gc_gcmsd consumable and maintenance

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

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Page 1: GC_GCMSD Consumable and Maintenance

Maximize your efficiency. Minimize your downtime.Get the results you need.

Maintaining your Agilent GC and GC/MS Systems

Operate your lab at peak performance

Troubleshoot difficult problems

Select the right Agilent supplies

Plan preventative maintenance

Page 2: GC_GCMSD Consumable and Maintenance

VIDEO

This icon denotes a video that is available to view on our website.Just visit www.agilent.com/chem/techsupport to view how-tovideos and obtain more information.

1 www.agilent.com/chem

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

2 Gas Management3 Gas Types

4 Contaminants & Purities

4 Gas Purification Systems

12 Regulators

13 Tubing

14 Leak Detection

15 Flow Rates

18 Sample IntroductionConsumables & GC InletsSample Introduction

19 Vials

21 Syringes

Inlet Types

26 Packed-Column

28 Split/Splitless

31 Cool On-Column

34 Programmed TemperatureVaporizer PTV

Inlet Accessories

36 Septa

42 Ferrules

47 Liners

52 Flip Top Inlet Sealing System

54 Parts & Supplies

56 Columns57 Column Maintenance

57 Column Selection

58 Column Installation/Setup& Conditioning

59 Column Performance

63 Columns Types andCharacteristics

68 Detectors69 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 Systems83 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 & Support105 Expert Service, Training

& Support

Don’t Miss…GC Maintenance Schedule (inside back cover)

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 challengeof operating with a reduced staff. That’s why we’re committed to bringing you theworld’s best GC and GC/MS systems — plus the critical information you need to keepthem running properly.

In this newly updated Maintenance Guide, we share everything from essential serviceschedules … 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 cankeep your downtime to a minimum, and get the results you need.

TIPS AND TOOLS

This icon denotes a helpful hint that provides useful information you can find throughout this guide and online at www.agilent.com/chem.

Page 3: GC_GCMSD Consumable and Maintenance

Gas ManagementThe use of quality carrier gases is essentialfor consistent and accurate GC analyses.Proper gas management is key to achievingthis goal. Agilent provides a diverse line ofhigh quality gas management products —gas purifiers, regulators, leak detectors and flowmeters — all designed to preventcolumn damage, improve detector life, andimprove the quality and consistency of yourGC separations. This section explains howcommon contaminants like oxygen, moistureand hydrocarbons can damage your GCcolumn, and helps you understand how toprevent it. Also, look for practical informationabout 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 YamaguchiApplications Support Manager

CATALOG

For a complete selection of gas management supplies, see Agilent’s2005-2006 Essential Chromatography Catalog. Or, visit our onlinecatalog at www.agilent.com/chem/4ecatalog.

www.agilent.com/chem 2

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GAS MANAGEMENT

Gas Types

Carrier GasesThe most frequently used carrier gases arehelium and hydrogen, although nitrogenand argon can be used. Purity is essentialfor these gases since they sweep thesample through the column where it isseparated into its component parts andthen through the detector for componentquantification. Carrier gas purity is alsocritical to prevent degradation ofchromatographic hardware.

Contaminants in carrier gases can have a significant effect on column life andsubsequent analyte detection. Harmfuleffects of impure gases includecontaminant peaks and elevated column

bleed, along with column and/or detectordamage. The following sections describethe gases and purities that are necessaryfor gas chromatography carrier gases, aswell as other support gases.

Support GasesSupport gases may be specific fordetectors or for applications. These gasesinclude fuels, oxidants, coolants, detectorgases, and pneumatic gases. The degree of purity required for support gases isdependent on how that gas is being used,and whether or not it will make contactwith the sample. Coolant gases (carbon

dioxide) and pneumatic gases (air ornitrogen) generally do not come in contactwith the sample or detector. Therefore,these non-contact gases do not have to be the highest purity available.

Fuels, oxidants and detector gases, in mostcases, do come in contact with the sampleand detector, and require higher puritygases. Unfortunately, gas nomenclature asit relates to purity is not consistent acrossspecialty gas suppliers. It is important torecognize the impurities in your gassupplier’s products, and to utilize theappropriate Agilent gas purificationproducts (see next section).

Sample Gas Type Function Contact Purity Required*

Air Pneumatics No Low Grade

Nitrogen Pneumatics No Low Grade

Limit of Detection required:

Trace (0-1 ppm) 1-1000 ppm 1000 ppm-1% 1%-100%

Hydrogen Carrier or fuel gas for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero

Hydrogen/Helium Mix Fuel gas for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero

Methane/Argon Carrier or make-up or Nitrogen for ECD Yes Research Research Research N/A

Air Oxidant for detector No Ultra-Pure Ultra-Pure UHP/Zero UHP/Zero

Nitrogen, Helium, Carrier or or Argon make-up gas Yes Research Ultra-Pure Ultra-Pure UHP/Zero

*Purities of gases depend upon the type of detector that is used. Use this table as a general guide only and refer to your detector manual for specific gas purities that are needed.Low Grade = Specialty or industrial gases (≤99.998%)UHP/Zero Grade (99.999%)Ultra-Pure Grade (99.9995%)Research Grade (99.9999%)

Carrier and Support Gases

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GAS MANAGEMENT

Contaminants in gases are majorcontributors to capillary columndegradation and detector noise, and can interfere with chromatographic results. Concentration of thesecontaminants vary by the grade of gas.

Analytical gases are available in manygrades of quality, from high purity(99.995%) to chromatography grade purity(99.9995+%). The higher the purity, thehigher the cost.

Identifying ContaminantsTo make a proper purity choice it is helpful to understand the contaminantsmost common in GC gases and how they can affect your analysis. Commoncontaminants are:

Hydrocarbons and Halocarbons

• decrease detector sensitivity byincreasing detector background noise

• can also cause baseline drift or wander,contaminant peaks, and noisy or highoffsets of baselines

Moisture• can be introduced by improper handling

and/or installation of plumbing

• a common cause of column stationaryphase degradation

• can damage instrument

Oxygen• most common contaminant

• a common cause of column stationaryphase and inlet liner degradation

• can cause decomposition of labileanalytes

• opportunity for introduction at everyfitting present in the gas line or duringuse of gas permeable tubing.

In some cases it may be difficult todetermine which contaminant presents the biggest problem in a given analysis. Ifunsure, a call to your gas supplier may behelpful. Once the problem contaminantshave been identified and a generalcontaminant level is determined, the nextstep is to choose a gas purity level thatcomes closest to these requirements.

Keep in mind that higher grades of gasgenerally cost more. The greatest costsavings can be achieved by using thelowest purity gas which will neitherinterfere with the analysis nor damage your equipment. Using the proper gaspurification equipment to remove commoncontaminants and achieve the desiredpurity level is essential.

Agilent brings the highest performance and largest variety of gas purifiers (traps) to gas chromatographers. Purifiers areavailable in a variety of sizes andconfigurations to remove commoncontaminants like oxygen, moisture, and hydrocarbons. In-line gas purifiers,including refillable, indicating, S-shaped,and metal body types, are made to removespecific contaminants. Agilent also offersgas purification systems with removablecartridges. These systems provide theability to design the right combination of filters needed for your application toachieve the proper gas purity.

The illustration on the next page shows the most common gas purificationconfigurations used in gas chromatography.

Regardless of which purification system is employed, proper installation andmaintenance is required to achieve optimal performance from the purificationsystem(s). A purifier that is not maintainedwill eventually expire and becomeineffective, or worse, a source ofcontamination.

Other Considerations• determine desired purity level

• keep number of fittings in gas line to a minimum

• install purifiers in a convenient locationclose to the GC

• purifier log books are useful fordetermining maintenance schedule

• use indicating traps closest to the GC soyou can determine when to change thetraps that are upstream

Gas Purification Systems

Contaminants & Purities

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GAS MANAGEMENT

Gas TrapsThe purpose of gas traps is to removedetrimental impurities from the carrier and detector gases. Moisture (water),oxygen and hydrocarbon traps are the most common traps used with GC systems. A few combination traps areavailable which remove moisture, oxygenand/or organics with a single trap. Theeffectiveness of the traps depends on theinitial quality of the gas. Littleenhancement by traps to the GC system isobtained by traps when using very highpurity gases (e.g., ultra-high purity orsimilar grades) while obvious improvementis obtained with lower grades of gas.

Constant exposure of capillary columns tooxygen and moisture, especially at hightemperatures, results in rapid and severecolumn damage. The use of oxygen andmoisture traps for the carrier gas mayextend column life and protect theinstrument. Traps may provide someprotection if there is a leak at or around the gas cylinder. Any moisture or oxygenintroduced into the gas stream due to theleak will be removed by the trap until itexpires. This creates an opportunity todetect and fix the leak before column orinstrument damage occurs.

Carrier Gas Purification

Key:1 = Moisture Trap2 = Hydrocarbon Trap3 = Oxygen Trap4 = Indicating Oxygen Trap5 = Gas Purification System6 = Combination Trap for

moisture, oxygen, and hydrocarbon removal

Detector Gas Purification

In-Line Gas Purifiers

Gas Purification System

Combination Trap

-OR-

-OR-

FID make-up, air,and H2

Gas supply

Gas supply

Gas supply = cylinder, in-house line, or gas generator

Regulator = Brass dual stage regulator

Vent

ECD make-up

ELCD reaction gas

MS carrier gas

TIPS AND TOOLS

Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.

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GAS MANAGEMENT

Big Moisture TrapRefillable Moisture Trap

Size H2O Removal Maximum Effluent H2O 1/8 in. 1/4 in.Description (cc) Capacity (g) Concentration (ppb) Part No. Part No.

Molecular Sieve 13X and Indicating 4Å – Economy, with plastic Lexan body (other packings available, see Agilent catalog)

Refillable Moisture Trap 200 36 18 MT200-2 MT200-4

Adsorbent Refill (1 pint) for MT Series MSR-1 MSR-1

Glass Indicating Moisture Traps (larger size is available, see Agilent catalog)

Glass Indicating Moisture Traps 100 16.3 6 GMT-2-HP GMT-4-HP

Molecular Sieve Refill for GMT Series 250 GMSR GMSR

Moisture Removal S-Trap – can be reconditioned in the GC oven

Moisture S-Trap – preconditioned 5060-9084

Big Moisture Traps – for the Ultimate Moisture Capacity

Big Moisture Trap 750 BMT-2 BMT-4

Refill for BMT Series (2 refills) BMSR-1 BMSR-1

Moisture Removal Traps

Moisture (Water) TrapsThere are several different adsorbents and indicating materialsused in moisture traps. Moisture traps can be easily refilled.Adsorbent refills are typically 1/4 to 1/2 the cost of a new trapmaking refilling a more economical (and less wasteful) option.

Indicating moisture traps are available in plastic and glass bodies.Glass body traps are used when potential contaminants fromplastic trap bodies are a concern. Glass traps are normallyencased in a protective, plastic shrink wrap or a high impactplastic shield (outer trap body). Glass and plastic bodied traps areusually pressure tested at 150 psi, thus they are safe for use at thetypical pressures required by the GC.

Refillable Glass Moisture Trap

Moisture S-Trap

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GAS MANAGEMENT

Hydrocarbon TrapsHydrocarbon traps remove organics, suchas hydrocarbons and halocarbons, from the gas stream. The adsorbent is usuallyactivated carbon or an impregnated carbonfilter media. Carbon removes organicsolvents from the gas stream, including thetypical solvents used in nearly every lab.Hydrocarbon-moisture combination trapsare also available which remove water in

1/8 in. 1/4 in.Description Size (cc) Part No. Part No.

Hydrocarbon Traps – General Purpose

Refillable Hydrocarbon Trap 200 HT200-2 HT200-4

Adsorbent Refill (1 pint, 2 refills) ACR ACR

Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity

Big Hydrocarbon Trap 750 BHT-2 BHT-4

Refill for Big Hydrocarbon Trap (2 refills) BACR 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 100 HT3-2 HT3-4

Adsorbent Refill (1 pint, 3 refills) ACR ACR

Hydrocarbon Traps

Oxygen TrapsOxygen traps usually include a metal-containing inert support reagent. Mostoxygen traps reduce the oxygenconcentration to below 15-20 ppb. Thecapacity of a standard oxygen trap isapproximately 30mg of oxygen per 100cc of trap volume. Oxygen traps can alsoremove some small organic and sulfurcompounds from gas streams, but this isnot their primary application.

Metal (usually aluminum) trap bodies arerecommended for GC analyses. Some

plastics are permeable to air and containcontaminants that can degrade gas quality.In addition, many of the metal bodiedoxygen traps can withstand high pressures(up to 2000 psi). Some oxygen traps alsoremove moisture from the gas streamwithout affecting the oxygen removalcapability.

Indicating oxygen traps change color whenoxygen is present in the gas at harmfullevels. Indicating traps are not intended tobe the primary oxygen removal trap, butshould be used in conjunction with a highcapacity non-indicating oxygen trap. Theyare installed after the high capacity oxygentrap in the gas line to indicate when thehigh capacity trap has expired and needsto be changed. Expired oxygen traps needto be immediately changed since they cancontaminate the gas, in addition to failingto remove oxygen.

1/8 in. 1/4 in.Description Size (cc) Part No. Part No.

Indicating Oxygen Traps – glass body with plastic safety shield

Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP

Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller sizeavailable, see Agilent catalog)

Big Oxygen Trap 750 BOT-2 BOT-4

Oxygen Traps

Big Oxygen Trap

Indicating Oxygen Trap

Hydrocarbon Trap

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GAS MANAGEMENT

1/8 in. 1/4 in.Description Size (cc) Part No. Part No.

Oxygen/Moisture Traps

Agilent OT3 Trap 100 OT3-2 OT3-4

Hydrocarbon/Moisture Traps

Refillable Hydro-Moisture Trap 200 HMT200-2 HMT200-4

Refill for Hydrocarbon/Moisture Trap (1 pint, 2 refills) HCRMS HCRMS

Big Universal Traps – for the Ultimate in Gas Purification, removes oxygen, moisture,hydrocarbons, CO, and CO2

Big Universal Trap – Helium purged (also recommended for GC Mass Spec) 750 RMSH-2 RMSH-4

Big Universal Trap – Hydrogen purged 750 RMSHY-2 RMSHY-4

Big Universal Trap – Nitrogen purged 750 RMSN-2 RMSN-4

Big Mounting Clip for mounting Big Traps 2/pk UMC-5-2 UMC-5-2

Combination TrapsAgilent carries several Combination Trapsthat provide multiple contaminant removalin a single trap. These traps offer:

• Optimized adsorbents for maximumsurface area and capacity

• Leak-free, one-piece design to eliminatepotential leaks from using multiple traps

Hydrocarbon Moisture Trap

Big Universal Trap

Hydrocarbon Traps continued

addition to organics as described in the nextsection. Capillary grade hydrocarbon trapsare purged with ultra-high purity helium and packed with a very efficient activatedcarbon material. Metal trap bodies are usedto prevent any contaminants in plastic trapbodies from contaminating the carbonadsorbent. Most hydrocarbon traps can be refilled by the end user.

Big Hydrocarbon Trap

Hydrocarbon S-Trap

• Efficient design which preventschanneling and promotes efficientscrubbing

• The ultimate in purification with a singletrap (Big Universal Trap)

Agilent OT3 Trap

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GAS MANAGEMENT

High Capacity

Gas Purification System

Three Cartridge System

• Agilent’s highest capacity and mosteconomical gas purification system.

• Provides low-cost gas contaminantremoval for up to 18 cylinders of carrier gas.

• Includes a manifold with cartridgemounts and three replaceable cartridges:one moisture/hydrocarbon cartridge; oneoxygen cartridge; and one oxygenindicating cartridge.

• Consists of a permanent all-weldedstainless steel manifold to minimize the potential for leaks.

• Suitable for bench or wall mounting.

Description Part No.

Three Cartridge System–Includes manifold for wall or bench mount and 3 cartridges (H2O/hydrocarbon, oxygen, and indicating O2)

With 1/8 in. fittings 5183-1907

With 1/4 in. fittings 5182-9776

Replacement Cartridge Kit–Includes all three cartridges for 5182-9780above system

Single Cartridge System–Includes single cartridge manifold brackets for wall or bench mount, and a triple combination cartridge (H2O/hydrocarbon, and O2 )

With 1/8 in. fittings 5183-4598

With 1/4 in. fittings 5183-4599

Triple combination replacement cartridge for single cartridge system 5183-4600

High Capacity Gas Purification System

Three Cartridge High Capacity

Gas PurificationSystem

Single-Cartridge System

• Contains a triple-combination cartridgethat offers the same highly efficientcontaminant removal properties fromeight cylinders of carrier gas but withoutthe visual indicator.

• Other cartridges are also available fordetector gas supplies and as individualfilters for specialized requirements.

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GAS MANAGEMENT

Description Fitting (in.) Part No.

4-Head

O2, indicating O2, HC, H2O 1/8 RQC-P

Quick Change Plus (QC+) – Point of Operation Panels

Description Part No.

High capacity oxygen GC-1

High capacity moisture GC-2

Indicating moisture GC-2-I

Hydrocarbon GC-3

Indicating oxygen GC-4

Replacement Cartridges

Quick Change Plus (QC+) Point of

Operation PanelThe QC+ Point of Operation Panel containspurifier cartridges that can be quicklychanged. The cartridges are removed fromthe panel without interruption of gas flowto the system, drastically minimizing costlyinstrument downtime.

Filter cartridges are of all metal or glassconstruction, eliminating infusion andresultant signal noise associated withfilters constructed from plastics. Cartridgesare quickly installed via a simple knurledretaining nut, with no wrenches needed.As many as four cartridges can be replacedin a matter of seconds, and because thereis low dead volume, a minimal amount ofgas system purge is required afterinstallation.

RQC-P

EASY ONLINE ORDERING

From oxygen traps to purification systems, you can find all yourgas management supplies … all in one place.

Just visit www.agilent.com/chem/4ecatalog

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GAS MANAGEMENT

Universal/External Split Vent TrapSplit vent traps stop environmentalpollution. The split vent trap was designedto protect the lab environment from thecontaminants released by split injectionsystems, which can vent up to 500 timesthe amount of sample reaching thedetector into the laboratory's air. Areplaceable, impregnated carbon filtermedia traps and eliminates a broad rangeof contaminants. The traps are also easy to change and come with three packs ofreplacement cartridges each. Replaceapproximately every six months.

Description Part No.

Universal/external split vent trap with 3 cartridges(1/8 in. Swagelok fitting) RDT-1020

Replacement cartridges (3/pk) RDT-1023

Description Part No.

Carrier Gas Purification System: Single position system perfect for GC/MS, ECD and NPD detectors. Includes the triple filter cartridge. 5182-9704

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. 5182-0816

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. 5182-9705

Filter cartridge bundle of 4 (oxygen, moisture, and 2 hydrocarbon) 5183-4770

Super-Clean Gas Purification SystemsAvailable with 1/8" fittings only

Split Vent Trap and Cartridges

Super-Clean Gas Filter SystemSuper-Clean gas filter systems aredesigned to provide the utmost inconvenience and contamination reduction. The system is tested for leak-tightness and the glass and metalconstruction of the cartridges eliminatesdiffusion of contaminants into the gasstream. During cartridge replacement,check valves and close off the system tothe atmosphere, further minimizing theentry of contaminants.

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GAS MANAGEMENT

Brass Body Regulator

Regulators Pressure regulators are an integralcomponent in any gas handling system.Their function is to reduce the pressurefrom a high pressure source, such as acylinder, to a suitable use pressure.Although regulators are very good atcontrolling pressure, they do not controlflow. They have a maximum flow ratewhich is dictated by the design. Basically,the flow is determined by the pressure drop across the regulator.

Types of RegulatorsThere are primarily two types of regulators:single stage and dual (or two) stage. The difference is that a dual stageregulator is actually two regulatorsconnected in a series.

Dual stage regulators provide more preciseand consistent pressure control than singlestage regulators. The reason is that in asingle stage regulator, as the gas cylinderempties and the inlet pressure to theregulator decreases (inlet decay), thepressure on the diaphragm is reduced.Without proper adjustment, the outletpressure might slowly rise.

A dual stage regulator overcomes thisproblem by connecting two regulatorstogether. The first stage regulates thepressure to the second stage, thus creatinga constant pressure and allowing minimalinlet decay. Agilent recommends usingtwo-stage regulators with our GC Systemsto provide the proper pressure control foroptimal use.

Regulator MaterialsRegulators are usually constructed of brassor stainless steel. The choice of materialfollows the same guidelines as the choiceof tubing. Generally, it is not recommendedthat the materials be interchanged. Ifstainless steel tubing were chosen due to purity considerations, then a stainlesssteel regulator should be chosen for thesame reasons. Steel regulators are moreexpensive, which is why Agilent offersbrass regulators for less demandingapplications.

No matter which material is chosen for theregulator body, be sure to specify one withstainless steel diaphragms for criticalapplications such as use on carrier, fuel ordetector gases. Agilent recommends usingour economical brass body, dual stainless

steel diaphragm regulators for most GCapplications. These regulators, combinedwith the proper gas purification system,provide proper gas pressure control andpurity for gas chromatography.

When ordering a regulator, be sure tospecify the proper connections. In the US, most gas manufacturers follow CGAconnection guidelines. In Europe, there are a number of organizations designatingcylinder connections that are specific toindividual countries. It is best to contactyour local supplier for the properconnection designation.

Description Part No.

Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*

CGA 346, 125 psig max (8.6 bar), Air 5183-4641

CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642

CGA 540, 125 psig max (8.6 bar), O2 5183-4643

CGA 580, 125 psig max (8.6 bar), He, Ar, N2 5183-4644

CGA 590, 125 psig max (8.6 bar), Air 5183-4645

*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below

Regulator Outlet Adapters – Female NPT to Swagelok-style

1/4 in. to 1/8 in. brass (included with brass regulators) 0100-0118

1/4 in. to 1/4 in. brass** 0100-0119

** Required for plumbing 1/4 in. tubing to regulators above

TIPS AND TOOLS

Always depressurize a regulator before closing byadjusting knob and removing the regulator from thecylinder.

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GAS MANAGEMENT

Description Part No.

Copper tubing, 1/8 in., 50 ft. 5180-4196

Copper tubing, 1/8 in., 12 ft. 5021-7107

Tubing–Precleaned

TubingWhen constructing or maintaining a gasdelivery system for GC, choosing theproper tubing material is very importantand will help to eliminate potentialproblems and improve the overall quality ofthe gas system. Although there are manycommon tubing materials available, somepose safety or cleanliness problems.

Non-metallic types of tubing such aspolyethylene and Teflon are notrecommended 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 ofappropriate tubing materials has beennarrowed down to two: copper andstainless steel. Agilent recommends usingcopper tubing for most applications, since it is easy to bend and plumb and is lessexpensive than stainless steel. Usestainless steel tubing only for crucialapplications that require very high purity, or where building codes mandate its use.

Cleaning TubingBefore 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 canlead to contamination of the system withdisastrous results.

Cleaning tubing requires the use ofsuitable detergents and solvents alongwith nitrogen and a purgeable oven fordrying. This may be done easily for smalllengths of tubing, but in larger systems thecleaning procedure sometimes becomesunwieldy, leaving behind a large quantity of solvent requiring proper disposal.

Fortunately, Agilent provides clean, highquality GC grade tubing for large systemsas an economical alternative.

Tubing Type Diameter Recommended Pressure Drop(inches) Max. Length (feet) (psig)

Copper 1/8* 50 2

Copper 1/4* 300 0.5

*Recommended when multiple instruments are connected to the same source

Determining Tubing LengthParameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig

Spectra-Link Tubing Connecting Systemon a two-stage regulator

MAINTENANCE MINDER

Always replace cylinders at around 500 psi, to reduce the risk of having a drastic pressure drop right in the middle of an important analysis.

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GAS MANAGEMENT

Gas Leak Detector

Leak DetectionLeaks allow oxygen and othercontaminants to enter the gas stream.Therefore, GC instrument maintenanceshould include checking fittings andconnections with a gas leak detector.Agilent’s Gas Leak Detector enables quickand easy detection and measurement of

Description Part No.

Leak detector includes probe, extended flexible probe, range extension nozzle,probe clip and template, cable, AC power adapter/battery charger, battery, usermanual, cleaning wipe, and carrying case (available in 115 V or 220 V).

Gas leak detector, 115 V 5182-9646

Gas leak detector, 220 V 5182-9648

Description Part No.

Cylinder wall bracket with strap and chain 5183-1941(cylinder size up to 14 in., 35 cm)

Cylinder Bracket

Description Part No.

Spectra-Link with 1/8 in. fittings and 36 in. SS tubing SL-8

Spectra-Link with 1/4 in. fittings and 36 in. SS tubing SL-4

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

Gas Leak Detector Kit

gas leaks for 12 common gases. Based on adual cell micro volume thermal conductivitysystem, this unit provides very highsensitivity and eliminates contaminationcaused by soap solution methods.

