maintaining your agilent gc and gc ms systems

121
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

Upload: ahmed-samy

Post on 16-Nov-2015

80 views

Category:

Documents


1 download

DESCRIPTION

Maintaining Your Agilent GC and GC MS Systems

TRANSCRIPT

  • 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

  • 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 800 227 9770

    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

    Dont MissGC 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 todays labs face the challengeof operating with a reduced staff. Thats why were committed to bringing you theworlds 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.

    Weve 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.

  • 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. Its 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 Agilents2005-2006 Essential Chromatography Catalog. Or, visit our onlinecatalog at www.agilent.com/chem/4ecatalog.

    www.agilent.com/chem 800 227 9770 2

  • 3 www.agilent.com/chem 800 227 9770

    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 gassuppliers 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

  • www.agilent.com/chem 800 227 9770 4

    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

  • 5 www.agilent.com/chem 800 227 9770

    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 Agilents 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.

  • www.agilent.com/chem 800 227 9770 6

    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. Price

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

    Refillable Moisture Trap 200 36 18 MT200-2 MT200-4 $104

    Adsorbent Refill (1 pint) for MT Series MSR-1 MSR-1 $ 55

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

    Glass Indicating Moisture Traps 100 16.3 6 GMT-2-HP GMT-4-HP $119

    Molecular Sieve Refill for GMT Series 250 GMSR GMSR $ 63

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

    Moisture S-Trap preconditioned 5060-9084 $226

    Big Moisture Traps for the Ultimate Moisture Capacity

    Big Moisture Trap 750 BMT-2 BMT-4 $235

    Refill for BMT Series (2 refills) BMSR-1 BMSR-1 $ 58

    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

  • 7 www.agilent.com/chem 800 227 9770

    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. Price

    Hydrocarbon Traps General Purpose

    Refillable Hydrocarbon Trap 200 HT200-2 HT200-4 $106

    Adsorbent Refill (1 pint, 2 refills) ACR ACR $ 63

    Big Hydrocarbon Traps for the Ultimate Hydrocarbon Capacity

    Big Hydrocarbon Trap 750 BHT-2 BHT-4 $235

    Refill for Big Hydrocarbon Trap (2 refills) BACR BACR $ 52

    Hydrocarbon Removal S-Trap can be reconditioned in the GC oven

    Hydrocarbon S-Trap 5060-9096 $232

    Capillary Grade Hydrocarbon Traps for crucial capillary applications

    Capillary Grade Hydrocarbon Trap 100 HT3-2 HT3-4 $ 98

    Adsorbent Refill (1 pint, 3 refills) ACR ACR $ 63

    Hydrocarbon 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. Price

    Indicating Oxygen Traps glass body with plastic safety shield

    Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP $143

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

    Big Oxygen Trap 750 BOT-2 BOT-4 $235

    Oxygen Traps

    Big Oxygen Trap

    Indicating Oxygen Trap

    Hydrocarbon Trap

  • www.agilent.com/chem 800 227 9770 8

    GAS MANAGEMENT

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

    Oxygen/Moisture Traps

    Agilent OT3 Trap 100 OT3-2 OT3-4 $104

    Hydrocarbon/Moisture Traps

    Refillable Hydro-Moisture Trap 200 HMT200-2 HMT200-4 $ 98

    Refill for Hydrocarbon/Moisture Trap (1 pint, 2 refills) HCRMS HCRMS $ 63

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

    Big Universal Trap Helium purged (also recommended for GC Mass Spec) 750 RMSH-2 RMSH-4 $261

    Big Universal Trap Hydrogen purged 750 RMSHY-2 RMSHY-4 $261

    Big Universal Trap Nitrogen purged 750 RMSN-2 RMSN-4 $261

    Big Mounting Clip for mounting Big Traps 2/pk UMC-5-2 UMC-5-2 $ 21

    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

  • 9 www.agilent.com/chem 800 227 9770

    GAS MANAGEMENT

    High Capacity

    Gas Purification System

    Three Cartridge System

    Agilents 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. Price

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

    With 1/8 in. fittings 5183-1907 $612

    With 1/4 in. fittings 5182-9776 $567

    Replacement Cartridge KitIncludes all three cartridges for 5182-9780 $393above system

    Single Cartridge SystemIncludes 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 $239

    With 1/4 in. fittings 5183-4599 $255

    Triple combination replacement cartridge for single cartridge system 5183-4600 $136

    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.

