Maintaining your Agilent GC and GC/MS Systems

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Operate your lab at peak performance

Troubleshoot difficult problems

Select the right Agilent supplies

Plan preventative maintenance

Maintaining your Agilent

GC and GC/MS Systems

Maximize your efficiency. Minimize your downtime.

Get the results you need.

Our GC and GC/MS Maintenance Guide puts nearly 40 years of Agilent knowledge at your fingertips.

At Agilent Technologies, we understand that many of today’s labs face the challenge of operating with a reduced staff. That’s why we’re committed to bringing you the world’s best GC and GC/MS systems — plus the critical information you need to keep them running properly.

In this newly updated Maintenance Guide, we share everything from essential service schedules … to invaluable troubleshooting tips and problem-solving methods.

We’ve even included easy guides to help you order Agilent parts and supplies — which have 40 years of high quality and technical experience built right in. So you can keep your downtime to a minimum, and get the results you need.

1

Maintaining Your Agilent GC and GC/MS Systems

Maximize your efficiency. Minimize your downtime.

Get the results you need.

TIPS AND TOOLS

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

VIDEO

This icon denotes a video that is available to view on our website.

Just visit www.agilent.com/chem/techsupport to view how-to videos and obtain more information.

2 Gas Management

3 Gas Types

4 Contaminants & Purities

4 Gas Purification Systems

12 Regulators

13 Tubing

14 Leak Detection

15 Flow Rates

18 Sample Introduction

Consumables & GC Inlets

Sample Introduction

19 Vials

21 Syringes

Inlet Types

26 Packed-Column

28 Split/Splitless

31 Cool On-Column

34 Programmed Temperature

Vaporizer PTV

Inlet Accessories

36 Septa

42 Ferrules

47 Liners

52 Flip Top Inlet Sealing System

54 Parts & Supplies

56 Columns

57 Column Maintenance

57 Column Selection

58 Column Installation/Setup

& Conditioning

59 Column Performance

63 Columns Types and

Characteristics

68 Detectors

69 Flame Ionization Detector (FID)

Thermal Conductivity Detector

(TCD)

72 Electron-Capture Detector

(ECD)

74 Thermal Conductivity Detector

(TCD)

76 Flame Photometric Detector

(FPD)

78 Nitrogen-Phosphorus Detector

(NPD)

82 GC/MS Systems

83 Maintaining Mass Selective

Detectors (MSDs)

87 Mass Spectrometer Symptoms

88 Ion Source

93 Vacuum Systems & Pumps

96 Electron Multipliers &

Replacement Horn

97 Maintaining the MS Engine

99 Ion Source Parts & Supplies

100 General GC/MS Supplies

101 Test & Performance Samples

104 Services & Support

105 Expert Service, Training

& Support

Don’t Miss…

GC Maintenance Schedule (inside back cover) www.agilent.com/chem • 800 227 9770

www.agilent.com/chem • 800 227 9770

Gas Management

The use of quality carrier gases is essential for consistent and accurate GC analyses.

Proper gas management is key to achieving this goal. Agilent provides a diverse line of high quality gas management products — gas purifiers, regulators, leak detectors and flowmeters — all designed to prevent column damage, improve detector life, and improve the quality and consistency of your

GC separations. This section explains how common contaminants like oxygen, moisture and hydrocarbons can damage your GC column, and helps you understand how to prevent it. Also, look for practical information about regulators, the importance of clean

GC-tubing, and minimizing the likelihood of GC system contamination.

“Gas management is more than just selecting the highest quality carrier gas available. It’s about selecting the appropriate carrier gas for your needs, and taking steps to prevent system contamination. Agilent understands this and provides products that make gas management easy to implement in your lab.”

Kenji Yamaguchi

Applications Support Manager

CATALOG

For a complete selection of gas management supplies, see Agilent’s

2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.

2

GAS MANAGEMENT

Gas Types

Carrier Gases

The most frequently used carrier gases are helium and hydrogen, although nitrogen and argon can be used. Purity is essential for these gases since they sweep the sample through the column where it is separated into its component parts and then through the detector for component quantification. Carrier gas purity is also critical to prevent degradation of chromatographic hardware.

Contaminants in carrier gases can have a significant effect on column life and subsequent analyte detection. Harmful effects of impure gases include contaminant peaks and elevated column bleed, along with column and/or detector damage. The following sections describe the gases and purities that are necessary for gas chromatography carrier gases, as well as other support gases.

Support Gases

Support gases may be specific for detectors or for applications. These gases include fuels, oxidants, coolants, detector gases, and pneumatic gases. The degree of purity required for support gases is dependent on how that gas is being used, and whether or not it will make contact with the sample. Coolant gases (carbon dioxide) and pneumatic gases (air or nitrogen) generally do not come in contact with the sample or detector. Therefore, these non-contact gases do not have to be the highest purity available.

Fuels, oxidants and detector gases, in most cases, do come in contact with the sample and detector, and require higher purity gases. Unfortunately, gas nomenclature as it relates to purity is not consistent across specialty gas suppliers. It is important to recognize the impurities in your gas supplier’s products, and to utilize the appropriate Agilent gas purification products (see next section).

Carrier and Support Gases

Gas Type

Air

Nitrogen

Function

Pneumatics

Pneumatics

Sample

Contact

No

No

Purity Required*

Low Grade

Low Grade

Limit of Detection required:

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

Hydrogen

Hydrogen/Helium Mix

Methane/Argon or Nitrogen

Air

Carrier or fuel gas for detector

Fuel gas for detector

Carrier or make-up for ECD

Oxidant for detector

Yes

Yes

Yes

No

Research

Research

Research

Ultra-Pure

Ultra-Pure

Ultra-Pure

Research

Ultra-Pure

Nitrogen, Helium, or Argon

Carrier or make-up gas Yes Research Ultra-Pure

*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%)

Ultra-Pure

Ultra-Pure

Research

UHP/Zero

Ultra-Pure

1%-100%

UHP/Zero

UHP/Zero

N/A

UHP/Zero

UHP/Zero

3 www.agilent.com/chem • 800 227 9770

GAS MANAGEMENT

Contaminants & Purities

Contaminants in gases are major contributors to capillary column degradation and detector noise, and can interfere with chromatographic results. Concentration of these contaminants vary by the grade of gas.

Analytical gases are available in many grades of quality, from high purity

(99.995%) to chromatography grade purity

(99.9995+%). The higher the purity, the higher the cost.

Identifying Contaminants

To make a proper purity choice it is helpful to understand the contaminants most common in GC gases and how they can affect your analysis. Common contaminants are:

Hydrocarbons and Halocarbons

• decrease detector sensitivity by increasing detector background noise

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

Moisture

• can be introduced by improper handling and/or installation of plumbing

• a common cause of column stationary phase degradation

• can damage instrument

Oxygen

• most common contaminant

• a common cause of column stationary phase and inlet liner degradation

• can cause decomposition of labile analytes

• opportunity for introduction at every fitting present in the gas line or during use of gas permeable tubing.

In some cases it may be difficult to determine which contaminant presents the biggest problem in a given analysis. If unsure, a call to your gas supplier may be helpful. Once the problem contaminants have been identified and a general contaminant level is determined, the next step is to choose a gas purity level that comes closest to these requirements.

Keep in mind that higher grades of gas generally cost more. The greatest cost savings can be achieved by using the lowest purity gas which will neither interfere with the analysis nor damage your equipment. Using the proper gas purification equipment to remove common contaminants and achieve the desired purity level is essential.

Gas Purification Systems

Agilent brings the highest performance and largest variety of gas purifiers (traps) to gas chromatographers. Purifiers are available in a variety of sizes and configurations to remove common contaminants like oxygen, moisture, and hydrocarbons. In-line gas purifiers, including refillable, indicating, S-shaped, and metal body types, are made to remove specific contaminants. Agilent also offers gas purification systems with removable cartridges. These systems provide the ability to design the right combination of filters needed for your application to achieve the proper gas purity.

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

Regardless of which purification system is employed, proper installation and maintenance is required to achieve optimal performance from the purification system(s). A purifier that is not maintained will eventually expire and become ineffective, or worse, a source of contamination.

Other Considerations

• determine desired purity level

• keep number of fittings in gas line to a minimum

• install purifiers in a convenient location close to the GC

• purifier log books are useful for determining maintenance schedule

• use indicating traps closest to the GC so you can determine when to change the traps that are upstream www.agilent.com/chem • 800 227 9770 4

GAS MANAGEMENT

Carrier Gas Purification

In-Line Gas Purifiers

Gas supply

-OR-

Gas Purification System

Gas supply

-OR-

Vent

Combination Trap

Key:

1 = Moisture Trap

2 = Hydrocarbon Trap

3 = Oxygen Trap

4 = Indicating Oxygen Trap

5 = Gas Purification System

6 = Combination Trap for moisture, oxygen, and hydrocarbon removal

Detector Gas Purification

FID make-up, air, and H

2

ECD make-up

ELCD reaction gas

MS carrier gas

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

Regulator = Brass dual stage regulator

Gas Traps

The purpose of gas traps is to remove detrimental impurities from the carrier and detector gases. Moisture (water), oxygen and hydrocarbon traps are the most common traps used with GC systems. A few combination traps are available which remove moisture, oxygen and/or organics with a single trap. The effectiveness of the traps depends on the initial quality of the gas. Little enhancement by traps to the GC system is obtained by traps when using very high purity gases (e.g., ultra-high purity or similar grades) while obvious improvement is obtained with lower grades of gas.

Constant exposure of capillary columns to oxygen and moisture, especially at high temperatures, results in rapid and severe column damage. The use of oxygen and moisture traps for the carrier gas may extend column life and protect the instrument. Traps may provide some protection if there is a leak at or around the gas cylinder. Any moisture or oxygen introduced into the gas stream due to the leak will be removed by the trap until it expires. This creates an opportunity to detect and fix the leak before column or instrument damage occurs.

5

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.

www.agilent.com/chem • 800 227 9770

GAS MANAGEMENT

Moisture (Water) Traps

There are several different adsorbents and indicating materials used in moisture traps. Moisture traps can be easily refilled.

Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap making refilling a more economical (and less wasteful) option.

Indicating moisture traps are available in plastic and glass bodies.

Glass body traps are used when potential contaminants from plastic trap bodies are a concern. Glass traps are normally encased in a protective, plastic shrink wrap or a high impact plastic shield (outer trap body). Glass and plastic bodied traps are usually pressure tested at 150 psi, thus they are safe for use at the typical pressures required by the GC.

Refillable Glass Moisture Trap

Moisture Removal Traps

Description

Size

(cc)

H

2

O Removal Maximum Effluent H

2

Capacity (g) Concentration (ppb)

O 1/8 in.

Part No.

1/4 in.

Part No.

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

Refillable Moisture Trap

Adsorbent Refill (1 pint) for MT Series

200 36 18 MT200-2

MSR-1

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

Glass Indicating Moisture Traps 100

Molecular Sieve Refill for GMT Series 250

16.3

6 GMT-2-HP

GMSR

MT200-4

MSR-1

GMT-4-HP

GMSR

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

Moisture S-Trap – preconditioned

Big Moisture Traps – for the Ultimate Moisture Capacity

Big Moisture Trap

Refill for BMT Series (2 refills)

750

5060-9084

BMT-2

BMSR-1

BMT-4

BMSR-1

Price

$226

$235

$ 58

$104

$ 55

$119

$ 63

Refillable Moisture Trap www.agilent.com/chem • 800 227 9770

Moisture S-Trap Big Moisture Trap

6

GAS MANAGEMENT

Indicating Oxygen Trap

Big Oxygen Trap

Oxygen Traps

Oxygen traps usually include a metalcontaining inert support reagent. Most oxygen traps reduce the oxygen concentration to below 15-20 ppb. The capacity of a standard oxygen trap is approximately 30mg of oxygen per 100cc of trap volume. Oxygen traps can also remove some small organic and sulfur compounds from gas streams, but this is not their primary application.

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

Oxygen Traps

Description Size (cc)

1/8 in.

Part No.

Indicating Oxygen Traps – glass body with plastic safety shield

1/4 in.

Part No.

Price

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

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

Big Oxygen Trap 750 BOT-2 BOT-4

$143

$235 plastics are permeable to air and contain contaminants that can degrade gas quality.

In addition, many of the metal bodied oxygen traps can withstand high pressures

(up to 2000 psi). Some oxygen traps also remove moisture from the gas stream without affecting the oxygen removal capability.

Indicating oxygen traps change color when oxygen is present in the gas at harmful levels. Indicating traps are not intended to be the primary oxygen removal trap, but should be used in conjunction with a high

capacity non-indicating oxygen trap. They are installed after the high capacity oxygen trap in the gas line to indicate when the high capacity trap has expired and needs to be changed. Expired oxygen traps need to be immediately changed since they can contaminate the gas, in addition to failing to remove oxygen.

7

Hydrocarbon Traps

Description Size (cc)

1/8 in.

1/4 in.

Part No.

Part No.