Cylinder Wall Bracket

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GAS MANAGEMENT

ADM 1000 features include:• Accuracy ± 3%

• Operating temperature range–0 to 45ºC for the instrument, -70 to 135ºC for the tubing

• Calibration–traceable to NIST primarystandards

• Real time, split ratio measurement

• CE mark certified

• Measures flow rates from 0.5 to 1000 mL/min

• Split ratios–compare the ratio from one gas measurement to another (i.e., injection port split ratios)

ADM 2000In addition to the features of the ADM1000, the ADM 2000 includes:

• Mass flow measurements–measure flowrate, independent of atmosphericpressure and temperature (calculated)

• Data output through RS-232 port

• 9V battery and AC power adapter (120 or 220 VAC)

Selecting a FlowmeterAgilent manufactures the largest selectionof volumetric and mass flowmeters forchromatography. We have developedflowmeters for measuring capillary columnflows, calibrating air pumps and flowcontrollers, and verifying instrument gasflows. All flowmeters are calibrated toNIST-traceable standards.

Description Part No.

FlowTracker 1000 Flowmeter 5183-4779

FlowTracker 2000 Flowmeter and Leak Detector 5183-4780

FlowTracker Universal AC Adapter (optional, not supplied with FlowTracker units) 5183-4781

FlowTracker Flowmeters – volumetric, multimode flowmeters

Flow RatesSetting and maintaining GC flow ratesgreatly affect the instrument accuracy and sensitivity. During maintenance, verify carrier and support gas flows with the proper flowmeter. Choosing aflowmeter for your application dependsupon measurement speed, ease of use,accuracy, and flow rate range.

FlowTracker 2000

ADM 1000

ADM 2000

Page 17: GC_GCMSD Consumable and Maintenance

www.agilent.com/chem 16

GAS MANAGEMENT

Flow Rate (mL/min) Gases Accuracy Power RS-232 DataDescription Low High Measured (%) Supply Output Part No.

ADM Flowmeters – volumetric, measures all gases*

ADM1000 0.5 1000 All ± 3 9V Battery None 220-1170

ADM2000 0.5 1000 All ± 3 Battery or 120 VAC Yes 220-1171-U

ADM2000E 0.5 1000 All ± 3 Battery or 220 VAC Yes 220-1171-E

Electronic Mass Flowmeter – dedicated mass flowmeter, very accurate for specific gases*

Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery(110 V) 5.0 500 N2, Air ± 3 or 110 VAC Yes HVF-500

Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery(220 V) 5.0 500 N2, Air ± 3 or 220 VAC Yes HVF-500-2

Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters**

Optiflow 420 0.1 50 All +/- 3 9V Battery None HFM-420

Optiflow 570 0.5 700 All +/- 3 9V Battery None HFM-570

Optiflow 650 5.0 5,000 All +/- 2 9V Battery None HFM-650

*non-corrosive gases only

**non-corrosive and mildly corrosive gases only

Flowmeters

Optiflow 420Veri-Flow 500

TIPS AND TOOLS

Tap Agilent’s GC knowledge over the phone, online, in the classroom,even at your site. See pages 104-115 for more information about ourservices and support.

Page 18: GC_GCMSD Consumable and Maintenance

You asked … we listened!

Announcing the launch of our new Life Sciences and Chemical Analysis website. Based on customer feedback, we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.

• A coherent page design – that automatically detectsscreen resolution and optimizes the page size for less scrolling.

• An expanded navigation – that includes links to product literature, technical support, education, events, and news.

• A newly designed online store – with fast access topricing, order status, quotes, and local sales information.

• Direct links – to the services, parts, and consumables thatkeep your instruments running in top condition.

The new site features:

To experience these exciting new changes for yourself, go to www.agilent.com/chem.

Page 19: GC_GCMSD Consumable and Maintenance

Gas Management

The use of quality carrier gases is essentialfor consistent and accurate GC analyses.Proper gas management is key to achievingthis goal. Agilent provides a diverse line ofhigh quality gas management products – gaspurifiers, regulators, leak detectors and flowmeters – all designed to preventcolumn damage, improve detector life, andimprove the quality and consistency of yourGC separations. This section explains howcommon contaminants like oxygen, moistureand hydrocarbons can damage your GCcolumn, and helps you understand how toprevent it. Also, look for practical informationabout regulators, the importance of clean GC-tubing, and minimizing the likelihood of GC system contamination.

“Good sample introduction helps ensuregood reproducibility, optimal peak shape,and accurate sample delivery. Agilent’scommitment to offering the highest qualitysupplies means accurate, reliable results.Time after time.”

Bryan Bente, Ph.D.Technology Development Manager

Sample IntroductionConsumables & GC Inlets

Agilent offers a wide range of high-qualitysample vials, septa, syringes, liners andinlets for a broad range of gas-phaseapplications. Just as you depend on ourmeticulously engineered GC and GC/MSinstruments, you can count on Agilentconsumables. This section reviews thesecritical components. Also, look for usefulinfofrom proper syringe use and cleaningtechniques to a detailed discussion onoptimized inlet settings.

www.agilent.com/chem 18

CATALOG

For a complete selection of vials, syringes, and inlets, see Agilent’s2005-2006 Essential Chromatography Catalog. Or, visit our onlinecatalog at www.agilent.com/chem/4ecatalog.

Page 20: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Introduction

VialsAgilent’s wide opening vials are designedspecifically for analyzing samples with yourGC. They have specially designed vial neckangles, bottom design and height to ensurecompatibility with Agilent autosamplerswith rotating or robotic arm trays. Agilentoffers a large variety of autosampler vials in different closures, cap colors, septachoices and package options. Agilent alsooffers convenience packs with 500 vialsand caps in a reusable blue storage box.

For small sample sizes, Agilent offers avariety of options. You can use microvolumeinserts with the wide opening vials or, foradded convenience, use vials with smallvolume capacity.

Vial FillingWhen filling sample vials, keep in mind:

• if you need to test a large amount ofsample over repeated injections, dividethe sample among several vials to obtainreliable results

• when sample volume in the vial is low,contaminants from the previous sampleinjection or solvent washes may have agreater impact on the sample.

The airspace in the vial is necessary toavoid forming a vacuum when sample is withdrawn. This could affectreproducibility.

Glass–for general purposeuse and for use with acids

Silanized–for use withsamples that bind to glass,and for trace analyses

Polypropylene –for usewith alcohols and aqueoussolvents

Amber Vials–for use withlight-sensitive samples

Microvolume Inserts–foruse with very small samplevolumes

High Recovery Vials–for use with limited samplevolumes

Recommended fill volumes for sample vials

Vial Options

3.6 mm*

*Needle position based on standard sampling depth.

1 mL 50 µL

100 µL vial

TIPS AND TOOLS

Do not inject air into the vials to prevent the vacuum. This often damages the cap seal.

Page 21: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Selecting Vial Septa MaterialsVial cap septa are critically important to optimal analysis. Each septumcomplements the overall system andenhances chemical performance. Agilent’s vial cap septa are specificallyformulated and constructed for optimumsystem performance, with minimal coringand superior chemical inertness.

Red Rubber/Teflon• Routine analysis

• Moderate resealing

• Excellent chemical inertness

• Not recommended for multiple injections or storage of samples

• Least expensive

Silicone/Teflon• Excellent resealing

• Resists coring

• Good for multiple injections

Teflon/Silicone/Teflon• Used in trace analysis applications

• Above average resealing

• Most resistant to coring

• Least evaporation

• Use with large diameter, blunt tip syringe needles

Teflon Disc• Good for MS and ECD analysis

• Good for large-volume injections

• Chemically inert

• No resealing

• Single injection

• No long-term sampling storage

Viton• Chlorinated solvents

• Organic acids

• Limited resealing

• Not suitable for 32 gauge syringe

Determining Your Quantity Needs

To determine potential septa orderingquantities, consider:

• the number of samples run during aday/week

• if samples are run in small or largebatches

• if samples are run manually or with anautosampler

• if samples are run overnight, unattended

Description Quantity Part No.

Vials

2 mL Crimp top vial convenience pack with silver AI caps with Teflon/Red rubber septa 500/pk 5181-3400

2 mL Screw top vial conveniencepack with blue screw caps andTeflon/Red rubber septa 500/pk 5182-0732

2 mL Snap top vial convenience packwith clear polypropylene snap capsand Teflon/Red rubber septa 500/pk 5182-0547

100 µL Insert for wide opening vials 100/pk 5181-1270

250 µL Polypropylene flat bottom inserts 500/pk 5183-2087

100 µL Glass lined polypropylene vials 100/pk 9301-0977

Less than 5 µL dead volume, Micro-V vial, clear crimp top 100/pk 5184-3551

30 µL reservoir volume, High recoveryvial, crimp top 100/pk 5182-3454

Vials

Unattended autosamplerruns require a precise fit foruninterrupted operation.Typically, automated sampleruns use a higher quality andquantity of vials.

TIP

S A

ND

TO

OLS

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

SyringesSyringe type and design are important forchromatography to ensure reproduciblesample injections for consistent results.The Agilent line of syringes include avariety of plunger and needle choices to use with your autosamplers.

Agilent syringes are designed:

• for reproducible sample volume delivery

• specifically for the Agilent inlet orautosampler

• to maximize inlet septum lifetime

Selecting Syringes1. Select the syringe type based on the

inlet (injection port) you are using andthe volume of sample you want to inject.

2. Select a syringe. Refer to your automaticliquid sampler operating documentationfor available syringe sizes andcorresponding injection volumes.

3. Select the appropriate syringe needle gauge.

Inlet Needle Gauge Column Type

Packed, split orsplitless (including PTV) 23 gauge or 23/26 gauge tapered any

Cool on-column 23/26 gauge tapered or 26 gauge 530 µm

Cool on-column 26/32 gauge tapered 320 µm

Cool on-column 26/32 gauge tapered 250 µm

Needle Gauge Selection

Sharp tip

Use syringe needles with an Agilent dual-taper needle or a conical tip. Sharp-tippedneedles tend to tear the inlet septum andcause leaks. Also, a sharp-tipped needletends to leave residual amounts of sampleon the septum as it exits, resulting in alarge solvent tail on the chromatogram.

Tapered needle

Cone tip

Needle tips

Needle ShapeNeedle Tip

TIPS AND TOOLS

For best results, use the Agilent Cone Tip (HP Point Style) with Agilent’s Centerguide Septa, page 38.

Page 23: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Advantage Limitations Recommended Use

5 µL, fitted • Most accurate • Thinnest plunger, • 1 µL injectionsplunger syringe for 1µL can bend • Clean samples

injection more easily • Routine analysis• No hardware • Not ideal for higher

modification needed viscosity samplesfor 0.5 µL injection • Plunger not

replaceable

10 µL, fitted • Most economical • Most accurate only • General purposeplunger • Most reliable fitted for 1 µL and larger syringe

plunger syringe injections • Clean samples• Less bending • Plunger not • Routine analysis• Better for high replaceable

viscosity samples

10 µL, • Replaceable plunger • More expensive • Dirty samplesgas-tight for reduced than fitted plunger • Gases and volatile

repair cost • Not available in samples• Less plunger binding 5 µL size • Reactive samples

than fitted plunger• Tight seal between

plunger and barrel

Syringe Characteristics and Recommended Uses

To insert a needle into a syringe barrel:

1. Unscrew the syringe barrel cap andremove the spring.

2. Make sure the needle has the Teflondisk. If the syringe barrel does not have the Teflon disk, use the instructionsin the syringe box to wrap the needleyourself.

3. Slide the spring and the cap down overthe needle.

4. Insert the needle into the syringe barrel.

5. Screw the cap back on the syringe barrel.

Replacing On-column Syringe NeedlesThe stainless steel needles used for 250-µm and 320-µm injections must be inserted into a glass syringe barrel.Select the correct size needle for thecolumn you plan to use.

TIPS AND TOOLS

Failure to use an on-column syringe when injecting into an on-column inlet could damage the injector, syringe and column.

Page 24: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Tips• Make sure to input the proper syringe

size when setting up the injection sectionof your data handling device.

• Rinse syringes and clean their plungersbefore use to maximize syringe lifetime.

• Rinse the syringe 5-8 times betweeninjections to minimize sample carryover.

• Pump sample in and out of the syringe atleast 5 times to remove any air bubbles,and for maximum reproducibility andaccuracy.

• A 26-gauge syringe can be used for on-column injections into a 0.53mm idcolumn. Always check that on-columnsyringe needles fit inside the capillarycolumn before installing the column and syringe in the GC.

• For on-column injections, always use the proper septum nut and stainless steelinsert for the column dimension you areusing. Use a septum with a moldedthrough-hole with injections onto 0.32mmand 0.25mm columns.

• The more polar the solvent, the morelikely it is to contain water. Traceamounts of water, especially whencombined with water-extractablematerials from samples, can acceleratesyringe wear dramatically. With thesetypes of samples, use a Teflon tippedsyringe plunger. Even better, proactivelyreplace syringes, since plunger bendsmay be inevitable.

• Remove a gas-tight plunger from thesyringe for long-term storage to keep theTeflon tip leak-free. If a gas-tight plungerdoes not fit properly, place it in hot waterfor about 10 minutes then press the tipuniformly on a clean, hard surface and letcool to room temperature. The plungershould reseal correctly to provide 10-25%more injections.

• To maximize the lifetime of standardplungers, rinse the syringe and wipe the plunger with solvent (isopropanol or acetone) and a lint-free wipe, asspecified in the syringe cleaningprocedure included with each syringe.

NEW! Agilent Gold Standard GC Autosampler Syringes

see page 25

VIDEO

To view a video on syringe installation, visit www.agilent.com/chem/techsupport.

Page 25: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Troubleshooting GuideProper care, cleaning, and handling of each syringe will help ensure correct performance and long life. When cleaning your syringe, it is best to use solvents that effectively dissolve the sample you are working with. Try to avoid cleaning agents that are alkaline, contain phosphates, or are strongly acidic.

Problem

Bent plungers or stuck syringes

Bent needles

Blocked needles

RustNote: even minor rust can cause the plungerto become stuck in the barrel.

“Ring around the neck” (A dark ring betweenthe top of the barrel and the end of thevolume scale.)

Loose plungers – accompanied by syringeleaks and area count reproducibility problems.

Possible Cause(s)

• Particles such as dust, leftover samples, salts,metal, or glass can fill the narrow gap betweenthe plunger shaft and the inside wall of thebarrel.

• Improper needle alignment.

• Narrow-gauge needles (26 gauge) bend moreeasily than larger (23 gauge) needles.

• Needles tend to bend when inserted into thesample vial – not the inlet port. This can becaused by septa that are too “tough.”

• If the needle has been slightly bent whenmounted in the autosampler – or when thesyringe is installed into the autosampler – thenit is more likely to bend further when it pushesthrough the septa on the sample vial caps.

• Sample material or contaminants may betrapped inside the needle.

• The needle may not have been properly cleaned.

• During normal use, the shaft rubs against theglass walls of the barrel. This gradually wearsaway the rust-resistant metal on the shaft’ssurface.

• Rusting happens most rapidly when using wateror solvents that may contain (or absorb) water.

• Skin oils and other organic material.

• Fine metal and glass particles from the syringeplunger and barrel may be rubbing together.Once this happens, the plunger may bend ifused further.

• The syringe is nearing the end of its useful life.

Suggested Action(s)

• If the plunger’s movement feels “gritty,”remove the plunger from the barrel, flush theshaft with solvent, and wipe it dry with a lint-free cloth. Then, carefully insert the plungerback into the barrel. Finally, submerge the tipof the needle into a container of solvent, andcycle the plunger to pull the solvent into andout of the barrel.

• Never cycle the plunger in a dry syringe.

• Do not “mix & match” plungers and barrels.

• Always clean syringes after use.

• Use only Agilent autosamplers. They areprecision-designed to ensure properalignment with the syringe needle.

• Use 23 to 26-gauge tapered needles to getthe combined benefits of greater septa lifeand fewer bent needles.

• Only use Agilent vials and septa.

• Remove the plunger and use a secondsyringe to fill the blocked syringe withsolvent. Then, insert the plunger and gentlypush solvent through needle. Important: Tryto use a cleaning agent that is appropriate forthe contaminant. Common choices aremethanol, methylene chloride, acetonitrile,and acetone.

• To slow this process, remove the water fromthe syringe at the end of each day.

1. Rinse the syringe several times with a “dry”solvent, such as acetone.

2. Remove the syringe from the autosampler,and wipe the plunger dry with a lint-freecloth

3. Let syringe and plunger air dry.

• Never touch the plunger shaft with yourfingers.

• If build-up appears when water is thesolvent: rinse syringe with acetone and wipethe plunger clean at the end of each day.

• Replace the syringe. Note: Plungers normally feel “loose” whennon-polar solvents (like hexane and toluene)are used.

Page 26: GC_GCMSD Consumable and Maintenance

25 www.agilent.com/chem

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Description Unit Part No.

Miscellaneous Autosampler Supplies

4 mL Clear screw top wash vials with screw caps (no Septa) 144/pk 9301 0723

Septa for 4 mL vial 144/pk 9301-1031

Diffusion caps for 4 mL vials 12/pk 07673-40180

4 mL wash vial with fill marking, caps 25/pk 5182-0551

Screw for mounting syringe 07673-20570

Quadrant kit (4 tray sections) 18596-40015

7673/83 Basic Supply Kit contains: 10 mL syringes (6/ea), 23/26 gauge needles, 4 mL vials with diffusion caps (144/pk), 2 mL automatic sampler vials with screw caps (1,000/pk), GC septa (25/pk), Vial racks (5/pk) 07673-60840

GC Automatic Liquid Sampler Supplies

Description Gauge/Length Quantity Part No.

Tapered Needle Syringes(use for split/splitless or on-column injections with 0.53 mm id columns)

10 µL Tapered Fixed Needle 23-26s/42 6/pk 5181-3360

5 µL Tapered Fixed Needle 23-26s/42 6/pk 5181-8810

Straight Needle Syringes(use with Merlin Microseal)

10 µL Straight Fixed Needle 23/42 6/pk 9301-0725

5 µL Straight Fixed Needle 23/42 6/pk 5182-0875

Gold Standard GC Autosampler Syringes

Gold Standard GC ALS Syringe FeaturesLot Numbers ensure certified performance to all specifications

Gold protective cap prevents chipping of the glass syringe barrel as it contacts the septum retainer nut

Black ink and gold illuminating backdropfor easier viewing of the volume scale

Individually sealed packaging forcontaminant-free use

Page 27: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

LeaksSince packed-column inlets are usuallyflow-controlled, septum and column leakswill have a direct impact on retention timesand peak areas. Sample can be lostthrough the leak holes, and air can diffuseback into the inlet to cause columndegradation. Change the septum on aregular basis and check columnconnections at the first stage of problems.To prevent stationary phase decomposition,make sure that the oven and inlet are atroom temperature when not in use andwhen changing the septum.

Packed-Column InletsPacked-column direct inlets are verypopular. Packed-column analysis isfrequently done when high efficiencyseparations are not needed or when gasesare analyzed by gas-solid chromatography.Packed-column inlets are simple in bothdesign and use. Few parameters need tobe set, and all carrier gas flow flushesthrough the inlet into the column in thestandard configuration.

Parameter Selection/Setting Rationale

Inlet temperature BP of solvent +50˚C Ensures flash vaporizationBP of major solute(s) Use for neat samples

Insert type 1/8-inch stainless steel Use for ss column only1/4-inch stainless steel Inserts permit connection of

columns up to 1/4-inch od.

Liner Glass Use to lower activity (replaceable)

Initial column temperature programming Sharpens peaks and temperature reduces run time

Column type 1/8-inch packed stainless Will not break1/4-inch packed glass Better for polar or labile

compounds

Carrier gas flow 20-40 mL/min Use with N2 carrier gas30-60 mL/min Use with He or

H2 carrier gas

Packed-Column Inlet Procedures/Practices

TroubleshootingMost problems with packed-column inletsinvolve sample decomposition, flashback,or leaks.

DecompositionSince packed-column inlets are active,especially if glass liners are not used, polarsample components will often tail ordegrade in the inlet. Sample decompositioncaused by the inlet is easily diagnosed; thedecomposition products will have peaks atthe same retention times as standards forthe decomposition product.

When inlet-caused decomposition issuspected, try intracolumn direct injection,deactivated glass liners, or lower inlettemperatures, and remove any columnpacking in the inlet zone.

The inherent activity of packed-columninlets is somewhat mediated by the factthat they usually have low internal volume.When this is coupled with the relativelyfast flow rates used with packed columns,the residence time of sample in the inlet isshort and decomposition is reduced incomparison to the decomposition thatoccurs with some capillary inlets (forexample, splitless inlets).

FlashbackThe negative side of low inlet volume,however, means that excessively largesample injections will easily exceed thecapacity of the liner and will flash back intogas supply lines and onto the septum. Thiscan cause several maladies, includingghost peaks, sample losses, irreproduciblepeak areas, and decomposition.

Page 28: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Item Description Unit Part No.

1 Septum nut 18740-60835

2 Septa Bleed temperature, optimized, 11 mm 50/pk 5183-4757

3 Top insert weldment 19243-80570

4 Viton O-rings 12/pk 5080-8898

5 Glass liner, disposable 25/pk 5080-8732

Glass liner, disposable/deactivated 5/pk 5181-3382

6 Vespel/graphite ferrules, 1/4 in. id 10/pk 5080-8774

7 Tubing nut, 1/4 in. brass 10/pk 5180-4105

Adapters with glass liners

8 0.53 mm column adapter 19244-80540

1/8 in. column adapter 19243-80530

1/4 in. column adapter 19243-80540

9 Upper insulation 19243-00067

10 Nut warmer cup with insulation 19234-60720

11 Column nut for 0.53 mm column 2/pk 5181-8830

For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.* For Model 6890/6850 only

Inside ofOven

1

2

3

4

5

6

8

9

10

11

1/4 in. nut

1/4 in. Vespel/

1/8 in. or 1/4 in.stainless steel liner

Liner

7

graphite ferrule

6890/6850 Series GC Packed Port Supplies*

5890 Packed-Column Inlet Supplies

Description Unit Part No.

Nonpurging septum nut assembly for manual flow control only, not EPC 19243-60570

Adapters without glass liners

1/8 in. column adapter 19243-80510

1/4 in. column adapter 19243-80520

Universal Packed-Column Inlet (non-purged)

Septum retainer nut forheadspace sampling, nonpurging 19243-605050

Brass nut, 1/4 in. 10/pk 5180-4105TIPS

AN

D T

OO

LS

Tap Agilent’s GC knowledge over the phone,online, in the classroom, even at your site. See pages 104-115 for more informationabout our services and support.

Inside of Oven

1/4 in. Vespel/ graphite ferrule1/4 in. Vespel/ graphite ferrule

1/8 in. or 1/4 in.stainless steel liner

1/4 in. nut

Page 29: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Split/Splitless InletsThe combined “split/splitless” inlet is themost popular inlet for capillary column gaschromatography. Because it can be used ineither split or splitless mode, it provides avery effective combination that can covermost analysis requirements.

Split ModeSplit injection is an effective way tointroduce small amounts of sample withoutoverloading the column. Split injection isrequired for samples that:

• cannot be diluted for analysis (forexample, solvents)

• are gases that cannot be focused, or that have long injection times (valveinjections)

• have important minor peaks elutingdirectly before the solvent peak (as insolvent analysis)

Split injection is also good for screeningsamples of which little is known or forthose that have widely differingconcentrations, since the split ratio can be adjusted easily. Split inlets are also a good choice for dirty samples.

Parameter Selection/Setting Rationale

Inlet temperature Try 250˚C or BP of Ensures flash vaporizationlast eluting compound Minimizes inlet discrimination

Inlet liner Large volume, deactivated Minimizes flashbackMinimizes degradation

Inlet packing Silanized glass wool Retains non-volatilesMinimizes inlet discrimination

Glass beads or frit Less active than woolNone Least active

Injection volume 0.5-3 µL liquid Split easily adjusted0.10-10 mL gas Split adjusted accordingly

Injection technique Fast autoinjection Less needle discriminationHot-needle fast manual Reproducible discriminationinjection

Split ratio 50:1 to 500:1 Depends on sample and injection volume, and column ID

Initial column Not critical Narrow initial peakstemperatures

Septum purge 2-3 mL/min Minimizes ghosting

Split Mode Variables, Practices, and Rationales

A majority of the problems encounteredwith split inlets are related to discriminationand decomposition. Both analyticalaccuracy and reproducibility decrease with the increases in discrimination and decomposition. Split inlets suffer from both needle discrimination and inlet discrimination.

TroubleshootingSplit inlets are spared from most band-broadening phenomena, since narrowpeaks are generated as part of the splittingprocess. Therefore, any peak broadening or tailing observed with split injection isusually due to improper columninstallation, low split flow, (<20 mL/min on 6890) or low inlet temperature. If yoususpect that the inlet temperature may betoo low, increase it by 50˚C and comparethe results to the lower temperatureanalysis. Repeat if results are positive until no further improvement is seen.