  • www.agilent.com/chem 800 227 9770 10

    GAS MANAGEMENT

    Description Fitting (in.) Part No. Price

    4-Head

    O2, indicating O2, HC, H2O 1/8 RQC-P $1604

    Quick Change Plus (QC+) Point of Operation Panels

    Description Part No. Price

    High capacity oxygen GC-1 $ 64

    High capacity moisture GC-2 $ 64

    Indicating moisture GC-2-I $106

    Hydrocarbon GC-3 $ 64

    Indicating oxygen GC-4 $155

    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

  • 11 www.agilent.com/chem 800 227 9770

    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. Price

    Universal/external split vent trap with 3 cartridges(1/8 in. Swagelok fitting) RDT-1020 $ 94

    Replacement cartridges (3/pk) RDT-1023 $ 45

    Description Part No. Price

    Carrier Gas Purification System: Single position system perfect for GC/MS, ECD and NPD detectors. Includes the triple filter cartridge. 5182-9704 $ 398

    Super-Clean Gas Purification System: For your most demanding GC application, includes four position baseplate manifold with four filter cartridges: oxygen, moisture (both with indicator), and two hydrocarbon cartridges. 5182-0816 $1291

    Replacement Filter Cartridges

    Triple Filter Cartridge: A single carrier gas filter now with hydrocarbon, moisture, and oxygen trapping capability. Includes moisture and oxygen indicator so you know exactly when to replace the cartridge. 5182-9705 $ 186

    Filter cartridge bundle of 4 (oxygen, moisture, and 2 hydrocarbon) 5183-4770 $ 530

    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.

  • www.agilent.com/chem 800 227 9770 12

    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. Price

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

    CGA 346, 125 psig max (8.6 bar), Air 5183-4641 $275

    CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642 $275

    CGA 540, 125 psig max (8.6 bar), O2 5183-4643 $275

    CGA 580, 125 psig max (8.6 bar), He, Ar, N2 5183-4644 $275

    CGA 590, 125 psig max (8.6 bar), Air 5183-4645 $275

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

    Regulator Outlet Adapters Female NPT to Swagelok-style

    1/4 in. to 1/8 in. brass (included with brass regulators) 0100-0118 $ 14

    1/4 in. to 1/4 in. brass** 0100-0119 $ 15

    ** 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.

  • 13 www.agilent.com/chem 800 227 9770

    GAS MANAGEMENT

    Description Part No. Price

    Copper tubing, 1/8 in., 50 ft. 5180-4196 $56

    Copper tubing, 1/8 in., 12 ft. 5021-7107 $28

    TubingPrecleaned

    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: 70F; 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.

  • www.agilent.com/chem 800 227 9770 14

    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.Agilents Gas Leak Detector enables quickand easy detection and measurement of

    Description Part No. Price

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

    Gas leak detector, 115 V 5182-9646 $1915

    Gas leak detector, 220 V 5182-9648 $1915

    Description Part No. Price

    Cylinder wall bracket with strap and chain 5183-1941 $ 60(cylinder size up to 14 in., 35 cm)

    Cylinder Bracket

    Description Part No. Price

    Spectra-Link with 1/8 in. fittings and 36 in. SS tubing SL-8 $496

    Spectra-Link with 1/4 in. fittings and 36 in. SS tubing SL-4 $496

    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

  • 15 www.agilent.com/chem 800 227 9770

    GAS MANAGEMENT

    ADM 1000 features include: Accuracy 3%

    Operating temperature range0 to 45C for the instrument, -70 to 135C for the tubing