Price

Hydrocarbon Traps – General Purpose

Refillable Hydrocarbon Trap

Adsorbent Refill (1 pint, 2 refills)

200 HT200-2

ACR

Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity

HT200-4

ACR

$106

$ 63

Big Hydrocarbon Trap

Refill for Big Hydrocarbon Trap (2 refills)

750 BHT-2

BACR

BHT-4

BACR

$235

$ 52

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

Hydrocarbon S-Trap 5060-9096

Capillary Grade Hydrocarbon Traps – for crucial capillary applications

Capillary Grade Hydrocarbon Trap

Adsorbent Refill (1 pint, 3 refills)

100 HT3-2

ACR

HT3-4

ACR

$232

$ 98

$ 63

Hydrocarbon Traps

Hydrocarbon traps remove organics, such as hydrocarbons and halocarbons, from the gas stream. The adsorbent is usually activated carbon or an impregnated carbon filter media. Carbon removes organic solvents from the gas stream, including the typical solvents used in nearly every lab.

Hydrocarbon-moisture combination traps are also available which remove water in

Hydrocarbon Trap www.agilent.com/chem • 800 227 9770

GAS MANAGEMENT

Hydrocarbon Traps continued

addition to organics as described in the next section. Capillary grade hydrocarbon traps are purged with ultra-high purity helium and packed with a very efficient activated carbon material. Metal trap bodies are used to prevent any contaminants in plastic trap bodies from contaminating the carbon adsorbent. Most hydrocarbon traps can be refilled by the end user.

Big Hydrocarbon Trap

Hydrocarbon S-Trap

Combination Traps

Agilent carries several Combination Traps that provide multiple contaminant removal in a single trap. These traps offer:

• Optimized adsorbents for maximum surface area and capacity

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

• Efficient design which prevents channeling and promotes efficient scrubbing

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

Description

Oxygen/Moisture Traps

Size (cc)

1/8 in.

Part No.

1/4 in.

Part No.

Price

Agilent OT3 Trap

Hydrocarbon/Moisture Traps

100 OT3-2 OT3-4 $104

Refillable Hydro-Moisture Trap

Refill for Hydrocarbon/

Moisture Trap (1 pint, 2 refills)

200 HMT200-2

HCRMS

HMT200-4

HCRMS

$ 98

$ 63

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

2

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

Big Universal Trap – Hydrogen purged 750

Big Universal Trap – Nitrogen purged 750

Big Mounting Clip for mounting Big Traps 2/pk

RMSHY-2

RMSN-2

UMC-5-2

RMSHY-4

RMSN-4

UMC-5-2

$261

$261

$ 21

Agilent OT3 Trap

Big Universal Trap

Hydrocarbon Moisture Trap www.agilent.com/chem • 800 227 9770 8

9

GAS MANAGEMENT

Three Cartridge

High Capacity

Gas Purification

System

High Capacity Gas Purification System

Description Part No.

Three Cartridge System–Includes manifold for wall or bench mount and 3 cartridges

(H

2

O/hydrocarbon, oxygen, and indicating O

2

)

With 1/8 in. fittings 5183-1907

With 1/4 in. fittings

Replacement Cartridge Kit–

Includes all three cartridges for above system

5182-9776

5182-9780

Single Cartridge System–Includes single cartridge manifold brackets for wall or bench mount, and a triple combination cartridge

(H

2

O/hydrocarbon, and O

2

)

With 1/8 in. fittings 5183-4598

5183-4599 With 1/4 in. fittings

Triple combination replacement cartridge for single cartridge system 5183-4600

High Capacity

Gas Purification System

Three Cartridge System

• Agilent’s highest capacity and most economical gas purification system.

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

• Includes a manifold with cartridge mounts and three replaceable cartridges: one moisture/hydrocarbon cartridge; one oxygen cartridge; and one oxygen indicating cartridge.

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

• Suitable for bench or wall mounting.

Single-Cartridge System

• Contains a triple-combination cartridge that offers the same highly efficient contaminant removal properties from eight cylinders of carrier gas but without the visual indicator.

• Other cartridges are also available for detector gas supplies and as individual filters for specialized requirements.

Price

$239

$255

$136

$612

$567

$393 www.agilent.com/chem • 800 227 9770

Quick Change Plus (QC+) Point of

Operation Panel

The QC+ Point of Operation Panel contains purifier cartridges that can be quickly changed. The cartridges are removed from the panel without interruption of gas flow to the system, drastically minimizing costly instrument downtime.

Filter cartridges are of all metal or glass construction, eliminating infusion and resultant signal noise associated with filters constructed from plastics. Cartridges are quickly installed via a simple knurled retaining nut, with no wrenches needed.

As many as four cartridges can be replaced in a matter of seconds, and because there is low dead volume, a minimal amount of gas system purge is required after installation.

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

Fitting (in.) Part No.

Description

4-Head

O

2

, indicating O

2

, HC, H

2

O 1/8 RQC-P

Price

$1604

Replacement Cartridges

Description

High capacity oxygen

High capacity moisture

Indicating moisture

Hydrocarbon

Indicating oxygen

Part No.

GC-1

GC-2

GC-2-I

GC-3

GC-4

Price

$ 64

$ 64

$106

$ 64

$155

RQC-P

GAS MANAGEMENT

www.agilent.com/chem • 800 227 9770

EASY ONLINE ORDERING

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

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

10

11

GAS MANAGEMENT

Super-Clean Gas Filter System

Super-Clean gas filter systems are designed to provide the utmost in convenience and contamination reduction. The system is tested for leak-tightness and the glass and metal construction of the cartridges eliminates diffusion of contaminants into the gas stream. During cartridge replacement, check valves and close off the system to the atmosphere, further minimizing the entry of contaminants.

Super-Clean Gas Purification Systems

Available with 1/8" fittings only

Description

Carrier Gas Purification System: Single position system perfect for GC/MS,

ECD and NPD detectors. Includes the triple filter cartridge.

Super-Clean Gas Purification System:

For your most demanding GC application, includes four position baseplate manifold with four filter cartridges: oxygen, moisture (both with indicator), and two hydrocarbon cartridges.

Replacement Filter Cartridges

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

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

Part No.

5182-9704

5182-0816

5182-9705

5183-4770

Price

$ 398

$1291

$ 186

$ 530

Description

Universal/external split vent trap with 3 cartridges

(1/8 in. Swagelok fitting)

Replacement cartridges (3/pk)

Part No.

RDT-1020

RDT-1023

Price

$ 94

$ 45

Universal/External Split Vent Trap

Split vent traps stop environmental pollution. The split vent trap was designed to protect the lab environment from the contaminants released by split injection systems, which can vent up to 500 times the amount of sample reaching the detector into the laboratory's air. A replaceable, impregnated carbon filter media traps and eliminates a broad range of contaminants. The traps are also easy to change and come with three packs of replacement cartridges each. Replace approximately every six months.

Split Vent Trap and Cartridges www.agilent.com/chem • 800 227 9770

GAS MANAGEMENT

Regulators

Pressure regulators are an integral component in any gas handling system.

Their function is to reduce the pressure from a high pressure source, such as a cylinder, to a suitable use pressure.

Although regulators are very good at controlling pressure, they do not control flow. They have a maximum flow rate which is dictated by the design. Basically, the flow is determined by the pressure drop across the regulator.

Types of Regulators

There are primarily two types of regulators: single stage and dual (or two) stage.

The difference is that a dual stage regulator is actually two regulators connected in a series.

Dual stage regulators provide more precise and consistent pressure control than single stage regulators. The reason is that in a single stage regulator, as the gas cylinder empties and the inlet pressure to the regulator decreases (inlet decay), the pressure on the diaphragm is reduced.

Without proper adjustment, the outlet pressure might slowly rise.

A dual stage regulator overcomes this problem by connecting two regulators together. The first stage regulates the pressure to the second stage, thus creating a constant pressure and allowing minimal inlet decay. Agilent recommends using two-stage regulators with our GC Systems to provide the proper pressure control for optimal use.

Regulator Materials

Regulators are usually constructed of brass or stainless steel. The choice of material follows the same guidelines as the choice of tubing. Generally, it is not recommended that the materials be interchanged. If stainless steel tubing were chosen due to purity considerations, then a stainless steel regulator should be chosen for the same reasons. Steel regulators are more expensive, which is why Agilent offers brass regulators for less demanding applications.

No matter which material is chosen for the regulator body, be sure to specify one with stainless steel diaphragms for critical applications such as use on carrier, fuel or detector gases. Agilent recommends using our economical brass body, dual stainless

Brass Body Regulator steel diaphragm regulators for most GC applications. These regulators, combined with the proper gas purification system, provide proper gas pressure control and purity for gas chromatography.

When ordering a regulator, be sure to specify the proper connections. In the

US, most gas manufacturers follow CGA connection guidelines. In Europe, there are a number of organizations designating cylinder connections that are specific to individual countries. It is best to contact your local supplier for the proper connection designation.

Description Part No.

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

CGA 346, 125 psig max (8.6 bar), Air

CGA 350, 125 psig max (8.6 bar), H

2

, Ar/Me

CGA 540, 125 psig max (8.6 bar), O

2

CGA 580, 125 psig max (8.6 bar), He, Ar, N

2

CGA 590, 125 psig max (8.6 bar), Air

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

5183-4641

5183-4642

5183-4643

5183-4644

5183-4645

Regulator Outlet Adapters – Female NPT to Swagelok-style

1/4 in. to 1/8 in. brass

(included with brass regulators)

1/4 in. to 1/4 in. brass**

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

0100-0118

0100-0119

Price

$ 14

$ 15

$275

$275

$275

$275

$275

TIPS AND TOOLS

Always depressurize a regulator before closing by adjusting knob and removing the regulator from the cylinder.

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

13

GAS MANAGEMENT

Spectra-Link Tubing Connecting System on a two-stage regulator

Tubing Type Diameter

(inches)

Recommended

Max. Length (feet)

Copper

Copper

1/8 *

1/4*

50

300

*Recommended when multiple instruments are connected to the same source

Pressure Drop

(psig)

2

0.5

Tubing–Precleaned

Tubing

When constructing or maintaining a gas delivery system for GC, choosing the proper tubing material is very important and will help to eliminate potential problems and improve the overall quality of the gas system. Although there are many common tubing materials available, some pose safety or cleanliness problems.

Non-metallic types of tubing such as polyethylene and Teflon are not recommended for GC applications due to their gas permeability and difficulty in cleaning. This type of tubing can be used for non-critical applications, such

Determining Tubing Length

Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig as pressurizing pneumatic lines; however, be aware of its pressure limitations.

In view of these problems, the list of appropriate tubing materials has been narrowed down to two: copper and stainless steel. Agilent recommends using copper tubing for most applications, since it is easy to bend and plumb and is less expensive than stainless steel. Use stainless steel tubing only for crucial applications that require very high purity, or where building codes mandate its use.

Cleaning Tubing

Before any tubing is placed into service, or if it becomes contaminated with use, it is essential that it be properly cleaned.

Unclean or improperly cleaned tubing can lead to contamination of the system with disastrous results.

Cleaning tubing requires the use of suitable detergents and solvents along with nitrogen and a purgeable oven for drying. This may be done easily for small lengths of tubing, but in larger systems the cleaning procedure sometimes becomes unwieldy, leaving behind a large quantity of solvent requiring proper disposal.

Fortunately, Agilent provides clean, high quality GC grade tubing for large systems as an economical alternative.

Description Part No.

Price

Copper tubing, 1/8 in., 50 ft.

Copper tubing, 1/8 in., 12 ft.

5180-4196

5021-7107

$56

$28

MAINTENANCE MINDER

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

www.agilent.com/chem • 800 227 9770

Spectra-Link is No Ordinary Flexible Tubing!

• Stainless Steel: no outgassing or permeation through polymeric materials

• Quick Connection: prevents air from entering gas lines during tank changeover

• Tested: each system has leak rates lower than 1x10 -5 cc/sec

Description

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

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

Part No.

SL-8

SL-4

Price

$496

$496

Cylinder Bracket

Description

Cylinder wall bracket with strap and chain

(cylinder size up to 14 in., 35 cm)

Part No.

5183-1941

Price

$ 60

Leak Detection

Leaks allow oxygen and other contaminants to enter the gas stream.

Therefore, GC instrument maintenance should include checking fittings and connections with a gas leak detector.

Agilent’s Gas Leak Detector enables quick and easy detection and measurement of gas leaks for 12 common gases. Based on a dual cell micro volume thermal conductivity system, this unit provides very high sensitivity and eliminates contamination caused by soap solution methods.

Gas Leak Detector Kit

Description Part No.

Price

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

Gas leak detector, 115 V

Gas leak detector, 220 V

5182-9646

5182-9648

$1915

$1915

Cylinder Wall Bracket

GAS MANAGEMENT

Gas Leak Detector www.agilent.com/chem • 800 227 9770 14

GAS MANAGEMENT

Flow Rates

Setting and maintaining GC flow rates greatly affect the instrument accuracy and sensitivity. During maintenance, verify carrier and support gas flows with the proper flowmeter. Choosing a flowmeter for your application depends upon measurement speed, ease of use, accuracy, and flow rate range.

Selecting a Flowmeter

Agilent manufactures the largest selection of volumetric and mass flowmeters for chromatography. We have developed flowmeters for measuring capillary column flows, calibrating air pumps and flow controllers, and verifying instrument gas flows. All flowmeters are calibrated to

NIST-traceable standards.

15

FlowTracker 2000

ADM 1000

FlowTracker Flowmeters – volumetric, multimode flowmeters

Description Part No.