TIPS AND TOOLS

For fast and easy liner changes, check out Agilent’s new Flip Top Inlet Sealing System on page 52.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Splitless ModeFor splitless injection, a conventional splitinjector is operated in a nonsplitting modeby closing the split valve during injection.The sample is flash-vaporized in the liner,and sample vapors are carried into thecolumn by the carrier gas where they arerecondensed at temperatures below theboiling point of the solvent. After most ofthe sample has been transferred into thecolumn, vapors remaining in the liner arecleared by opening the split vent whichremains open for the duration of the run.

The most important benefit of splitlessinjection is that a majority of the injectedsample is introduced into the column. Thisresults in much higher sensitivity than thatachieved using split injection.

Solvent EffectOne requirement of splitless injections isthat the initial column temperature shouldbe kept at least 10˚C below the boilingpoint of the sample solvent. This allowsthe sample solvent to condense at thefront of the column trapping the solventmolecules into a tight, narrow band.Additionally, use a solvent that is similar inpolarity to the column stationary phase,and avoid mixed solvents. Breaking theserules may result in split peaks.

Splitless injection is routinely used in areas such as:

• environmental analysis

• pesticide monitoring of foods

• drug screening

In these applications, sample preparationrequirements are significant, and it is notalways possible or economically justifiableto clean up a sample extensively. Socolumn protection becomes as importantas sensitivity. Also, samples with tracequantities of important solutes that eluteon the solvent tail may be focused by thesolvent to yield more sensitive analyses.

Parameter Selection/Setting Rationale

Inlet temperature Just above highest Ensures flash vaporizationboiling point of Reduce if degradation occurssolutes (+20˚C) Use higher for dirty samples

and higher-boiling solutes

Inlet liner Large volume >0.8mL Use with autoinjectorSmall volume <0.2mL Use only for slow manual

injections, and gas injections

Inlet packing None Use only with slow injectionDecreases degradation

Silanized glass wool Use for fast autoinjection & dirty samples

Injection volume 0.5-2 µL liquid Depends on solvent, liner, & conditions

Injection technique Fast autoinjection Most reproducibleLess needle discrimination

Hot-needle slow manual Inject 1-2µL.sec if narrow liner is used and >1µL injection

Hot-needle fast manual Use for <1µL injections

Purge flow 20-50 mL/min Higher if using constant flow

Purge delay time 20-80 sec Adjust according to column flow rate/liner type & sample conditions

Oven temperature 10-25˚C below solvent BP Necessary for solvent focusing

Column flow >2mL/min when possible Clears inlet fastReduces backflash and decomposition

Septum purge 2-3mL/min Reduces ghosting

Quantification Internal standard Maximizes reproducibilityStandard addition Use only with constant

injection volume

Retention gap 1-3m, deactivated Reduces peak distortion(1-2m per µL injected) Promotes solvent and

stationary phase focusing

Split Mode Variables, Practices, and Rationales

VIDEO

To view a video on liner and gold seal replacement, visitwww.agilent.com/chem/techsupport.

Page 31: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

DecompositionLoss of peak area or generation of newpeaks, can sometimes be dramaticallyreduced by changing liner type or bydeactivating the liner and inlet withsilanizing reagents. Removing or reducingthe amount of liner packing can alsodecrease inlet activity.

Item Description Unit Part No.

1 Septum retainer nut 18740-60835

2 Septa See page 36

3 Insert Weldment G1544-60575

4 Liner O-ring See page 52

5 Liner See page 47

6 Split vent trap assembly (6890/6850 only) G1544-80550

7 Retaining nut (6890/6850 only) G1544-20590Retaining nut (5890 only) 19251-20620

8 SS seal 18740-20880Gold-plated seal 18740-20885

9 Washer, 0.375 in. od 12/pk 5061-5869

10 Reducing nut 18740-20800

11 Insulation (requires 3) 19243-00067

12 Lower insulation cover 19243-00070

13 Ferrule

14 Column nut (6890/5890 only) 2/pk 5181-8830

Column nut (6850 only) 2/pk 5183-4732

Angled wrench for split/splitless inlet 19251-00100

* For a complete parts breakdown, see the 6890/6850 Series GC Instrument User and/or Service Manuals.

1

2

4

56

3

7

89

10

11

12

1314

6890/6850 Split/Splitless Inlet Supplies*

TroubleshootingMost problems encountered with splitlessinjection are related to incorrect purgetime, degradation, improper focusing, andflashback.

Appropriate initial column temperature iscritical. Sample vapors can be lost throughthe septum purge line if the insert isoverfilled with sample vapor (either toolarge injection volume or too small linervolume), leading to irreproducibility andnonlinearity of peak areas. Match inlettemperature, liner volume, and injectionvolume carefully to avoid backflash.

TIPS AND TOOLS

A guard column or retention gap is often beneficial for splitless injections,improving peak shape and extending column life when analyzing dirty samples.(See page 61).

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Cool On-Column InletsCool on-column injection is superior inmany ways to other sample introductiontechniques.

Advantages:• elimination of sample discrimination

• elimination of sample alteration

• solvent focusing of early eluting solutes

• high analytical precision

If done properly, cool on-column injectionprovides the most accurate and preciseresults of the available inlets. Syringediscrimination is completely eliminated.Moreover, inlet-related discrimination doesnot occur, since the liquid is introduceddirectly into the column. Automated on-column injection provides even higheranalytical precision. Add to this theelimination of thermal decomposition andrearrangement reactions, and it becomesapparent that cool on-column injectionshould be considered whenever highprecision and accurate results are required.

Parameter Selection/Setting Rationale

Initial inlet temperature = or 3˚C above column oven temperature Ensures sample focusing in solvent front

Initial inlet temperature ramp Same as oven (oven track) Faster than oven Simple and effective Narrows initial peak width

Injection volume 0.1-2.0 µL liquid Use smaller injections for small id columns;Depends on column capacity

Injection technique Fast autoinjection Projects droplets away from syringe tipFused silica needle Use for manual injection into small id columns

Oven temperature Inlet temperature or slightly lower Prevents backflash

Column flow 50-80cm/sec Use for H2 carrier gas30-50cm/sec Use for He carrier gas

Septum purge 12-15mL/min Use if installed to prevent ghosting

Quantification All methods Inherently reproducible techniqueLack of discrimination

Retention gap requirements 1-3m, deactivated Corrects peak distortionProtects column from non-volatile componentsPermits autoinjection with narrow-bore columns

Cool On-Column Inlet Procedures/Practices

Limitations:• maximum sample volumes are smaller compared

with other inlets (0.5 µL to 2.0 µL)

• solute peaks eluting just before the solventcannot be focused and are difficult to determine

• capillary columns (especially those with a largephase ratio or small inner diameter) can be easilyoverloaded with sample

• parameters such as initial column temperature,solvent nature, and injection rate must often beoptimized

TIPS AND TOOLS

Since the sample is directly deposited into the column, nonvolatile sample componentscan accumulate at the head of the column and will degrade efficiency and/or interact withsubsequent injections.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample ConsiderationsSample preparation is important for on-column injection because of:

• the potential for column overload, column contamination,

• the incompatibility of some solvents with the stationary phase,

• dependence of the initial columntemperature on the boiling point of the solvent.

Many of the problems associated with these variables can be resolved by using a retention gap ahead of theanalytical column.

TroubleshootingThe major problems found with cool on-column injection are associated withcolumn overload, solvent/stationary phaseincompatibility, and column contamination.

If the flooded zone after injection is toolong (large injections, poor wettability),peaks will be broad or split. A retention gapusually will resolve this problem. Loss ofcolumn efficiency with on-column injectionusually is caused by contamination ordegradation of the stationary phase at thehead of the column. Only columns with animmobilized stationary phase should beused with cool on-column injection toprevent displacement of the stationaryphase by solvents.

Immobilized stationary phases can bewashed to remove contaminants andrenew performance. If column performancedoes not improve after washing, cut 0.5moff the inlet side of the column. If that doesnot return column performance, thecolumn must be replaced and a retentiongap should be used for all further injectionsof dirty samples.

Description Unit Part No.

Column nut 2/pk 5181-8830

250 µm graphite/Vespel ferrule 10/pk 5181-3323

320 µm 0.5 mm graphite/Vespel ferrule 10/pk 5062-3514

250 µm retention gap (one 5 m piece) 160-2255-5

320 µm retention gap (one 5 m piece) 160-2325-5

530 µm retention gap (one 5 m piece) 160-2535-5

Quartz deactivated column connector fits 0.18-0.53 mm 5/pk 5181-3396

Column/Retention Gap Installation Consumables

VIDEO

To view a video on cool on-column installation and septum replacement,visit www.agilent.com/chem/techsupport.

TIPS AND TOOLS

Sample degradation can occur with cool on-column injection if columnor retention gap activity is high. Use only well-deactivated retentiongaps and high quality capillary columns from Agilent.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Item Description Unit Part No.

Manual injection

1c Cooling tower assembly 19320-80625

1d Duckbill septum 10/pk 19245-40050

Fused silica syringe needles 6/pk 19091-63000

Syringe barrel for use with fused-silica needles,10 µL 9301-0658

Common Supplies

3 Spring 19245-60760

4 Inserts for capillary columns

For 200 µm columns (one ring) 19245-20510

For 250 µm columns (six rings) 19245-20515

For 320 µm columns (five rings) 19245-20525

For 530 µm columns (no rings) 19245-20580

For 530 µm Al clad columns (four rings) 19245-207804

5 Ferrule 5080-8853

6 Column nut 2/pk 5181-8830

6890 Series GC Cool On-Column Inlet Supplies

Automatic Injection

1a Septum nut base for 320 mm assembly 19245-80521

1b Septum nut base for 530 mm assembly G1545-80520

2 Advanced green 5 mm through hole septa 50/pk 5183-4760BTO 5 mm through hole septa 50/pk 5183-4758

5890 Series Cool On-Column Inlet Supplies

Automatic Injection

1a Septum nut (5890 Series II GC) 19245-80520

1b Needle guide (for 7673A only) 19245-20670

* For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.

6890 Series Cool On-Column Inlet Supplies*

1b

2

5

6

1c1a

34

1d

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

PTV inlets combine the benefits of split,splitless and on-column inlets. The sample isusually injected into a cool liner, so syringeneedle discrimination does not occur. Thenthe inlet temperature is increased to vaporizethe sample. The user programs vent timesand temperature to achieve the equivalent ofsplit or splitless transfer of sample vapors tothe column. PTV injection is considered themost universal sample introduction systembecause of its flexibility.

Advantages• no syringe-needle discrimination

• minimal inlet discrimination

• no special syringe needed

• use of large injection volumes

• removal of solvent and low boilingcomponents

• trapping of nonvolatile components in liner

• split or splitless operation

• retention time and area reproducibilityapproaching cool on-column injection

PTV inlets are actively cooled before andduring injection by Peltier devices or byforced gases (air, liquid N2, or liquid CO2).Cryogenic cooling of the inlet can reduceinlet temperature enough to thermallyfocus gas injections from other samplingdevices in the liner. This is a distinctadvantage of using PTV inlets incomparison to conventional inlets forcoupling auxiliary sampling devices tocapillary columns.

Post-injection, PTV inlets are heated using electrical heaters or preheatedcompressed air. Depending on design, inlet temperature ramps are either ballistic (i.e., ramped to the maximumtemperature at an uncontrolled maximumrate) or programmable.

Parameter Selection/Setting Rationale

Injection mode Cold split For general use and sample screening

Cold splitless For trace analysis

Inlet temperature Adjustable (i.e., 2˚C/sec Use slower ramp rates for ramp rate to 12˚C/sec) labile, complex, or large

volume samples Use faster ramp rates for most samples Use faster ramp rates to shorten splitless purge delay time

Ballistic Simpler, less expensive instrumentation

Inlet liner Straight with silanized wool For general useBaffled For labile samplesPacked with an adsorbent For focusing gaseous

injections from auxiliary sampling devices

Injection volume 0.1-1.5µL Use lower volumes for volatile solvents and fast ramp ratesUse volumes larger than 1.5µL only in solvent- elimination mode

Sample Injection Autosampler or manual, Not critical for cold split technique fast or slow & splitless modes

Oven temperature 10-25˚C below solvent BP For proper solvent effect insplitless mode

Sample dependent For split mode

Column flow 30-50 cm/sec Clears inlet fasterLess backflash

Septum purge 1-5mL/min Minimizes ghosting

Quantification Any method Inherently reproducibleLow discrimination in coldinjection modes

Retention gap 1-3m, deactivated Compensates for extended flooded zone and solvent-column incompatibility

Programmed Temperature Vaporizer (PTV) Inlets

PTV Inlet Procedures/Practices (cold split/splitless modes)

VIDEO

To view a video on PTV column installation, liner installation and silverseal replacement, visit www.agilent.com/chem/techsupport.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Item Description Column ID Unit Part No.

1 Septumless head G2617-60507

2 Septum head G2618-80500

3 Septum nut 18740-60835

4 PTV inlet assy G2617-60506

5 PTV LCO2 cooling jacket G2617-60508

6 PTV LN2 cooling jacket G2619-60501

7 Silver seal 5/pk 5182-9763

8 Graphpak inlet adapter 0.20 mm 5182-9754

0.25-0.33 mm 5182-9761

0.53 mm 5182-9762

9 Ferrules for 0.20 mm 10/pk 5182-9756

Graphpak inlet 0.25 mm 10/pk 5182-9768

0.32 mm 10/pk 5182-9769

0.53 mm 10/pk 5182-9770

10 Split nut for inlet adapters 5062-3525

11 PTV insulation block G2617-20510

PTV cryo insulator (not shown) G2617-60510

Teflon ferrule (needle seal) 5182-9748

Kalrez seal 5182-9759

Valve body 5182-9757

Pressure spring 5182-9758

Viton seal 5182-9775

Sealing element 5182-9760

CO2 Cryo inline filter 3150-0602

Service kit for septumless head 5182-9747contains Kalrez seal, valve body, and pressure springGraphpak 3D ferrules 5/pk 5182-9749

Installation tool for 3D ferrules G2617-80540

1

2

3

4

5, 6

78910

11

6890 PTV Inlet

PTV Liners

Description Part No.

PTV Liner Single Baffle, 2 mm id 180 µL volume, deactivated, glasswool 5183-2038

PTV Liner Single Baffle, 2 mm id 200 µL volume, deactivated 5183-2036

PTV Liner Multi Baffle, 1.5 mm id 150 µL volume, deactivated 5183-2037

PTV Liner Fritted Glass, 1.5 mm id 150 µL volume, deactivated 5183-2041

There are few choices in liner design for PTV inlets.However, liner volume andactivity are still key issues tobe considered when selectingamong the few available PTVliners. PTV liners requirepacking or a modified surfaceto hold the liquid sample inplace before and during thevaporizing process.

TIP

S A

ND

TO

OLS

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa One of the key components of sampleintroduction is the inlet septum. Allcolumns must have carrier gas headpressure to establish flow through thecolumn. Septa maintain the leak-free sealand exclude air from the inlet. They comein many different sizes and are made frommany different types of material specific to inlet type and analysis needs.

Septa are usually available according totheir recommended upper temperature limits. Lower temperature septa areusually softer, seal better, and canwithstand more punctures (injections)than their high-temperature counterparts.If used above their recommendedtemperatures, however, they can leak ordecompose. This causes sample losses,lower column flow, decreased column lifeand ghosting.

What is the Function The septum isolates the sample flow pathfrom the outside world. It must provide abarrier that is readily penetrated by theinjector needle while maintaining internalpressure without contaminating theanalysis. They are generally made ofspecial high-temperature, low-bleedsilicone rubber formulations.

Why ReplaceSepta should be replaced regularly to avoid:• leaks• decomposition• sample loss• reduced column or split vent flow• ghost peaks• column degradation

How to Minimize ProblemsAvoid problems by:• using within the recommended

temperature range• changing regularly• installing “hand tight”• using septum purge when available• using autoinjectors• using sharp syringe needles

Agilent Introduces InnovativePackaging for Inlet Septa

Agilent has recently introduced a newand innovative packaging design for inlet septa. This new packaging is a tri-fold blister pack that providescleanliness, convenience, andconsistency for our complete line of 11 mm and 9.5 mm septa.

Your 50th Septum will be as Clean as Your 1st!

The primary benefit behind the newpackaging is that each septum isindividually packaged for the ultimatecleanliness. Each septum is easilydispensed one at a time by pushing itthrough the back foil, as is commonlydone with pharmaceutical capsules andtablets. No longer do you need to reachinto a jar and wonder how clean thesepta are or if you are contaminatingother septa.

In addition, the new packaging deliversthe following features and added value:

• No more clumping or sticking: Septadon’t stick to each or the jar

• Easy to see exactly how many areleft: Know exactly when to reorder

• Compact storage size: Fits easily intodrawers

• Convenient quantities: All septa arepackaged in either 50 or 100 packs

• High quality PET packaging: Tested byGC-FID, GC/MS, and GC-ECD toensure the absence of interferingbackground peaks

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Symptom

Extra Peaks/Humps

Normal Problem

Baseline Change After Large Peak

Normal Problem Problem(flow increase) (flow decrease)

Retention Times Prolonged

Normal Problem Problem

Possible Cause

Septum bleed.

Large leak at septum during injection andfor a short time thereafter (common withlarge diameter needles).

Carrier gas leaks at septum or columnconnection.

Remedy

Turn off injector heater. If extra peaksdisappear, clean the inlet and change theliner. If cored septa particles are present,use a centerguide septa and a 23-26 gaugetapered syringe. Important: always use theseptum specified for higher temperature oranalyze at lower inlet temperature.

Replace septum and use smaller diameterneedles.

Check for leaks. Replace septum or tightenconnections if necessary.

Septa Troubleshooting

MAINTENANCE MINDER

After repeated injections, septa can become prone to leakage. To maintain system integrity, change septa regularly.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Our premium non-stick septa have a recess on the injection side, to guide the syringeneedle to the same point with every injection.

• Proprietary plasma treatment ensures non-stick septa without the use of potentiallydamaging 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

Premium Non-Stick Septa

Other suppliers coat their septa with powder to prevent sticking. However, thiscoating can accumulate inside split vent lines and interfere with the analysis ofactive analytes.

But Agilent’s new non-stick septa are plasma coated, which eliminates chemicalbleed and contamination from foreign substances. So your GC system will maintainits integrity, stay cleaner and require less maintenance.

Available in Bleed Optimized, Long-Life, and Advance Green.

Introducing Agilent Premium Non-Stick Septa – featuring a proprietary plasma coating that won’tstick or clump.

Agilent’s plasma-treated non-stick septa

Competitor “non-stick” septa

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Agilent’s premium GC inlet septa are not garden-variety septa

stamped out in large sheets, creating variations in geometry. Rather,

each Agilent premium septum is molded to a perfectly uniform size

and shape.

Individual molding lets us put a dimple in the center of each septumto guide the syringe needle into the inlet.

With the dimpled CenterGuide, the syringe needle enters theseptum at precisely the same spot each time.

The result: minimal coring (see Figure 1).

• Less chance that a cone of material will be punched out of thebottom during the first few injections

• Virtually no septa material falling into the inlet liner, improving chromatographic quality

• Up to 1,000 autoinjections under optimal conditions before failurewith HP Point syringes. The HP Point syringe yields optimalperformance and reliability and reduces coring by parting, notcutting, the septum.

Agilent septa are made of highly durable, high-temperature tested silicone rubber.

Each lot is tested to ensure low bleed at high temperatures.

Because bleed from septa can be a major contributor to the overallsignal, a high-quality septum is an absolute necessity for analysesdemanding increased sensitivity.

Summary of Inlet Septum Characteristics

TEMPERATURESEPTUM TYPE BLEED LIFETIME LIMIT

BTO ✔✔✔ ✔ to 400ºC(Bleed and (optimized forTemperature high temperature)Optimized)

Long Life ✔ ✔✔✔ to 350ºC

Advanced Green ✔✔ ✔✔ to 350ºC

✔✔✔ = best ✔✔ = very good ✔ = good

Figure 1. Comparison of Coring, With and Without CenterGuide

(30x magnification)

High-Temperature Septa Without CenterGuide: Major Coring Before 100 Autoinjections

1 autoinjection 100 autoinjections 700 autoinjections

Agilent BTO Septa With CenterGuide: Very Little Coring Even After 700 Autoinjections

Page 41: GC_GCMSD Consumable and Maintenance

• While general purpose septa do not havethe centerguide of premium septa, they are made of durable material tominimize the risk of contamination and the need for reconditioning

• Convenient blister packs of 50 or 100septa minimize risk of contamination and need for reconditioning

www.agilent.com/chem 40

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

General Purpose SeptaAgilent’s General Purpose Septa are made from an enhanced injection-moldedsilicone rubber material. The septa material,dark red or gray in color, is specified towithstand over 200 automatic injections at an injection port temperature of 350ºC. You can have confidence in yourchromatographic results knowing that each lot of septa is placed through ademanding QC test to ensure that only the highest quality product is delivered to your laboratory.

Agilent’s General Purpose red/graysepta are cost-effective choiceswhich provide:

• Low bleed for reduced instrumentmaintenance downtime and increasedlaboratory productivity

• Less frequent replacement for longlifetime and the ability to withstand morethan 200 autosampler injections atmaximum injection port temperatures

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

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 Temperature350ºC

• Soft, 45 Durometer, Easy On Autosampler Needles

Agilent Bleed and TemperatureOptimized Non-Stick Septa (BTO) • Extended temperature range, low-bleed

• Maximum Injection Port Temperature400ºC

• Virtually eliminates injection-port sticking

• Pre-conditioned; packaged in glass to prevent contamination

• Ideal for use with low-bleed, “Mass Spec” capillary columns

p/n 5183-4757 p/n 5183-4761 p/n 5183-4759

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Ordering Information

Part No.

Premium Non-Stick SeptaAgilent Bleed and Temperature Optimized Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-475711 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4757-1005 mm septa through-hole for on-column in glass jar (50/pk) 5183-4758

Agilent Advanced Green Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-475911 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4759-1005 mm septa through-hole for on-column in glass jar (50/pk) 5183-4760

Agilent Long-Life Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-476111 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4761-1005 mm septa through-hole for on-column in glass jar (50/pk) 5183-4762

General Purpose Septa

Gray Septa

11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk) 5080-8896-5011 mm for 5880, 5890, 6850 and 6890 GCs (100/pk) 5080-8894-100 9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5080-8728-50 9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5080-8728-100

Red Septa

11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk) 5181-1263-50 11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk) 5181-1263-100 11 mm with partial through-hole for 5880, 5890, (50/pk) 5181-3383-50 6850 and 6890 GCs11 mm with partial through-hole for 5880, 5890, (100/pk) 5181-3383-100 6850 and 6890 GCs9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5181-1283-50 9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5181-1283-100 5 mm through-hole for on-column inlets, (25/pk) 5181-1260 automatic or manual injections* 5 mm solid for high column backpressure, on-column inlets* (25/pk) 5181-1261 * 5 mm septa are packaged in glass jars

EASY ONLINE ORDERING

Our online store offers every GC inlet and consumable that your systemmight need – including pieces that are hard to find.

Just visit www.agilent.com/chem/4ecatalog

Page 43: GC_GCMSD Consumable and Maintenance

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

How to Minimize ProblemsGeneral technique for installing ferrules:• don’t overtighten – finger-tighten column

nut, 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, chips, or other damage beforereusing them

• change ferrules when new columns orinjector/detector parts are installed

FerrulesUsing the wrong ferrule or a worn-outferrule to seal your column connection can result in inconsistent and unreliablechromatography. An improper ferrule can cause leaks which allow air and other contaminants to enter theinstrument through the column seal,causing major interference with columnand detector performance. For optimumperformance, ferrules should be replacedevery time the column is replaced andwhen performing column maintenance.

Agilent offers a comprehensive selectionof ferrules made of different materials andconfigurations for a leak-free connectionbetween the column and injector.

Three main types of ferrules are used withcapillary GC columns: graphite, Vespel andVespel-graphite composites. Graphiteferrules can withstand temperatures ashigh as 450ºC, and Vespel and Vespel-graphite ferrules are rated to 280ºC and350ºC, respectively.

What is the Function Ferrules seal the connection of the columnor liner to the system. The ideal ferruleprovides a leak-free seal, accommodatesvarious column outer diameters, seals withminimum torque, will not stick to thecolumn or fittings, and will toleratetemperature cycling.

Why ReplaceSignals that a ferrule is damaged include:

• background noise from oxygen diffusinginto the system

• column bleed catalyzed by oxygen• sample degradation• loss of sample• increase in detector signal/noise• poor retention time reproducibility

Column Ferrule Types

Advantages Limitations

Graphite Easy-to-use, stable seal Soft, easily deformed or destroyed

Higher temperature limit • possible system contamination

• not for use with GC/MStransfer-lines

Vespel or Mechanically robust Flows at elevated temperature

Vespel-graphite Long lifetime • must retighten frequently

• prone to leakage

Polymer bleed problematic withsome detectors (NPD and ECD)

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Normal Peaks

Correct column positioning in both injection port and FID

Tailing Solvent Peaks

Column positioned incorrectly in theinjection port, or possible ferrule or septumparticle in the carrier gas flow path

100% Graphite FerrulesReusing a ferrule – or using off-brandferrules – may be a costly mistake. That’sbecause you’ll increase the likelihood ofdangerous leaks that can damage the GCcolumn and sensitive detector parts.

