has been in operation should have a pool 9 mm plus or minus 1 mm deep. but can vary depending upon applications.com/chem . Therefore. For the 5973 use the sight glass to determine the depth of the fluid. Description Rough pump oil. Importance of the Fluid Level The amount of fluid in the pump affects the amount of vapor and the temperature of the base plate. 5972 or 5971/GCD) Molecular sieve (5973. the best time to check the fluid is when the instrument is already vented for other maintenance. The recommended total fluid charge is approximately 37 ml. It will also lower the pumping speed because there is less fluid vapor available to pump away gases which can especially affect operation in CI Mode due to higher flow rates. 5972 or 5971/GCD) Oil mist filter RV3/E1M18/E2M18/E2M2 Oil mist filter E2M1. Unplug the MSD power cord. if the fluid is discolored or contains particulate material. 2. How to Check the Fluid Level 1. Avoid contact with the pump oil. Inspect the pump fluid. Fluid in freshly charged pumps will be 12 mm deep.agilent. If it is not vented already. The MSD must be vented in order to check the diffusion pump fluid (except for the 5973). 6b.5 Oil mist filter E2M18 95 Part No. The recommended total fluid charge for the 5971/5972 is 18 ml (plus or minus 2 ml). 6040-0798 6040-0834 9301-1104 3162-1056 G1099-80037 5063-5224 www. the fluid must be changed.
This displaces old oil from the internal pump cavities. and all vacuum system procedures to keep pump fluid background to a minimum. PFTBA can result in higher background over an extended period of time. Switch on for 2 or 3 seconds. while reducing sensitivity and linearity. Remove the fill cap from the top of the pump to expose the fill hole. 5972. To maximize electron multiplier life: • Maintain the best possible vacuum. Disconnect the power cord again. Avoid contact with the fluid. 6. Always dispose of used oil properly.GC/MS SYSTEMS General Instructions on How to Replace the Pump Oil 1. allow four hours for pumpdown and thermal equilibration before scanning. 05971-80103 G1099-80001 05971-80102 Symptom • Voltage is over 2500 volts • Poor vacuum Corrective Action • Replace electron multiplier TIPS AND TOOLS Use only Agilent replacement multipliers and horns for Agilent MSDs. Reinstall the fill cap. 9. 7. TIPS AND TOOLS Use chemical-resistant gloves and safety glasses when replacing pump fluid. Reinstall the drain plug and pour pump oil into the fill hole. Description Electron multiplier replacement horn (5973. • Don’t tune excessively. 5. Shutdown and vent the MSD. 2. Start up and pump down the MSD according to the Instrument Manual procedure. 5971/GCD) High energy dynode (5973 only) Electron multiplier kit (5972. • Use extreme caution and be conservative with venting. especially in the analyzer manifold. 5971/GCD only) Part No. pumpdown. 8. Other manufacturers’ products can increase noise.com/chem 96 . 4. and then switch it off again. www. Place a container under the drain plug on the foreline pump.agilent. 3. • Actively look for background contamination and leaks and repair them immediately. Remove the drain plug from the pump. • After venting. Reconnect the MSD to its power source. Electron Multipliers and Replacement Horn Maximize Lifetime The lifetime of an EM is directly related to the current that flows through it and the extent of contamination or condensation that it experiences. Reconnect the MSD power cord.