Price

FlowTracker 1000 Flowmeter

FlowTracker 2000 Flowmeter and

Leak Detector

5183-4779

5183-4780

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

$ 816

$1143

$ 43

ADM 1000 features include:

• Accuracy ± 3%

• Operating temperature range–

0 to 45ºC for the instrument, -70 to

135ºC for the tubing

• Calibration–traceable to NIST primary standards

• Real time, split ratio measurement

• CE mark certified

• Measures flow rates from 0.5 to

1000 mL/min

• Split ratios–compare the ratio from one gas measurement to another

(i.e., injection port split ratios)

ADM 2000

In addition to the features of the ADM

1000, the ADM 2000 includes:

• Mass flow measurements–measure flow rate, independent of atmospheric pressure and temperature (calculated)

• Data output through RS-232 port

• 9V battery and AC power adapter

(120 or 220 VAC)

ADM 2000 www.agilent.com/chem • 800 227 9770

GAS MANAGEMENT

Flowmeters

Description

Flow Rate (mL/min)

Low High

Gases

Measured

Accuracy

(%)

Power

Supply

RS-232 Data

Output

ADM Flowmeters – volumetric, measures all gases*

ADM1000

ADM2000

ADM2000E

0.5

0.5

0.5

1000

1000

1000

All

All

All

± 3

± 3

± 3

9V Battery

Battery or 120 VAC

Battery or 220 VAC

None

Yes

Yes

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

Veri-Flow 500

(110 V)

Veri-Flow 500

(220 V)

5.0

5.0

500

500

He, H

2

, Ar/CH

4

N

2

, Air

He, H

2

, Ar/CH

4

N

2

, Air

± 3

± 3

Rechargeable Battery or 110 VAC

Rechargeable Battery or 220 VAC

Yes

Yes

Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters**

Optiflow 420 0.1

50 All +/- 3 9V Battery

Optiflow 570

Optiflow 650

0.5

5.0

700

5,000

*non-corrosive gases only

**non-corrosive and mildly corrosive gases only

All

All

+/- 3

+/- 2

9V Battery

9V Battery

None

None

None

Part No.

220-1170

220-1171-U

220-1171-E

HVF-500

HVF-500-2

HFM-420

HFM-570

HFM-650

Price

$620

$725

$725

$681

$681

$573

$573

$677

Veri-Flow 500 www.agilent.com/chem • 800 227 9770

Optiflow 420

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.

16

You asked … we listened!

Announcing the launch of our new Life Sciences and

Chemical Analysis website.

Based on customer feedback, we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.

The new site features:

• A coherent page design – that automatically detects

screen resolution and optimizes the page size for less scrolling.

• An expanded navigation – that includes links to

product literature, technical support, education, events, and news.

• A newly designed online store – with fast access to

pricing, order status, quotes, and local sales information.

• Direct links – to the services, parts, and consumables that

keep your instruments running in top condition.

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

Consumables &

for consistent and accurate GC analyses.

prevent it. Also, look for practical information about regulators, the importance of clean

GC-tubing, and minimizing the likelihood of GC system contamination.

www.agilent.com/chem • 800 227 9770

“Good sample introduction helps ensure good reproducibility, optimal peak shape, and accurate sample delivery. Agilent’s commitment to offering the highest quality supplies means accurate, reliable results.

Time after time.”

Bryan Bente, Ph.D.

Technology Development Manager

CATALOG

For a complete selection of vials, syringes, and inlets, see Agilent’s

2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.

18

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Introduction

Vials

Agilent’s wide opening vials are designed specifically for analyzing samples with your

GC. They have specially designed vial neck angles, bottom design and height to ensure compatibility with Agilent autosamplers with rotating or robotic arm trays. Agilent offers a large variety of autosampler vials in different closures, cap colors, septa choices and package options. Agilent also offers convenience packs with 500 vials and caps in a reusable blue storage box.

For small sample sizes, Agilent offers a variety of options. You can use microvolume inserts with the wide opening vials or, for added convenience, use vials with small volume capacity.

Vial Filling

When filling sample vials, keep in mind:

• if you need to test a large amount of sample over repeated injections, divide the sample among several vials to obtain reliable results

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

The airspace in the vial is necessary to avoid forming a vacuum when sample is withdrawn. This could affect reproducibility.

Vial Options

Glass –for general purpose use and for use with acids

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

Polypropylene –for use with alcohols and aqueous solvents

Amber Vials –for use with light-sensitive samples

Microvolume Inserts –for use with very small sample volumes

High Recovery Vials – for use with limited sample volumes

Recommended fill volumes for sample vials

19

TIPS AND TOOLS

Do not inject air into the vials to prevent the vacuum.

This often damages the cap seal.

1 mL

3.6 mm*

*Needle position based on standard sampling depth.

50 µL

100 µL vial www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Selecting Vial Septa Materials

Vial cap septa are critically important to optimal analysis. Each septum complements the overall system and enhances chemical performance.

Agilent’s vial cap septa are specifically formulated and constructed for optimum system performance, with minimal coring and superior chemical inertness.

Red Rubber/Teflon

• Routine analysis

• Moderate resealing

• Excellent chemical inertness

• Not recommended for multiple injections or storage of samples

• Least expensive

Silicone/Teflon

• Excellent resealing

• Resists coring

• Good for multiple injections

Teflon/Silicone/Teflon

• Used in trace analysis applications

• Above average resealing

• Most resistant to coring

• Least evaporation

• Use with large diameter, blunt tip syringe needles

Teflon Disc

• Good for MS and ECD analysis

• Good for large-volume injections

• Chemically inert

• No resealing

• Single injection

• No long-term sampling storage

Viton

• Chlorinated solvents

• Organic acids

• Limited resealing

• Not suitable for 32 gauge syringe

Determining Your Quantity Needs

To determine potential septa ordering quantities, consider:

• the number of samples run during a day/week

• if samples are run in small or large batches

• if samples are run manually or with an autosampler

• if samples are run overnight, unattended

Vials

Unattended autosampler runs require a precise fit for uninterrupted operation.

Typically, automated sample runs use a higher quality and quantity of vials.

Description Quantity Part No.

Vials

2 mL Crimp top vial convenience pack with silver AI caps with

Teflon/Red rubber septa

2 mL Screw top vial convenience pack with blue screw caps and

Teflon/Red rubber septa

2 mL Snap top vial convenience pack with clear polypropylene snap caps and Teflon/Red rubber septa

100 µL Insert for wide opening vials

500/pk

500/pk

5181-3400

5182-0732

30 µL reservoir volume, High recovery vial, crimp top

500/pk

100/pk

5182-0547

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

100/pk 5182-3454

Price

$115

$183

$154

$ 88

$ 57

$158

$ 69

$109 www.agilent.com/chem • 800 227 9770 20

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringes

Syringe type and design are important for chromatography to ensure reproducible sample injections for consistent results.

The Agilent line of syringes include a variety of plunger and needle choices to use with your autosamplers.

Agilent syringes are designed:

• for reproducible sample volume delivery

• specifically for the Agilent inlet or autosampler

• to maximize inlet septum lifetime

Selecting Syringes

1. Select the syringe type based on the inlet (injection port) you are using and the volume of sample you want to inject.

2. Select a syringe. Refer to your automatic liquid sampler operating documentation for available syringe sizes and corresponding injection volumes.

3. Select the appropriate syringe needle gauge.

Needle Tip

Sharp tip

Needle Gauge Selection

Inlet

Packed, split or splitless (including PTV)

Cool on-column

Cool on-column

Cool on-column

Needle Gauge Column Type

23 gauge or 23/26 gauge tapered any

23/26 gauge tapered or 26 gauge 530 µm

26/32 gauge tapered

26/32 gauge tapered

320 µm

250 µm

Needle Shape

Needle tips

Cone tip

Tapered needle

Use syringe needles with an Agilent dualtaper needle or a conical tip. Sharp-tipped needles tend to tear the inlet septum and cause leaks. Also, a sharp-tipped needle tends to leave residual amounts of sample on the septum as it exits, resulting in a large solvent tail on the chromatogram.

21

TIPS AND TOOLS

For best results, use the Agilent Cone Tip (HP Point Style) with

Agilent’s Centerguide Septa, page 38. www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Characteristics and Recommended Uses

Syringe

5 µL, fitted plunger

Advantage Limitations Recommended Use

• Most accurate syringe for 1µL injection

• Thinnest plunger, • 1 µL injections can bend more easily

• Clean samples

• Routine analysis

• No hardware • Not ideal for higher modification needed viscosity samples for 0.5 µL injection • Plunger not replaceable

10 µL, fitted • Most economical plunger • Most reliable fitted plunger syringe

• Less bending

• Better for high viscosity samples

• Most accurate only • General purpose for 1 µL and larger syringe injections • Clean samples

• Plunger not replaceable

• Routine analysis

10 µL, gas-tight

• Replaceable plunger • More expensive • Dirty samples for reduced repair cost than fitted plunger • Gases and volatile

• Not available in samples

• Reactive samples • Less plunger binding 5 µL size than fitted plunger

• Tight seal between plunger and barrel

Replacing On-column Syringe Needles

The stainless steel needles used for

250-µm and 320-µm injections must be inserted into a glass syringe barrel.

Select the correct size needle for the column you plan to use.

To insert a needle into a syringe barrel:

1. Unscrew the syringe barrel cap and remove the spring.

2. Make sure the needle has the Teflon disk. If the syringe barrel does not have the Teflon disk, use the instructions in the syringe box to wrap the needle yourself.

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

4. Insert the needle into the syringe barrel.

5. Screw the cap back on the syringe barrel.

TIPS AND TOOLS

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

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

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Tips

• Make sure to input the proper syringe size when setting up the injection section of your data handling device.

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

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

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

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

• For on-column injections, always use the proper septum nut and stainless steel insert for the column dimension you are using. Use a septum with a molded through-hole with injections onto 0.32mm

and 0.25mm columns.

• The more polar the solvent, the more likely it is to contain water. Trace amounts of water, especially when combined with water-extractable materials from samples, can accelerate syringe wear dramatically. With these types of samples, use a Teflon tipped syringe plunger. Even better, proactively replace syringes, since plunger bends may be inevitable.

• Remove a gas-tight plunger from the syringe for long-term storage to keep the

Teflon tip leak-free. If a gas-tight plunger does not fit properly, place it in hot water for about 10 minutes then press the tip uniformly on a clean, hard surface and let cool to room temperature. The plunger should reseal correctly to provide 10-25% more injections.

• To maximize the lifetime of standard plungers, rinse the syringe and wipe the plunger with solvent (isopropanol or acetone) and a lint-free wipe, as specified in the syringe cleaning procedure included with each syringe.

NEW! Agilent Gold Standard

GC Autosampler Syringes

see page 25

23

VIDEO

To view a video on syringe installation, visit www.agilent.com/chem/techsupport. www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Troubleshooting Guide

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

Problem

Bent plungers or stuck syringes

Possible Cause(s)

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

Suggested Action(s)

• If the plunger’s movement feels “gritty,” remove the plunger from the barrel, flush the shaft with solvent, and wipe it dry with a lintfree cloth. Then, carefully insert the plunger back into the barrel. Finally, submerge the tip of the needle into a container of solvent, and cycle the plunger to pull the solvent into and out of the barrel.

• Never cycle the plunger in a dry syringe.

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

• Always clean syringes after use.

Bent needles

Blocked needles

• Improper needle alignment.

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

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

• If the needle has been slightly bent when mounted in the autosampler – or when the syringe is installed into the autosampler – then it is more likely to bend further when it pushes through the septa on the sample vial caps.

• Use only Agilent autosamplers. They are precision-designed to ensure proper alignment with the syringe needle.

• Use 23 to 26-gauge tapered needles to get the combined benefits of greater septa life and fewer bent needles.

• Only use Agilent vials and septa.

• Sample material or contaminants may be trapped inside the needle.

• The needle may not have been properly cleaned.

• Remove the plunger and use a second syringe to fill the blocked syringe with solvent. Then, insert the plunger and gently push solvent through needle. Important: Try to use a cleaning agent that is appropriate for the contaminant. Common choices are methanol, methylene chloride, acetonitrile, and acetone.

Rust

Note: even minor rust can cause the plunger to become stuck in the barrel.

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

• During normal use, the shaft rubs against the glass walls of the barrel. This gradually wears away the rust-resistant metal on the shaft’s surface.

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

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

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

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

3. Let syringe and plunger air dry.

• Skin oils and other organic material.

• Fine metal and glass particles from the syringe plunger and barrel may be rubbing together.

Once this happens, the plunger may bend if used further.

Loose plungers – accompanied by syringe leaks and area count reproducibility problems.

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

• Never touch the plunger shaft with your fingers.

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

• Replace the syringe.

Note: Plungers normally feel “loose” when non-polar solvents (like hexane and toluene) are used. www.agilent.com/chem • 800 227 9770 24

25

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Gold Standard GC Autosampler Syringes

Description Gauge/Length Quantity

Tapered Needle Syringes

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

10 µL

5 µL

Tapered

Tapered

Fixed Needle

Fixed Needle

23-26s/42

23-26s/42

Straight Needle Syringes

(use with Merlin Microseal)

10 µL

5 µL

Straight

Straight

Fixed Needle

Fixed Needle

23/42

23/42

6/pk

6/pk

6/pk

6/pk

Part No.