For best results, always use new Agilentferrules, which feature the highest qualitydesign, and are supported by decades oftechnical expertise.

Wrong Peak Ratios

Column positioned incorrectly in the inlet(either too far or not far enough; verify 4-6mm installation distance)

Two different types of Agilent column nutscan be used with these ferrules:

• The universal column nut (p/n 5181-8830) has a hexagonal head requiring theuse of a wrench to tighten it completely.

• The finger-tight column nut (p/n 5020-8293 for 530um columns and p/n 5020-8292 for columns 320µm or less) doesnot require a wrench to tighten. It can only be used with the 100%graphite ferrules.

Ferrule Troubleshooting

Problems possible after changing ferrules

Normal Peaks Tailing Solvent Peaks Wrong Peak Ratios

TIPS AND TOOLS

Do not use 100% graphite ferrules in GC/MS transfer lines. They willdeform and leak over time, due to the softness of the graphite.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Vespel/Graphite(85%/15%) FerrulesThe combination of graphite and Vespelresults in a ferrule having low oxygen diffusion rates which does not shrink tothe same extent as pure Vespel. Theseferrules are recommended for use withGC/MS or other oxygen sensitivedetectors, like the ECD, but are alsocompatible with other detectors like FIDand NPDs.

In addition, the Vespel/graphite ferrulesprovide added confidence of leak-free connections when installed correctly.Proper installation requires a finger-tightturn on the nut, then an additional 1/4 – 1/2turn with a wrench.

These ferrules are very hard and cannotbe deformed sufficiently to seal multiplecolumn diameters. The ferrule hole mustmatch the column OD exactly to ensure aleak-free seal. For capillary columnapplications, there is a specific ferrule foreach column diameter. Choosing a ferrulewith a larger hole than is specified for agiven column dimension can result in alarge leak. If left unchecked, an improperseal at the injector will result in highcolumn bleed and a shortened columnlifetime. An improper seal at the detectorcan result in increased detectorsignal/noise. In the case of the MSD itcan also contribute to oxidation of the ionsource which can increase the frequencyof detector maintenance.

Two different lengths of Vespel/graphiteferrules are available for capillary columnuse. The standard sized ferrule iscompatible with the universal column nut.The second ferrule size is slightly longerand is specifically designed to fit with theMS interface nut used for the GC/MStransfer line connection. The larger ferrulecan also be used to make columnconnections to inlets and other detectorsbut requires a specially designed columnnut (p/n 05988-20066) to accommodate the longer ferrule.

When using Vespel/graphite ferrules,Agilent recommends tightening the columnnut to a 1/4 turn after the first temperatureprogram runs. Even preconditioned ferrulescan exhibit some shrinkage after atemperature programmed run.

Vespel/Graphite Nut & Ferrule Combinations

Standard ferrule and standard nut

Universal Column Nut + Vespel/Graphite Ferrules

5181-8830 5181-3323 (0.1, 0.2, 0.25 mm ID columns)

5062-3514 (0.32 mm)

5062-3512 (0.45 and 0.53 mm)

Longer ferrule with MS interface nut

MS Interface Column Nut + Vespel/Graphite Ferrules

05988-20066 5062-3508 (0.1, 0.2, and 0.25 mm ID columns)

5062-3506 (0.32 mm)

5062-3538 (0.45 and 0.53 mm)

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

100% Vespel Ferrules Vespel is a high-temperature polyimide basedmaterial which is very hard. This material hasthe lowest permeability to oxygen, making it anexcellent sealing material when making metalor glass connections. These ferrules do notdeform easily. So, it is important to match the ferrule hole size to the proper column diameter.

The main disadvantage of 100% Vespel ferrulesis the shrinkage of the material when exposedto temperature cycling conditions. 100% Vespelferrules should only be used for isothermalapplications.

Agilent Ferrule Selection Recommendations

Ferrule/Seal Upper Usages LimitationsType Temperature

Limit------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Graphite 450ºC General purpose Not for MS or (100%) for capillary columns. oxygen sensitive

Suitable for FID and NPD. detectors.Recommended for high temperature and cool on-column applications. Can be removed easily.

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel/Graphite 350ºC General purpose for Not reusable.(85%/15%) capillary columns.

Recommended for MS or oxygen sensitive detectors. Most reliable leak-free connection.

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel 280ºC Isothermal operation. Leaks after(100%) temperature cycle.------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------SilTite N/A Use only with SilTite Nut Kits Not Reusable(100% metal)

VIDEO

To view a video on ferrules, visit www.agilent.com/chem/techsupport.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Ordering Information

Ferrule Id Column Id Quantity Part No.(mm) (mm)

General Purpose Graphite Ferrules (Short Ferrules)0.5 0.1, 0.2, 0.25, 0.32 10/pk 5080-88531.0 0.53 10/pk 5080-87730.4 0.05-0.25 10/pk 500-21140.8 0.45, 0.53 10/pk 500-2118

85% Vespel, 15% Graphite Ferrules (Short Ferrules)0.80.3 0.1, 0.2 10/pk 5062-35160.80.4 0.1, 0.2, 0.25 10/pk 5181-33230.80.5 0.32 10/pk 5062-35140.80.8 0.45, 0.53 10/pk 5062-3512

Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)0.3 0.1 10/pk 5062-35070.4 0.1, 0.2, 0.25 10/pk 5062-35080.5 0.32 10/pk 5062-35060.8 0.53 10/pk 5062-3538

These ferrules are recommended for use with GC/MS.

100% Vespel High-Performance Ferrules (Short Ferrules)0.4 0.1, 0.2, 0.25 10/pk 5181-33220.5 0.32 10/pk 5062-35130.8 0.45, 0.53 10/pk 5062-3511

These ferrules are recommended for use in isothermal analysis only.

Specialty Ferrules, 85% Vespel, 15% GraphiteTwo Hole 0.4 ID holes 0.1, 0.2, 0.25 10/pk 5062-3580

0.5 ID holes 0.32 10/pk 5062-3581No Hole 10/pk 5181-3308

SilTite Metal FerrulesFor use with 0.20-0.25 mm ID 0.4 10/pk 5184-3569capillary columns. Includes 2 column nutsFor use with 0.32 mm ID capillary 0.5 10/pk 5184-3570columns. Includes 2 column nutsFor use with 1/16 in. od 10/pk 5184-3571SS tubing. Includes 2 column nutsFor use with 0.53 mm ID capillary columns. 0.8 10/pk 5188-2789Includes 2 nuts

Column NutsShort NutsUniversal column nut, 1/16 in. hex 2/pk 5181-8830Finger-tight column nut for 0.53 mm columns* 1 ea 5020-8293Finger-tight column nut for 0.32 mm columns* and smaller 1 ea 5020-8292Blanking plug, finger-tight style 1 ea 5020-82946850 Column Nut 2/pk 5183-4732

Long NutsMS interface column nut 1 ea 05988-20066Column nut for GC/MS ferrules 1 ea 05921-21170Column nut wrench, 1 /4 in. and 5 /16 in. 1 ea 8710-0510* For use with graphite ferrules only.Always match short nuts with short ferrules and long nuts with long ferrules.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

LinersAgilent offers a complete selection of GC split and splitless inlet liners thatdeliver consistent quality. So you can getconsistent results.

And unlike other manufacturer’s liners,Agilent liners are built to Agilent’s preciseinlet tolerances which helps ensureoptimal dimensional accuracy andinertness toward demanding compounds.

Choosing the proper liner for a specificapplication can be a difficult and challenging task. 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 inletor sample vaporization

What is the Function Liners are the centerpiece of the inlet system in which the sample is evaporatedand brought into the gas phase.

Why ReplaceThese problems will occur if the liner is notchanged on a regular basis or if the correctliner is not used:

• peak shape degradation

• solute discrimination

• poor reproducibility

• sample decomposition

• ghost peaks

• reduced column life

How to Minimize ProblemsChange 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, visit www.agilent.com/chem/techsupport.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Discussion of LinerCharacteristics

Liner VolumeThe purpose of the injection port is to allowthe introduction of a sample into the gaschromatograph in an accurate, reproduciblemanner. The vaporized sample should be a true representation of the liquid sampleand, unless specifically desired, should be injected without chemical change. Theelevated temperatures used in the inletvaporize the liquid sample to a gas fortransfer to the head of the column. Thisphase transition is accompanied by a verysignificant volume change. The volume ofthe resulting vapor must be small enoughto fit within the volume of the liner. If thevolume is too great for the liner, it couldresult in backflash, or sample loss causedby expansion into the septum purge or splitvent lines. Both can compromisereproducibility and sensitivity. Backflashalso frequently results in sample carryover.

Larger volume liners (> 800 µL) are characterized by larger inside diameters(ID) and are typically used with injectionsizes of 1 µL or more. The small volume liners have a smaller ID and are usuallyused with small injection sizes (< 1 µL), fast 100 µm ID columns, gas samples, orwhen using external sampling devices like headspace and purge and trap.

Liner DeactivationActive sites on inlet liners can adsorb sample components and cause peak tailing,and potential loss of sensitivity andreproducibility. Deactivation agents areused to cover or react with active sites onthe glass surface of the liner. Agilent linersare deactivated using deactivationprocedures that produce reproducible andinert liners, with long lifetimes. For splitlessapplications or when even slightly polarcompounds must be analyzed, adeactivated liner should be used.

With use, even deactivated liners canbegin to exhibit activity. When this occurs,the liner should be replaced. Liners can becleaned to remove particulate material orsolvent rinsed to remove less volatilecomponents. However, choosing theproper liner cleaning procedure can bedifficult. Some solvents may remove thedeactivation layer, and tools might scratchthe glass surface of the liner, resulting inthe generation of unwanted active sites.A new liner almost always outperforms a cleaned and re-deactivated one –especially for trace analysis.

TIPS AND TOOLS

Agilent offers a free software tool that calculates the vapor volume of an extended list ofcommon solvents, based on your choice of inlet temperatures and pressures for a givenAgilent inlet liner. To download, go to www.agilent.com/chem/techsupport. Click “UserContributed Software;” then, click “GC Pressure/Flow Calculator.”

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Design FeaturesDimensions • The outside diameter (OD) of the liner

determines if the liner is more effectivelyused in split or splitless mode

• Larger OD liners are designed for splitlessoperation, fit tightly and limit sample contact with metal parts of the inlet

• Larger OD liners improve analyte recoveryby retaining more sample inside the liner

• Agilent splitless liners are all designedwith exacting dimensional tolerances tofit tightly in the inlet and minimize samplecontact with metal surfaces

• Smaller OD liners are designed for splitinjection because they produce lessresistance to carrier and split flowthrough the inlet

• Large volume liners are used for splitinjections with enforced dimensional stability for a wide range of split ratios

TapersTapering or narrowing the liner internaldiameter (ID) is done for a number ofpurposes:

• Bottom taper focuses sample onto thehead of the column

• Bottom taper minimizes contact withmetal parts of the inlet

• Center taper positions glass wool correctly

• Top taper minimizes sample backflash

To operate properly, the column must beinstalled correctly in the injection port withthe tip of the column ideally located abouthalfway into the taper, or about 4-6 mmfrom the column tip to the top of the ferrule(See Figure 1). Some applications will work better with different column installationdepths. Therefore, you should check theinstrument manual for proper installationdistances and determine which distance is appropriate for your application.Reproducible positioning is important for repeatable quantitative results.

Packing

Glass WoolMany liner designs use deactivated glass wool packing. The glass wool ispositioned or held in place near the center of the liner to:

• Provide additional surface area for complete volatilization of the sample tominimize thermal discrimination

• Trap non-volatile components and septumparticles before they reach the column

• Wipe any sample from the syringe needle,thereby increasing reproducibility and preventing sample residue build-up at theseptum

Glass wool liners that have glass wool nearthe center of the liner, such as Agilent PartNos. 5183-4647 and 5183-4711, arerecommended for automatic injections.

If glass wool is positioned at the bottom ofthe liner, its main purpose is simply to trapnon-volatile components. Glass wool isgenerally not recommended for the following analytes:

• phenols• organic acids• pesticides• amines• drugs of abuse• reactive polar compounds• thermally labile compounds

Glass CupsAnother design feature used to helpvolatilize the sample and provide good mixing is the incorporation of a glass cupinside the liner. Glass cup liners are alsoavailable with additional glass wool andinert packing to increase reproducibility and limit sample discrimination. Notrecommended for use with ElectronicPressure Control Inlets on 6890 or 6850 GCs.

Figure 1.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner TroubleshootingSymptom

Tailing Peaks

Normal Problem

Baseline Rise Before or After Peak

Normal Problem Problem

Baseline Change After Large Peak

Normal Problem Problem

Unresolved Peaks

Normal Problem Problem

Possible Cause

Sample components adsorbed by column,inlet liner or contaminated gold inlet seal.

Needle hitting and breaking packing ininlet liner.

Column end poorly cut (sample absorption).Broken or chipped inlet liner.

Inlet flow too low.

Sample decomposing.

Column and inlet liner misaligned. See also”Septum Troubleshooting,” page 37

Column or inlet liner contaminated or column deteriorating.

Remedy

Use new, deactivated liner or clean oldliner and replace glass wool.

Partially remove packing from liner or usewithout packing.

Remove column. Make a clean, square cut using a reliable capillary fused silicacutting tool (such as a ceramic wafer orthe Agilent Column Cutter), then reinstallcolumn.

Make sure total flow in inlet is above 40 mL/min.

Remove inlet liner and check cleanliness.Use new, deactivated liner or replace glasswool and packing. Column/sampleresidues could also be the problem.

Check installation of column end and inletliner; adjust if necessary.

Use a guard column to prolong column life.Remove inlet liner and check cleanliness.Use new, deactivated liner or replace glasswool and packing. Trim the front end of thecolumn a minimum of 6 inches.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Agilent LinersOur engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Intensive linerdevelopment and testing have resulted in a set of liners that we recommend whenever new methods are being developed, when methods are being optimized, or when problems with existing methods are encountered. These liners are:

Split injection:Agilent low-pressure-drop split liner withglass wool, bottom taper, glass bead foreasy positioning, and deactivated, AgilentPart No. 5183-4647 (with extraordinarilytight dimensional control for optimum split performance).

Splitless injection:Single tapered liner without glass wool,deactivated, Agilent Part No. 5181-3316EN.

Note: For pesticide analysis – especiallyDDT and Endrin, where breakdown is aproblem – we recommend Agilent PartNos. 5181-3316EN and 5181-3315EN.

General purpose split/splitless injection: Similar design to Agilent Part No. 5183-4647, but with an outer diameter thatcompromises for both split and splitlessinjections, Agilent Part No. 5183-4711.

Direct injection:Straight liner without glass wool,deactivated, Agilent Part No. 5181-8818(use only for gas samples, headspace, orpurge and trap applications).

Direct ConnectDirect Connect liners are ideal forcustomers running highly sensitivecompounds, or for users who requiremaximum inertness performance andminimal inlet discrimination for trace GCand GC/MS applications. Direct Connectliners also eliminate sample exposure tometal parts, minimizing inlet-relateddegradation. These liners are included inour new 8270 EPA Applications kitdesigned specifically for optimizing a6890/5973 GC/MSD to this method.

The liners are deactivated, come in either a single or double taper, and utilize a pressfit connection to the column. In addition,there is a small, drilled hole in the side of the liner whose size and placement wasoptimized by Agilent R&D engineers toallow them to work with EPC.

Focus LinerImprove reproducibility, improve results.The Focus Liner traps a precisely controlledamount of glass wool in the ideal positionin the injection port liner. At the point ofinjection, the glass wool provides extrasurface area for vaporization, trapsnonvolatile sample residue, and wipes any residual sample from the sampleneedle – reproducibility is the result.

In addition to these liners we offer a broad selection of liners for your specificapplication needs.

Liner O-RingsLiners are sealed in the inlet with O-ringsor graphite seals. O-ring seals are easier toremove and to replace than graphite thatdeforms and flakes apart. The graphiteseals should be used when inlettemperatures exceed 350ºC.

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Flip Top Inlet Sealing SystemAgilent’s NEW Flip Top Inlet Sealing System is the faster, smarter way to changeinlet 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 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. Do you change liners more than 2-3 times per week?

2. How long does it take you to change a liner (total downtime)?

3. Do you want to increase your productivity and column life?

4. 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/MSsystem is changing the inlet liners. A hot inlet may have to be opened on each system every24 to 48 hours to change a dirty inlet liner. The special wrench used for this operation is oftenmisplaced, bent at an odd angle, too thin, or simply awkward to use. In addition, the inlet nutis usually too hot to handle so it must be turned several times with the wrench before it willrelease the top assembly of the injection port.

Once the dirty liner is replaced, the inlet nut must be replaced on the injection port andoccasionally the wrench slips off the nut leading to scrapes, burns, and cuts. It can take atleast 5 minutes of wrestling with this hot injection port nut and wrench combination just totake out the old liner and put in a new one. By the time the operator finishes the procedureand re-equilibrates, it can result in 15 minutes of downtime!

Of course, doing this with a GC/MS causes even more problems as ambient air is drawn into thecapillary column, through the hot MS interface, and into the heated source resulting in multipleproblems for the operator including shortened column life and air background in the MS.

The Easiet Way to Change Inlet Liners!Agilent’s new Flip Top Inlet Sealing System is a device designed to allow the user to safelyand reliably change an inlet liner in as little as 30 seconds without tools in a consistent leak-free manner. No longer will you have to contend with frustrating searches for wrenches orburning your fingers on hot inlets.

Available exclusively from Agilent, the Flip Top has a levered arm that attaches to any6890/6850/5890 insert weldment and locks to the injection port using an adapter ringscrewed onto the inlet. Once installed, the user simply lifts the arm of the Flip Top whichreleases the insert weldment from the injection port, and allows instant access to the liner.The process is simply reversed to re-seal the weldment to the port.

Description Part No.

Flip Top Inlet Sealing System 5188-2717

Liner O-rings (10/pk) 5188-2741

VIDEO

To view videos on the Flip Top Inlet Sealing System,visit www.agilent.com/chem/fliptop2

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Ordering Information

Application Liner Single 5/pk 25/pkVolume(µl) Liner

Agilent Choice LinersLiner, split, low press. drop, For split injection 870 5183-4647 5183-4701 5183-4702glass wool, taper, deactivated

Liner, splitless, single-taper, For splitless injection 900 5181-3316 5183-4695 5183-4696no glass wool, deactivated

NEW! Liner, Splitless, For trace pesticide 900 5181-3316EN Single-taper, no glass wool, analysispolymerically deactivated

Liner, direct, 2 mm ID, For direct injection 250 5181-8818 5183-4703 5183-4704deactivated (use for gas samples,

headspace, or purgeand trap applications)

Liner, general purpose For split/splitless 870 5183-4711 5183-4712 5183-4713split/splitless, glass wool, injectiontaper, deactivated

Splitless Inlet LinersLiner, splitless, single-taper, glass wool, deactivated 900 5062-3587 5183-4693 5183-4694

Liner, splitless, double-taper, no glass wool, deactivated 800 5181-3315 5183-4705 5183-4706

NEW! Liner, Splitless, For trace pesticide 800 5181-3315EN double-taper, no glass wool, analysispolymerically deactivated

Direct Inlet LinersLiner, direct, 2 mm ID, non-deactivated, quartz 250 18740-80220 5183-4707 5183-4708

Liner, direct, 1.5 mm ID, non-deactivated 140 18740-80200 5183-4709 5183-4710[use for gas samples, headspace, or purgeand trap applications]

Liner, straight, splitless 4.0 mm ID 990 210-3003 210-3003-5

Split Inlet Liner 990 19251-60540 5183-4691 5183-4692Liner, split, glass wool, non-deactivated

Split Inlet Liners For Manual Injection 800 18740-80190 5183-4699 5183-4700Liner, split, with cup, no glass wool

Liner, split, with cup, glass wool, and packing 800 18740-60840 5183-4697 5183-4698[not recommended for use with electronic pressure control (EPC)], for manual injection

Direct Connect LinersPart No.

Single taper direct connect liner, 4 mm ID, deactivated G1544-80730Dual taper direct connect liner, 4 mm ID, deactivated G1544-80700

Focus LinersID Wool Dimensions Part No.

Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4004-5Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4022-5

Liner O-Rings Part No.Fluorocarbon O-ring (12/pk) 5180-4182Graphite O-ring for splitless liner (10/pk) 5180-4173Graphite O-ring for split liner (10/pk) 5180-4168Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk) 5188-2741

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Instrument Inlet Parts and SuppliesWhen it comes to inlet replacement parts for your Agilent GCs, don’tsettle for imitations; choose only genuine Agilent parts.

Our inlets are backed by the same 40 years of design experience thatyou’ve come to expect from our instruments. So you get optimalperformance, plus the reproducible results that your lab demands.

What’s more, Agilent supplies every replacement part that yoursystem might need – not just a few select pieces. So you can get allyour consumables, all in one place.

Septum See page 36

Split/Splitless Inlet Weldment Part No. G1544-60575, for 6890 GC with EPC

Septum NutPart No. 18740-60835

Viton O-RingPart No. 5180-4182, 12/pk

Liners See page 47

Column Nut for 6890 GCPart No. 5181-8830, 2/pk

Heater-Sensor AssemblyPart No. G1544-61140

Gold-Plated Seal (Splitless)See page 55

Washer Part No. 5061-5869, 12/pk

Reducing Nut Part No. 18740-20800,

1 each

Ferrules (85% Vespel, 15% Graphite)– Part No. 5062-3516, 0.37 mm I.D.,

for 100-200 µm Columns, 10/pk

– Part No. 5181-3323, 0.40 mm I.D., for 250 µm Columns, 10/pk

– Part No. 5062-3514, 0.50 mm I.D., for 320 µm Columns, 10/pk

– Part No. 5062-3512, 0.74 mm I.D., for 530 µm Columns, 10/pk

TIPS AND TOOLS

For a complete parts breakdown, see the5890, 6890, and 6850 series GC InstrumentUser and/or Service Manuals, or visitwww.agilent.com/chem.

Retaining Nut Part No. G1544-20590

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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Part No.

6890/6850 Split/Splitless Insert AssembliesStandard manual pneumatics 19251-60575Original standard EPC using 1/4" split vent filter. G1544-60575Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to G1544-80580clean carrier gas for ECD operation.S/SL insert weldment. Used with large charcoal canister type filter G1544-60585for 6890/6850.Similar to G1544-60575 except carrier lines separated for interface to valved G1580-60575systems of a G1540A instrument.S/SL insert assembly for G1540A with valved system option. This insert assembly G1580-60585uses the large charcoal canister split vent filter for 6890/6850.

5890 Split/Splitless Multimode Inlet SuppliesSeptum retainer nut 18740-60835Retainer nut for headspace sampling 18740-60830Retaining nut 19251-20620Reducing nut 18740-20800For a complete parts breakdown, see the 5890, 6890 and 6850 series GC Instrument User and/or Service Manuals.

Liner Seals and WashersStainless steel 18740-20880Gold-plated seal 18740-20885Gold-plated seal with cross 5182-9652Washers (12 pk) 5061-5869

Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity. Other manufacturers’ seals are notmachined, and may compromise your results.

Gold-plated seal p/n 18740-20885 Gold-plated seal with cross p/n 5182-9652Use when inlet flow exceeds 400 ml/min.

TopBottom

Page 57: GC_GCMSD Consumable and Maintenance

“Agilent lets you choose from over 1,000different columns. It’s no wonder that, for nearly 40 years, customers have builtproducts – and entire businesses – aroundthe results they get from our DB- and HP-capillary GC columns.”

Phil Stremple, GC Columns Program Manager

ColumnsChoosing the right GC column andfollowing Agilent’s simple column carerecommendations will maximize GC columnperformance and lifetime. In this section ourexperts offer practical advice on how toselect, install and store your GC column,plus give helpful hints about avoiding thermaland oxygen degradation. Because GC columncontamination is the primary cause ofshortened column lifetime, we’ve alsoincluded a detailed discussion about theprevention of non-volatile and semi-volatilecontamination, as well as appropriaterecovery measures.

www.agilent.com/chem 56

CATALOG

For a complete selection of GC columns and parts, see Agilent’s 2005-2006 Essential Chromatography Catalog. Or, visit our online catalog atwww.agilent.com/chem/4ecatalog.

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COLUMNS

While GC column maintenance is simple, the frequency and type of column maintenance that is required varies due to many system and samplefactors. Instead of simply following a

Column Maintenancepredefined timetable of maintenance items,the main focus should be how to obtain the highest performance and lifetime from a capillary column. This depends onchoosing the right column, correct

installation/system setup, and avoiding the primary factors that cause columnperformance degradation (breakage,thermal damage, oxygen damage, chemicaldamage and contamination).

PhasesAll phases can be used with conventionalGC systems, and most stationary phasescan be used with a GC/MS system.However, it is a good idea to choose aphase for your application that has thelowest amount of column bleed aspossible. Column bleed is the naturaldegradation of the stationary phase thatoccurs at higher temperatures, whichappears as an elevated baseline as thetemperature rises to the column’s upperthermal limit. Column bleed will deposit inthe MSD ion source, which can decreaseMSD performance. By minimizing theamount of column bleed, you will helpreduce the frequency of required ionsource maintenance.