This makes it easier to detect variances from normal operation and to take corrective action. if you are removing the ion source for cleaning. 1 liter SantoVac 5. Cleaning the Ion Source There is not a regular interval for ion source cleaning. MS Engine Pump Lubricants and Oils 5989 or 5988 Thermo or Electro Spray 5985 or 5987 5999x. place them on clean. • If you must set parts down. Symptoms of a dirty ion source include poor sensitivity and inadequate abundances at high masses. Common maintenance tasks are listed on page 83. • Keep parts covered so that dust does not accumulate on them.agilent. not directly onto a laboratory bench. For example. Keep a record (logbook) of system performance characteristics and maintenance operations performed. 5993x or 5995x Lubricant Oil Turbo pump lubricant: Balzers turbo pump lubricant. nylon gloves when handling parts which will come in contact with the sample stream. 1 gal Inland 45 Rough pump oil. 0.com/chem . Fomblin 6040-0798 6040-0834 6040-0730 97 www. put the vacuum manifold cover back in its normal position after you have removed the source. Re-establish a low vacuum in the vacuum manifold until you need to reinstall the ion source. lint-free.25 liter Part No. See the Troubleshooting chapter in your hardware manual for more information about these symptoms.GC/MS SYSTEMS Maintaining the MS Engine Maintenance Schedule • Always wear clean. Oil from your fingers is a particularly difficult contaminant to remove. 128 ml 6040-0370 6040-0819 Rough pump oil: Rough pump oil. • Do not leave the interior of the vacuum system open to the atmosphere. 6040-0468 • • • • • • • • • • • • • • • • • Diffusion pump oil: SantoVac 5. 1 liter Inland 45 Particle Beam pump oil. The ion source should be cleaned when symptoms indicate. lint-free cloths or clean aluminum foil. Performing these tasks on a regular basis can reduce overall operating costs.
agilent. pump oil Replace mech. That way. Task Every Week Every 3 Months Every 6 Months As Needed Autotune or manual tune (save results) • • • • • We recommend keeping a separate set of tools that have been thoroughly cleaned for working with the MS engine. pump traps Check diffusion pump fluid Degas ion gauge tube Replace ion gauge tube Replace seals & O-rings • • • • • • • • • • • Analyzer Maintenance Clean ion source Replace filament Replace ion source heater Replace mass filter heater Replace electron multiplier horn GC/MS Interface Maintenance Refill EI calibration vial Refill CI calibration vial Replace interface heater TIPS AND TOOLS 98 • • • www. Cabinet Maintenance Clean the cabinet Inspect hoses and cords Vacuum the fan filter Vacuum System Maintenance Check mech. The most common maintenance tasks are listed in the table below. These tools are needed to prevent contamination when reassembling or installing clean assemblies such as the ion source.com/chem .GC/MS SYSTEMS We strongly recommend keeping a log of all system performance and routine maintenance operations. pump oil Replace mech. problems that might impact performance can be identified and resolved quickly.
05989-20110 05989-67002 05989-20111 05989-20109 05989-20145 05989-20119 05989-20165 05985-60179 05989-60098 E F 5989 Repeller Assembly Replacement Parts and Supplies The electron multiplier lifetime on the 5989 may be 6 to 9 months or shorter. 05989-80043 05971-80103 Parts and Supplies Ion gauge tube. with no jet separator • Extensive CI • High sensitivity work with high EM voltage Description 5989 Electron multiplier kit Electron multiplier replacement horn Part No.agilent. K-25 flange 0960-0799 O-rings and Seals Insulating ring O-ring. detector flange (5/pk) Diffusion pump fluid fitting fill and drain cap O-ring (12/pk) KF 25 centering ring and O-ring O-ring. B A 5989 Lens Stack C D Description (A) Clamp insulator. ion source (B) Entrance lens (C) Lens insulator. manifold window 05989-20705 5181-3367 0905-1145 3162-0110 0905-1189 99 www. ion source (D) Plate insulator. The following tables list common consumable parts and supplies used in the maintenance of the MS Engine.GC/MS SYSTEMS Ion Source Parts and Supplies Many of the tools and supplies needed to service the 5989 MS Engine are included in the installation kit supplied with the instrument. especially with the following applications: • Thermospray • Particle Beam • Purge and trap. ion source (E) EI/CI repeller (F) Repeller insulator Filament block Filament assembly Heater cartridge Part No.com/chem .