5181-3360

5181-8810

9301-0725

5182-0875

Price

$198

$303

$191

$292

GC Automatic Liquid Sampler Supplies

Description Unit Part No.

Miscellaneous Autosampler Supplies

4 mL Clear screw top wash vials with screw caps (no Septa)

Septa for 4 mL vial

Diffusion caps for 4 mL vials

4 mL wash vial with fill marking, caps

Screw for mounting syringe

Quadrant kit (4 tray sections)

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)

144/pk

144/pk

9301 0723

9301-1031

12/pk 07673-40180

25/pk 5182-0551

07673-20570

18596-40015

07673-60840

Price

$755

$ 64

$ 21

$ 19

$ 26

$ 13

$ 75

Gold Standard GC

ALS Syringe Features

Lot Numbers ensure certified performance to all specifications

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

Black ink and gold illuminating backdrop for easier viewing of the volume scale

Individually sealed packaging for contaminant-free use www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Packed-Column Inlets

Packed-column direct inlets are very popular. Packed-column analysis is frequently done when high efficiency separations are not needed or when gases are analyzed by gas-solid chromatography.

Packed-column inlets are simple in both design and use. Few parameters need to be set, and all carrier gas flow flushes through the inlet into the column in the standard configuration.

Packed-Column Inlet Procedures/Practices

Parameter Selection/Setting Rationale

Inlet temperature BP of solvent +50˚C

BP of major solute(s)

Ensures flash vaporization

Use for neat samples

Insert type 1/8-inch stainless steel

1/4-inch stainless steel

Use for ss column only

Inserts permit connection of columns up to 1/4-inch od.

Liner

Initial column temperature

Column type

Carrier gas flow

Glass Use to lower activity

(replaceable) temperature programming Sharpens peaks and reduces run time

1/8-inch packed stainless Will not break

1/4-inch packed glass Better for polar or labile compounds

20-40 mL/min

30-60 mL/min

Use with N

2 carrier gas

Use with He or

H

2 carrier gas

Troubleshooting

Most problems with packed-column inlets involve sample decomposition, flashback, or leaks.

Decomposition

Since packed-column inlets are active, especially if glass liners are not used, polar sample components will often tail or degrade in the inlet. Sample decomposition caused by the inlet is easily diagnosed; the decomposition products will have peaks at the same retention times as standards for the decomposition product.

When inlet-caused decomposition is suspected, try intracolumn direct injection, deactivated glass liners, or lower inlet temperatures, and remove any column packing in the inlet zone.

The inherent activity of packed-column inlets is somewhat mediated by the fact that they usually have low internal volume.

When this is coupled with the relatively fast flow rates used with packed columns, the residence time of sample in the inlet is short and decomposition is reduced in comparison to the decomposition that occurs with some capillary inlets (for example, splitless inlets).

Flashback

The negative side of low inlet volume, however, means that excessively large sample injections will easily exceed the capacity of the liner and will flash back into gas supply lines and onto the septum. This can cause several maladies, including ghost peaks, sample losses, irreproducible peak areas, and decomposition.

Leaks

Since packed-column inlets are usually flow-controlled, septum and column leaks will have a direct impact on retention times and peak areas. Sample can be lost through the leak holes, and air can diffuse back into the inlet to cause column degradation. Change the septum on a regular basis and check column connections at the first stage of problems.

To prevent stationary phase decomposition, make sure that the oven and inlet are at room temperature when not in use and when changing the septum.

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

27

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890/6850 Series GC Packed Port Supplies*

Item Description Unit Part No.

Price

1

2

3

4

5

9

10

11

Septum nut

Septa Bleed temperature, optimized, 11 mm

Top insert weldment

Viton O-rings

50/pk

12/pk

Glass liner, disposable 25/pk

Glass liner, disposable/deactivated 5/pk

6

7

Vespel/graphite ferrules, 1/4 in. id 10/pk

Tubing nut, 1/4 in. brass 10/pk

Adapters with glass liners

8 0.53 mm column adapter

1/8 in. column adapter

1/4 in. column adapter

Upper insulation

Nut warmer cup with insulation

Column nut for 0.53 mm column 2/pk

18740-60835

5183-4757

19243-80570

5080-8898

5080-8732

5181-3382

5080-8774

5180-4105

19244-80540

19243-80530

19243-80540

19243-00067

19234-60720

5181-8830

$ 37

$119

$ 99

$141

$ 5

$ 54

$ 25

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

* For Model 6890/6850 only

$ 67

$132

$ 12

$ 37

$ 14

$ 42

$ 13

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.

5890 Packed-Column Inlet Supplies

Description Unit

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

Adapters without glass liners

1/8 in. column adapter

1/4 in. column adapter

Universal Packed-Column Inlet (non-purged)

Septum retainer nut for headspace sampling, nonpurging

Brass nut, 1/4 in.

10/pk

9

10

11

5

6

7

8

1

2

3

4

Liner

Part No.

1/4 in. Vespel/ graphite ferrule

Price

19243-60570 $100

19243-80510

19243-80520

$ 88

$128

19243-60505

5180-4105

$ 70

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

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Split/Splitless Inlets

The combined “split/splitless” inlet is the most popular inlet for capillary column gas chromatography. Because it can be used in either split or splitless mode, it provides a very effective combination that can cover most analysis requirements.

Split Mode

Split injection is an effective way to introduce small amounts of sample without overloading the column. Split injection is required for samples that:

• cannot be diluted for analysis (for example, solvents)

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

• have important minor peaks eluting directly before the solvent peak (as in solvent analysis)

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

Troubleshooting

Split inlets are spared from most bandbroadening phenomena, since narrow peaks are generated as part of the splitting process. Therefore, any peak broadening or tailing observed with split injection is usually due to improper column installation, low split flow, (<20 mL/min on 6890) or low inlet temperature. If you suspect that the inlet temperature may be too low, increase it by 50˚C and compare the results to the lower temperature analysis. Repeat if results are positive until no further improvement is seen.

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

Split Mode Variables, Practices, and Rationales

Parameter Selection/Setting Rationale

Inlet temperature Try 250˚C or BP of last eluting compound

Inlet liner Large volume, deactivated

Ensures flash vaporization

Minimizes inlet discrimination

Minimizes flashback

Minimizes degradation

Inlet packing

Injection volume

Silanized glass wool

Glass beads or frit

None

0.5-3 µL liquid

0.10-10 mL gas

Injection technique Fast autoinjection

Split ratio

Hot-needle fast manual injection

50:1 to 500:1

Retains non-volatiles

Minimizes inlet discrimination

Less active than wool

Least active

Split easily adjusted

Split adjusted accordingly

Less needle discrimination

Reproducible discrimination

Not critical

Depends on sample and injection volume, and column ID

Narrow initial peaks Initial column temperatures

Septum purge 2-3 mL/min Minimizes ghosting

TIPS AND TOOLS

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

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

29

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Split Mode Variables, Practices, and Rationales

Inlet temperature

Inlet liner

Inlet packing

Just above highest boiling point of solutes (+20˚C)

Large volume >0.8mL

Small volume <0.2mL

None

Silanized glass wool

Ensures flash vaporization

Reduce if degradation occurs

Use higher for dirty samples and higher-boiling solutes

Use with autoinjector

Use only for slow manual injections, and gas injections

Use only with slow injection

Decreases degradation

Use for fast autoinjection

& dirty samples

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

& conditions

Injection technique Fast autoinjection Most reproducible

Less 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

Purge delay time

20-50 mL/min

20-80 sec

Higher if using constant flow

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 fast

Reduces backflash and decomposition

Septum purge

Quantification

2-3mL/min

Internal standard

Standard addition

Reduces ghosting

Maximizes reproducibility

Use only with constant injection volume

Retention gap 1-3m, deactivated

(1-2m per µL injected)

Reduces peak distortion

Promotes solvent and stationary phase focusing

Splitless Mode

For splitless injection, a conventional split injector is operated in a nonsplitting mode by closing the split valve during injection.

The sample is flash-vaporized in the liner, and sample vapors are carried into the column by the carrier gas where they are recondensed at temperatures below the boiling point of the solvent. After most of the sample has been transferred into the column, vapors remaining in the liner are cleared by opening the split vent which remains open for the duration of the run.

The most important benefit of splitless injection is that a majority of the injected sample is introduced into the column. This results in much higher sensitivity than that achieved using split injection.

Solvent Effect

One requirement of splitless injections is that the initial column temperature should be kept at least 10˚C below the boiling point of the sample solvent. This allows the sample solvent to condense at the front of the column trapping the solvent molecules into a tight, narrow band.

Additionally, use a solvent that is similar in polarity to the column stationary phase, and avoid mixed solvents. Breaking these rules 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 preparation requirements are significant, and it is not always possible or economically justifiable to clean up a sample extensively. So column protection becomes as important as sensitivity. Also, samples with trace quantities of important solutes that elute on the solvent tail may be focused by the solvent to yield more sensitive analyses.

VIDEO

To view a video on liner and gold seal replacement, visit

www.agilent.com/chem/techsupport.

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Troubleshooting

Most problems encountered with splitless injection are related to incorrect purge time, degradation, improper focusing, and flashback.

Appropriate initial column temperature is critical. Sample vapors can be lost through the septum purge line if the insert is overfilled with sample vapor (either too large injection volume or too small liner volume), leading to irreproducibility and nonlinearity of peak areas. Match inlet temperature, liner volume, and injection volume carefully to avoid backflash.

Decomposition

Loss of peak area or generation of new peaks, can sometimes be dramatically reduced by changing liner type or by deactivating the liner and inlet with silanizing reagents. Removing or reducing the amount of liner packing can also decrease inlet activity.

6

7

8

9

10

4

5

1

2

3

6890/6850 Split/Splitless Inlet Supplies*

Item Description Unit Part No.

Price

6

7

4

5

1

2

3

8

9

10

11

12

13

14

Septum retainer nut

Septa

Insert Weldment

Liner O-ring

Liner

Split vent trap assembly (6890/6850 only)

Retaining nut (6890/6850 only)

Retaining nut (5890 only)

SS seal

Gold-plated seal

Washer, 0.375 in. od

Reducing nut

Insulation (requires 3)

Lower insulation cover

Ferrule

Column nut (6890/5890 only)

Column nut (6850 only)

12/pk

2/pk

2/pk

Angled wrench for split/splitless inlet

18740-60835

See page 36

G1544-60575

See page 52

See page 47

G1544-80550

G1544-20590

19251-20620

18740-20880

18740-20885

5061-5869

18740-20800

19243-00067

19243-00070

5181-8830

5183-4732

19251-00100

$ 39

$216

$128

$ 26

$ 31

$ 26

$ 33

$ 8

$ 34

$ 5

$ 15

$ 26

$ 47

$ 29

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

11

12

13

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

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).

30

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Cool On-Column Inlets

Cool on-column injection is superior in many ways to other sample introduction techniques.

Advantages:

• elimination of sample discrimination

• elimination of sample alteration

• solvent focusing of early eluting solutes

• high analytical precision

If done properly, cool on-column injection provides the most accurate and precise results of the available inlets. Syringe discrimination is completely eliminated.

Moreover, inlet-related discrimination does not occur, since the liquid is introduced directly into the column. Automated oncolumn injection provides even higher analytical precision. Add to this the elimination of thermal decomposition and rearrangement reactions, and it becomes apparent that cool on-column injection should be considered whenever high precision and accurate results are required.

Limitations:

• maximum sample volumes are smaller compared with other inlets (0.5 µL to 2.0 µL)

• solute peaks eluting just before the solvent cannot be focused and are difficult to determine

• capillary columns (especially those with a large phase ratio or small inner diameter) can be easily overloaded with sample

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

Cool On-Column Inlet Procedures/Practices

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

Injection volume 0.1-2.0 µL liquid

Simple and effective

Narrows initial peak width

Use smaller injections for small id columns;

Depends on column capacity

Injection technique

Oven temperature

Column flow

Septum purge

Quantification

Fast autoinjection

Fused silica needle

Inlet temperature or slightly lower

50-80cm/sec

30-50cm/sec

12-15mL/min

All methods

Projects droplets away from syringe tip

Use for manual injection into small id columns

Prevents backflash

Use for H

2 carrier gas

Use for He carrier gas

Use if installed to prevent ghosting

Retention gap requirements 1-3m, deactivated

Inherently reproducible technique

Lack of discrimination

Corrects peak distortion

Protects column from non-volatile components

Permits autoinjection with narrow-bore columns

31

TIPS AND TOOLS

Since the sample is directly deposited into the column, nonvolatile sample components can accumulate at the head of the column and will degrade efficiency and/or interact with subsequent injections.

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Considerations

Sample 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 column temperature 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 the analytical column.

Troubleshooting

The major problems found with cool oncolumn injection are associated with column overload, solvent/stationary phase incompatibility, and column contamination.

If the flooded zone after injection is too long (large injections, poor wettability), peaks will be broad or split. A retention gap usually will resolve this problem. Loss of column efficiency with on-column injection usually is caused by contamination or degradation of the stationary phase at the head of the column. Only columns with an immobilized stationary phase should be used with cool on-column injection to prevent displacement of the stationary phase by solvents.

Immobilized stationary phases can be washed to remove contaminants and renew performance. If column performance does not improve after washing, cut 0.5m

off the inlet side of the column. If that does not return column performance, the column must be replaced and a retention gap should be used for all further injections of dirty samples.