There are a few simple rules for choosingcolumns with lower bleed levels:• Choose a low-bleed phase for your

application – Agilent has developedseveral low-bleed versions of the mostpopular phases. These are chemicallydesigned to possess minimal levels ofcolumn bleed possible and often havethe benefit of an increased upper-temperature limit.

• If a low-bleed column is not available,choose a low-polarity column with amoderate film thickness. The amount ofbleed will rise with increases in polarity,film thickness, and length.

• Use more polar phases when difficultisomer separations are required. (Choosea more polar phase when you must, buttry to make it the least polar column thatwill do the job)

DimensionsAll dimensions can be used withconventional GC systems. Many types of GCcolumn phases can be used with the MSD,but there are some dimensionalconsiderations. The maximum allowableflow rate and optimal sensitivity flow rateswill vary depending upon the type of pump.In general, the column flow should be1mL/min (2mL/min for Performance TurboPumps). Therefore, column length and internal diameter combinations arerestricted to provide the appropriate flow to the GC/MS.• Narrow-bore columns (0.25mm i.d. and

smaller) can be installed directly into theGC interface.

Selection of Capillary Columns for GC and GC/MS

Primary“Quantion”

is hidden

Primary“Quantion” is enhanced

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COLUMNS

• Wide-bore columns (0.32mm i.d.) that are30m or longer can be installed directlyinto the 5973 GC interface (other MSDsmay require 50m or longer). If using awide-bore column with a shorter length,an effluent splitter or jet separator shouldbe utilized.

• Columns with internal diameters greaterthan 0.32mm should not be directlyinterfaced into the GC interface. For thesecolumns, an effluent splitter or jetseparator should be installed.

Description Part No.

DB-1ms, 0.25mm i.d., 30m, 0.25µm 122-0132

HP-5ms, 0.25mm i.d., 30m, 0.25µm 19091S-433

DB-XLB, 0.25mm i.d., 30m, 0.25µm 122-1232

DB-35ms, 0.25mm i.d., 30m, 0.25µm 122-3832

HP-INNOWax, 0.25mm i.d., 30m, 0.25µm 19091N-133

Column Installation, Setup, & 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.

• Avoid re-using ferrules.

• Use an appropriate column cutting tool such as a ceramic wafer or diamond tipped scribe.

• Make sure column ends are cleanly cut and free of particulate matter before installing into the injector and detector.

• Install the column the appropriatedistance into the injector and detector as specified by the GC manufacturer.

• The column should be placed on a column hanger and no portion of the capillary tubing should touch the oven walls.

• Verify that all fittings are leak-free and the carrier gas is oxygen-free beforeheating the oven.

• Briefly conditioning a column beforeinstalling it into the GC/MS interface isrecommended. When the column andinlet are first heated, volatile materialswithin the flow-path and a small portionof the column stationary phase move intothe gas phase. These materials are thencarried by the carrier gas into the MSDand can deposit in the MSD ion source.This can decrease MSD performance.Conditioning the column briefly prior toinstallation into the MSD will minimizethe contamination brought into the ionsource.

Popular Column Choices

TIPS AND TOOLS

Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.

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COLUMNS

Bad

Good

Example of column cuts

• Check the installation and set the linear velocity by injecting a non-retainedcompound.

• Condition the column as specified in theliterature provided with each column.

Description Part No.

Ceramic wafer (4/pk) 5181-8836

20x Magnifier 430-1020

General Purpose Graphite ferrule (0.5mm ID, for column IDs ≤ 0.32mm) 10/pk 5080-8853

General Purpose Graphite ferrule (1.0mm ID, for 0.45-0.53mm ID columns) 10/pk 5080-8773

Gas leak detector 115V 5182-9646 Gas leak detector 220V 5182-9648

Column BreakageFused silica columns can break whereverthere are small scratches or abrasions inthe protective polyimide coating.Continuous heating and cooling of theoven, vibrations caused by the oven fan as well as being wound on a circularcage all place stress on the tubing. While under these stresses, flaws will propagate until breakage occurs.

NOTE: Larger diameter columns (0.45- 0.53mm id) are more prone to breakage.

Description Part No.

Fused Silica Union, Universal 2-way (5/pk) 705-0905

Quartz deactivated column connector (5/pk) 5181-3396

Polyimide Sealing resin (5 grams) 500-1200

Causes of Performance Degradation

Column Installation & Setup continued

Prevention

• Avoid scratches and abrasions by notexposing the column to sharp edges suchas column hangers and tags, metal edgesin the GC oven, column cutters and othermiscellaneous items on the lab bench.

• Avoid winding or bending the column too tightly.

Recovery

• If a broken column has been heated,damage to the stationary phase is verylikely. Discard the back of the column (the column half without carrier gas). Trim 6 inches off the end of the column and reinstall.

• If the broken column has not beenheated, connect the two pieces with a low volume union. No more than 2-3 unions should be installed for one column.

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COLUMNS

Description Part No.

FlowTracker 2000 Flowmeter and Leak Detector 5183-4780

Big Oxygen Trap (750 cc, 1/8" fitting) BOT-2

Big Moisture Trap (750 cc, 1/8" fitting) BMT-2

Big Universal Trap (Combination Trap) (750cc, 1/8" fitting, He) RMSH-2

Advanced Green Septa (11mm, 50/pk) 5183-4759

Thermal DamageExceeding a column’s upper temperaturelimit results in accelerated degradation ofthe stationary phase and tubing surface.This results in the premature onset ofexcessive column bleed, peak tailing foractive compounds and/or loss of efficiency(resolution).

Prevention • Do not exceed the columns specified

upper temperature limits:

– Isothermal limit: temperature that the column can be held at for anindefinite time

– Programmed limit: maximum columntemperature; column should only beheld there for about 5-10 minutes

• Set the GC maximum oven temperaturefunction at or a few degrees above thetemperature limit of the column. Withtwo columns in the oven be sure to setthe maximum temperature to thetemperature limit of the column with thelowest value.

Recovery

• Disconnect column from detector

• Heat the column 8-16 hours at theisothermal limit

• Remove 10-15 cm from the column end

• Reinstall into the detector and conditionas usual

NOTE: Thermal damage cannot be reversed.The column usually does not return to itsoriginal performance; however, it is oftenstill functional. The life of the column willbe reduced after thermal damage.

Oxygen DamageOxygen is an enemy to all capillary GCcolumns. Constant exposure to oxygendoes not damage the column at or nearambient temperatures; however, severedamage occurs as the column temperatureincreases. A leak in the carrier gas flowpath (e.g., gas lines, fittings, injector,septa) is the most common source ofoxygen exposure. As the column is heated,very rapid degradation of the stationaryphase occurs. This results in the prematureonset of excessive column bleed, peaktailing for active compounds and/or loss ofefficiency (resolution).

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.

PreventionMaintain 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 arecompletely empty

Recovery Perform column “bakeout” as describedunder thermal damage recovery.

NOTE: Oxygen damage occurs very rapidly.In less severe cases, the column may stillbe functional but at a reduced performancelevel. In more severe cases, the column isirreversibly damaged.

TIPS AND TOOLS

Install a moisture trap upstream of the oxygen trap to increase the oxygen trap lifetime.

Page 62: GC_GCMSD Consumable and Maintenance

61 www.agilent.com/chem

COLUMNS

GUARD COLUMNA guard column is a piece of fused silica tubing attached with a union tothe front of the analytical column with the following characteristics:

• Material should be deactivated fused silica tubing to minimize soluteinteractions.

• Length should be from 1-10 meters. Typical lengths of 5-10 meters allowsubstantial trimming before the entire guard column has to replaced.

• Internal diameter are generally the same as the column. Guard columns with larger ids can be used for additional residue capacity.

• A low volume union should be used to attach the tubing to the column.Glass pressfit unions are inexpensive and easy to install. DuraGuardcolumns offer the guard column built into the analytical column as asingle piece of fused silica, eliminating the need for unions.

Guard columns are used to minimize the effect of non-volatile residues on the analysis. The non-volatile residues deposit in the guard column andnot in the analytical column. This greatly reduces the interaction betweenthe residues and the sample. Periodic cutting or trimming of the guardcolumn is usually required upon a build-up of residues. The onset of peakshape problems is the usual indicator that the guard column needstrimming or changing.

Guard column installation instructions are available at www.agilent.com/chem.

Click on “Technical Support,” then “GC Reference Library.” The procedure can be

found under “General Information.”

Guard Column

Chemical DamageInorganic or mineral acids and bases arethe primary sources of chemical damage to stationary phases. Most of these acidsand bases have low volatility andaccumulate at the front of the column. If allowed to remain, the acids or basesdamage the stationary phase. The onlyorganic compounds that have beenreported to chemically damage stationaryphases are perfluoroacids and these needto be present at high levels (e.g., 1% orhigher). This results in the premature onset of excessive column bleed, peaktailing for active compounds and/or loss of efficiency (resolution).

NOTE: Hydrochloric acid and ammoniumhydroxide are the least harmful of the group as both tend to follow any water that is present in the sample. Thus, if HCl or NH4OH are present in a sample,minimizing water retention will renderthese compounds relatively harmless to the column.

Prevention• Perform sample preparation to remove

inorganic acids and bases from thesample

• Install guard column and trim frequently

• If acids or bases must be used choose anorganic alternative or HCl or NH4OH

Recovery• Remove 0.5 to 1 meter from the front

of the column

• Severe cases may require the removal of 5 or more meters

Column ContaminationColumn contamination is the mostcommon problem encountered in capillaryGC. Unfortunately, it mimics most otherchromatographic problems and is oftenmisdiagnosed. A contaminated column is usually not damaged, but it may berendered unusable. There are two basictypes of contaminants: nonvolatile andsemivolatile.

INJECTOR DETECTOR

Column

Union

Guard Column

Page 63: GC_GCMSD Consumable and Maintenance

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COLUMNS

Nonvolatile Contaminants Nonvolatile contaminants or residues donot elute and accumulate in the column(most often confined to the first fewmeters). The column becomes coated withthese residues which interfere with theproper partitioning of solutes in and out of the stationary phase. Also, the residuesmay interact with active solutes resulting in peak adsorption problems (evident aspeak tailing or loss of peak size). Activesolutes are those containing a hydroxyl (-OH) or amine (-NH) group, and somethiols (-SH) and aldehydes.

Prevention • Perform sample cleanup to remove

nonvolatile materials from the sample

• Use injection port liners packed withglass wool (may not be feasible whenanalyzing 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 0.5 to 1 meter of thefront of the column

• Turn the column around (install detectorend into injector). Not recommended forsensitive ECD, NPD, and MS detectors.

• Solvent rinse the column

• Cut the column in half and use the backhalf (detector side)

Semivolatile ContaminantsSemivolatile contaminants or residuesaccumulate in the column, but eventuallyelute. Hours to days may elapse beforethey completely leave the column. Likenonvolatile residues, they may cause peakshape and size problems and, in addition,are usually responsible for many baselineproblems (instability, wander, drift, ghostpeaks, etc.).

Prevention• Perform sample cleanup to remove

semi-volatile materials from the sample

• Increase the final temperature of the GC run (not to exceed the temperaturelimit of the column)

• Change septa regularly

Recovery • Bakeout the column: limit 1-2 hours

(excess baking may polymerize somecontamination and reduce columnlifetime)

• Solvent rinse the column

Does Your Sample Have Residues?Perform this simple test.

1. Place 20-30 µL of the sample onto amicroscope slide.

2. Put the slide over the heated GC inletfor 20 minutes.

3. Hold the slide up to the light.

If you can see anything where the dropwas, your sample has residues.

Description Part No.

Split/Splitless Inlet liner: glass wool,taper, deactivated (5/pk) 5183-4712

Splitless Inlet liner: single-taper, no glass wool, deactivated (5/pk) 5183-4695

Quartz deactivated column connector (5/pk) 5181-3396

Polyimide sealing resin (5 grams) 500-1200

Deactivated Fused silica, 10m, 0.53mm i.d. 160-2535-10

Deactivated Fused silica, 10m, 0.25mm i.d. 160-2255-10

Capillary column rinse kit 430-3000

Column StorageCapillary columns should be stored in theiroriginal box when removed from the GC.Place GC septa over the ends to preventdebris from entering the tubing. Uponreinstallation of the column, the columnends need to be trimmed by 2-4 cm toensure that a small piece of septa is notlodged in the column.

If a column is left in a heated GC, thereshould always be carrier gas flow throughthe column. The carrier gas flow can beturned off only if the oven, injector,detector and transfer lines are turned off(i.e., not heated). Without carrier gas flow,damage to the heated portion of thecolumn occurs.

Page 64: GC_GCMSD Consumable and Maintenance

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COLUMNS

DB-1ms• 100% Dimethylpolysiloxane• Identical selectivity to DB-1• Nonpolar• Very low bleed characteristics• Improved acid performance compared to

standard 100% Dimethylpolysiloxanecolumns

• Improved signal-to-noise ratio for bettersensitivity and mass spectral integrity

• Excellent general purpose column• Bonded and cross-linked• Solvent rinsable

I.D. Length Film Part No.

0.10 10 0.10 127-01120.10 10 0.40 127-01130.10 20 0.10 127-01220.10 20 0.40 127-0123

0.20 12 0.33 128-01120.20 25 0.33 128-0122

0.25 30 0.10 122-01310.25 30 0.25 122-01320.25 60 0.25 122-0162

0.32 30 0.10 123-01310.32 30 0.25 123-01320.32 60 0.25 123-0162

DB-1ms Order Guide Temperature Limits (-60 to 340/360°C)

Column Types and Characteristics

Similar PhasesHP-1ms, Rtx-1ms, CP-Sil 5CB

ApplicationsGeneral purpose: Amines, hydrocarbons,pesticides, PCBs, phenols, sulfurcompounds, flavors and fragrances.

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COLUMNS

I.D. Length Film Part No.

0.20 12 0.33 19091S-1010.20 25 0.33 19091S-1020.20 50 0.33 19091S-105

0.25 15 0.10 19091S-3310.25 15 0.25 19091S-4310.25 15 1.00 19091S-2310.25 30 0.10 19091S-3330.25 30 0.25 19091S-433*0.25 30 0.50 19091S-1330.25 60 0.10 19091S-3360.25 60 0.25 19091S-436

0.32 15 1.00 19091S-2110.32 25 0.52 19091S-1120.32 30 0.10 19091S-3130.32 30 0.25 19091S-4130.32 30 0.50 19091S-1130.32 60 0.10 19091S-3160.32 60 0.25 19091S-416

HP-5ms Order Guide Temperature Limits (-60 to 325/350°C)

* This column is shipped with the 5973 MSD.

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

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

Similar PhasesRtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms,BPX-5, Rtx-5 Amine

ApplicationsSemivolatiles, alkaloids, drugs, FAMEs,halogenated compounds, pesticides,herbicides

I.D. Length Film Part No.

0.18 20 0.18 121-55220.18 40 0.18 121-5542

0.20 25 0.33 128-55220.20 50 0.33 128-5552

0.25 25 0.25 122-55220.25 25 0.40 122-552A0.25 30 0.10 122-55310.25 30 0.25 122-55320.25 30 0.50 122-55360.25 50 0.25 122-55520.25 60 0.10 122-55610.25 60 0.25 122-5562

0.32 30 0.10 123-55310.32 30 0.25 123-55320.32 30 0.50 123-55360.32 50 0.25 123-55520.32 60 0.10 123-55610.32 60 0.25 123-5562

DB-5ms Order Guide Temperature Limits (-60 to 325/360°C)

Similar PhasesRtx-5ms, HP-5ms, PTE-5, CP-Sil 8CBms,BPX-5

ApplicationsSemivolatiles, alkaloids, drugs, FAMEs,halogenated compounds, pesticides, herbicides

Page 66: GC_GCMSD Consumable and Maintenance

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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, herbicides, PCBs

and PAHs • Certified for MS • Bonded and cross-linked • Solvent rinsable

I.D. Length Film Part No.

0.18 20 0.18 121-12220.18 30 0.18 121-1232

0.20 12 0.33 128-12120.20 25 0.33 128-1222

0.25 15 0.10 122-12110.25 15 0.25 122-12120.25 15 1.00 122-12130.25 30 0.10 122-12310.25 30 0.25 122-12320.25 30 0.50 122-12360.25 30 1.00 122-12330.25 60 0.25 122-1262

0.32 30 0.10 123-12310.32 30 0.25 123-12320.32 30 0.50 123-12360.32 60 0.25 123-1262

DB-XLB Order Guide Temperature Limits (30 to 340/360°C)

Similar PhaseMDN-12

ApplicationsPCB congeners, pesticides, chlorinatedherbicides, phenoxy acid methyl esters,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

Similar PhasesRtx-35, SPB-35, AT-35, Sup-Herb

ApplicationsAroclors, PCBs, amines, pesticides,chlorinated herbicides, haloacetic acids,pharmaceuticals, drugs of abuse

I.D. Length Film Part No.

0.20 15 0.33 128-38120.20 25 0.33 128-3822

0.25 15 0.25 122-38120.25 30 0.15 122-38310.25 30 0.25 122-38320.25 60 0.25 122-3862

0.32 30 0.25 123-38320.32 60 0.25 123-3862

DB-35ms Order Guide Temperature Limits (50 to 340/360°C)

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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-225ms• Equivalent to (50%-Cyanopropylphenyl)-

methylpolysiloxane• Mid/high polarity• Excellent for separations of cis- and

trans-fatty acid methyl esters (FAMEs)• Low bleed• Bonded and cross-linked• Solvent rinsable• Close equivalent to USP Phase G7

Similar PhasesDB-17, HP-50+, Rtx-50, 007-17, SP-2250,SPB-50, BPX-50, SPB-17

ApplicationsDrugs, glycols, pesticides, steroids

Similar PhasesHP-225, SP-2330, CP-Sil 43CB, RSL-500,Rtx-225, BP-225, CB-225, OV-225, 007-225

ApplicationsAlditol acetates, FAMEs, neutral sterols

I.D. Length Film Part No.

0.18 20 0.18 121-4722

0.25 15 0.15 122-47110.25 15 0.25 122-47120.25 30 0.15 122-47310.25 30 0.25 122-47320.25 60 0.25 122-4762

0.32 30 0.15 123-47310.32 30 0.25 123-4732

I.D. Length Film Part No.

0.25 15 0.25 122-29120.25 30 0.25 122-29320.25 60 0.25 122-2962

0.32 30 0.25 123-2932

DB-225ms Order Guide Temperature Limits (40 to 240°C)

DB-17ms Order Guide Temperature Limits (40 to 320/340°C)

EASY ONLINE ORDERING

Need a column that’s custom-designed for your lab?

Just visit www.agilent.com/chem/4ecatalog

Page 68: GC_GCMSD Consumable and Maintenance

67 www.agilent.com/chem

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

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

I.D. Length Film Part No.

0.20 25 0.20 19091N-1020.20 25 0.40 19091N-2020.20 50 0.20 19091N-1050.20 50 0.40 19091N-205

0.25 30 0.15 19091N-0330.25 30 0.25 19091N-1330.25 30 0.50 19091N-2330.25 60 0.15 19091N-0360.25 60 0.25 19091N-1360.25 60 0.50 19091N-236

0.32 30 0.15 19091N-0130.32 30 0.25 19091N-1130.32 30 0.50 19091N-2130.32 60 0.15 19091N-0160.32 60 0.25 19091N-1160.32 60 0.50 19091N-216

I.D. Length Part No.

0.32 30 113-43320.32 60 113-4362

HP-INNOWax Order Guide Temperature Limits (40 to 260/270°C)

GS-GasPro Order Guide Temperature Limits (-80 to 260/300°C)

Similar PhasesHP-20M, SUPELCOWAX 10, CP-WAX 52CB,SUPEROX II, CB-WAX, Stabilwax, BP-20,007-CW, Carbowax, DB-WAXetr

ApplicationsAlcohols, aromatics, essential oils, solvents

Similar PhaseCP-Silica PLOT

ApplicationsC1 to C12 hydrocarbons, CO2, trace-levelsulfurs, hydride gases, inorganic gases,halocarbons, SF6, oxygen/nitrogenseparation at -80°C.

Page 69: GC_GCMSD Consumable and Maintenance

“GC detectors are highly sensitive systemsthat are often compromised by varioustypes of contamination. By implementingsome recommended detectormaintenance routines, you can minimizeinstrument downtime and keep your GCsystem working at peak efficiency.”

Bernhard RothweilerApplications Chemist

DetectorsMost detectors require simple but periodiccleaning to maintain peak performance. This is especially true for highly sensitive GC detectors. Without routine detectormaintenance, GC system performance willdeteriorate and can cause detector failure.Detailed procedures on how to clean,maintain and replace common detectors,including FID, TCD, NPD, ECD, and FPD aresummarized in this section. Also included are special handling techniques and specificrecommendations to maximize specificdetector operations. For example, learn howto resolve flame ignition problems associatedwith your flame photometric detector andtest electron capture detectors forradioactivity leaks.

CATALOG

For a complete selection of Detector supplies, see Agilent’s 2005-2006Essential Chromatography Catalog. Or, visit our online catalog atwww.agilent.com/chem/4ecatalog.

www.agilent.com/chem 68

Page 70: GC_GCMSD Consumable and Maintenance

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DETECTORS

Cleaning & ReplacementEven with normal use, deposits develop inthe jet and detector (usually white silicafrom column bleed or black carbonaceoussoot). These deposits reduce sensitivityand cause chromatographic noise andspikes. Although you can clean the jet, it isusually more practical to replace dirty jetswith new ones. If you do clean the jet, becareful not to scratch the jet internally;scratches will ruin the jet

Flame Ionization Detectors require littlemaintenance to keep them performing atsatisfactory levels. The primary task is tooccasionally measure hydrogen, air andmakeup gas flows. They can drift over timeor be changed unintentionally withoutknowledge of it occurring. Each gas flowshould be independently measured toobtain the most accurate values.

CondensationSince the FID combustion process results in water formation, the detectortemperature must be kept above 100˚C toprevent condensation. Such condensation,especially when combined with chlorinatedsolvents or samples, causes corrosion andsensitivity loss.

Hardware ProblemsIf the flame goes out or will not light:

• Check the column flow rate. It may be too high. Decrease the flow rate orpressure. Switch to a more restrictivecolumn (longer or with a smaller id). If you must use a large id column, firstcool the GC oven to below 50˚C, then turnoff the carrier flow long enough to allowthe FID to light. Check for partially orcompletely plugged jet.

• Check that the right type of jet is installedfor the column you are using.

• Injecting large volumes of aromaticsolvent or water can cause the flame togo out. Switch to a nonaromatic solventor inject less solvent.

• The lit offset value may be too low or toohigh. Adjust the value.

Flame Ionization Detector (FID)

FID Cleaning Kit, P/N 9301-0985

Igniter Glow Plug Assembly

Collector Assembly

Collector Body

FID Jets

FID Ferrules

VIDEO

To view a video on FID column installation, jet replacement, collector maintenance, or ignitor replacement, visitwww.agilent.com/chem/techsupport.

Page 71: GC_GCMSD Consumable and Maintenance

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DETECTORS

Item Description Unit Part No.

1 PTFE chimney (optional)** 19231-21050

2 Collector nut 19231-20940

3 Spring washer 10/pk 5181-3311

4 Ignitor castle 19231-20910

Optional Hastelloy Ignitor Castle* 19231-21060

5 Ignitor glow plug assembly 19231-60680

6 Collector insulator G1531-20700

7 Collector body G1531-20690Hastelloy Collector Body 61531-21090

9 FID collector assembly 1 G1531-60690

Detector insulation assembly G1531-20700

FID collector cleaning brush 2/pk 8710-1346

Collector Housing G1531-20740

FID retainer nut wrench 19301-00150(5880, 5890, 6890)

1/4 in. Nut Driver for FID jet-drilled shaft 8710-1561

FID supplies kit-Includes: 5182-3450Jet, packed standard 3 each 18710-20119FID performance evaluation sample kit 2 each 18710-60170Ignitor glow plug assembly 2 each 19231-60680Jet, cap. series 530 µm 3 each 19244-80560FID flow measuring insert 2 each 19301-60660Cleaning wires for 0.03 in. ID jet 5180-4150Cleaning wires: 0.018 in. ID/530 µm jet 1/pk 5180-4152Wire, jet cleaning, 5 each 19301-20720Capillary inlet cleaning wires 5180-4153Detector cleaning kit 9301-0985

**Not included in assembly.*Hastelloy components may be used when analyzing highly corrosive materials.

1 Does not include Hastelloy component.

6890/6850 Ionization Detector (FID) SuppliesJet Cleaning Procedure (using Agilent’s FID Cleaning Kit #9301-0985)

1. Run a cleaning wire through the top ofthe jet. Run it back and forth a few timesuntil it moves smoothly. Be careful not toscratch the jet. (Do not force too large awire or probe into the jet opening or theopening will become distorted. A loss ofsensitivity, poor peak shape and/orlighting difficulties may result if theopening is deformed.)