    Calibrationtraceable to NIST primarystandards

    Real time, split ratio measurement

    CE mark certified

    Measures flow rates from 0.5 to 1000 mL/min

    Split ratioscompare 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 measurementsmeasure 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. Price

    FlowTracker 1000 Flowmeter 5183-4779 $ 816

    FlowTracker 2000 Flowmeter and Leak Detector 5183-4780 $1143

    FlowTracker Universal AC Adapter (optional, not supplied with FlowTracker units) 5183-4781 $ 43

    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

  • www.agilent.com/chem 800 227 9770 16

    GAS MANAGEMENT

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

    ADM Flowmeters volumetric, measures all gases*

    ADM1000 0.5 1000 All 3 9V Battery None 220-1170 $620

    ADM2000 0.5 1000 All 3 Battery or 120 VAC Yes 220-1171-U $725

    ADM2000E 0.5 1000 All 3 Battery or 220 VAC Yes 220-1171-E $725

    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 $681

    Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery(220 V) 5.0 500 N2, Air 3 or 220 VAC Yes HVF-500-2 $681

    Optiflow Flowmeters Gas Flowmeters versatile volumetric flowmeters**

    Optiflow 420 0.1 50 All +/- 3 9V Battery None HFM-420 $573

    Optiflow 570 0.5 700 All +/- 3 9V Battery None HFM-570 $573

    Optiflow 650 5.0 5,000 All +/- 2 9V Battery None HFM-650 $677

    *non-corrosive gases only

    **non-corrosive and mildly corrosive gases only

    Flowmeters

    Optiflow 420Veri-Flow 500

    TIPS AND TOOLS

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

  • You asked we listened!

    Announcing the launch of our new Life Sciences and Chemical Analysis website. Based on customer feedback, weve 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.

  • 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. Agilentscommitment 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 800 227 9770 18

    CATALOG

    For a complete selection of vials, syringes, and inlets, see Agilents2005-2006 Essential Chromatography Catalog. Or, visit our onlinecatalog at www.agilent.com/chem/4ecatalog.

  • 19 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Sample Introduction

    VialsAgilents 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.

    Glassfor general purposeuse and for use with acids

    Silanizedfor use withsamples that bind to glass,and for trace analyses

    Polypropylene for usewith alcohols and aqueoussolvents

    Amber Vialsfor use withlight-sensitive samples

    Microvolume Insertsforuse with very small samplevolumes

    High Recovery Vialsfor 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 L

    100 L vial

    TIPS AND TOOLS

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

  • www.agilent.com/chem 800 227 9770 20

    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. Agilents 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. Price

    Vials

    2 mL Crimp top vial convenience pack with silver AI caps with Teflon/Red rubber septa 500/pk 5181-3400 $115

    2 mL Screw top vial conveniencepack with blue screw caps andTeflon/Red rubber septa 500/pk 5182-0732 $183

    2 mL Snap top vial convenience packwith clear polypropylene snap capsand Teflon/Red rubber septa 500/pk 5182-0547 $154

    100 L Insert for wide opening vials 100/pk 5181-1270 $ 88

    250 L Polypropylene flat bottom inserts 500/pk 5183-2087 $ 57

    100 L Glass lined polypropylene vials 100/pk 9301-0977 $158

    Less than 5 L dead volume, Micro-V vial, clear crimp top 100/pk 5184-3551 $ 69

    30 L reservoir volume, High recoveryvial, crimp top 100/pk 5182-3454 $109

    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

  • 21 www.agilent.com/chem 800 227 9770

    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 m

    Cool on-column 26/32 gauge tapered 320 m

    Cool on-column 26/32 gauge tapered 250 m

    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 Agilents Centerguide Septa, page 38.

  • www.agilent.com/chem 800 227 9770 22

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Syringe Advantage Limitations Recommended Use

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

    injection more easily Routine analysis No hardware Not ideal for higher

    modification needed viscosity samplesfor 0.5 L injection Plunger not

    replaceable

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

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

    viscosity samples

    10 L, 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 L 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-m and 320-m 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.