com/chem and do a library search for 5989-1510EN. part no. dual taper. part no. www. pub. 5181-3316 • Direct Connect Liner.agilent. single taper. Contents: • Start-Up Guide. With the kit. pub. no. deactivated.d. “Improvements in the Agilent 6890/5973 GC/MSD System for use with USEPA Method 8270”.GC/MS SYSTEMS General GC/MS Supplies G2860A 8270 Semi-Volatiles Applications Kit The G2860A 8270 Semi-Volatiles Applications Kit is designed for use in Agilent 6890/5973A and 6890/5973N GC/MSD Systems.d. 4mm i.. 30m x 250um x 0. For another option that also features 5973 MSD Electronics upgrades. deactivated.5um HP-5 MS. visit www.com/chem0 100 .. G1544-80730 • Direct Connect Liner. No. G2860A LIBRARY There are many ways to perform semi-volatile analysis. deactivated. system linearity is maximized and activity is minimized. part no. 4mm i. 5988-3072EN • Ultra Ion Source Chamber • Ultra Repeller • Ultra Large Aperture Drawout Plate • Pre-tested column. 19091S – 139 • Single-taper splitless liner. part no. 4mm i.agilent.d. 5988-3073EN • Application Note.. The kit provides modified and/or pretested components to improve system performance for USEPA Method 8270. G1544-80700 • Floppy Disk with tuning macros Description 8270 Semi-Volatiles Applications Kit Part No.
com/chem/4ecatalog for one-click access to: • Product pricing links (when available) • Local sales contact information • Online quote requests • Order status updates … and more 101 www.agilent.agilent. Tuning Samples MSD EI Tune CI Tune EI Verification Samples Performance Negative Mode CI Positive Mode CI Checkout Samples Semi-Volatile Volatile 5973 5972 5971 GCD PFTBA PFTBA PFTBA PFTBA PFDTD PFTBA PFTBA NA OFN 1 pg/µL HCB 10 pg/µL HCB 10 pg/µL Sample A (10 ng/µL) OFN 1 pg/µL NA NA NA Benzophenone 100 pg/µL Benzophenone 100 pg/µL Benzophenone 100 pg/µL NA DFTPP DFTPP DFTPP DFTPP BFB BFB BFB BFB MS Engine 5989A 5989B PFTBA PFTBA PFTBA PFTBA HCB 50 pg/µL HCB 20 pg/µL OFN 1 pg/µL OFN 500 fg/µL Benzophenone 100 pg/µL Benzophenone 100 pg/µL DFTPP DFTPP BFB BFB EASY ONLINE ORDERING Visit the Agilent website at www.GC/MS SYSTEMS Test and Performance Samples Each GC/MS has a specific test and performance sample.com/chem . Refer to the chart below for the exact sample.
10 g 0. and methyl palmitate in isooctane. 1 vial (Sample B.5 mL 10 g 100 pg/µL. 5 ampoules 10 pg/µL. Benzidine. mix of HCB. 100 pg/µL). OFN 1 pg/µL. PFTBA not certified Octafluoronapthalene (OFN) 8500-6405 1 ng/µL (2 ea) 1 pg/µL. 1 mL ampoule 05970-60045 GC/MS Tuning Standard contains: DFTPP. 4 ampoules 1 ng/µL. and p. Evaluation Sample for GC/MS Systems Contains 6 vials: 4 vials (Sample A.5 g. fomblin oil 1 bottle. 5 ampoules 500 fg/µL 25 µg/mL 05990-60075 8500-5441 8500-6572 8500-5851 Octafluoronapthalene (OFN) p-Bromofluorobenzene (BFB) www.agilent. HCB 20 pg/mL.p’-DDT 1 mg/mL in methylene chloride 8500-5995 5989 Installation Sample Kit contains: HCB 50 pg/µL. Pentachlorophenol.com/chem 102 . p-chlorodiphenyl. OFN and Benzophenone 5 ng/µL Extended Mass Performance Sample PFTBA certified PFTBA Sample Kit PFDTD Benzophenone 0.GC/MS SYSTEMS Description Quantity Part No. 10 ng/µL). 2 ampoules 20 pg/µL 8500-6406 8500-5500 8500-0656 05971-60571 8500-8130 8500-5440 8500-5808 Hexachlorobenzene Hexachlorobenzene Methyl stearate (in methanol). Benzophenone 100 pg/µL. and 1 vial (Sample C. 100 ng/µL) each of dodecane biphenyl.