2. Fill an ultrasonic cleaning bath withaqueous detergent, and place the jet inthe bath. Sonicate for five minutes.

3. Use a jet reamer to clean the inside ofthe jet.

4. Sonicate again for five minutes.

NOTE: From this point on, handle the partsonly with forceps!

5. Remove the jet from the bath and rinse itthoroughly, first with hot tap water andthen with a small amount of GC-grademethanol.

6. Blow the jet dry with a burst ofcompressed air or nitrogen, and thenplace the jet on a paper towel and allowit to air dry.

Plugged FID jet

EASY ONLINE ORDERING

Here’s another time-saving reason to place your order through ourwebsite: 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

Page 72: GC_GCMSD Consumable and Maintenance

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DETECTORS

Description Length(mm) Part No.

Jets for capillary dedicated FID

Capillary jet (0.011 in./0.29 mm ID tip) 48 G1531-80560

High-temperature jet (SimDIS 0.018 in. ID tip) 48 G1531-80620

Adaptable FID

Capillary 0.53 mm jet (0.011 in. ID tip) 61.5 19244-80560

Packed (0.018 in. ID tip) 63.5 18710-20119

Packed (0.030 in. ID tip) 63.5 18789-80070

0.53 mm high temp (0.018 in. ID tip) for SimDIS 61.5 19244-80620

Description Unit Part No.

FID flow measuring insert 19301-60660

FID ignitor cable G1531-60680

FID Performance evaluation sample kit, 0.03% C14, 18710-60170C15, and C16 normal alkanes in hexane

O-rings 12/pk 5080-4978

Cleaning wire 19301-20720

Jet cleaning wire for 0.03 in. ID jet 5/pk 5180-4150

Jet cleaning wire for Series 530 mm and 0.018 in. ID jet 5/pk 5180-4152

FID Jets

Agilent FID Jets (from top to bottom): Dedicatedcapillary, Adaptable capillary, Adaptable packed

4

6

7

1

2

3

5

6

8

6890 Series GC FID Detector

Collector Body, P/N G1531-20690

FID Consumables

TIPS AND TOOLS

Different size jets are available to optimize flame shape for capillary columns, orreduce contamination build-up for high molecular weight eluents. Usually, smallbore jets produce the greatest signal, but can plug up or contaminate more easilyrelative to large jets, so compromise may be necessary.

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DETECTORS

Radioactivity Leak TestElectron capture detectors must be testedfor radioactive leakage at least every sixmonths. Records of tests and results mustbe maintained for possible inspection bythe Nuclear Regulatory Commission and/orthe responsible local agency. More frequenttests may be conducted when necessary.

The procedure used is a “wipe test.” Awipe test kit is supplied with each newdetector. Refer to the information cardsupplied in the Wipe Test Kit forinstructions on performing the test.

Gas PurityFor successful EC detection, it’s importantthat the carrier and purge gases are veryclean and dry (99.9995%). Moisture,oxygen, or other contaminants can improvesensitivity, but at a cost of linear range.Always precondition the column beforeconnection to the detector.

Agilent provides two types of electroncapture detectors. The regular detector(ECD) has a larger internal volume(approximately 10 times) than the micro-cell detector (µ-ECD). These two types canbe distinguished by the top cover of thedetector – the ECD has a solid cover andthe µ-ECD has a perforated cover.

Thermal CleaningIf your baseline is noisy or the output value is abnormally high and you havedetermined that these problems are notbeing caused by leaks in the GC system,you may have contamination in thedetector from column bleed and sampleresidues. To remove contamination, youshould perform a thermal cleaning(bakeout) of the detector.

Warning: Detector disassembly and/orcleaning procedures other than thermalshould be performed only by personneltrained and licensed appropriately tohandle radioactive materials. Traceamounts of radioactive 63Ni may beremoved during other procedures, causing possible hazardous exposure to ß and x-radiation.

Electron-Capture Detector (ECD)

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. For this reason the cell

must be handled with care. Radioactive leak tests must be performed at the

required intervals, the inlet and outlet fittings must be capped when the detector

is not in use, corrosive chemicals must not be introduced into the detector, and

the effluent from the detector must be vented outside the laboratory environment.

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DETECTORS

Item Description Part No.

1 ECD makeup gas adapter* G1533-80565

2, 3 Nut warmer cup with insulation 19234-60720

ECD adapter replacement liner, fused silica 19233-20625

ECD end cap 19233-20755

ECD chemical sample kit, 3 ampoules 18713-60040solution of 33 pg/mL (0.033 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

Electron-Capture Detector (ECD) Supplies

TIPS AND TOOLS

Tap Agilent’s GC knowledge over the phone, online, in the classroom,even at your site. See pages 104-115 for more information about ourservices and support.

ECD Wipe Test: A wipe test kit (P/N 18713-60050) is supplied with each new ECD. The kitincludes an information card with instructions for performing the test. Records of tests andresults must be maintained for possible inspection by the NRC (Nuclear RegulatoryCommission) and/or responsible state agency.

1

2

3

6890 Series GC ECD Detector

Page 75: GC_GCMSD Consumable and Maintenance

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DETECTORS

Description Unit Part No.

6890/6850/5890 Common TCD Supplies

TCD replacement cell (6890/6850 only) G1532-60675

TCD cap column adapter seal 10/pk 18740-20950

TCD cap column adapter 18740-20960

Graphite ferrules, 1.0 mm id 10/pk 5080-8773

Graphite ferrules, 0.5 mm id 10/pk 5080-8853

Capillary column nut, for 6890 2/pk 5181-8830

Capillary column nut, for 6850 2/pk 5183-4732

TCD packed column adapter (6890/6850 only) G1532-20710

TCD chemical sample kit, 3 ampoules, 0.5 mL, 5 solution of 0.3% C14, C15, and C16, normalalkanes in hexane 18711-60060

5890 TCD Supplies

Makeup gas adapter, TCD 19232-80550

TCD column adapter, 1/8 to 1/4 in. glass 19302-80020

TCD replacement cartridge 19232-60676

The TCD compares the thermalconductivities of two gas flows – purecarrier gas (also called the reference gas)and carrier gas plus sample components(also called column effluent).

Filament MaintenanceThe primary maintenance for a TCDinvolves the filament. Most proceduresinvolve improving filament life or keepingthe filament from becoming damaged orcontaminated.

A constant presence of oxygen canpermanently damage filaments throughoxidative processes. The most commonsource of oxygen is a leak(s) near thedetector – or in the carrier or makeup gas line fittings. Oxygen traps arerecommended for the carrier and makeupgases to reduce oxygen levels. Propercolumn installation techniques and regularleak checks (especially after columninstallation) help to keep leak problems toa minimum.

The damage caused by oxygen is moresevere at high filament currents.Chemically active sample components such as acids and halogenated compoundsmay attack and damage the filaments.Avoiding these compounds when possibleincreases filament life. Turning off orsubstantially reducing the filament currentwhen the TCD is not in use also prolongsfilament life.

Increasing Filament LifetimeIncreased filament lifetime will result if thefollowing startup process is used:

1. Purge the detector with carrier andmakeup gas for 10-15 minutes beforeturning on the filaments. This preventsoxidation of the filaments due to thepresence of oxygen that has diffusedinto the cell under no flow conditions.

2. Turn on the filaments at the lowestpossible current setting, then increasethe filament current in severalincrements to the desired value. Thisreduces the power surge upon currentintroduction and prolongs filamentlifetime.

Cell Contamination Cell contamination is a problem when alower detector temperature is used toimprove sensitivity. Also, low filamentcurrents promote contamination since the filament is maintained at a lowertemperature at lower currents. If the cellbecomes contaminated, a solvent flush of the detector may help to remove thecondensed material.

Thermal Conductivity Detector (TCD)

Thermal Conductivity Detector (TCD) Supplies

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DETECTORS

Solvent Flush Procedure1. Cool the cell to room temperature and

remove the column.

2. Place a septum in a nut or fittingassembly that fits onto the detectorentrance.

3. Place the nut or assembly on thedetector fitting and tighten. Verify the presence of makeup gas flow.

4. Inject 20-100 µL volumes of toluene orbenzene into the detector through theseptum. Inject a total volume of at least 1mL of solvent. Do not injecthalogenated solvents such as methylenechloride and chloroform into thedetector.

5. After the final injection, allow makeupgas to flow for 10 minutes or more.Slowly raise the temperature of the cellto 20-30˚C above the normal operatingtemperature.

6. After 30 minutes, decrease thetemperature to the normal value andinstall the column as usual.

Thermal CleaningThe TCD can become contaminated withdeposits from such things as column bleedor dirty samples. A wandering baseline,increased noise level, or changes inresponse on a checkout chromatogram allindicate contamination. Thermal cleaning,or bakeout (heating the detector block toevaporate the contaminant), should beperformed only after you have confirmedthat the carrier gas and the flow systemcomponents are leak-free andcontaminant-free.

Watch out for decreased sensitivity causedby samples that react with the filament,originating from oxygen-contaminatedcarrier gas, leaks in plumbing, or columnbleeding. Samples with active components,such as acids and halogenated compoundscan chemically attack the filament as well. Also, sample condensation willcontaminate the detector cell if thetemperature is too low.

Some types of contaminants can beremoved by temperature bakeout. Also, in non-modulated designs, wanderingbaselines due to temperature variation canbe corrected by making sure the detectortemperature remains constant.

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DETECTORS

MaintenanceFlame Photometric Detectors requireminimal maintenance to keep themperforming at satisfactory levels. Thehydrogen, air and makeup gas flows shouldbe measured occasionally. They can driftover time or be changed unintentionallywithout knowledge of it occurring. Each gasflow should be measured independently toobtain the most accurate values.

Cleaning & Parts ReplacementThe FPD requires periodic cleaning. In most cases, this only involves the jet, andless frequently, the filter. Agilent providesbrushes and wires that simplify thecleaning of all detector parts (see FPDSupplies on page 77). The brushes areused to dislodge particulates clinging tothe metal surfaces. A fine wire is used toclean the jet opening of particulates. Donot force too large a wire or probe into thejet opening or the opening may becomedistorted. A loss of sensitivity, poor peakshape, and/or lighting difficulties mayresult if the opening is deformed. The filteror any of the window parts should behandled gently. Scratches or other surfacedeformities reduce the amount of lightpassing through the filter, thus reducingresponse. The filter and related partsshould be clean and free from fingerprints.

The Photo Multiplier Tube (PMT) needsperiodic replacement. The PMT is defectiveand needs to be rebuilt or replaced if:

• high voltage is on and the flame is lit

• low or no signal and/or noise notattributed to any other source such asbad cables are observed

• light leaks occur

• high temperatures are used

• defective signal boards are present

High detector temperatures reduce thePMT life. When not in use, turn off thePMT to maximize its usable lifetime. SomePMTs may have a shelf life and should notbe stored for prolonged periods before use.

Column bleed and/or effluent cancontaminate the first quartz window (heatshield) nearest the detector module. Dust,fingerprints, and atmosphericcontaminants can dirty both quartzwindows, the filter, and/or thephotomultiplier tube window.Contamination anywhere along the lightpath between flame and PMT can reducedetector sensitivity.

If a response problem is encountered(sensitivity, noise, selectivity) the FPD jetshould be inspected for deposits and, ifnecessary, cleaned or replaced. To properlyservice the jet, the detector module shouldbe removed from the instrument, andfollowed by appropriate service (see jetcleaning procedure on page 70).

Occasionally, the transfer line fused silicaliner between the column and FPD modulemust be inspected, cleaned and/or replaced.

Flame Ignition ProblemsIf the FPD flame won’t light or stay lit:

• Be sure there is a problem. Ignition is bestconfirmed by holding a mirror or shinysurface near the aluminum exhaust tube,with the rubber drip tube removed, andobserve condensation if the flame is lit.

• Check Lit Offset. If it is zero, autoignitionis turned off. If it is too large, the GC willnot know that the flame is lit and willshut down the detector.

• Increase the air supply pressure to thepneumatics module. This makes theflame easier to light but does not affectthe air flow rate setpoint.

• If the flame doesn’t light at all, check theglow plug circuit. Observe the visualdisplay, which will momentarily go togreater than 65500 counts when theflame lights. If the display doesn’tchange, check the pin connections at theprinted circuit board, the lead connectionon the glow plug and the appropriate 5Afuse on the GC main circuit board.

• The flame is easier to light at higherdetector temperatures.

• Under some operating conditions, theflame may be more easily lit with therubber drip tube removed. After lightingthe flame, reinstall the drip tube.

• If the flame still won’t light, there couldbe a large leak in the system. This resultsin measured flow rates being differentfrom actual flow rates, causing non-idealignition conditions. Thoroughly leakcheck the whole system.

Flame Conditions & Gas FlowsThe flame conditions are critical tosuccessful operation. Since the detectionzone is above the flame, the gas flows andjet diameter must be optimized so thatcomponents burned (activated) in theflame will emit in the detection zone.

Gas flows are also critical for optimizedselectivity and sensitivity. The most criticalparameters are the hydrogen/air orhydrogen/oxygen ratio, and the total gasflow, which effects flame temperature.

Flame Photometric Detector (FPD)

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DETECTORS

Item Description Unit Part No.

1 Exit tube assembly 19256-60700

2 Nut, brass, 1/4 in. 10/pk 5180-4105

4 Weldment, block 19256-80560

5 O-ring, ignitor, Kalrez 0905-1610

6 Spacer, ignitor 19256-20590

7 FPD Ignitor Replacement Kit 19256-60800

8 Ignitor cable assembly (6890 only) G1535-60600

9 Gasket, heat shield 19256-80045

10 Window, first heat shield 19256-80030

11 Disk, heat shield 19256-20580

12 Coupling, SS 19256-20550

14 Screw, M3 x 12 (4 required) 0515-0911

15 Clamp 19256-00090

16 O-ring, inner window 12/pk 5061-5886

17 Window, second heat shield 19256-80060

18 O-ring, outer window 12/pk 5061-5891

19 Flange adapter 19256-20510

20 Flange ring 19256-00200

21 O-ring, Viton, 1.239 in. id 12/pk 5061-5890

Adapter weldment, 1/8 in. columns 19256-80590

Adapter weldment, capillary 19256-80570

Start-up kit (5890 only) 19256-60500

FPD O-ring (5890 only) 12/pk 5061-5867

Liner/ferrule kit 19256-60590

Sulfur filter 19256-80000

Phosphorus filter 19256-80010

Kalrez O-ring, size 2-002 0905-1609

Kalrez O-ring, size 2-011 0905-1608

Fluorocarbon Elastomer O-ring, brown, 0.926 in. id 12/pk 5061-5889

FPD Performance Evaluation Sample: Solution of 20 ng/mL (20 ppm) dodecanethiol and tributylphosphate in isooctane, 3 ampoules 19305-60580

1

2

3

4

56

7

8

16

910

11

12

1314

15

1718

19

20

21

6890/5890 FPD Supplies

Install the correct opticalfilter, depending on thechoice of Sulfur orPhosphorus mode. For Sulfur Mode, use the 393 nanometer filter. For Phosphorus Mode, use the 525 nanometer filter.

MA

INTE

NA

NC

E M

IND

ER

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DETECTORS

Bead MaintenanceNPDs are temperamental and requirefrequent maintenance. Small changes in anyof a number of parameters can significantlychange the performance characteristics ofan NPD. The bead requires the mostmaintenance. It needs to be changedfrequently, thus a spare is a necessity.

The beads have to be kept dry which limitstheir storage life to about six months. Whena new bead is installed, slowly raise thedetector temperature and bead current.Rapid heating can crack or break the beadespecially if it has been stored under humidconditions. It has been observed that higherhydrogen flows and bead currents decreasebead life. If the NPD is not in use, thehydrogen flow and bead current should bereduced or turned off to increase bead life.Make sure there is some type of gas flow ina heated detector or when there is current tothe bead.

Bead LifeTo extend the life of the bead:

• Use the lowest practical adjust offset orbead voltage.

• Run clean samples and keep the inlet/linerclean to minimize contamination.

• Turn off the bead when not in use.

• Keep the detector temperature high (320 – 335˚C).

• Turn off the hydrogen flow during solventpeaks and between runs.

• If the NPD is off for an extended period of time in a high humidity environment,water may accumulate in the detector. To evaporate this water, set the detectortemperature to 100˚C and maintain it for 30 minutes. Then set the detectortemperature to 150˚C and maintain it for another 30 minutes.

Gas FlowThe hydrogen, air and makeup gas flowsshould be measured frequently. They candrift over time or be changed unintentionallywithout knowledge of it occurring. Each gasflow should be measured independently toobtain the most accurate values. NPDs arevery sensitive to changes in the gas flowsand consistent flows are necessary tomaintain performance levels.

Gas PurityBecause of its high sensitivity, the NPDrequires very pure gases (99.999% or better).We strongly recommend that moisture andhydrocarbon traps be used on the carriergas and all detector gases, including thedetector hydrogen, air, and makeup gases.Dirty gases will not only give poorchromatographic performance, but willshorten the bead life as well.

Nitrogen-Phosphorus Detector (NPD)

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DETECTORS

Description Length (mm) Part No.

Capillary jet (0.011 in./0.29 mm id tip)(6890 only, dedicated) 48 G1531-80560

6890/5890 Adaptable

Capillary 0.53 mm jet (0.011 in. id tip) 61.5 19244-80560

Packed (0.018 in. id tip) 63.5 18710-20119

NPD Jets

Cleaning & Replacement

The NPD requires periodic cleaning. In mostcases, this only involves the collector andthe jet. Agilent provides brushes and wiresthat simplify the cleaning of all detectorparts (see NPD Supplies on page 79). Thebrushes are used to dislodge particulatesclinging to the metal surfaces. A fine wire isused to clean the jet opening of particulates.Do not force too large a wire or probe intothe jet opening or the opening will becomedistorted. A loss of sensitivity or poor peakshape may result if the opening is deformed.The various parts can be ultrasonicated aftercleaning with a brush. Eventually the jetneeds to be replaced, so it is stronglyrecommended to have spare jets on hand.

Over time, residue from the bead or samplecan build up in the collector and causebaseline problems. You should clean thecollector after you have changed the beadtwo or three times.

The metal C-rings wear slightly with eachassembly and disassembly. After severalassemblies and disassemblies (five or more),the rings may not seal effectively, causing anerratic baseline. A ceramic insulator and sealkit is available. Always cool the detector tonear-ambient when changing seals andinsulators.

Because there is no flame in the NPD, thejet does not collect silica and soot as doesthe FID jet. Although you can clean the jet, itis usually more practical to simply replacedirty jets with new ones. If you do clean thejet, use the cleaning wire, taking care not todamage the inside of the jet. You can alsouse a sonicator bath to clean the jet.

ContaminantsSome chemical problems can also arisewhen using the NPD. Because it is a tracedetector, be careful not to contaminate theanalytical system.

Glassware Glassware must be very clean. Phosphatedetergents should be avoided, so acidwashing of glassware followed by distilledwater and solvent rinsing is recommended.

Solvents Solvents should be checked for purity.Chlorinated solvents and silanizing reagentscan decrease the useful lifetime of the alkalisource; excess reagent should be removedprior to injection, if possible.

Other Contamination SourcesPhosphate-containing leak detectors,phosphoric acid-treated columns or glasswool, polyimide-coated columns, ornitrogen-containing liquid phases can addnoise to the system and should be avoided.

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DETECTORS

14

18

17

1

3

45

6

8

13

15

7

2

9

1011

12

16

Item Description Part No.

6890 NPD Supplies

1 Screws, M3 x 0.5 x 8 mm (Pozidriv) 0515-0655

2 NPD white ceramic bead assembly* G1534-60570

NPD black ceramic bead assembly** 5183-2007

3 Lid weldment G1534-80510

4 Metal C-ring, top 0905-2580

5 Alumina insulator, upper G1534-40020

6 Collector funnel G1534-20530

7 Alumina insulator, lower G1534-40030

8 Metal C-ring bottom and top 0905-1284

9 Screw, M4 x 10 mm 0515-2495

10 J-Clamp 1400-0015

11 Screw, M4 x 10 mm 0515-2495

12 NPD interconnect assembly G1534-60610

13 Mounting pallet G1531-40020

14 Jets (see page 79)

15 Base weldment, Capillary NPD G1534-80500

Base Weldment, Packed NPD G1534-80540

16 Lid stop G1534-20590

NPD Ceramic Insulator Kit includes items 4, 5, 7, and 8 5182-9722

17 Column adapters for packed NPD

18 Nut warmer cup with insulation 19234-60720

5890 NPD Supplies

NPD collector (NPD bead) 19234-60540

Recoating kit, sufficient for 10 collectors 5080-8872

Detector Trap Replacement Kit 19231-60790

*This bead is more sensitive, but exhibits some tailing for phosphorous compounds. Quantity discounts available.

**The black bead is potentially a little less sensitive, but does not exhibit peak tailing and typically has a longer lifetime.

Nitrogen-Phosphorous Detector (NPD) Supplies

Page 82: GC_GCMSD Consumable and Maintenance

You asked … we listened!

Our new e-Catalog makes onlineordering easier than ever. We’ve streamlined our online store to complement the design and content of our 2005-2006 EssentialChromatography Catalog.

Visit www.agilent.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

Page 83: GC_GCMSD Consumable and Maintenance

GC/MS SystemsYour mass spectrometer is a sensitive, highly specialized device that offers more functionality – and requires moremaintenance – than other GC detectors.Therefore, we have devoted an entire section of this guide to MSDs.

“We offer intelligent, creative solutions to help our customers maximize theperformance of their GC/MS systems.”

Jim McCurrySenior Applications Chemist

CATALOG

For a complete selection of gas management supplies, see Agilent’s2005-2006 Essential Chromatography Catalog. Or, visit our onlinecatalog at www.agilent.com/chem/4ecatalog.

www.agilent.com/chem 82

Page 84: GC_GCMSD Consumable and Maintenance

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GC/MS SYSTEMS

Some parts of the MSD require regularly scheduled maintenance.

Common maintenance tasks are listed in the table below. It is advisable to keep a log bookof system performance, Autotune, and maintenance operations performed. This makes iteasier to identify variations from normal performance and to take corrective action. Subtledifferences may exist between MSD models. Consult your hardware manual for specificinstruction.

Every dayCheck, and if necessary, replace theseptum. Check the injection port liners.Check the tightness of the column nuts.Hint: With Agilent’s new Flip Top InletSealing System, you don’t have to check orchange liners. So you save time and effort.See page 52 for ordering information.

Every weekCheck the foreline pump oil level and diffusion pump fluid. Change the injectionport liners and O-rings. Gas ballast theforeline pump.

Every monthClean the split/splitless inlet vent line trap. Check for leaks (inlet and columnconnections).

Every three monthsReplace gas cylinders (when below 500 psig).

Every six monthsReplace the foreline pump oil. Check, and if necessary, refill the calibration vial.

Every yearReplace the diffusion pump fluid.Recondition or replace internal and externaltraps and chemical filters on the GC.

As neededTune the MSD. Clean the ion source.Replace the carrier gas trap. Replace worn-out parts (filaments, EM, etc.).Replace the column. Lubricate seals.

Monitor Record all tune values such as electronmultiplier and ion source parameters in a log book to monitor instrumentperformance. In addition note the highvacuum and foreline vacuum pressures.

Maintaining Mass Selective Detectors (MSDs)

TASK EVERY EVERY EVERY ASWEEK 6 MONTHS YEAR NEEDED

Tune the MSD •Change injection port liners •*Check the foreline pump oil level •Gas ballast the foreline pump •Check the calibration vial •Replace the foreline pump oil •Check the diffusion pump fluid •Replace the diffusion pump fluid •Replace the traps and filters •Clean the ion source •Change the carrier gas trap(s) and purifier •Replace the worn out parts •Lubricate seals (where appropriate) •Replace column •

*For more information on inlet maintenance, see pages 26-34.

Page 85: GC_GCMSD Consumable and Maintenance

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GC/MS SYSTEMS

Air LeaksAir leaks are a problem for any instrumentthat requires a vacuum to operate. Leaksare generally caused by vacuum seals thatare damaged or not fastened correctly.

ContaminationContamination is usually identified by excessive background in themass spectra. It can come from the GC or from the MSD. The source of the contamination can sometimes be determined by identifying thecontaminants. Some contaminants are much more likely to originate in the GC, others are more likely to originate in the MSD.

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 ofcontamination and the level of contamination. Minor contamination by wateror solvents can usually be removed by allowing the system to pump (with aflow of clean carrier gas) overnight. Serious contamination by rough pumpoil, diffusion pump fluid or fingerprints is much more difficult to remove; itmay require extensive cleaning. For further details contact your AgilentCustomer Engineer (CE).

Symptoms of leaks include:• higher than normal vacuum manifold

pressure or foreline pressure• higher than normal background• peaks characteristic of air (m/z 18, 28,

32, and 44 or m/z 14 and 16)• poor sensitivity• low relative abundance of m/z 502

(this varies with the tune program and MSD used)

Page 86: GC_GCMSD Consumable and Maintenance

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 theinterface attaches to the vacuummanifold)

• diffusion pump co-seal and/or baffleadapter O-ring

• turbomolecular pump O-ring

• new Vespel/graphite ferrules contractwhen heated

Corrective Action• Check interface nut for tightness.