  • 23 www.agilent.com/chem 800 227 9770

    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.

  • www.agilent.com/chem 800 227 9770 24

    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 shaftssurface.

    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 plungers 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 drysolvent, 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.

  • 25 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Description Unit Part No. Price

    Miscellaneous Autosampler Supplies

    4 mL Clear screw top wash vials with screw caps (no Septa) 144/pk 9301 0723 $ 64

    Septa for 4 mL vial 144/pk 9301-1031 $ 21

    Diffusion caps for 4 mL vials 12/pk 07673-40180 $ 19

    4 mL wash vial with fill marking, caps 25/pk 5182-0551 $ 26

    Screw for mounting syringe 07673-20570 $ 13

    Quadrant kit (4 tray sections) 18596-40015 $ 75

    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 $755

    GC Automatic Liquid Sampler Supplies

    Description Gauge/Length Quantity Part No. Price

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

    10 L Tapered Fixed Needle 23-26s/42 6/pk 5181-3360 $198

    5 L Tapered Fixed Needle 23-26s/42 6/pk 5181-8810 $303

    Straight Needle Syringes(use with Merlin Microseal)

    10 L Straight Fixed Needle 23/42 6/pk 9301-0725 $191

    5 L Straight Fixed Needle 23/42 6/pk 5182-0875 $292

    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

  • www.agilent.com/chem 800 227 9770 26

    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 +50C 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.

  • 27 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Item Description Unit Part No. Price

    1 Septum nut 18740-60835 $ 37

    2 Septa Bleed temperature, optimized, 11 mm 50/pk 5183-4757 $ 67

    3 Top insert weldment 19243-80570 $132

    4 Viton O-rings 12/pk 5080-8898 $ 12

    5 Glass liner, disposable 25/pk 5080-8732 $ 37

    Glass liner, disposable/deactivated 5/pk 5181-3382 $ 14

    6 Vespel/graphite ferrules, 1/4 in. id 10/pk 5080-8774 $ 42

    7 Tubing nut, 1/4 in. brass 10/pk 5180-4105 $ 13

    Adapters with glass liners

    8 0.53 mm column adapter 19244-80540 $119

    1/8 in. column adapter 19243-80530 $ 99

    1/4 in. column adapter 19243-80540 $141

    9 Upper insulation 19243-00067 $ 5

    10 Nut warmer cup with insulation 19234-60720 $ 54

    11 Column nut for 0.53 mm column 2/pk 5181-8830 $ 25

    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. Price

    Nonpurging septum nut assembly for manual flow control only, not EPC 19243-60570 $100

    Adapters without glass liners

    1/8 in. column adapter 19243-80510 $ 88

    1/4 in. column adapter 19243-80520 $128

    Universal Packed-Column Inlet (non-purged)

    Septum retainer nut forheadspace sampling, nonpurging 19243-60505 $ 70

    Brass nut, 1/4 in. 10/pk 5180-4105 $ 13TIP

    S A

    ND

    TO

    OLS

    Tap Agilents 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

  • www.agilent.com/chem 800 227 9770 28

    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 250C 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 L 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, (

  • 29 www.agilent.com/chem 800 227 9770

    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 10C 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 (+20C) Use higher for dirty samples

    and higher-boiling solutes

    Inlet liner Large volume >0.8mL Use with autoinjectorSmall volume 1L injection

    Hot-needle fast manual Use for 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 L 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.

  • www.agilent.com/chem 800 227 9770 30

    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. Price

    1 Septum retainer nut 18740-60835 $ 39

    2 Septa See page 36

    3 Insert Weldment G1544-60575 $216

    4 Liner O-ring See page 52

    5 Liner See page 47

    6 Split vent trap assembly (6890/6850 only) G1544-80550 $128

    7 Retaining nut (6890/6850 only) G1544-20590 $ 26Retaining nut (5890 only) 19251-20620 $ 31

    8 SS seal 18740-20880 $ 26Gold-plated seal 18740-20885 $ 33

    9 Washer, 0.375 in. od 12/pk 5061-5869 $ 8

    10 Reducing nut 18740-20800 $ 34

    11 Insulation (requires 3) 19243-00067 $ 5

    12 Lower insulation cover 19243-00070 $ 15

    13 Ferrule

    14 Column nut (6890/5890 only) 2/pk 5181-8830 $ 26

    Column nut (6850 only) 2/pk 5183-4732 $ 47

    Angled wrench for split/splitless inlet 19251-00100 $ 29

    * 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).