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We stand behind our products with … • Immediate technical assistance by phone or online." Yukiko Sameshima Customer Engineer www. and regulatory requirements. including maintenance. So you can spend more time running samples. developing methods and meeting production deadlines – and less time arranging for instrument services. repair. and consultation.com/chem 104 . • Industry-leading training courses to help increase your lab’s overall knowledge base. business processes. • A variety of service options.Services & Support Every Agilent GC and GC/MS system is backed by our nearly 40 years of experience with instrument design. “Our customers know they can rely on Agilent's expertise and resources to keep their instruments running at top performance. Our professionals are standing by to help you solve problems and optimize your resources.agilent. compliance. • Prompt onsite service from Agilent-certified Engineers. lab operations.
You can rest assured that the engineer who arrives at your site will perform the requested service with optimum skill. • Use only Agilent factory-approved replacement parts. which includes preventative maintenance. • Continually update their training and qualifications. most Agilent engineers are part of the Agilent product development team. Agilent service agreements operate under a yearly fixed cost. compliance. this fixed cost covers it all – at no additional charge. maintenance. and repair. A Total Commitment to Your Lab for One Fixed Cost. maintenance. you can also consolidate instrument maintenance and repair services into multi-year agreements for administrative ease and greater cost savings. and labor. That’s because Agilent engineers … • Are experts in instrument operation. and compliance are built into your GC and GC/MS systems right from the start. as well as Agilent hardware and software qualification protocols. No matter how many service visits or replacement parts you need. • Carry calibrated.com/chem . telephone support. The Unmatched Expertise of Fully Trained Engineers. repairs. columns.agilent. in-depth documentation • Reduced administrative burdens 105 www. The Flexibility to Select The Solution That’s Right for You.SERVICES & SUPPORT Our focus is on keeping your lab running at peak performance. and supplies to ensure peak instrument reliability. compliance. traceable tools and testing equipment. If you choose. parts. So you can be certain that ease of repair. What’s more. Our team will work with you to help your laboratory achieve … • Maximum uptime • High productivity • Total compliance • Extended instrument life • Fast problem resolution • Verified system performance • The skills and knowledge you need for efficient operation and maintenance • Consistent.
• Available parts option. • A convenient way to keep up with the latest software enhancements. and inspection of your instrument. • Travel expenses and labor.agilent. Offsite Instrument Repair For selected Agilent analysis instruments • Option 1: Replacement with an identical instrument (your fastest choice). • Optional coverage for consumables used during repair. • Low cost.com/chem 106 . • Fast identification and resolution of software problems. • Fast and easy. • A single cost-effective source for telephone support and software updates. • Less expensive than onsite repair. • A fixed annual cost for parts makes budget management more predictable. • Extended instrument life. Software Service • Telephone access to trained technical professionals. factory-trained Agilent service professionals. www. • Enhancements to the original application software purchase. • You can choose the response method that fits your business needs and budget. • Option 2: Return to Agilent for repair. • Software bulletins that identify discovered defects and recommend workarounds. Onsite Instrument Repair • Hardware telephone support with access to skilled. • Confidence in the integrity of your measurements.SERVICES & SUPPORT Agilent Services Telephone Service Features • Telephone access to skilled Agilent service professionals. • Travel expenses and labor. • A fixed annual cost for software upgrades makes budget management more predictable. • Includes extensive diagnostics and testing that are not feasible with onsite maintenance or repair. Preventative Maintenance For selected Agilent analysis instruments • Expert cleaning. adjustment. • Maximum uptime. Advantages to You • Fast identification and resolution of hardware problems. • Coverage for consumables used. lubrication.