Replace if necessary.

• Check leak/test the GC injection port.

85 www.agilent.com/chem

GC/MS SYSTEMS

Cleaning SolventsIt is common to see cleaning solvent peaksin the mass spectra shortly after the ionsource is cleaned.

FingerprintsFingerprints contain hydrocarbons that canappear in mass spectra. Hydrocarboncontamination is characterized by a seriesof mass peaks 14 amu apart. Theabundances of these peaks decrease aspeak mass increases. Fingerprintcontamination is usually caused by thefailure to wear lint-free, nylon gloves duringion source cleaning, GC inlet maintenance,or from installing the column. Use specialcare to avoid recontamination of parts afteryou clean them. This typically occurs aftersome maintenance or part replacement.

Diffusion Pump FluidIf the diffusion pump is allowed to operatewith no column (carrier gas) flow into thevacuum system, vapor from the diffusionpump fluid can drift up into the vacuummanifold. A more serious problem is whenfluid is back streamed into the vacuum

Corrective Action• Dry all cleaned metal parts in the GC

oven before reassembling and reinstallingthem. Refer to specific cleaningprocedures in your MSD HardwareManual.

Corrective Action• Reclean using clean, nylon gloves and

proper cleaning techniques.

manifold by sudden or improper venting ofthe vacuum system. If a diffusion pumphas back streamed, a prominent peak willoften be seen at m/z 446 and the spectralbaseline will exhibit increased backgroundnoise.

• Use a temperature that’s just above the boiling point of the solvent.

Corrective Action• If m/z 446 appears please call Agilent

for assistance.

Description Part No.

MS interface column nut 05988-20066

Column nut for GC/MS and two-hole ferrules 05921-21170

Universal Column Nut (2/pk) 5181-8830

Description Part No.

Nylon gloves, lint-free, Large 8650-0030Nylon gloves, lint-free, Small 8650-0029

TIPS AND TOOLS

The most likely point for an air leak is a seal you recently opened.

Page 87: GC_GCMSD Consumable and Maintenance

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GC/MS SYSTEMS

Common Contaminants

Foreline Pump OilForeline pump oil contamination ischaracterized by peaks spaced 14 amuapart (hydrocarbons). Contamination withforeline pump oil is less common thancontamination with diffusion pump fluid.

Corrective Action• Call Agilent for assistance.

Ions (m/z) Compound Possible Source

13,14,15,16 Methane CI gas

18, 28, 32, 44 or 14, 16 H2O, N2, O2, CO2 or N, O Residual air and water, air leaks, outgassing from Vespel™ ferrules

31, 51, 69, 100, 119, 131, 169, PFTBA and related ions PFTBA (tuning compound)181, 214, 219, 264, 376, 414,426, 464, 502, 576, 614

31 Methanol Cleaning solvent

43, 58 Acetone Cleaning solvent

78 Benzene Cleaning solvent

91, 92 Toluene or xylene Cleaning solvent

105, 106 Xylene Cleaning solvent

151, 153 Trichloroethane Cleaning solvent

69 Foreline pump fluid or Foreline pump oil vapor or calibration valve leakPFTBA

73, 147, 207, 221, 281, Dimethylpolysiloxane Septum bleed or methyl silicone column coating295, 355, 429

77, 94, 115, 141, 168, 170, Diffusion pump fluid Diffusion pump fluid and related ions262, 354, 446

149 Plasticizer (phthalates) Vacuum seals (O-rings) damaged by high temperatures, use of vinyl or plastic gloves

Peaks spaced 14 amu apart Hydrocarbons Fingerprints, foreline pump oil

Contamination IdentificationThe following table lists some of the more common contaminants, the ion characteristic of those contaminants, and the likely sourcesof those contaminants.

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GC/MS SYSTEMS

This section describes some of thesymptoms you might observe – either inthe spectra of samples or in a tune report.Typically, these symptoms fall into twobroad classes:

1. those that affect the systemsensitivity.

2. those that affect the repeatability of a measurement.

Some symptoms can be corrected byfollowing the suggested corrective actions.Others require the services of an AgilentCustomer Engineer.

Sensitivity

Symptoms Corrective Action

Wrong retention time Check GC, method, application and carrier gas velocity

Low signal Check GC, tune vacuum system

Leaking injection port Clean the injection portReplace the injection port liner and septa

Air leak Check and tighten interface nut, leak test GC injection port

Peak widths Do Autotune, check flow rate and temperature stability

Interfering peaks Check time parameters, coeluting peaks, column type

Excessive background Do Autotune and compare to background specificationsCheck time parameters

Incorrect mass assignment Retune

Abnormal spectra – Check for contaminationexcessive backgroundcontamination

Incorrect tuning Check tune file, retune, check sample

Repeller voltage is too low Raise voltage to test for response

Dirty ion source Clean source

Symptoms Corrective Action

Dirty syringe needle Clean or replace the syringe

Wrong syringe needle Replace syringe and septa

Leaking injection port Perform injection port maintenanceReplace the injection port liner, septa, and liner o-ring

Injection is too large Check method and injection volume, split ratio and/or splitless purge time

Loose column connections Tighten column nuts on injection port or transfer lineReplace column nuts and ferrule

Variations in pressure, Ensure the MSD is located in an environment where column flow, the temperature is stableand temperature – 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

Dirty ion source Clean source

Loose connections Check internal and external analyzer wiring connections,in the analyzer make sure all are secure

Ground loops Check main electrical lines

Repeatability

Mass Spectrometer Symptoms

Page 89: GC_GCMSD Consumable and Maintenance

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GC/MS SYSTEMS

Ion Source

Maintaining the Ion SourceCleaning procedures for MSDs vary. Referto your MSD Hardware Manual for specificion source cleaning procedures.

Common measures of instrument performance:• abundance of certain ions (e.g.

percentage of the 502 ion from theAutotune 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 CleaningThe cleaning frequency is determined by:• the number of samples run (throughput)• the type of samples• unique, established laboratory protocol

The ion source operates by electronionization (EI) or chemical ionization (CI).The sample enters the ion source from theGC/MSD interface. Electrons emitted by afilament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample mole-

Selecting a Cleaning MethodThe primary action of any cleaningprocedure is to remove contamination from surfaces. Removing this contaminationrestores the electrostatic properties of theion source lensing system. Numerouscleaning methods have been developed forrestoring ion source performance. Thecleaning 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 cleanstainless steel ion source parts is aluminum oxide. It is available in eitherpowder form or an abrasive film. After thecritical surfaces have been abrasivelycleaned, the loose particles must beremoved. One method of removing particlesis swabbing with a cotton swab or a cleancloth dipped in acetone. A clean swabshould be used for each element followedby a sonication. These cleaning suppliesare listed on page 89.

cules, ionizing and fragmenting them. Thepositive voltage on the repeller pushes thepositive ions into the lens stack, wherethey pass through several electrostaticlenses. These lenses concentrate the ionsinto a tight beam, which is directed into themass filter.

Preparing to CleanPrior to cleaning, the mass spectrometermust be vented and the ion source must beremoved. Before venting the system, thefollowing 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 routineto run its full course. Improper venting maycause diffusion pump fluid to be depositedinto the analyzer (backstreaming). It canalso reduce the life of the multiplier, orother sensitive MS parts.

5973 Ion Source Assembly (EI)

TIPS AND TOOLS

Agilent’s new MS Inert Ion Source improves inertness – and maintains it over multiple cleanings. For more information see page 90.

Page 90: GC_GCMSD Consumable and Maintenance

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GC/MS SYSTEMS

Description Part No.

Cleaning and Maintenance

Nylon gloves, lint-free, Large 8650-0030

Nylon gloves, lint-free, Small 8650-0029

Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk) 9310-4828

Generic ion source cleaning kit for all GC/MS types 5181-8863Includes: 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) 05980-60051

Abrasive Sheets, aluminum oxide green lapping paper for ion source 5061-5896cleaning, 600 mesh (5 sheets)

Alumina powder, abrasive 8660-0791

PFTBA sample, certified (10 g) 8500-0656

PFTBA sample kit, 1 mL 05971-60571

Activated alumina, absorbent pellets for Edwards 8500-1233rough pump traps, non-LC/MS (1 lb can)

PFTBA glass vial 05980-20018

Cotton swabs (100/pk) 5080-5400

ToolsScrewdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws 8710-0899

Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws 8710-0900

Wrench, open-end, 1/4 x 5/16 in. 8710-0510

Screwdriver, TORX, T15 8710-1622

Screwdriver, TORX, T10 5182-3466

Ferrules and O-ringsTeflon 1/4 in. ferrule (back) 0100-0160

Teflon 1/4 in. ferrule (front) 0100-0787

Retainer rings (10/pk) 5181-1258

5973 One Year Maintenance Kit (for diffusion pump systems) 5183-2096Includes: 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 05971-60561Includes: 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)

Cleaning and Maintenance Supplies

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B

H

H

I

I

JK

L

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5973 Repeller Assembly (EI).

5973 Ion Source Parts (EI).

A

C

D

E

F G

HLM

M

Description 5973 Part No.

(A) Ion source body G1099-20130

(B) Repeller G1099-20132

(C) Interface socket G1099-20136

(D) Drawout plate 05971-20134

(E) Drawout cylinder G1072-20008

(F) Ion focus lens 05971-20143

(G) Entrance lens 05971-20126

(H) Repeller insulator G1099-20133

(I) Set screw 0515-1446

(J) Washer, M3 (1/pk) 3050-0891

(K) Nut, 5.5 mm 0535-0071

(L) Ion Source Sensor G1099-60104

(M) Lens insulator, (2/pk) 05971-20130

Ion source assembly G1099-60106

Source heater assembly G1099-60177

Repeller assembly G1099-60170

Screw (for filament on the source) 0515-1046

5973 MSD Ion Source Parts (EI)

MS Inert Ion Source Parts

Description 5973A 5973N 5973 inert**

Drawout plate – 3 mm Inert G2589-20100

Drawout plate – 6 mm Inert** G2589-20045 G2589-20045 G2589-20045

EI High Temp Filament G2590-60053

Repeller assembly, Inert source G1099-60170 G1099-60170 G2589-60102

Screws for filament High Temp 0515-1046 0515-1046 G1999-20021

Source body, Inert G1099-20130 G1099-20130 G2589-20043

Source Washer, Inert G2589-20101

**used in G2860A and G2860B extended linearity kits

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5972/5971/GCD MSD Ion Source Parts (EI)

Description 5972/5971/GCD Part No.

(A) Entrance lens 05971-20126

(B) Lens insulator, (2/pk) 05971-20130

(C) Ion focus lens 05971-20143

(D) Drawout cylinder G1072-20008

(E) Drawout plate 05971-20134

(F) Ion source body 05971-20128

(G) Set screw 0515-1446

(H) Repeller assembly 05971-60170

(I) Screw (for filament on the source) 0515-1046

Ion source assembly 5972 Part No.

05972-60226

Transfer line tip, gold-plated 5972/5971 Part No. GCD Part No.

05971-20305 G1800-20305

A

B

B

C

D

E

F

G

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5972/5971/GCD Ion Source (EI)

MSD Flowrates (ml/min)

Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowratesbelow for flow limitations.

Min Max Diff Pump Max Turbo Pump Tuning Max5973 0.1 2.0 4.0 2.05972 0.1 2.0 NA 2.05971 0.1 1.5 NA 1.0GCD 0.1 1.0 NA 1.0

TIPS AND TOOLS

It is good practice to replace scratched lenses and other ion source parts.Scratched source parts lead to poor performance.

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FilamentsTwo filaments are located on oppositesides outside of the ion source. The activefilament carries an adjustable ac emissioncurrent. The emission current heats the filament, causing it to emit electrons; theseelectrons ionize the sample molecules. Inaddition, for the 5973 and 5972, bothfilaments have an adjustable dc biasvoltage. The bias voltage determines theenergy on the electrons, usually -70 eV.

Maintaining the FilamentsLike the filament in an incandescent lightbulb, the ion source filaments willeventually burn out. Certain practices willreduce the chance of early failure:

Quadrupole Mass FilterThe mass filter does not require periodicmaintenance. It should not be removedfrom the radiator or distributed in any way.

Tips to increase filament life• When setting up data acquisition

parameters, set the solvent delay so thatthe analyzer will not turn on while thesolvent peak is eluting.

• When the software prompts Overridesolvent delay at the beginning of a run,always select “No.”

• Never put the quadrupole in anultrasonic cleaner.

• Never change the physical orientation ofthe quadrupole mass filter.

• The fused-quartz quadrupole is fragileand will break if dropped or handledroughly.

• The material in the cusps of thequadrupole is very hygroscopic. Ifexposed to water, the quadrupole mustbe dried very slowly to prevent damage.

• Higher emission current will reducefilament life.

• If you are controlling your MSD from theEdit Parameters screen, always selectMS Off before changing any of thefilament parameters.

• Cleaning techniques appropriate for othermanufacturers’ instruments are notsuitable for Agilent MSDs – and mayactually harm the mass filter.

• To save time and effort, use only AgilentMSD mass filters, which do not requireperiodic cleaning or maintenance.

• In case of extreme contamination,contact a trained Agilent servicerepresentative to perform the mass filter cleaning.

Filament Assembly

Description Unit Part No.

Filament, 5973 (EI) 05972-60053

Filament, 5973 (CI) 2/pk G1099-80053

Filament, EI High Temperature for the 5973 inert G2590-60053

Filament, 5972 (EI/CI) 05972-60053

Filament, 5971 (EI/CI) / GCD (EI) 05971-60140

TIPS

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It is very useful to switch fromone filament to the other everythree months so that when onefilament fails, you know theother will fail soon. This willallow you to change bothfilaments at the same time,which helps to maximize yourinstrument uptime.

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Vacuum System OperationThe vacuum system creates the high vacuum (low pressure) required for theMSD to operate. Without this vacuum, the molecular mean free path is too short.

Ions cannot travel from the ion sourcethrough the mass filter to the electronmultiplier (detector) without colliding withother molecules.

CalibrationThe calibration valve is an electromechanicalvalve with a vial that contains a tuningcompound. Perfluorotribuylamine (PFTBA) is the most commonly used tuningcompound. It is required for automatictuning of the MSD in EI mode. The tuningcompound is usually a liquid but can bevolatile or semi-volatile solid.

The major components of the vacuumsystem 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

How to RefillThe calibration vial can be refilled withoutventing the system. Fill the vial to 0.5 cmfrom the top. DO NOT overfill. Air istrapped in the vial when it is refilled.

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

This sometimes causes an “Excess sourcepressure” error message during the firsttune after refilling. This is more likely if thevial is overfilled. Be sure to purge the airupon refilling the vial.

Keeping a pan under the vacuum pump helps todetect and identify the origin of oil leaks.

Vacuum Systems and Pumps

Description Part No.

PFTBA sample, certified (10 g) (EI) 8500-0656PFDTD sample (10 g) (CI) 8500-8130

MAINTENANCE MINDER

MAINTENANCE MINDER

If using the 5973 with a CI source, use Perfluorodimethyltrioxadodecane(PFDTD) sample.

Page 95: GC_GCMSD Consumable and Maintenance

Pressure SymptomsThis section describes unusual pressurereadings and their possible causes. Thesymptoms in this section are based ontypical pressures. At typical column flowrates (0.5 – 2.0 ml/minute), the forelinepressure will be approximately 20 to 100mTorr. The vacuum manifold pressure willbe approximately 1 x 10-6 to 1.4 x 10-4 Torr.

The vacuum manifold pressures can only bemeasured if your system is equipped withthe optional gauge controller.

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GC/MS SYSTEMS

These pressures can vary widely frominstrument to instrument so it is importantthat you are familiar with the pressuresthat are typical for your instrument at agiven carrier gas flow and oventemperature.

The foreline pressures listed can only bemeasured on diffusion pump-equippedsystems. Turbomolecular pumps arecontrolled according to their speed and do not have foreline pressure gauges.

Foreline pressure is too high

Symptom • Pressure is above 100 mTorr.• Pressure for a given column flow has

increased over time.

Possible Cause • 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.• Pressure for a given column flow has

increased over time.

Possible Cause • 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

Foreline pressure is too low

Symptom • Pressure is below 20 mTorr.

Possible Cause • 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.

Vacuum manifold pressure is too low

Symptom • Pressure is below 1.4 x 10-6 Torr.

Possible Cause • 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.

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Diffusion PumpIt is not necessary to change the diffusionpump fluid more than once a year, unlessyou observe symptoms that suggest aproblem with the diffusion pump fluid. TheMSD must be vented in order to check thediffusion pump fluid (except for the 5973).Therefore, the best time to check the fluidis when the instrument is already ventedfor other maintenance.

Importance of the Fluid LevelThe amount of fluid in the pump affects the amount of vapor and the temperature of the base plate. Too little fluid will causethe pump to run at a higher temperaturebecause there is less fluid to carry away theheat resulting in fluid cracking or degradationand loss of high vacuum. It will also lowerthe pumping speed because there is lessfluid vapor available to pump away gases which can especially affect operation in CI Mode due to higher flow rates.

Foreline PumpThe oil in the foreline or rough pumpshould be replaced on average once everysix months, but can vary depending uponapplications. After oil replacement, if theforeline trap is present, the molecularsieves should be replaced.

How to Check the Fluid Level1. If it is not vented already, shut down and

vent the MSD according to instrumentmanual.

2. Unplug the MSD power cord.

3. Remove the pump and cover the topwith aluminum foil.

4. 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, remove the stack parts.

5. Inspect the pump fluid, if the fluid is discolored or contains particulatematerial, the fluid must be changed.

Avoid contact with the pump oil. Theresidue from some samples may be toxic.Dispose of used oil properly.

6a. Use a metal ruler to determine thedepth of the fluid. A pump that hasbeen in operation should have a pool 9 mm plus or minus 1 mm deep. Fluidin freshly charged pumps will be 12mm deep. It is normal that up to 2 ml of oil may be in the rear portion of thevacuum manifold. The recommendedtotal fluid charge for the 5971/5972 is18 ml (plus or minus 2 ml).

6b. For the 5973 use the sight glass to determine the depth of the fluid. The recommended total fluid charge is approximately 37 ml.

Description Part No.

Diffusion pump fluid: SantoVac Ultra 5P, 18.5 ml (5973, 5972 or 5971/GCD) 6040-0809

Ion gauge controller (5973/5972A) 59864B

Ion gauge tube for measuring vacuum (5971/5972) 0960-0376

Triode gauge tube for measuring vacuum (5972/5973) 0960-0897

Description Part No.

Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD) 6040-0798

Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD) 6040-0834

Molecular sieve (5973, 5972 or 5971/GCD) 9301-1104

Oil mist filter RV3/E1M18/E2M18/E2M2 3162-1056

Oil mist filter E2M1.5 G1099-80037

Oil mist filter E2M18 5063-5224

Page 97: GC_GCMSD Consumable and Maintenance

General Instructions on How to Replace thePump Oil

1. Shutdown and vent the MSD.

2. Place a container under the drain plug on theforeline pump.

3. Remove the fill cap from the top of the pump toexpose the fill hole.

4. Remove the drain plug from the pump.

5. Reconnect the MSD to its power source. Switchon for 2 or 3 seconds, and then switch it offagain. This displaces old oil from the internalpump cavities. Disconnect the power cord again.

6. Reinstall the drain plug and pour pump oil intothe fill hole.

7. Reinstall the fill cap.

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GC/MS SYSTEMS

8. Reconnect the MSD power cord.

9. Start up and pump down the MSDaccording to the Instrument Manualprocedure.

Maximize LifetimeThe lifetime of an EM is directly related to the current thatflows through it and the extent of contamination orcondensation that it experiences. To maximize electronmultiplier life:

• Maintain the best possible vacuum, especially in theanalyzer manifold.

• Use extreme caution and be conservative with venting,pumpdown, and all vacuum system procedures to keeppump fluid background to a minimum.

• After venting, allow four hours for pumpdown andthermal equilibration before scanning.

• Actively look for background contamination and leaksand repair them immediately.

• Don’t tune excessively. PFTBA can result in higherbackground over an extended period of time.

Symptom• Voltage is over 2500 volts• Poor vacuum

Corrective Action• Replace electron multiplier

Electron Multipliers and Replacement Horn

Description Part No.

Electron multiplier replacement horn 05971-80103

(5973, 5972, 5971/GCD)

High energy dynode (5973 only) G1099-80001

Electron multiplier kit (5972, 5971/GCD only) 05971-80102

TIPS AND TOOLS

Use chemical-resistant gloves and safety glasses when replacing pumpfluid. Avoid contact with the fluid. Always dispose of used oil properly.

TIPS AND TOOLS

Use only Agilent replacement multipliers and horns for Agilent MSDs.Other manufacturers’ products can increase noise, while reducingsensitivity and linearity.

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Maintaining the MS Engine

Maintenance Schedule• Always wear clean, lint-free, nylon gloves

when handling parts which will come incontact with the sample stream. Oil fromyour fingers is a particularly difficultcontaminant to remove.

• If you must set parts down, place them onclean, lint-free cloths or clean aluminumfoil, not directly onto a laboratory bench.

• Keep parts covered so that dust does notaccumulate on them.

• Do not leave the interior of the vacuumsystem open to the atmosphere. Forexample, if you are removing the ion sourcefor cleaning, put the vacuum manifold coverback in its normal position after you haveremoved the source. Re-establish a lowvacuum in the vacuum manifold until youneed to reinstall the ion source.

Common maintenance tasks are listed onpage 83. Performing these tasks on a regularbasis can reduce overall operating costs.Keep a record (logbook) of systemperformance characteristics andmaintenance operations performed. This makes it easier to detect variances from normal operation and to take corrective action.

Cleaning the Ion SourceThere is not a regular interval for ion sourcecleaning. The ion source should be cleanedwhen symptoms indicate. Symptoms of adirty ion source include poor sensitivity andinadequate abundances at high masses. See the Troubleshooting chapter in yourhardware manual for more information aboutthese symptoms.

MS Engine Pump Lubricants and Oils

5989 or Thermo or 5985 or 5999x, 5993xLubricant Oil 5988 Electro Spray 5987 or 5995x Part No.

Turbo pump lubricant:Balzers turbo pump lubricant, 0.25 liter • • 6040-0468

Diffusion pump oil:SantoVac 5, 1 liter • • • 6040-0370SantoVac 5, 128 ml • • • 6040-0819

Rough pump oil:Rough pump oil, 1 gal Inland 45 • • • • 6040-0798Rough pump oil, 1 liter Inland 45 • • • • 6040-0834Particle Beam pump oil, Fomblin • 6040-0730

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We strongly recommend keeping a log of all system performance and routine maintenanceoperations. That way, problems that might impact performance can be identified andresolved quickly.

The most common maintenance tasks are listed in the table below.

Task Every Every Every As Week 3 Months 6 Months Needed

Autotune or manual tune (save results) •

Cabinet Maintenance

Clean the cabinet •Inspect hoses and cords •Vacuum the fan filter •

Vacuum System Maintenance

Check mech. pump oil •Replace mech. pump oil •Replace mech. 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

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LSWe recommendkeeping a separateset of tools that havebeen thoroughlycleaned for workingwith the MS engine.These tools areneeded to preventcontamination whenreassembling orinstalling cleanassemblies such asthe ion source.

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The electron multiplier lifetime on the 5989may be 6 to 9 months or shorter, especiallywith the following applications:

• Thermospray• Particle Beam• Purge and trap, with no jet separator• Extensive CI• High sensitivity work with high EM voltage

Ion Source Parts and Supplies

5989 Lens Stack

5989 Repeller Assembly

Replacement Parts and Supplies

Description Part No.

(A) Clamp insulator, ion source 05989-20110(B) Entrance lens 05989-67002(C) Lens insulator, ion source 05989-20111(D) Plate insulator, ion source 05989-20109(E) EI/CI repeller 05989-20145(F) Repeller insulator 05989-20119Filament block 05989-20165Filament assembly 05985-60179Heater cartridge 05989-60098

Description Part No.

5989Electron multiplier kit 05989-80043Electron multiplier replacement horn 05971-80103

Parts and SuppliesIon gauge tube, K-25 flange 0960-0799

O-rings and SealsInsulating ring 05989-20705O-ring, detector flange (5/pk) 5181-3367Diffusion pump fluid fittingfill and drain cap O-ring (12/pk) 0905-1145KF 25 centering ring and O-ring 3162-0110O-ring, manifold window 0905-1189

E

F

A

B

C

D

Many of the tools and supplies needed toservice the 5989 MS Engine are included in the installation kit supplied with theinstrument. The following tables listcommon consumable parts and suppliesused in the maintenance of the MS Engine.