Column/Retention Gap Installation Consumables

Description

Column nut

250 µm graphite/Vespel ferrule

320 µm 0.5 mm graphite/Vespel ferrule

250 µm retention gap (one 5 m piece)

320 µm retention gap (one 5 m piece)

530 µm retention gap (one 5 m piece)

Quartz deactivated column connector fits 0.18-0.53 mm

Unit

2/pk

10/pk

10/pk

5/pk

Part No.

5181-8830

5181-3323

5062-3514

160-2255-5

160-2325-5

160-2535-5

5181-3396

Price

$ 26

$ 55

$ 51

$ 39

$ 42

$ 59

$ 94

TIPS AND TOOLS

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

www.agilent.com/chem • 800 227 9770

VIDEO

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

32

33

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 Series Cool On-Column Inlet Supplies*

Item Description

Manual injection

1c Cooling tower assembly

1d Duckbill septum

Fused silica syringe needles

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

Common Supplies

3 Spring

Unit

10/pk

6/pk

Part No.

19320-80625

19245-40050

19091-63000

9301-0658

Price

$175

$ 29

$ 41

$ 90

19245-60760 $ 9

4 Inserts for capillary columns

For 200 µm columns (one ring)

For 250 µm columns (six rings)

For 320 µm columns (five rings)

For 530 µm columns (no rings)

19245-20510 $ 89

19245-20515 $114

19245-20525 $ 78

19245-20580 $ 55

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

5 Ferrule 5080-8853

6 Column nut 2/pk 5181-8830

$ 47

$ 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

2 Advanced green 5 mm through hole septa

BTO 5 mm through hole septa

50/pk

50/pk

G1545-80520

5183-4760

5183-4758

$ 63

$ 62

$ 72

5890 Series Cool On-Column Inlet Supplies

Automatic Injection

1a Septum nut (5890 Series II GC)

1b Needle guide (for 7673A only)

19245-80520

19245-20670

$ 91

$ 35

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

1a

1b

1d

1c

2

3

4

5

6 www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Programmed Temperature Vaporizer (PTV) Inlets

PTV inlets combine the benefits of split, splitless and on-column inlets. The sample is usually injected into a cool liner, so syringe needle discrimination does not occur. Then the inlet temperature is increased to vaporize the sample. The user programs vent times and temperature to achieve the equivalent of split or splitless transfer of sample vapors to the column. PTV injection is considered the most universal sample introduction system because 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 boiling components

• trapping of nonvolatile components in liner

• split or splitless operation

• retention time and area reproducibility approaching cool on-column injection

PTV inlets are actively cooled before and during injection by Peltier devices or by forced gases (air, liquid N

2

, or liquid CO

2

).

Cryogenic cooling of the inlet can reduce inlet temperature enough to thermally focus gas injections from other sampling devices in the liner. This is a distinct advantage of using PTV inlets in comparison to conventional inlets for coupling auxiliary sampling devices to capillary columns.

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

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

Parameter Selection/Setting Rationale

Injection mode Cold split

Cold splitless

For general use and sample screening

For trace analysis

Inlet temperature ramp rate

Adjustable (i.e., 2˚C/sec to 12˚C/sec)

Ballistic

Use slower ramp rates for labile, complex, or large volume samples

Use faster ramp rates for most samples

Use faster ramp rates to shorten splitless purge delay time

Simpler, less expensive instrumentation

Inlet liner

Injection volume

Sample Injection technique

Oven temperature

Straight with silanized wool For general use

Baffled For labile samples

Packed with an adsorbent For focusing gaseous injections from auxiliary sampling devices

0.1-1.5µL Use lower volumes for volatile solvents and fast ramp rates

Use volumes larger than

1.5µL only in solvent- elimination mode

Autosampler or manual, fast or slow

Not critical for cold split

& splitless modes

10-25˚C below solvent BP

Column flow

Sample dependent

30-50 cm/sec

For proper solvent effect in splitless mode

For split mode

Clears inlet faster

Less backflash

Septum purge

Quantification

Retention gap

1-5mL/min

Any method

1-3m, deactivated

Minimizes ghosting

Inherently reproducible

Low discrimination in cold injection modes

Compensates for extended flooded zone and solventcolumn incompatibility

VIDEO

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

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

35

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 PTV Inlet

Item Description

3

4

5

1

2

6

7

8

9

10

11

Septumless head

Septum head

Septum nut

PTV inlet assy

PTV LCO

2 cooling jacket

PTV LN

2 cooling jacket

Silver seal

Column ID Unit Part No.

G2617-60507

G2618-80500

18740-60835

G2617-60506

G2617-60508

G2619-60501

5182-9763

Ferrules for

Graphpak inlet

5/pk

Graphpak inlet adapter 0.20 mm

0.25-0.33 mm

0.53 mm

5182-9754

5182-9761

5182-9762

0.20 mm 10/pk 5182-9756

0.25 mm 10/pk 5182-9768

0.32 mm 10/pk 5182-9769

Split nut for inlet adapters

0.53 mm 10/pk 5182-9770

5062-3525

PTV insulation block

PTV cryo insulator (not shown)

G2617-20510

G2617-60510

Teflon ferrule (needle seal)

Kalrez seal

Valve body

Pressure spring

Viton seal

Sealing element

CO

2

Cryo inline filter

Service kit for septumless head contains Kalrez seal, valve body, and pressure spring

Graphpak 3D ferrules

Installation tool for 3D ferrules

5/pk

5182-9748

5182-9759

5182-9757

5182-9758

5182-9775

5182-9760

3150-0602

5182-9747

5182-9749

G2617-80540

Price

$ 166

$ 146

$ 159

$ 61

$ 53

$ 137

$ 110

$ 91

$ 6

$ 24

$ 73

$ 137

$ 224

$2661

$1078

$ 39

$4850

$ 544

$ 473

$ 62

$ 173

$ 152

$ 146

$ 158

$ 166

$ 143

$ 208

1

3

2

4

5, 6

7

8

9

10

11

There are few choices in liner design for PTV inlets.

However, liner volume and activity are still key issues to be considered when selecting among the few available PTV liners. PTV liners require packing or a modified surface to hold the liquid sample in place before and during the vaporizing process.

PTV Liners

Description

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

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

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

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

Part No.

5183-2038

5183-2036

5183-2037

5183-2041

Price

$ 25

$ 20

$ 29

$ 55 www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa

One of the key components of sample introduction is the inlet septum. All columns must have carrier gas head pressure to establish flow through the column. Septa maintain the leak-free seal and exclude air from the inlet. They come in many different sizes and are made from many different types of material specific to inlet type and analysis needs.

Septa are usually available according to their recommended upper temperature limits. Lower temperature septa are usually softer, seal better, and can withstand more punctures (injections) than their high-temperature counterparts.

If used above their recommended temperatures, however, they can leak or decompose. This causes sample losses, lower column flow, decreased column life and ghosting.

What is the Function

The septum isolates the sample flow path from the outside world. It must provide a barrier that is readily penetrated by the injector needle while maintaining internal pressure without contaminating the analysis. They are generally made of special high-temperature, low-bleed silicone rubber formulations.

Why Replace

Septa should be replaced regularly to avoid:

• leaks

• decomposition

• sample loss

• reduced column or split vent flow

• ghost peaks

• column degradation

How to Minimize Problems

Avoid problems by:

• using within the recommended temperature range

• changing regularly

• installing “hand tight”

• using septum purge when available

• using autoinjectors

• using sharp syringe needles

Agilent Introduces Innovative

Packaging for Inlet Septa

Agilent has recently introduced a new and innovative packaging design for inlet septa. This new packaging is a tri-fold blister pack that provides cleanliness, convenience, and consistency 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 new packaging is that each septum is individually packaged for the ultimate cleanliness. Each septum is easily dispensed one at a time by pushing it through the back foil, as is commonly done with pharmaceutical capsules and tablets. No longer do you need to reach into a jar and wonder how clean the septa are or if you are contaminating other septa.

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

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

• Easy to see exactly how many are left: Know exactly when to reorder

• Compact storage size: Fits easily into drawers

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

• High quality PET packaging: Tested by

GC-FID, GC/MS, and GC-ECD to ensure the absence of interfering background peaks www.agilent.com/chem • 800 227 9770 36

37

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Troubleshooting

Symptom

Extra Peaks/Humps

Possible Cause

Septum bleed.

Remedy

Turn off injector heater. If extra peaks disappear, clean the inlet and change the liner. If cored septa particles are present, use a centerguide septa and a 23-26 gauge tapered syringe. Important: always use the septum specified for higher temperature or analyze at lower inlet temperature.

Normal Problem

Baseline Change After Large Peak

Large leak at septum during injection and for a short time thereafter (common with large diameter needles).

Replace septum and use smaller diameter needles.

Normal Problem Problem

(flow increase) (flow decrease)

Retention Times Prolonged

Carrier gas leaks at septum or column connection.

Check for leaks. Replace septum or tighten connections if necessary.

Normal Problem Problem

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

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Premium Non-Stick Septa

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

• Proprietary plasma treatment ensures non-stick septa without the use of potentially damaging talcum powder

• Center point guides the needle for easy penetration and less coring

• Reduce needle bending

• Precision molding assures accurate fit in the inlet

• Each batch tested on an Agilent 6890 GC-FID for bleed

Agilent’s plasma-treated non-stick septa

Introducing Agilent Premium Non-Stick Septa – featuring a proprietary plasma coating that won’t stick or clump.

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

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

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

Competitor “non-stick” septa www.agilent.com/chem • 800 227 9770 38

39

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

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

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 septum to guide the syringe needle into the inlet.

With the dimpled CenterGuide, the syringe needle enters the septum 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 the bottom 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 failure with HP Point syringes. The HP Point syringe yields optimal performance and reliability and reduces coring by parting, not cutting, 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.

Figure 1. Comparison of Coring, With and Without CenterGuide

(30x magnification)

High-Temperature Septa Without CenterGuide: Major Coring Before 1

00 Autoinjections

1 autoinjection 100 autoinjections 700 autoinjections

Agilent BTO Septa With CenterGuide: Very Little Coring Even After

700 Autoinjections

Summary of Inlet Septum Characteristics

SEPTUM TYPE

BTO

(Bleed and

Optimized)

Long Life

Advanced Green

✔✔✔ = best

BLEED

✔✔✔

(optimized for

LIFETIME

TEMPERATURE

LIMIT to 400ºC

✔✔

✔✔✔

✔✔

✔✔ = very good ✔ = good to 350ºC to 350ºC www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

p/n 5183-4757

Agilent Bleed and Temperature

Optimized Non-Stick Septa (BTO)

• Extended temperature range, low-bleed

• Maximum Injection Port Temperature

400ºC

• Virtually eliminates injection-port sticking

• Pre-conditioned; packaged in glass to prevent contamination

• Ideal for use with low-bleed,

“Mass Spec” capillary columns p/n 5183-4761

Agilent Long-Life Non-Stick Septa

• Pre-pierced for extended life and reduced coring

• The preferred Septum for Autosamplers

• Ideal for Overnight Runs

• Up to 400 Injections Per Septum injection

• Maximum Injection Port Temperature

350ºC

• Soft, 45 Durometer, Easy On

Autosampler Needles p/n 5183-4759

Agilent Advance Green

Non-Stick Septa

• True Long-Life, High Temperature

Green Septum

• More Injections per Septum

• Reduced Injection Port Sticking

• Maximum Injection Port Temperature

350ºC

• Packaged in glass vials for high purity

• Economical alternative to competitor’s

“Green” Septa

General Purpose Septa

Agilent’s General Purpose Septa are made from an enhanced injection-molded silicone rubber material. The septa material, dark red or gray in color, is specified to withstand over 200 automatic injections at an injection port temperature of

350ºC. You can have confidence in your chromatographic results knowing that each lot of septa is placed through a demanding QC test to ensure that only the highest quality product is delivered to your laboratory.

Agilent’s General Purpose red/gray septa are cost-effective choices which provide:

• Low bleed for reduced instrument maintenance downtime and increased laboratory productivity

• Less frequent replacement for long lifetime and the ability to withstand more than 200 autosampler injections at maximum injection port temperatures

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

• Convenient blister packs of 50 or 100 septa minimize risk of contamination and need for reconditioning www.agilent.com/chem • 800 227 9770 40

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Ordering Information

Premium Non-Stick Septa

Agilent Bleed and Temperature Optimized Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)

11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)

5 mm septa through-hole for on-column in glass jar (50/pk)

Agilent Advanced Green Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)

11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)

5 mm septa through-hole for on-column in glass jar (50/pk)

Agilent Long-Life Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)

11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)

5 mm septa through-hole for on-column in glass jar (50/pk)

General Purpose Septa

Gray Septa

11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk)

11 mm for 5880, 5890, 6850 and 6890 GCs (100/pk)

9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)

9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)

Red Septa

11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk)

11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk)

11 mm with partial through-hole for 5880, 5890, (50/pk)

6850 and 6890 GCs

11 mm with partial through-hole for 5880, 5890, (100/pk)

6850 and 6890 GCs

9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)

9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)

5 mm through-hole for on-column inlets, (25/pk) automatic or manual injections*

5 mm solid for high column backpressure, on-column inlets* (25/pk)

* 5 mm septa are packaged in glass jars

41

EASY ONLINE ORDERING

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

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

Part No.