relevant. • A comprehensive test of the repaired module using established conditions and known sample characteristics to ensure the basic accuracy and precision of your module. • Efficient system requalification by performing the appropriate tests based on the components repaired. • Assurance that all instrument subsystems are performing within specifications. • Consistent. • Verification that a system is performing at operation specifications after repair. • Minimal system downtime after completion of instrument repair. • Comprehensive system and application software verification tests. • Meaningful. • Complete system operation testing.com/chem . ISO 9000. Operational Qualification/Performance Verification (OQ/PV) For selected Agilent analysis instruments Note: We recommend Preventative Maintenance before OQ/PV. • Procedures and documentation that fit the requirements of GLP.SERVICES & SUPPORT Agilent Services Installation Qualification (IQ) Features • Qualification and documentation of shipment completeness. and understandable system tests. • Supplies the evidence you need to satisfy regulatory agencies. • Measuring equipment that is traceable to national and international standards. 107 www. • Less risk of financial loss due to noncompliance. • No need to write your own SOPs to qualify Agilent instruments – or to train your staff. Advantages to You • Supplies the evidence you need to satisfy regulatory agencies. Requalification (RQ) After Repair For instruments that have their operational performance verified by an annual OQ/PV. • Delivered by professionals with training certification.agilent. • Confidence in the integrity of your measurements. • Helps fulfill the master validation plan – and change-control SOP requirements – for the IQ phase. • Measuring equipment is traceable to national and international standards. • All procedures and documentation meet regulatory agency requirements. traceable results among all your laboratories – and improved method transfer. and other regulatory agencies. based on the type and extent of the repair. • Full automation to increase the qualification scope without excess time requirements. with traceable. Note: only a subset of the Operational Qualification test is performed. • Verification and documentation of an instrument’s ability to meet specified criteria. documented chains from sample introduction to reporting.
SERVICES & SUPPORT Agilent Services Network Qualification Features • Network definition and performance testing using established Agilent Design.com/chem 108 . and Operational Qualification protocols.agilent. • Increased control – Agilent will verify known elements and identify unknown network contingency states that may impact application performance.Long Duration Network Characterization. created using hardware and software network testing tools. . • Reduced regulatory exposure – audit-ready documentation establishes evidence of network system control. • Improved consistency – network qualification protocols are developed according to a quality lifecycle.A graphical network topology map. • Increased uptime – issues that might impact application performance are quickly identified and resolved. and evaluates its operation over a controlled range of traffic conditions. Protocols include: . • Efficient cleaning with minimal downtime. . www. . which analyzes each function in its operating environment. integrity. Mass Spectrometer Ion Source Cleaning For selected Agilent analysis instruments • Onsite disassembling • Cleaning • Reassembling • Testing • Your staff can devote more time to chemistry. not instrument maintenance. and are maintained under version and revision control. supportability. which monitors the network over time.A physical and logical inventory. Advantages to You • Significant time savings. which documents reserve capacity and stability over a range of operating demands. • Documentation of the definition. • Completed protocols. and health of high-risk network segments. We’ll also provide the following reports: . Installation Qualification.Performance Predictability Analysis.A snapshot of network health. • Network Operational Qualification testing. as installed.
Directory structure . you would have to reload and reconfigure your software – a process that can take days.agilent.com/chem/service.Customizations .Simple backup software .5-in.SERVICES & SUPPORT Agilent Services Software Backup Features • Telephone or onsite factory support to facilitate restoration. Normally.Analytical hardware .User settings and operations .agilent.Printers and peripherals .Network information .Security information Advantages to You • Fast and easy – you simply insert a disk … reboot … and you’ll be back in operation in as little as two hours. 109 www.Settings .Application software . please visit www.Operating system . • Captures the unique system settings for all software components needed to reconstruct your system including: .Configurations .System registry .Ten CD-ROMs . • A complete solution – the initial configuration backup includes: .com/chem .One full system backup . floppy disks .A storage case .Ten 3.Installation of the backup software and optional CD writer TIPS AND TOOLS To learn more about Agilent’s complete portfolio of services.