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Contents:

• Start-Up Guide, pub. No. 5988-3073EN• Application Note, “Improvements in the

Agilent 6890/5973 GC/MSD System foruse with USEPA Method 8270”, pub. no.5988-3072EN

• Ultra Ion Source Chamber• Ultra Repeller• Ultra Large Aperture Drawout Plate

• Pre-tested column, 30m x 250um x 0.5umHP-5 MS, part no. 19091S – 139

• Single-taper splitless liner, 4mm i.d.,deactivated, part no. 5181-3316

• Direct Connect Liner, single taper, 4mmi.d., deactivated, part no. G1544-80730

• Direct Connect Liner, dual taper, 4mmi.d., deactivated, part no. G1544-80700

• Floppy Disk with tuning macros

G2860A 8270 Semi-VolatilesApplications Kit

The G2860A 8270 Semi-VolatilesApplications Kit is designed for use inAgilent 6890/5973A and 6890/5973NGC/MSD Systems. The kit providesmodified and/or pretested components toimprove system performance for USEPAMethod 8270. With the kit, system linearityis maximized and activity is minimized.

General GC/MS Supplies

Description Part No.

8270 Semi-Volatiles Applications Kit G2860A

LIBRARY

There are many ways to perform semi-volatile analysis. For another option thatalso features 5973 MSD Electronics upgrades, visit www.agilent.com/chemand do a library search for 5989-1510EN.

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Each GC/MS has a specific test and performance sample. Refer to the chart below for the exact sample.

Test and Performance Samples

EI CI Negative Positive MSD Tune Tune EI Mode CI Mode CI Semi-Volatile Volatile

5973 PFTBA PFDTD OFN 1 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL DFTPP BFB

5972 PFTBA PFTBA HCB 10 pg/µL NA Benzophenone 100 pg/µL DFTPP BFB

5971 PFTBA PFTBA HCB 10 pg/µL NA Benzophenone 100 pg/µL DFTPP BFB

GCD PFTBA NA Sample A (10 ng/µL) NA NA DFTPP BFB

MS Engine

5989A PFTBA PFTBA HCB 50 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL DFTPP BFB

5989B PFTBA PFTBA HCB 20 pg/µL OFN 500 fg/µL Benzophenone 100 pg/µL DFTPP BFB

Tuning Samples Verification Samples Performance Checkout Samples

EASY ONLINE ORDERING

Visit the Agilent website at www.agilent.com/chem/4ecatalog forone-click access to: • Product pricing links (when available)• Local sales contact information• Online quote requests• Order status updates … and more

Page 103: GC_GCMSD Consumable and Maintenance

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Description Quantity Part No.

Evaluation Sample for GC/MS SystemsContains 6 vials: 4 vials (Sample A, 10 ng/µL), 1 vial (Sample B, 100 pg/µL),and 1 vial (Sample C, 100 ng/µL) each of dodecane biphenyl, p-chlorodiphenyl, and methyl palmitate in isooctane, 1 mL ampoule 05970-60045

GC/MS Tuning Standard contains:DFTPP, Benzidine, Pentachlorophenol, andp,p’-DDT 1 mg/mL in methylene chloride 8500-5995

5989 Installation Sample Kit contains:HCB 50 pg/µL, HCB 20 pg/mL, Benzophenone 100 pg/µL, OFN 1 pg/µL, mix of HCB, OFN and Benzophenone 5 ng/µL 8500-6406

Extended Mass Performance Sample 0.5 g, fomblin oil 8500-5500

PFTBA certified 1 bottle, 10 g 8500-0656

PFTBA Sample Kit 0.5 mL 05971-60571

PFDTD 10 g 8500-8130

Benzophenone 100 pg/µL, 5 ampoules 8500-5440

Hexachlorobenzene 10 pg/µL, 4 ampoules 8500-58081 ng/µL, 2 ampoules

Hexachlorobenzene 20 pg/µL 8500-6405

Methyl stearate (in methanol);

PFTBA not certified 1 ng/µL (2 ea) 05990-60075

Octafluoronapthalene (OFN) 1 pg/µL, 5 ampoules 8500-5441

Octafluoronapthalene (OFN) 500 fg/µL 8500-6572

p-Bromofluorobenzene (BFB) 25 µg/mL 8500-5851

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You asked … we listened!

Announcing the launch of our new Life Sciences and Chemical Analysis website. Based on customer feedback, we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.

• A coherent page design – that Automatically detectsscreen resolution and optimizes the page size for less scrolling.

• An expanded navigation – that includes links to product literature, technical support, education, events, and news.

• A newly designed online store – with fast access topricing, order status, quotes, and local sales information.

• Direct links – to the services, parts, and consumables thatkeep your instruments running in top condition.

The new site features:

To experience these exciting new changes for yourself, go to www.agilent.com/chem.

Page 105: GC_GCMSD Consumable and Maintenance

“Our customers know they can rely on Agilent's expertise and resources to keep their instruments running at top performance."

Yukiko SameshimaCustomer Engineer

Services & SupportEvery Agilent GC and GC/MS system is backedby our nearly 40 years of experience withinstrument design, lab operations, businessprocesses, and regulatory requirements.

We stand behind our products with …

• Immediate technical assistance by phone oronline.

• Prompt onsite service from Agilent-certifiedEngineers.

• A variety of service options, includingmaintenance, repair, compliance, andconsultation.

• Industry-leading training courses to helpincrease your lab’s overall knowledge base.

Our professionals are standing by to help yousolve problems and optimize your resources.So you can spend more time running samples,developing methods and meeting productiondeadlines – and less time arranging forinstrument services.

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SERVICES & SUPPORT

A Total Commitment to Your Lab for One Fixed Cost.

Agilent service agreements operate under a yearly fixed cost, which includespreventative maintenance, compliance,telephone support, repairs, parts, andlabor. No matter how many service visitsor replacement parts you need, this fixedcost covers it all – at no additional charge.

If you choose, you can also consolidateinstrument maintenance and repairservices into multi-year agreements for administrative ease and greater cost savings.

The Unmatched Expertise of Fully Trained Engineers.

You can rest assured that the engineerwho arrives at your site will perform therequested service with optimum skill.That’s because Agilent engineers …

• Are experts in instrument operation,maintenance, compliance, and repair.

• Continually update their training and qualifications.

• Use only Agilent factory-approvedreplacement parts, columns, andsupplies to ensure peak instrumentreliability.

• Carry calibrated, traceable tools andtesting equipment, as well as Agilenthardware and software qualificationprotocols.

What’s more, most Agilent engineers arepart of the Agilent product developmentteam. So you can be certain that ease ofrepair, maintenance, and compliance arebuilt into your GC and GC/MS systemsright from the start.

The Flexibility to Select TheSolution That’s Right for You.

Our team will work with you to help yourlaboratory achieve …

• Maximum uptime

• High productivity

• Total compliance

• Extended instrument life

• Fast problem resolution

• Verified system performance

• The skills and knowledge you need forefficient operation and maintenance

• Consistent, in-depth documentation

• Reduced administrative burdens

Our focus is on keeping your lab running at peak performance.

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SERVICES & SUPPORT

Agilent Services

Telephone Service

Software Service

Onsite Instrument Repair

Offsite Instrument RepairFor selected Agilent analysis instruments

Preventative MaintenanceFor selected Agilent analysis instruments

Features

• Telephone access to skilled Agilent serviceprofessionals.

• Available parts option.

• Telephone access to trained technicalprofessionals.

• Enhancements to the original applicationsoftware purchase.

• Software bulletins that identify discovereddefects and recommend workarounds.

• Hardware telephone support with accessto skilled, factory-trained Agilent serviceprofessionals.

• Travel expenses and labor.

• Optional coverage for consumables used during repair.

• Option 1: Replacement with an identicalinstrument (your fastest choice).

• Option 2: Return to Agilent for repair.

• Expert cleaning, adjustment, lubrication,and inspection of your instrument.

• Travel expenses and labor.

• Coverage for consumables used.

Advantages to You

• Fast identification and resolution of hardware problems.

• Low cost.

• Fast identification and resolution of software problems.

• A fixed annual cost for softwareupgrades makes budget managementmore predictable.

• A single cost-effective source for telephone support and software updates.

• A convenient way to keep up with the latest software enhancements.

• A fixed annual cost for parts makesbudget management more predictable.

• You can choose the response method that fits your business needs and budget.

• Less expensive than onsite repair.

• Fast and easy.

• Includes extensive diagnostics andtesting that are not feasible with onsitemaintenance or repair.

• Maximum uptime.

• Extended instrument life.

• Confidence in the integrity of your measurements.

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SERVICES & SUPPORT

Installation Qualification (IQ)

Operational Qualification/PerformanceVerification (OQ/PV)For selected Agilent analysis instruments

Note: We recommend PreventativeMaintenance before OQ/PV.

Requalification (RQ) After RepairFor instruments that have theiroperational performance verified by an annual OQ/PV.

• Qualification and documentation ofshipment completeness.

• Comprehensive system and applicationsoftware verification tests.

• Delivered by professionals with trainingcertification.

• Verification and documentation of aninstrument’s ability to meet specifiedcriteria.

• Procedures and documentation that fit therequirements of GLP, ISO 9000, and otherregulatory agencies.

• Full automation to increase thequalification scope without excess timerequirements.

• Measuring equipment that is traceable tonational and international standards.

• Verification that a system is performing at operation specifications after repair.

• Complete system operation testing.

Note: only a subset of the OperationalQualification test is performed, based on the type and extent of the repair.

• A comprehensive test of the repairedmodule using established conditions andknown sample characteristics to ensurethe basic accuracy and precision of yourmodule.

• Measuring equipment is traceable tonational and international standards.

• Supplies the evidence you need tosatisfy regulatory agencies.

• Helps fulfill the master validation plan –and change-control SOP requirements –for the IQ phase.

• Supplies the evidence you need tosatisfy regulatory agencies.

• No need to write your own SOPs toqualify Agilent instruments – or to trainyour staff.

• Consistent, traceable results among allyour laboratories – and improvedmethod transfer.

• Confidence in the integrity of yourmeasurements, with traceable,documented chains from sampleintroduction to reporting.

• Less risk of financial loss due tononcompliance.

• Meaningful, relevant, andunderstandable system tests.

• Minimal system downtime aftercompletion of instrument repair.

• Efficient system requalification byperforming the appropriate tests basedon the components repaired.

• Assurance that all instrumentsubsystems are performing withinspecifications.

• All procedures and documentation meetregulatory agency requirements.

Agilent Services Features Advantages to You

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SERVICES & SUPPORT

Network Qualification

Mass Spectrometer Ion Source CleaningFor selected Agilent analysis instruments

• Network definition and performancetesting using established Agilent Design,Installation Qualification, and OperationalQualification protocols.

• Documentation of the definition, integrity,supportability, and health of high-risknetwork segments.

• Completed protocols, created usinghardware and software network testingtools. Protocols include:

- A physical and logical inventory.- A graphical network topology map.- A snapshot of network health, as

installed.

• Network Operational Qualification testing,which monitors the network over time, andevaluates its operation over a controlledrange of traffic conditions. We’ll alsoprovide the following reports:

- Long Duration Network Characterization,which analyzes each function in itsoperating environment.

- Performance Predictability Analysis,which documents reserve capacity andstability over a range of operatingdemands.

• Onsite disassembling

• Cleaning

• Reassembling

• Testing

• Significant time savings.

• Increased uptime – issues that mightimpact application performance arequickly identified and resolved.

• Improved consistency – networkqualification protocols are developedaccording to a quality lifecycle, and aremaintained under version and revisioncontrol.

• Increased control – Agilent will verifyknown elements and identify unknownnetwork contingency states that mayimpact application performance.

• Reduced regulatory exposure – audit-ready documentation establishesevidence of network system control.

• Your staff can devote more time tochemistry, not instrument maintenance.

• Efficient cleaning with minimaldowntime.

Agilent Services Features Advantages to You

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SERVICES & SUPPORT

Software Backup • Telephone or onsite factory support tofacilitate restoration.

• Captures the unique system settings for allsoftware components needed toreconstruct your system including:

- Network information- Printers and peripherals- Configurations- User settings and operations- System registry- Application software- Settings- Operating system- Customizations- Analytical hardware- Directory structure- Security information

• Fast and easy – you simply insert a disk… reboot … and you’ll be back inoperation in as little as two hours.Normally, you would have to reload andreconfigure your software – a processthat can take days.

• A complete solution – the initialconfiguration backup includes:

- Simple backup software- Ten CD-ROMs- Ten 3.5-in. floppy disks- A storage case- One full system backup- Installation of the backup software

and optional CD writer

Agilent Services Features Advantages to You

TIPS AND TOOLS

To learn more about Agilent’s complete portfolio of services, pleasevisit www.agilent.com/chem/service.

Page 111: GC_GCMSD Consumable and Maintenance

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SERVICES & SUPPORT

6890 GC Split Inlet Mode Operation

6890 GC Splitless Inlet Mode Operation

6890 GC Purged Packed Inlet Operation

Self-paced;Four hours access

Self-paced;Four hours access

Self-paced;Four hours access

Reviews the basic theory and operation of the 6890 GC split/splitless capillaryinlet when running in split mode.

Clarifies flow paths, so you can gain the maximum benefit from this inletoperational mode.

Discusses typical problems and routinemaintenance procedures.

Reviews the basic theory and operation ofthe 6890 GC split/splitless capillary inletwhen running in splitless mode.

Clarifies flow paths, so you can gain the maximum benefit from this inletoperational mode.

Discusses typical problems and routinemaintenance procedures.

Reviews the basic theory and operation of the 6890 GC purged packed inlet.

Clarifies flow paths, so you can gain the maximum benefit from this inlet.

Discusses typical problems and routinemaintenance procedures.

Course Title Duration Description

Education & Training ServicesHighly trained lab professionals can boost your productivity, minimize errors andreruns, and expand your chromatography capabilities. And that’s why Agilent offersseveral training options that cover everything from troubleshooting and maintenanceto the most advanced operational techniques.

eLearning

Agilent’s e-Learning program features a series of focused, economical andindividualized instrument training modules designed to enhance and simplify yourlearning experience. From theory and operations... to common problems with yourinstruments... eLearning is available when you want it, where you want it, and howoften you want it. All you need is Internet access!

You can review and register for our e-Learning offerings by visitingwww.agilent.com/chem/elearning

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SERVICES & SUPPORT

6890 GC Keyboard Operation

6890 GC FID Theory and Operation

6890 GC ECD Theory and Operation

6890 GC TCD Theory and Operation

GC Automatic Liquid Sampler Operation

Self-paced;Four hours access

Self-paced;Four hours access

Self-paced;Four hours access

Self-paced;Four hours access

Instructor-led; 60-90 minutes

Reviews the basic operation of the 6890GC keyboard.

Thoroughly describes all keys, so you cangain the maximum benefit from your GC.

Reviews the basic theory and operation of the FID.

Covers proper column installation,keyboard setup, and flow optimization.

Discusses typical problems and routinemaintenance procedures.

Reviews the basic theory and operation of the ECD.

Covers proper column installation,keyboard setup, and flow optimization.

Discusses typical problems and routinemaintenance procedures.

Reviews the basic theory and operation of the TCD.

Covers proper column installation,keyboard setup, and flow optimization.

Discusses typical problems and routinemaintenance procedures.

Reviews the basic operation of the 7683Aautomatic liquid sampler system (ALS).

Shows you how to gain maximumproductivity from the ALS.

Discusses routine maintenanceprocedures, and how to return an ALS to Agilent for repair or exchange.

Course Title Duration Description

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SERVICES & SUPPORT

Logical GC Troubleshooting

Using the GC/MSD Security ChemStation to Achieve FDA CFR Part 11 Compliance

Managing and Administering theGC/MSD Security ChemStationto Meet FDA CFR Part 11 Compliance Requirements

Designed for systems administrators

Instructor-led; 60-90 minutes

Instructor-led; 60-90 minutes

Instructor-led; 60-90 minutes

Teaches a methodical process fortroubleshooting GC system problems.

Helps you identify the source of problemsquickly, making troubleshooting lessdaunting.

Note: This course does not discuss hardware-specific problems or solutions.

Describes in detail how to operate theGC/MSD Security ChemStation softwarein accordance with FDA CFR Part 11requirements.

Shows you how to manage the GC/MSDSecurity ChemStation software inaccordance with FDA CFR Part 11requirements.

Course Title Duration Description

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SERVICES & SUPPORT

Classroom Training

Agilent’s training courses for gaschromatography and mass spectrometryhelp new and experienced labprofessionals learn proper and efficientways to use analytical instruments andsoftware. These ISO-registered courses

also target those who want to broaden or sharpen their troubleshooting,maintenance, and system operation skills.

Contact Agilent today for more informationabout our training and services. Or visitwww.agilent.com/chem and select“Education.”

Course Title Course No. No. of Days Description

Technique

Introduction to Capillary GC H2615A 1 Provides an overview of capillary gas chromatography in alecture format.

Techniques of GC H4002A 5 Presents the fundamental concepts of gaschromatography.

Introduction to GC-MS H2609A 1 Introduces the technique of GC-MS in a lecture format thatincludes worksheet exercises.

Techniques of GC-MS H4040A 3 Reviews the key concepts of the GC-MS analysis process,as well as qualitative and quantitative GC-MS techniques.

Hardware/Software Operation

ChemStation Operation for the 6890 GC/ALS H5926A 5 Explains how to operate the Agilent 6890 GC using GCChemStation software.

Operation of the GC-MSD System Using the ChemStation for GC-MSD H4043A 5 Enhances an operator’s efficiency and productivity when

using the Agilent GC-MSD system.

Provides experience in data acquisition and analysis, librarysearching, reporting, and customizing the system to meetspecific laboratory or customer needs.

GC-MSD System for Environmental Applications H4050A 5 Increases an operator’s skill in using a mass selectivedetector with mass spectrometer EnviroQuant software.

Troubleshooting and Maintenance

6890 GC Maintenance H5308A 4 Addresses preventative maintenance and first-level repairfor the Agilent 6890 GC.

5890 GC Maintenance H4001A 4 Addresses preventative maintenance and first-level repairfor the Agilent 5890 GC.

6890 GC Troubleshooting and Preventative Maintenance H5309A 1 Introduces troubleshooting of the Agilent 6890 GC in a

lecture format.

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SERVICES & SUPPORT

Introduction to 5973 GC-MSD Troubleshooting and Preventative Maintenance H5947A 1 Demonstrates how to perform preventative

maintenance and troubleshooting to keep theAgilent 5973 GC-MSD system working properly.

Includes a discussion of typical vs. problemAuto-Tunes.

Offers class exercises that enhance understandingof troubleshooting and maintenance principles.

5973 GC-MSD Troubleshooting and Preventative Maintenance H2294A 3 Covers tuning and diagnostics, the vacuum

system, the 5973 MSD ion source, the quadrupolemass filter, and the 5973 MSD.

Includes hands-on laboratory exercises todemonstrate and practice the principles conveyed.

Data Analysis and Reporting

ChemStation for GC Data Analysis and Reporting H2606A 3 Teaches the operation of the Agilent GCChemStation software through instructorexplanations, combined with extensive hands-onand laboratory exercises.

Specifically focuses on data analysis and reporting.

Data Analysis and Reporting Using the ChemStation for GC-MSD H4076A 3 Enhances skills in using the Agilent ChemStation

for GC-MSD.

Makes users more efficient and productive, whileexpanding their ability to use ChemStationfeatures.

Describes how to customize the software forlaboratory and customer needs.

Data Analysis and Reporting Using the EnviroQuant ChemStation for GC-MSD H4053A 3 Improves proficiency in using the Agilent

EnviroQuant software.

Covers data analysis and reporting, includingcompletion of EPA-like forms.

Describes how to customize the software forlaboratory and customer needs.

Course Title Course No. No. of Days Description

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SERVICES & SUPPORT

Tap Agilent’s GC and GC/MSexpertise anytime.

Just give us a call to discuss hardware,software, application concerns, or basicoperation techniques.

Visit Agilent onlineFor a wealth of knowledge, tips, andinsights, go to www.agilent.com/chem.You’ll find:

• Frequently Asked Questions about Agilentinstruments and supplies.

• Interactive Troubleshooter A step-by-stepapproach to help you solve common problems.

• Find a Part Includes parts information,pricing, and availability, plus an illustratedparts breakdown.

• Software Downloads and Utilities Featurepatches and status bulletins, tools andutilities, firmware, and revision tables.

• How-to Videos Show you how to performcommon installation and maintenanceprocedures for Agilent products.

• Chromatogram Library A searchablecollection of GC, LC, and CEchromatograms for nearly a thousandchemical compounds.

• Instrument and Software Demos Such asproduct videos, 3D animations andinteractive software demos.

Support

a

Have a technical GC column, method, or troubleshooting question? Agilent’s technical GC and GC/MSexperts are available to answer your questions by phone, fax or e-mail for free. With years of experience inrunning samples, developing methods and troubleshooting GC systems, our chemists are promptly able tohelp you consistently achieve excellent performance and high productivity in your lab.

For GC Technical Support go to www.agilent.com/chem/techsupport and click on “Interactive Troubleshooter.”

Technical Support Consultation

Page 117: GC_GCMSD Consumable and Maintenance

You asked … we listened!

Our new e-Catalog makes onlineordering easier than ever. We’ve streamlined our online store to complement the design and content of our 2005-2006 EssentialChromatography Catalog.

Visit www.agilent.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

Page 118: GC_GCMSD Consumable and Maintenance

For more than 18 years, Separation Times hasbeen one of the scientific community’s mostrespected newsletters devoted to chemicalanalysis. And now, it’s available online!

Each issue is packed with …

• Application details geared toward specificindustries – such as environmental,chemical, petroleum, forensic, andagricultural.

• Handy tools, tips, and tricks designed tohelp your lab run more productively, and get reliable, reproducible results.

• Exclusive promotional offers and regionalevent announcements.

Best of all,Separation Times is absolutely FREE …and we’ll automatically e-mail it to you seven times per year.

To reserve your subscription today, go towww.agilent.com/chem/separationtimes

Receive a year’s worth of current chromatography insights with a

FREE subscription to Separation Times.

Page 119: GC_GCMSD Consumable and Maintenance

GC System Recommended Maintenance Schedule

Gas ManagementITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Gas purifiers Every 6-12 months Replacement schedule is based on capacity and grade of gases. (carrier gas & In general, replace non-indicating traps every 6-12 months or when detector gas) indicating traps start to change color. Replace indicating traps when

indicating material is spent.

Split vent trap Every 6 months* Replace.

Flowmeter Every 1-2 years Re-calibrate electronic flowmeters – follow recommended schedule forcalibration the unit (shown on calibration certificate).

Sample Introduction Consumables and GC InletsITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Syringes Every 3 months* Replace syringe if dirt is noticeable in the syringe, if it cannot beand/or syringe cleaned, if the plunger doesn’t slide easily, or if clogged. Replace needles needle if septa wear is abnormal or the needle becomes clogged.

Inlet liner Weekly* Check often. Replace when dirt is visible in the liner or if chromatography is degraded.

Liner O-rings Monthly* Replace with liner or with signs of wear.

Inlet septum Daily* Check often. Replace when signs of deterioration are visible (gaping holes, fragments in inlet liner, poor chromatography, low column pressure, etc.).

Inlet Hardware Every 6 months Check for leaks and clean.

Every year Check parts and replace when parts are worn, scratched, or broken.

Remember, the downtime for scheduled

maintenance is always less disruptive

than the downtime for unscheduled

maintenance and troubleshooting!

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ColumnsITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Front-end Weekly – monthly* Remove 1⁄2-1 meter from the front of the column when experiencing Maintenance chromatographic problems (peak tailing, decreased sensitivity, retention

time changes, etc.). Replace inlet liner, septum and clean inlet as necessary. Guard column may be useful for increasing column lifetime.

Solvent rinse As needed When chromatography degradation is due to column contamination. Only for bonded and cross-linked phases.

Replacement As needed When trimming and/or solvent rinsing no longer return chromatographicperformance.

Ferrules Replace ferrules when changing columns and inlet/detector parts.

DetectorsITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

FID/NPD Jets As needed Clean when deposits are present. Replace when they become scratched, & Collector bent or damaged, or when having difficulty lighting FID or keeping flame lit.

NPD Bead As needed Replace when signal drifts or there is a dramatic change in sensitivity.

FID Every 6 months Measure hydrogen, air, and makeup gas flows.

TCD As needed Thermally clean by “baking-out” when a wandering baseline, increased noise, or a change in response is present. Replace when thermal cleaning does not resolve the problem.

ECD Every 6 months Wipe test.As needed Thermally clean by “baking-out” when baseline is noisy, or the

output value is abnormally high. Replace when thermal cleaning does not resolve the problem.

FPD Every 6 months Measure hydrogen, air, and makeup gas flows.As needed Clean/replace FPD windows, and seals when detector sensitivity

is reduced.

MSD

Components require regular maintenance. For complete MSD maintenance schedule, please see page 83.

*Schedule is an approximation of average usage requirements. Frequency may vary widely based upon application and sample type.

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The information and pricing in this guide are subject to change without notice.

© Agilent Technologies, Inc. 2005Printed in USA February 15, 20055989-1925EN

www.agilent.com/chem

For detailed information about

supplies from Agilent, please

contact your local Agilent sales

representative, or your authorized

distributor, or visit us online.

Ask about Agilent’s other valuable

resources:

• Maintaining Your Agilent 1100 SeriesHPLC System

• Essential Chromatography Catalog

• Online Library and Tech Support