  • 31 www.agilent.com/chem 800 227 9770

    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 3C 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 L 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 L to 2.0 L)

    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.

  • www.agilent.com/chem 800 227 9770 32

    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. Price

    Column nut 2/pk 5181-8830 $ 26

    250 m graphite/Vespel ferrule 10/pk 5181-3323 $ 55

    320 m 0.5 mm graphite/Vespel ferrule 10/pk 5062-3514 $ 51

    250 m retention gap (one 5 m piece) 160-2255-5 $ 39

    320 m retention gap (one 5 m piece) 160-2325-5 $ 42

    530 m retention gap (one 5 m piece) 160-2535-5 $ 59

    Quartz deactivated column connector fits 0.18-0.53 mm 5/pk 5181-3396 $ 94

    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.

  • 33 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Item Description Unit Part No. Price

    Manual injection

    1c Cooling tower assembly 19320-80625 $175

    1d Duckbill septum 10/pk 19245-40050 $ 29

    Fused silica syringe needles 6/pk 19091-63000 $ 41

    Syringe barrel for use with fused-silica needles,10 L 9301-0658 $ 90

    Common Supplies

    3 Spring 19245-60760 $ 9

    4 Inserts for capillary columns

    For 200 m columns (one ring) 19245-20510 $ 89

    For 250 m columns (six rings) 19245-20515 $114

    For 320 m columns (five rings) 19245-20525 $ 78

    For 530 m columns (no rings) 19245-20580 $ 55

    For 530 m Al clad columns (four rings) 19245-20780 $ 54

    5 Ferrule 5080-8853 $ 47

    6 Column nut 2/pk 5181-8830 $ 26

    6890 Series GC Cool On-Column Inlet Supplies

    Automatic Injection

    1a Septum nut base for 320 mm assembly 19245-80521 $ 62

    1b Septum nut base for 530 mm assembly G1545-80520 $ 63

    2 Advanced green 5 mm through hole septa 50/pk 5183-4760 $ 62BTO 5 mm through hole septa 50/pk 5183-4758 $ 72

    5890 Series Cool On-Column Inlet Supplies

    Automatic Injection

    1a Septum nut (5890 Series II GC) 19245-80520 $ 91

    1b Needle guide (for 7673A only) 19245-20670 $ 35

    * 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

  • www.agilent.com/chem 800 227 9770 34

    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., 2C/sec Use slower ramp rates for ramp rate to 12C/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 0.1-1.5L Use lower volumes for volatile solvents and fast ramp ratesUse volumes larger than 1.5L only in solvent- elimination mode

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

    Oven temperature 10-25C 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.

  • 35 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Item Description Column ID Unit Part No. Price