5183-4757

5183-4757-100

5183-4758

5183-4759

5183-4759-100

5183-4760

5183-4761

5183-4761-100

5183-4762

5080-8896-50

5080-8894-100

$52

$93

5080-8728-50 $52

5080-8728-100 $93

5181-1263-50

5181-1263-100

$52

$93

5181-3383-50 $52

5181-3383-100 $93

5181-1283-50

5181-1283-100

$52

$93

5181-1260 $29

5181-1261 $29

Price

$72

$134

$72

$62

$107

$62

$84

$150

$84 www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrules

Using the wrong ferrule or a worn-out ferrule to seal your column connection can result in inconsistent and unreliable chromatography. An improper ferrule can cause leaks which allow air and other contaminants to enter the instrument through the column seal, causing major interference with column and detector performance. For optimum performance, ferrules should be replaced every time the column is replaced and when performing column maintenance.

Agilent offers a comprehensive selection of ferrules made of different materials and configurations for a leak-free connection between the column and injector.

Three main types of ferrules are used with capillary GC columns: graphite, Vespel and

Vespel-graphite composites. Graphite ferrules can withstand temperatures as high as 450ºC, and Vespel and Vespelgraphite ferrules are rated to 280ºC and

350ºC, respectively.

What is the Function

Ferrules seal the connection of the column or liner to the system. The ideal ferrule provides a leak-free seal, accommodates various column outer diameters, seals with minimum torque, will not stick to the column or fittings, and will tolerate temperature cycling.

Why Replace

Signals that a ferrule is damaged include:

• background noise from oxygen diffusing into the system

• column bleed catalyzed by oxygen

• sample degradation

• loss of sample

• increase in detector signal/noise

• poor retention time reproducibility

Column Ferrule Types

Advantages Limitations

Graphite Easy-to-use, stable seal

Higher temperature limit

Vespel or Mechanically robust

Vespel-graphite Long lifetime

Soft, easily deformed or destroyed

• possible system contamination

• not for use with GC/MS transfer-lines

Flows at elevated temperature

• must retighten frequently

• prone to leakage

Polymer bleed problematic with some detectors (NPD and ECD)

How to Minimize Problems

General 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 before reusing them

• change ferrules when new columns or injector/detector parts are installed www.agilent.com/chem • 800 227 9770 42

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Troubleshooting

Problems possible after changing ferrules

Normal Peaks Tailing Solvent Peaks

Normal Peaks Tailing Solvent Peaks

Wrong Peak Ratios

Wrong Peak Ratios

Correct column positioning in both injection port and FID

Column positioned incorrectly in the injection port, or possible ferrule or septum particle in the carrier gas flow path

Column positioned incorrectly in the inlet

(either too far or not far enough; verify

4-6mm installation distance)

100% Graphite Ferrules

Reusing a ferrule – or using off-brand ferrules – may be a costly mistake. That’s because you’ll increase the likelihood of dangerous leaks that can damage the GC column and sensitive detector parts.

For best results, always use new Agilent ferrules, which feature the highest quality design, and are supported by decades of technical expertise.

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

• The universal column nut (p/n 5181-

8830) has a hexagonal head requiring the use 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) does not require a wrench to tighten.

It can only be used with the 100% graphite ferrules.

43

TIPS AND TOOLS

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

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Vespel/Graphite

(85%/15%) Ferrules

The combination of graphite and Vespel results in a ferrule having low oxygen diffusion rates which does not shrink to the same extent as pure Vespel. These ferrules are recommended for use with

GC/MS or other oxygen sensitive detectors, like the ECD, but are also compatible with other detectors like FID and NPDs.

In addition, the Vespel/graphite ferrules provide added confidence of leak-free connections when installed correctly.

Proper installation requires a finger-tight turn on the nut, then an additional 1/

4 –

1/

2 turn with a wrench.

These ferrules are very hard and cannot be deformed sufficiently to seal multiple column diameters. The ferrule hole must match the column OD exactly to ensure a leak-free seal. For capillary column applications, there is a specific ferrule for each column diameter. Choosing a ferrule with a larger hole than is specified for a given column dimension can result in a large leak. If left unchecked, an improper seal at the injector will result in high column bleed and a shortened column lifetime. An improper seal at the detector can result in increased detector signal/noise. In the case of the MSD it can also contribute to oxidation of the ion source which can increase the frequency of detector maintenance.

Two different lengths of Vespel/graphite ferrules are available for capillary column use. The standard sized ferrule is compatible with the universal column nut.

The second ferrule size is slightly longer and is specifically designed to fit with the

MS interface nut used for the GC/MS transfer line connection. The larger ferrule can also be used to make column connections to inlets and other detectors but requires a specially designed column nut (p/n 05988-20066) to accommodate the longer ferrule.

When using Vespel/graphite ferrules,

Agilent recommends tightening the column nut to a 1/

4 turn after the first temperature program runs. Even preconditioned ferrules can exhibit some shrinkage after a temperature 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) www.agilent.com/chem • 800 227 9770 44

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

100% Vespel Ferrules

Vespel is a high-temperature polyimide based material which is very hard. This material has the lowest permeability to oxygen, making it an excellent sealing material when making metal or glass connections. These ferrules do not deform easily. So, it is important to match the ferrule hole size to the proper column diameter.

The main disadvantage of 100% Vespel ferrules is the shrinkage of the material when exposed to temperature cycling conditions. 100% Vespel ferrules should only be used for isothermal applications.

VIDEO

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

45

Agilent Ferrule Selection Recommendations

Ferrule/Seal

Type

Upper Usages

Temperature

Limit

Limitations

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------

Graphite 450ºC General purpose Not for MS or

(100%) for capillary columns.

Suitable for FID and NPD. oxygen sensitive 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 leak-free connection.

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------

Vespel

(100%)

280ºC

MS or oxygen sensitive detectors. Most reliable

Isothermal operation.

Leaks after temperature cycle.

------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------

SilTite N/A Use only with SilTite Nut Kits Not Reusable

(100% metal) www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Ordering Information

Ferrule Id

(mm)

General Purpose Graphite Ferrules (Short Ferrules)

0.5

1.0

0.4

0.8

Column Id

(mm)

Quantity

0.1, 0.2, 0.25, 0.32

10/pk

0.53

0.05-0.25

0.45, 0.53

10/pk

10/pk

10/pk

85% Vespel, 15% Graphite Ferrules (Short Ferrules)

0.80.3

0.80.4

0.80.5

0.80.8

0.1, 0.2

0.1, 0.2, 0.25

0.32

0.45, 0.53

Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)

0.3

0.4

0.5

0.8

0.1

0.1, 0.2, 0.25

0.32

0.53

These ferrules are recommended for use with GC/MS.

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

100% Vespel High-Performance Ferrules (Short Ferrules)

0.4

0.5

0.8

These ferrules are recommended for use in isothermal analysis only.

Specialty Ferrules, 85% Vespel, 15% Graphite

Two Hole 0.4 ID holes

0.5 ID holes

No Hole

SilTite Metal Ferrules

For use with 0.20-0.25 mm ID capillary columns. Includes 2 column nuts

For use with 0.32 mm ID capillary columns. Includes 2 column nuts

For use with 1/16 in. od

SS tubing. Includes 2 column nuts

For use with 0.53 mm ID capillary columns.

Includes 2 nuts

Column Nuts

Short Nuts

Universal column nut, 1/16 in. hex

Finger-tight column nut for 0.53 mm columns*

Finger-tight column nut for 0.32 mm columns* and smaller

Blanking plug, finger-tight style

6850 Column Nut

Long Nuts

MS interface column nut

Column nut for GC/MS ferrules

Column nut wrench, 1 /4 in. and 5 /16 in.

* For use with graphite ferrules only.

Always match short nuts with short ferrules and long nuts with long ferrules.

0.1, 0.2, 0.25

0.32

0.45, 0.53

0.1, 0.2, 0.25

0.32

0.4

0.5

0.8

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

10/pk

2/pk

1 ea

1 ea

1 ea

2/pk

1 ea

1 ea

1 ea www.agilent.com/chem • 800 227 9770a

Part No.

5080-8853

5080-8773

500-2114

500-2118

5062-3516

5181-3323

5062-3514

5062-3512

5062-3507

5062-3508

5062-3506

5062-3538

5181-3322

5062-3513

5062-3511

5062-3580

5062-3581

5181-3308

5184-3569

5184-3570

5184-3571

5188-2789

5181-8830

5020-8293

5020-8292

5020-8294

5183-4732

05988-20066

05921-21170

8710-0510

Price

$ 47

$ 38

$ 26

$ 26

$ 51

$ 55

$ 51

$ 53

$ 62

$ 62

$ 56

$ 48

$ 55

$ 51

$ 51

$ 79

$ 79

$ 47

$ 87

$ 87

$ 85

$135

$ 26

$ 18

$ 18

$ 12

$ 47

$ 13

$ 16

$ 24

46

47

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liners

Agilent offers a complete selection of

GC split and splitless inlet liners that deliver consistent quality. So you can get consistent results.

And unlike other manufacturer’s liners,

Agilent liners are built to Agilent’s precise inlet tolerances which helps ensure optimal dimensional accuracy and inertness toward demanding compounds.

Choosing the proper liner for a specific application 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 inlet or sample vaporization

What is the Function

Liners are the centerpiece of the inlet system in which the sample is evaporated and brought into the gas phase.

Why Replace

These problems will occur if the liner is not changed on a regular basis or if the correct liner is not used:

• peak shape degradation

• solute discrimination

• poor reproducibility

• sample decomposition

• ghost peaks

• reduced column life

How to Minimize Problems

Change liners on a regular basis determined by:

• previous use pattern

• sample cleanliness

• chromatographic abnormalities such as:

– peak shape changes

– peak discrimination

– poor reproducibility

– sample pyrolysis

– active analyte response loss or decomposition

VIDEO

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

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Discussion of Liner

Characteristics

Liner Volume

The purpose of the injection port is to allow the introduction of a sample into the gas chromatograph in an accurate, reproducible manner. The vaporized sample should be a true representation of the liquid sample and, unless specifically desired, should be injected without chemical change. The elevated temperatures used in the inlet vaporize the liquid sample to a gas for transfer to the head of the column. This phase transition is accompanied by a very significant volume change. The volume of the resulting vapor must be small enough to fit within the volume of the liner. If the volume is too great for the liner, it could result in backflash, or sample loss caused by expansion into the septum purge or split vent lines. Both can compromise reproducibility and sensitivity. Backflash also frequently results in sample carryover.

Larger volume liners (> 800 µL) are characterized by larger inside diameters

(ID) and are typically used with injection sizes of 1 µL or more. The small volume liners have a smaller ID and are usually used with small injection sizes (< 1 µL), fast 100 µm ID columns, gas samples, or when using external sampling devices like headspace and purge and trap.

Liner Deactivation

Active sites on inlet liners can adsorb sample components and cause peak tailing, and potential loss of sensitivity and reproducibility. Deactivation agents are used to cover or react with active sites on the glass surface of the liner. Agilent liners are deactivated using deactivation procedures that produce reproducible and inert liners, with long lifetimes. For splitless applications or when even slightly polar compounds must be analyzed, a deactivated liner should be used.

With use, even deactivated liners can begin to exhibit activity. When this occurs, the liner should be replaced. Liners can be cleaned to remove particulate material or solvent rinsed to remove less volatile components. However, choosing the proper liner cleaning procedure can be difficult. Some solvents may remove the deactivation layer, and tools might scratch the glass surface of the liner, resulting in the generation of unwanted active sites.

A new liner almost always outperforms a cleaned and re-deactivated one – especially for trace analysis.

www.agilent.com/chem • 800 227 9770

TIPS AND TOOLS

Agilent offers a free software tool that calculates the vapor volume of an extended list of common solvents, based on your choice of inlet temperatures and pressures for a given

Agilent inlet liner. To download, go to www.agilent.com/chem/techsupport. Click “User

Contributed Software;” then, click “GC Pressure/Flow Calculator.”

48

49

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Design Features

Dimensions

• The outside diameter (OD) of the liner determines if the liner is more effectively used in split or splitless mode

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

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

• Agilent splitless liners are all designed with exacting dimensional tolerances to fit tightly in the inlet and minimize sample contact with metal surfaces

• Smaller OD liners are designed for split injection because they produce less resistance to carrier and split flow through the inlet

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

Tapers

Tapering or narrowing the liner internal diameter (ID) is done for a number of purposes:

• Bottom taper focuses sample onto the head of the column

• Bottom taper minimizes contact with metal parts of the inlet

• Center taper positions glass wool correctly

• Top taper minimizes sample backflash

To operate properly, the column must be installed correctly in the injection port with the tip of the column ideally located about halfway into the taper, or about 4-6 mm from the column tip to the top of the ferrule

(See Figure 1). Some applications will work better with different column installation depths. Therefore, you should check the instrument manual for proper installation distances and determine which distance is appropriate for your application.

Reproducible positioning is important for repeatable quantitative results.

Packing

Glass Wool

Many liner designs use deactivated glass wool packing. The glass wool is positioned or held in place near the center of the liner to:

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

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

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

Glass wool liners that have glass wool near the center of the liner, such as Agilent Part

Nos. 5183-4647 and 5183-4711, are recommended for automatic injections.