Discusses typical problems and routine maintenance procedures. so you can gain the maximum benefit from this inlet operational mode. Clarifies flow paths. Discusses typical problems and routine maintenance procedures. Clarifies flow paths. so you can gain the maximum benefit from this inlet operational mode.com/chem 110 . and how often you want it. Clarifies flow paths. www.. economical and individualized instrument training modules designed to enhance and simplify your learning experience. Four hours access Description Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in split mode. All you need is Internet access! You can review and register for our e-Learning offerings by visiting www. to common problems with your instruments. eLearning Agilent’s e-Learning program features a series of focused.com/chem/elearning Course Title 6890 GC Split Inlet Mode Operation Duration Self-paced. where you want it. 6890 GC Purged Packed Inlet Operation Self-paced. Four hours access Reviews the basic theory and operation of the 6890 GC purged packed inlet..agilent. And that’s why Agilent offers several training options that cover everything from troubleshooting and maintenance to the most advanced operational techniques. From theory and operations. minimize errors and reruns. Four hours access Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in splitless mode.SERVICES & SUPPORT Education & Training Services Highly trained lab professionals can boost your productivity.agilent.. 6890 GC Splitless Inlet Mode Operation Self-paced. so you can gain the maximum benefit from this inlet. Discusses typical problems and routine maintenance procedures.. eLearning is available when you want it. and expand your chromatography capabilities.
agilent. Discusses typical problems and routine maintenance procedures. and how to return an ALS to Agilent for repair or exchange. 60-90 minutes Reviews the basic operation of the 7683A automatic liquid sampler system (ALS). Discusses typical problems and routine maintenance procedures. and flow optimization. Covers proper column installation. and flow optimization. Discusses typical problems and routine maintenance procedures. 6890 GC FID Theory and Operation Self-paced. 111 www. and flow optimization. 6890 GC ECD Theory and Operation Self-paced. keyboard setup. Covers proper column installation. Four hours access Reviews the basic theory and operation of the FID.com/chem . keyboard setup. keyboard setup. Four hours access Reviews the basic theory and operation of the ECD. Thoroughly describes all keys. Shows you how to gain maximum productivity from the ALS. so you can gain the maximum benefit from your GC. 6890 GC TCD Theory and Operation Self-paced. Discusses routine maintenance procedures. Covers proper column installation.SERVICES & SUPPORT Course Title 6890 GC Keyboard Operation Duration Self-paced. Four hours access Reviews the basic theory and operation of the TCD. Four hours access Description Reviews the basic operation of the 6890 GC keyboard. GC Automatic Liquid Sampler Operation Instructor-led.
com/chem 112 . Helps you identify the source of problems quickly. 60-90 minutes Describes in detail how to operate the GC/MSD Security ChemStation software in accordance with FDA CFR Part 11 requirements.SERVICES & SUPPORT Course Title Logical GC Troubleshooting Duration Instructor-led. Note: This course does not discuss hardwarespecific problems or solutions. 60-90 minutes www.agilent. Shows you how to manage the GC/MSD Security ChemStation software in accordance with FDA CFR Part 11 requirements. Managing and Administering the GC/MSD Security ChemStation to Meet FDA CFR Part 11 Compliance Requirements Designed for systems administrators Instructor-led. 60-90 minutes Description Teaches a methodical process for troubleshooting GC system problems. making troubleshooting less daunting. Using the GC/MSD Security ChemStation to Achieve FDA CFR Part 11 Compliance Instructor-led.
No.com/chem . Contact Agilent today for more information about our training and services. Provides experience in data acquisition and analysis. Presents the fundamental concepts of gas chromatography. Introduces the technique of GC-MS in a lecture format that includes worksheet exercises. These ISO-registered courses also target those who want to broaden or sharpen their troubleshooting. and customizing the system to meet specific laboratory or customer needs.” Course Title Technique Introduction to Capillary GC Techniques of GC Introduction to GC-MS Techniques of GC-MS Course No.agilent. Hardware/Software Operation ChemStation Operation for the 6890 GC/ALS Operation of the GC-MSD System Using the ChemStation for GC-MSD H5926A 5 Explains how to operate the Agilent 6890 GC using GC ChemStation software. Addresses preventative maintenance and first-level repair for the Agilent 5890 GC. as well as qualitative and quantitative GC-MS techniques. H4043A 5 GC-MSD System for Environmental Applications H4050A 5 Troubleshooting and Maintenance 6890 GC Maintenance 5890 GC Maintenance 6890 GC Troubleshooting and Preventative Maintenance H5308A H4001A 4 4 Addresses preventative maintenance and first-level repair for the Agilent 6890 GC. Increases an operator’s skill in using a mass selective detector with mass spectrometer EnviroQuant software. Enhances an operator’s efficiency and productivity when using the Agilent GC-MSD system. library searching. and system operation skills. Reviews the key concepts of the GC-MS analysis process. maintenance. of Days Description H2615A H4002A H2609A H4040A 1 5 1 3 Provides an overview of capillary gas chromatography in a lecture format.com/chem and select “Education. H5309A 1 113 www. Or visit www.SERVICES & SUPPORT Classroom Training Agilent’s training courses for gas chromatography and mass spectrometry help new and experienced lab professionals learn proper and efficient ways to use analytical instruments and software.agilent. Introduces troubleshooting of the Agilent 6890 GC in a lecture format. reporting.