    1 Septumless head G2617-60507 $2661

    2 Septum head G2618-80500 $1078

    3 Septum nut 18740-60835 $ 39

    4 PTV inlet assy G2617-60506 $4850

    5 PTV LCO2 cooling jacket G2617-60508 $ 544

    6 PTV LN2 cooling jacket G2619-60501 $ 473

    7 Silver seal 5/pk 5182-9763 $ 62

    8 Graphpak inlet adapter 0.20 mm 5182-9754 $ 173

    0.25-0.33 mm 5182-9761 $ 152

    0.53 mm 5182-9762 $ 146

    9 Ferrules for 0.20 mm 10/pk 5182-9756 $ 158

    Graphpak inlet 0.25 mm 10/pk 5182-9768 $ 166

    0.32 mm 10/pk 5182-9769 $ 166

    0.53 mm 10/pk 5182-9770 $ 146

    10 Split nut for inlet adapters 5062-3525 $ 159

    11 PTV insulation block G2617-20510 $ 61

    PTV cryo insulator (not shown) G2617-60510 $ 53

    Teflon ferrule (needle seal) 5182-9748 $ 137

    Kalrez seal 5182-9759 $ 110

    Valve body 5182-9757 $ 91

    Pressure spring 5182-9758 $ 6

    Viton seal 5182-9775 $ 24

    Sealing element 5182-9760 $ 73

    CO2 Cryo inline filter 3150-0602 $ 137

    Service kit for septumless head 5182-9747 $ 224contains Kalrez seal, valve body, and pressure springGraphpak 3D ferrules 5/pk 5182-9749 $ 143

    Installation tool for 3D ferrules G2617-80540 $ 208

    1

    2

    3

    4

    5, 6

    78910

    11

    6890 PTV Inlet

    PTV Liners

    Description Part No. Price

    PTV Liner Single Baffle, 2 mm id 180 L volume, deactivated, glasswool 5183-2038 $ 25

    PTV Liner Single Baffle, 2 mm id 200 L volume, deactivated 5183-2036 $ 20

    PTV Liner Multi Baffle, 1.5 mm id 150 L volume, deactivated 5183-2037 $ 29

    PTV Liner Fritted Glass, 1.5 mm id 150 L volume, deactivated 5183-2041 $ 55

    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

  • www.agilent.com/chem 800 227 9770 36

    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: Septadont 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

  • 37 www.agilent.com/chem 800 227 9770

    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.

  • www.agilent.com/chem 800 227 9770 38

    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 Agilents 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 wontstick or clump.

    Agilents plasma-treated non-stick septa

    Competitor non-stick septa

  • 39 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Agilents 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 400C(Bleed and (optimized forTemperature high temperature)Optimized)

    Long Life to 350C

    Advanced Green to 350C

    = 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

  • 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 800 227 9770 40

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    General Purpose SeptaAgilents 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 350C. 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.

    Agilents 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 350C

    Packaged in glass vials for high purity

    Economical alternative to competitorsGreen 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 Temperature350C

    Soft, 45 Durometer, Easy On Autosampler Needles

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

    Maximum Injection Port Temperature400C

    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

  • 41 www.agilent.com/chem 800 227 9770

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    Septa Ordering Information

    Part No. Price

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

    11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4757 $7211 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4757-100 $1345 mm septa through-hole for on-column in glass jar (50/pk) 5183-4758 $72

    Agilent Advanced Green Non-Stick Septa

    11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4759 $6211 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4759-100 $1075 mm septa through-hole for on-column in glass jar (50/pk) 5183-4760 $62

    Agilent Long-Life Non-Stick Septa

    11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4761 $8411 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4761-100 $1505 mm septa through-hole for on-column in glass jar (50/pk) 5183-4762 $84

    General Purpose Septa

    Gray Septa

    11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk) 5080-8896-50 $5211 mm for 5880, 5890, 6850 and 6890 GCs (100/pk) 5080-8894-100 $939.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5080-8728-50 $529.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5080-8728-100 $93

    Red Septa

    11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk) 5181-1263-50 $5211 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk) 5181-1263-100 $9311 mm with partial through-hole for 5880, 5890, (50/pk) 5181-3383-50 $526850 and 6890 GCs11 mm with partial through-hole for 5880, 5890, (100/pk) 5181-3383-100 $936850 and 6890 GCs9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5181-1283-50 $529.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5181-1283-100 $935 mm through-hole for on-column inlets, (25/pk) 5181-1260 $29automatic or manual injections* 5 mm solid for high column backpressure, on-column inlets* (25/pk) 5181-1261 $29* 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

  • www.agilent.com/chem 800 227 9770 42

    SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

    How to Minimize ProblemsGeneral technique for installing ferrules: dont overtighten finger-tighten column

    nut, then