If glass wool is positioned at the bottom of the liner, its main purpose is simply to trap non-volatile components. Glass wool is generally not recommended for the following analytes:

• phenols

• organic acids

• pesticides

• amines

• drugs of abuse

• reactive polar compounds

• thermally labile compounds

Glass Cups

Another design feature used to help volatilize the sample and provide good mixing is the incorporation of a glass cup inside the liner. Glass cup liners are also available with additional glass wool and inert packing to increase reproducibility and limit sample discrimination. Not recommended for use with Electronic

Pressure Control Inlets on 6890 or 6850 GCs.

Figure 1.

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Troubleshooting

Symptom

Tailing Peaks

Normal Problem

Baseline Rise Before or After Peak

Possible Cause

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

Needle hitting and breaking packing in inlet liner.

Column end poorly cut

(sample absorption).

Broken or chipped inlet liner.

Inlet flow too low.

Sample decomposing.

Remedy

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

Partially remove packing from liner or use without packing.

Remove column. Make a clean, square cut using a reliable capillary fused silica cutting tool (such as a ceramic wafer or the Agilent Column Cutter), then reinstall column.

Make sure total flow in inlet is above

40 mL/min.

Remove inlet liner and check cleanliness.

Use new, deactivated liner or replace glass wool and packing. Column/sample residues could also be the problem.

Normal Problem Problem

Baseline Change After Large Peak Column and inlet liner misaligned.

See also”Septum Troubleshooting,” page 37

Check installation of column end and inlet liner; adjust if necessary.

Normal Problem Problem

Unresolved Peaks Column or inlet liner contaminated or column deteriorating.

Use a guard column to prolong column life.

Remove inlet liner and check cleanliness.

Use new, deactivated liner or replace glass wool and packing. Trim the front end of the column a minimum of 6 inches.

Normal Problem Problem www.agilent.com/chem • 800 227 9770 50

51

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Agilent Liners

Our engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Intensive liner development 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 with glass wool, bottom taper, glass bead for easy positioning, and deactivated, Agilent

Part No. 5183-4647 (with extraordinarily tight dimensional control for optimum split performance).

Splitless injection:

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

Note: For pesticide analysis – especially

DDT and Endrin, where breakdown is a problem – we recommend Agilent Part

Nos. 5181-3316EN and 5181-3315EN.

General purpose split/ splitless injection:

Similar design to Agilent Part No. 5183-

4647, but with an outer diameter that compromises for both split and splitless injections, Agilent Part No. 5183-4711.

Direct injection:

Straight liner without glass wool, deactivated, Agilent Part No. 5181-8818

(use only for gas samples, headspace, or purge and trap applications).

Direct Connect

Direct Connect liners are ideal for customers running highly sensitive compounds, or for users who require maximum inertness performance and minimal inlet discrimination for trace GC and GC/MS applications. Direct Connect liners also eliminate sample exposure to metal parts, minimizing inlet-related degradation. These liners are included in our new 8270 EPA Applications kit designed specifically for optimizing a

6890/5973 GC/MSD to this method.

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

Focus Liner

Improve reproducibility, improve results.

The Focus Liner traps a precisely controlled amount of glass wool in the ideal position in the injection port liner. At the point of injection, the glass wool provides extra surface area for vaporization, traps nonvolatile sample residue, and wipes any residual sample from the sample needle – reproducibility is the result.

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

Liner O-Rings

Liners are sealed in the inlet with O-rings or graphite seals. O-ring seals are easier to remove and to replace than graphite that deforms and flakes apart. The graphite seals should be used when inlet temperatures exceed 350ºC.

www.agilent.com/chem • 800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Flip Top Inlet Sealing System

Agilent’s NEW Flip Top Inlet Sealing System is the faster, smarter way to change inlet liners on Agilent GC’s

• Cuts liner replacement time to as little as 30 seconds

• 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/MS system is changing the inlet liners. A hot inlet may have to be opened on each system every

24 to 48 hours to change a dirty inlet liner. The special wrench used for this operation is often misplaced, bent at an odd angle, too thin, or simply awkward to use. In addition, the inlet nut is usually too hot to handle so it must be turned several times with the wrench before it will release the top assembly of the injection port.

Once the dirty liner is replaced, the inlet nut must be replaced on the injection port and occasionally the wrench slips off the nut leading to scrapes, burns, and cuts. It can take at least 5 minutes of wrestling with this hot injection port nut and wrench combination just to take out the old liner and put in a new one. By the time the operator finishes the procedure and 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 the capillary column, through the hot MS interface, and into the heated source resulting in multiple problems 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 safely and reliably change an inlet liner in as little as 30 seconds without tools in a consistent leakfree manner. No longer will you have to contend with frustrating searches for wrenches or burning your fingers on hot inlets.

Available exclusively from Agilent, the Flip Top has a levered arm that attaches to any

6890/6850/5890 insert weldment and locks to the injection port using an adapter ring screwed onto the inlet. Once installed, the user simply lifts the arm of the Flip Top which releases the insert weldment from the injection port, and allows instant access to the liner.

The process is simply reversed to re-seal the weldment to the port.

Description

Flip Top Inlet Sealing System

Liner O-rings (10/pk) www.agilent.com/chem • 800 227 9770

Part No.

5188-2717

5188-2741

Price

$514

$19

VIDEO

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

52

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Ordering Information

Application Liner Single

Volume(µl) Liner

Agilent Choice Liners

Liner, split, low press. drop, glass wool, taper, deactivated

Liner, splitless, single-taper, no glass wool, deactivated

NEW! Liner, Splitless,

Single-taper, no glass wool, polymerically deactivated

For split injection

For splitless injection

For trace pesticide analysis

Liner, direct, 2 mm ID, deactivated

Liner, general purpose split/splitless, glass wool, taper, deactivated

For direct injection

(use for gas samples, headspace, or purge and trap applications)

For split/splitless injection

Splitless Inlet Liners

Liner, splitless, single-taper, glass wool, deactivated

Liner, splitless, double-taper, no glass wool, deactivated

NEW! Liner, Splitless, double-taper, no glass wool, polymerically deactivated

For trace pesticide analysis

Direct Inlet Liners

Liner, direct, 2 mm ID, non-deactivated, quartz

870

900

900

250

870

900

800

800

250

5183-4647

$35

5183-4701

$157

5181-3316

$29

5181-3316EN

$32

5183-4695

$124

5181-8818

$24

5183-4711

$27

5183-4703

$95

5183-4712

$112

5062-3587

$30

5181-3315

$36

5181-3315EN

$43

5183-4693

$129

5183-4705

$163

Liner, direct, 1.5 mm ID, non-deactivated

[use for gas samples, headspace, or purge and trap applications]

Liner, straight, splitless 4.0 mm ID

140

18740-80220 5183-4707

$28 $124

18740-80200 5183-4709

$17 $73

Split Inlet Liner

Liner, split, glass wool, non-deactivated

Split Inlet Liners For Manual Injection

Liner, split, with cup, no glass wool

Liner, split, with cup, glass wool, and packing

[not recommended for use with electronic pressure control (EPC)], for manual injection

Direct Connect Liners

Single taper direct connect liner, 4 mm ID, deactivated

Dual taper direct connect liner, 4 mm ID, deactivated

Focus Liners

Focus liner

Focus liner

ID

4.0 mm

4.0 mm

Wool

Yes

Yes

Dimensions

6.3 mm X 78.5 mm

6.3 mm X 78.5 mm

Liner O-Rings

Fluorocarbon O-ring (12/pk)

Graphite O-ring for splitless liner (10/pk)

Graphite O-ring for split liner (10/pk)

Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk)

990

800

800

990

$19

210-3003

$84

19251-60540 5183-4691

$19 $78

18740-80190 5183-4699

$40 $179

18740-60840 5183-4697

$43 $191

Part No.

G1544-80730

G1544-80700

Part No.

210-4004-5

210-4022-5

Part No.

5180-4182

5180-4173

5180-4168

Price

$62

$62

5183-4702

$700

5183-4696

$533

5183-4704

$414

5183-4713

$476

5183-4694

$560

5183-4706

$751

5183-4708

$533

5183-4710

$308

210-3003-5

5183-4692

$336

5183-4700

$784

5183-4698

$840

Price

$98

$108

Price

$13

$52

$52

5188-2741 $19

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

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Instrument Inlet Parts and Supplies

When it comes to inlet replacement parts for your Agilent GCs, don’t settle for imitations; choose only genuine Agilent parts.

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

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

Septum Nut

Part No. 18740-60835

Septum See page 36

Split/Splitless Inlet Weldment

Part No. G1544-60575, for 6890 GC with EPC

Viton O-Ring

Part No. 5180-4182, 12/pk

Liners See page 47

Heater-Sensor Assembly

Part No. G1544-61140

TIPS AND TOOLS

For a complete parts breakdown, see the

5890, 6890, and 6850 series GC Instrument

User and/or Service Manuals, or visit

www.agilent.com/chem.

Retaining Nut

Part No. G1544-20590

Washer

Part No. 5061-5869, 12/pk

Reducing Nut

Part No. 18740-20800,

1 each www.agilent.com/chem • 800 227 9770

Gold-Plated Seal (Splitless)

See page 55

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

Column Nut for 6890 GC

Part No. 5181-8830, 2/pk

54

55

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Part No.

6890/6850 Split/Splitless Insert Assemblies

Standard manual pneumatics

Original standard EPC using 1/4" split vent filter.

Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to clean carrier gas for ECD operation.

S/SL insert weldment. Used with large charcoal canister type filter for 6890/6850.

Similar to G1544-60575 except carrier lines separated for interface to valved systems of a G1540A instrument.

S/SL insert assembly for G1540A with valved system option. This insert assembly uses the large charcoal canister split vent filter for 6890/6850.

19251-60575

G1544-60575

G1544-80580

G1544-60585

G1580-60575

G1580-60585

5890 Split/Splitless Multimode Inlet Supplies

Septum retainer nut

Retainer nut for headspace sampling

Retaining nut

18740-60835

18740-60830

19251-20620

Reducing nut 18740-20800

For a complete parts breakdown, see the 5890, 6890 and 6850 series GC Instrument User and/or Service Manuals.

Liner Seals and Washers

Stainless steel

Gold-plated seal

Gold-plated seal with cross

Washers (12 pk)

18740-20880

18740-20885

5182-9652

5061-5869

$39

$106

$31

$35

$26

$33

$40

$8

Price

$230

$216

$73

$330

$261

$236

Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity. Other manufacturers’ seals are not machined, and may compromise your results.

Top

Gold-plated seal p/n 18740-20885

Bottom

Gold-plated seal with cross p/n 5182-9652

Use when inlet flow exceeds 400 ml/min.

www.agilent.com/chem • 800 227 9770

Columns

Choosing the right GC column and following Agilent’s simple column care recommendations will maximize GC column performance and lifetime. In this section our experts offer practical advice on how to select, install and store your GC column, plus give helpful hints about avoiding thermal and oxygen degradation. Because GC column contamination is the primary cause of shortened column lifetime, we’ve also included a detailed discussion about the prevention of non-volatile and semi-volatile contamination, as well as appropriate recovery measures. www.agilent.com/chem • 800 227 9770

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

Phil Stremple,

GC Columns Program Manager

CATALOG

For a complete selection of GC columns and parts, see Agilent’s 2005-

2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.

56

COLUMNS

Column Maintenance

While GC column maintenance is simple, the frequency and type of column maintenance that is required varies due to many system and sample factors. Instead of simply following a predefined timetable of maintenance items, the main focus should be how to obtain the highest performance and lifetime from a capillary column. This depends on choosing the right column, correct installation/system setup, and avoiding the primary factors that cause column performance degradation (breakage, thermal damage, oxygen damage, chemical damage and contamination).

57

Selection of Capillary Columns for GC and GC/MS

Phases

All phases can be used with conventional

GC systems, and most stationary phases can be used with a GC/MS system.

However, it is a good idea to choose a phase for your application that has the lowest amount of column bleed as possible. Column bleed is the natural degradation of the stationary phase that occurs at higher temperatures, which appears as an elevated baseline as the temperature rises to the column’s upper thermal limit. Column bleed will deposit in the MSD ion source, which can decrease

MSD performance. By minimizing the amount of column bleed, you will help reduce the frequency of required ion source maintenance.

Primary

“Quantion” is hidden

Primary

“Quantion” is enhanced

There are a few simple rules for choosing columns with lower bleed levels:

• Choose a low-bleed phase for your application – Agilent has developed several low-bleed versions of the most popular phases. These are chemically designed to possess minimal levels of column bleed possible and often have the benefit of an increased uppertemperature limit.

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

• Use more polar phases when difficult isomer separations are required. (Choose a more polar phase when you must, but try to make it the least polar column that will do the job)

Dimensions

All dimensions can be used with conventional GC systems. Many types of GC column phases can be used with the MSD, but there are some dimensional considerations. The maximum allowable flow rate and optimal sensitivity flow rates will vary depending upon the type of pump.

In general, the column flow should be

1mL/min (2mL/min for Performance Turbo

Pumps). Therefore, column length and internal diameter combinations are restricted to provide the appropriate flow to the GC/MS.

• Narrow-bore columns (0.25mm i.d. and smaller) can be installed directly into the

GC interface.

www.agilent.com/chem • 800 227 9770

• Wide-bore columns (0.32mm i.d.) that are

30m or longer can be installed directly into the 5973 GC interface (other MSDs may require 50m or longer). If using a wide-bore column with a shorter length, an effluent splitter or jet separator should be utilized.