combined with extensive hands-on and laboratory exercises. Specifically focuses on data analysis and reporting. the vacuum system. and the 5973 MSD. 5973 GC-MSD Troubleshooting and Preventative Maintenance H2294A 3 Data Analysis and Reporting ChemStation for GC Data Analysis and Reporting H2606A 3 Teaches the operation of the Agilent GC ChemStation software through instructor explanations. the quadrupole mass filter. Makes users more efficient and productive. Includes a discussion of typical vs. Offers class exercises that enhance understanding of troubleshooting and maintenance principles. including completion of EPA-like forms. of Days Description H5947A 1 Demonstrates how to perform preventative maintenance and troubleshooting to keep the Agilent 5973 GC-MSD system working properly.SERVICES & SUPPORT Course Title Introduction to 5973 GC-MSD Troubleshooting and Preventative Maintenance Course No. while expanding their ability to use ChemStation features. the 5973 MSD ion source. Covers tuning and diagnostics. Describes how to customize the software for laboratory and customer needs. Data Analysis and Reporting Using the ChemStation for GC-MSD H4076A 3 Data Analysis and Reporting Using the EnviroQuant ChemStation for GC-MSD H4053A 3 www. Includes hands-on laboratory exercises to demonstrate and practice the principles conveyed. Improves proficiency in using the Agilent EnviroQuant software. problem Auto-Tunes.agilent. Describes how to customize the software for laboratory and customer needs. Covers data analysis and reporting.com/chem 114 . No. Enhances skills in using the Agilent ChemStation for GC-MSD.
software.agilent. go to www. Technical Support Consultation a Have a technical GC column.agilent. • Interactive Troubleshooter A step-by-step approach to help you solve common problems. 3D animations and interactive software demos. method.com/chem. You’ll find: • Frequently Asked Questions about Agilent instruments and supplies. For GC Technical Support go to www. • Chromatogram Library A searchable collection of GC. and availability.agilent. tools and utilities. LC. developing methods and troubleshooting GC systems.com/chem/techsupport and click on “Interactive Troubleshooter. and insights. pricing. • Software Downloads and Utilities Feature patches and status bulletins. plus an illustrated parts breakdown. and revision tables. • Instrument and Software Demos Such as product videos. Just give us a call to discuss hardware. or troubleshooting question? Agilent’s technical GC and GC/MS experts are available to answer your questions by phone. Visit Agilent online For a wealth of knowledge.SERVICES & SUPPORT Support Tap Agilent’s GC and GC/MS expertise anytime. tips. • How-to Videos Show you how to perform common installation and maintenance procedures for Agilent products. • Find a Part Includes parts information. and CE chromatograms for nearly a thousand chemical compounds. With years of experience in running samples. or basic operation techniques. application concerns. fax or e-mail for free.” 115 www.com/chem . firmware. our chemists are promptly able to help you consistently achieve excellent performance and high productivity in your lab.
Visit www.com/chem/4ecatalog for one-click access to: • A time-saving “quick-buy” feature • Product pricing links (when available) • Local sales contact information • Online quote requests • Order status updates • Real-time customer support … and more . We’ve streamlined our online store to complement the design and content of our 2005-2006 Essential Chromatography Catalog.agilent.You asked … we listened! Our new e-Catalog makes online ordering easier than ever.
reproducible results. go to www. forensic. tips. • Handy tools. chemical. Separation Times is absolutely FREE … and we’ll automatically e-mail it to you seven times per year. Separation Times has been one of the scientific community’s most respected newsletters devoted to chemical analysis. and tricks designed to help your lab run more productively. And now. and agricultural. For more than 18 years. Best of all.agilent.Receive a year’s worth of current chromatography insights with a FREE subscription to Separation Times. To reserve your subscription today. and get reliable. it’s available online! Each issue is packed with … • Application details geared toward specific industries – such as environmental. petroleum.com/chem/separationtimes . • Exclusive promotional offers and regional event announcements.
In general. or broken. Weekly* Monthly* Daily* Inlet Hardware Every 6 months Every year Remember. if the plunger doesn’t slide easily.). Check often.GC System Recommended Maintenance Schedule Gas Management ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS Gas purifiers (carrier gas & detector gas) Split vent trap Flowmeter calibration Every 6-12 months Replacement schedule is based on capacity and grade of gases. if it cannot be cleaned. Replace when dirt is visible in the liner or if chromatography is degraded. Replace. scratched. Replace needle if septa wear is abnormal or the needle becomes clogged. etc. low column pressure. poor chromatography. Check often. replace non-indicating traps every 6-12 months or when indicating traps start to change color. Re-calibrate electronic flowmeters – follow recommended schedule for the unit (shown on calibration certificate). or if clogged. Check parts and replace when parts are worn. the downtime for scheduled maintenance is always less disruptive than the downtime for unscheduled maintenance and troubleshooting! . Check for leaks and clean. Replace when signs of deterioration are visible (gaping holes. Replace indicating traps when indicating material is spent. fragments in inlet liner. Every 6 months* Every 1-2 years Sample Introduction Consumables and GC Inlets ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS Syringes and/or syringe needles Inlet liner Liner O-rings Inlet septum Every 3 months* Replace syringe if dirt is noticeable in the syringe. Replace with liner or with signs of wear.
etc. Replace ferrules when changing columns and inlet/detector parts. or a change in response is present. Guard column may be useful for increasing column lifetime. Replace when they become scratched. septum and clean inlet as necessary. Replace inlet liner. When chromatography degradation is due to column contamination. Measure hydrogen. Thermally clean by “baking-out” when a wandering baseline. or when having difficulty lighting FID or keeping flame lit. Clean/replace FPD windows.Columns ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS Front-end Maintenance Weekly – monthly* Remove 1⁄2 -1 meter from the front of the column when experiencing chromatographic problems (peak tailing.). please see page 83. Only for bonded and cross-linked phases. Replace when thermal cleaning does not resolve the problem. For complete MSD maintenance schedule. Solvent rinse Replacement Ferrules As needed As needed Detectors ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS FID/NPD Jets & Collector NPD Bead FID TCD As needed As needed Every 6 months As needed Clean when deposits are present.agilent. Thermally clean by “baking-out” when baseline is noisy. When trimming and/or solvent rinsing no longer return chromatographic performance. Measure hydrogen. and makeup gas flows. air. increased noise. decreased sensitivity. Wipe test. Replace when signal drifts or there is a dramatic change in sensitivity. *Schedule is an approximation of average usage requirements. air. retention time changes. Replace when thermal cleaning does not resolve the problem. Frequency may vary widely based upon application and sample type. and seals when detector sensitivity is reduced.com/chem . www. or the output value is abnormally high. bent or damaged. ECD Every 6 months As needed FPD Every 6 months As needed MSD Components require regular maintenance. and makeup gas flows.
com/chem For detailed information about supplies from Agilent.agilent. or visit us online.www. 2005 5989-1925EN . 2005 Printed in USA February 15. Inc. or your authorized distributor. © Agilent Technologies. Ask about Agilent’s other valuable resources: • Maintaining Your Agilent 1100 Series HPLC System • Essential Chromatography Catalog • Online Library and Tech Support The information and pricing in this guide are subject to change without notice. please contact your local Agilent sales representative.
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