• Columns with internal diameters greater than 0.32mm should not be directly interfaced into the GC interface. For these columns, an effluent splitter or jet separator should be installed.

Popular Column Choices

DB-1ms, 0.25mm i.d., 30m, 0.25µm

HP-5ms, 0.25mm i.d., 30m, 0.25µm

DB-XLB, 0.25mm i.d., 30m, 0.25µm

DB-35ms, 0.25mm i.d., 30m, 0.25µm

HP-INNOWax, 0.25mm i.d.,

30m, 0.25µm

122-0132

19091S-433

122-1232

122-3832

$483

$483

$483

$483

19091N-133 $413

COLUMNS

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 appropriate distance 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 before heating the oven.

• Briefly conditioning a column before installing it into the GC/MS interface is recommended. When the column and inlet are first heated, volatile materials within the flow-path and a small portion of the column stationary phase move into the gas phase. These materials are then carried by the carrier gas into the MSD and can deposit in the MSD ion source.

This can decrease MSD performance.

Conditioning the column briefly prior to installation into the MSD will minimize the contamination brought into the ion source.

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.

www.agilent.com/chem • 800 227 9770 58

59

COLUMNS

Column Installation & Setup continued

Bad

Good

Example of column cuts

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

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

Description

Ceramic wafer (4/pk)

20x Magnifier

General Purpose Graphite ferrule

(0.5mm ID, for column IDs

0.32mm)

10/pk

General Purpose Graphite ferrule

(1.0mm ID, for 0.45-0.53mm

ID columns) 10/pk

Gas leak detector 115V

Gas leak detector 220V

Part No.

5181-8836

430-1020

5080-8853

5080-8773

5182-9646

5182-9648

Price

$ 15

$ 42

$ 47

$ 38

$1859

$1859

Causes of Performance Degradation

Column Breakage

Fused silica columns can break wherever there are small scratches or abrasions in the protective polyimide coating.

Continuous heating and cooling of the oven, vibrations caused by the oven fan as well as being wound on a circular cage 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.

Prevention

• Avoid scratches and abrasions by not exposing the column to sharp edges such as column hangers and tags, metal edges in the GC oven, column cutters and other miscellaneous 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 very likely. 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 been heated, connect the two pieces with a low volume union. No more than

2-3 unions should be installed for one column.

Description Part No.

Price

Fused Silica Union,

Universal 2-way

(5/pk) 705-0905 $ 50

Quartz deactivated column connector

(5/pk) 5181-3396 $ 94

Polyimide Sealing resin (5 grams) 500-1200 $ 24 www.agilent.com/chem • 800 227 9770

COLUMNS

Thermal Damage

Exceeding a column’s upper temperature limit results in accelerated degradation of the stationary phase and tubing surface.

This results in the premature onset of excessive column bleed, peak tailing for active 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 an indefinite time

– Programmed limit: maximum column temperature; column should only be held there for about 5-10 minutes

• Set the GC maximum oven temperature function at or a few degrees above the temperature limit of the column. With two columns in the oven be sure to set the maximum temperature to the temperature limit of the column with the lowest value.

Recovery

• Disconnect column from detector

• Heat the column 8-16 hours at the isothermal limit

• Remove 10-15 cm from the column end

• Reinstall into the detector and condition as usual

NOTE: Thermal damage cannot be reversed.

The column usually does not return to its original performance; however, it is often still functional. The life of the column will be reduced after thermal damage.

Oxygen Damage

Oxygen is an enemy to all capillary GC columns. Constant exposure to oxygen does not damage the column at or near ambient temperatures; however, severe damage occurs as the column temperature increases. A leak in the carrier gas flow path (e.g., gas lines, fittings, injector, septa) is the most common source of oxygen exposure. As the column is heated, very rapid degradation of the stationary phase occurs. This results in the premature onset of excessive column bleed, peak tailing for active compounds and/or loss of efficiency (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.

Prevention

Maintain an oxygen and leak-free system by:

• performing periodic leak checks

• changing septa regularly

• using high quality carrier gases

• installing and maintaining oxygen traps

• changing gas cylinders before they are completely empty

Recovery

Perform column “bakeout” as described under thermal damage recovery.

NOTE: Oxygen damage occurs very rapidly.

In less severe cases, the column may still be functional but at a reduced performance level. In more severe cases, the column is irreversibly damaged.

Description Part No.

FlowTracker 2000 Flowmeter and Leak Detector 5183-4780

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

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

Big Universal Trap (Combination Trap)

(750cc, 1/8" fitting, He)

Advanced Green Septa (11mm, 50/pk)

RMSH-2

5183-4759

Price

$1143

$ 235

$ 235

$ 261

$ 62

TIPS AND TOOLS

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

www.agilent.com/chem • 800 227 9770 60

61

COLUMNS

Chemical Damage

Inorganic or mineral acids and bases are the primary sources of chemical damage to stationary phases. Most of these acids and bases have low volatility and accumulate at the front of the column.

If allowed to remain, the acids or bases damage the stationary phase. The only organic compounds that have been reported to chemically damage stationary phases are perfluoroacids and these need to be present at high levels (e.g., 1% or higher). This results in the premature onset of excessive column bleed, peak tailing for active compounds and/or loss of efficiency (resolution).

NOTE: Hydrochloric acid and ammonium hydroxide are the least harmful of the group as both tend to follow any water that is present in the sample. Thus, if HCl or NH

4

OH are present in a sample, minimizing water retention will render these compounds relatively harmless to the column.

Prevention

• Perform sample preparation to remove inorganic acids and bases from the sample

• Install guard column and trim frequently

• If acids or bases must be used choose an organic alternative or HCl or NH

4

OH

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 Contamination

Column contamination is the most common problem encountered in capillary

GC. Unfortunately, it mimics most other chromatographic problems and is often misdiagnosed. A contaminated column is usually not damaged, but it may be rendered unusable. There are two basic types of contaminants: nonvolatile and semivolatile.

GUARD COLUMN

A guard column is a piece of fused silica tubing attached with a union to the front of the analytical column with the following characteristics:

• Material should be deactivated fused silica tubing to minimize solute interactions.

• Length should be from 1-10 meters. Typical lengths of 5-10 meters allow substantial 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. DuraGuard columns offer the guard column built into the analytical column as a single 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 and not in the analytical column. This greatly reduces the interaction between the residues and the sample. Periodic cutting or trimming of the guard column is usually required upon a build-up of residues. The onset of peak shape problems is the usual indicator that the guard column needs trimming or changing.

INJECTOR

Guard Column

DETECTOR

Guard Column

Column

Union

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

COLUMNS

Nonvolatile Contaminants

Nonvolatile contaminants or residues do not elute and accumulate in the column

(most often confined to the first few meters). The column becomes coated with these residues which interfere with the proper partitioning of solutes in and out of the stationary phase. Also, the residues may interact with active solutes resulting in peak adsorption problems (evident as peak tailing or loss of peak size). Active solutes are those containing a hydroxyl

(-OH) or amine (-NH) group, and some thiols (-SH) and aldehydes.

Prevention

• Perform sample cleanup to remove nonvolatile materials from the sample

• Use injection port liners packed with glass wool (may not be feasible when analyzing active compounds)

• Install a guard column and trim regularly

Recovery

• Do not bakeout the column

• Front End Maintenance:

– Clean or change the injection port liner

– Clean out the injector

– Cut off typically 0.5 to 1 meter of the front of the column

• Turn the column around (install detector end into injector). Not recommended for sensitive ECD, NPD, and MS detectors.

• Solvent rinse the column

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

Semivolatile Contaminants

Semivolatile contaminants or residues accumulate in the column, but eventually elute. Hours to days may elapse before they completely leave the column. Like nonvolatile residues, they may cause peak shape and size problems and, in addition, are usually responsible for many baseline problems (instability, wander, drift, ghost peaks, etc.).

Description

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

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

Quartz deactivated column connector (5/pk)

Polyimide sealing resin (5 grams)

Deactivated Fused silica,

10m, 0.53mm i.d.

Deactivated Fused silica,

10m, 0.25mm i.d.

Capillary column rinse kit

Prevention

• Perform sample cleanup to remove semi-volatile materials from the sample

• Increase the final temperature of the

GC run (not to exceed the temperature limit of the column)

• Change septa regularly

Recovery

• Bakeout the column: limit 1-2 hours

(excess baking may polymerize some contamination and reduce column lifetime)

• Solvent rinse the column

Does Your Sample Have Residues?

Perform this simple test.

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

2. Put the slide over the heated GC inlet for 20 minutes.

3. Hold the slide up to the light.

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

Part No.

5183-4712

5183-4695

5181-3396

500-1200

160-2535-10

160-2255-10

430-3000

Price

$112

$124

$ 94

$ 24

$110

$ 73

$ 78

Column Storage

Capillary columns should be stored in their original box when removed from the GC.

Place GC septa over the ends to prevent debris from entering the tubing. Upon reinstallation of the column, the column ends need to be trimmed by 2-4 cm to ensure that a small piece of septa is not lodged in the column.

If a column is left in a heated GC, there should always be carrier gas flow through the column. The carrier gas flow can be turned 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 the column occurs. www.agilent.com/chem • 800 227 9770 62

COLUMNS

Column Types and Characteristics

63

DB-1ms

• 100% Dimethylpolysiloxane

• Identical selectivity to DB-1

• Nonpolar

• Very low bleed characteristics

• Improved acid performance compared to standard 100% Dimethylpolysiloxane columns

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

• Excellent general purpose column

• Bonded and cross-linked

• Solvent rinsable

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

I.D.

Length Film Part No.

0.25

0.25

0.25

0.32

0.32

0.32

0.10

0.10

0.10

0.10

0.20

0.20

Similar Phases

HP-1ms, Rtx-1ms, CP-Sil 5CB

30

30

60

30

30

60

10

10

20

20

12

25

0.10

0.25

0.25

0.10

0.25

0.25

0.10

0.40

0.10

0.40

0.33

0.33

Price

127-0112

127-0113

127-0122

127-0123

128-0112

128-0122

122-0131

122-0132

122-0162

123-0131

123-0132

123-0162

Applications

General purpose: Amines, hydrocarbons, pesticides, PCBs, phenols, sulfur compounds, flavors and fragrances.

$483

$483

$823

$521

$521

$896

$343

$343

$495

$495

$261

$400 www.agilent.com/chem • 800 227 9770

COLUMNS

DB-5ms

• Phenyl Arylene polymer equivalent to a

(5%-Phenyl)-methylpolysiloxane

• Nonpolar

• Very low bleed characteristics

• Excellent inertness for active compounds

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

• Bonded and cross-linked

• Solvent rinsable

• Certified for MS

• Exact replacement of HP-5TA

• Close equivalent to USP Phase G27

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

I.D.

Length Film

0.18

0.18

0.20

0.20

0.32

0.32

0.32

0.32

0.32

0.32

0.25

0.25

0.25

0.25

0.25

0.25

0.25

0.25

Similar Phases

Rtx-5ms, HP-5ms, PTE-5, CP-Sil 8CBms,

BPX-5

50

60

60

30

30

30

30

50

60

60

25

25

30

30

20

40

25

50

0.18

0.18

0.33

0.33

0.10

0.25

0.50

0.25

0.10

0.25

0.25

0.40

0.10

0.25

0.50

0.25

0.10

0.25

Part No.

Price

121-5522

121-5542

128-5522

128-5552

122-5522

122-552A

122-5531

122-5532

122-5536

122-5552

122-5561

122-5562

123-5531

123-5532

123-5536

123-5552

123-5561

123-5562

Applications

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

$412

$740

$400

$674

$521

$521

$521

$804

$896

$896

$421

$421

$483

$483

$483

$753

$823

$823

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 Phases

Rtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms,

BPX-5, Rtx-5 Amine

Applications

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

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

I.D.

Length Film Part No.

0.20

0.20

0.20

0.25

0.25

0.25

0.25

0.25

0.25

0.25

0.25

0.32

0.32

0.32

0.32

0.32

0.32

0.32

* This column is shipped with the 5973 MSD.

30

30

30

60

60

15

15

15

12

25

50

30

60

60

15

25

30

30

0.33

0.33

0.33

0.10

0.25

1.00

0.10

0.25

0.50

0.10

0.25

1.00

0.52

0.10

0.25

0.50

0.10

0.25

19091S-101

19091S-102

19091S-105

19091S-331

19091S-431

19091S-231

19091S-333

19091S-433*

19091S-133

19091S-336

19091S-436

19091S-211

19091S-112

19091S-313

19091S-413

19091S-113

19091S-316

19091S-416

Price

$261

$400

$674

$295

$295

$295

$483

$483

$483

$823

$823

$319

$448

$521

$521

$521

$896

$896 www.agilent.com/chem • 800 227 9770 64

65

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

0.18

0.18

0.20

0.20

0.25

0.25

0.25

0.25

0.25

0.25

0.25

0.25

0.32

0.32

0.32

0.32

Similar Phase

MDN-12

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

I.D.

Length Film Part No.

30

30

30

30

60

15

15

15

30

30

30

60

20

30

12

25

0.18

0.18

0.33

0.33

0.10

0.25

1.00

0.10

0.25

0.50

1.00

0.25

0.10

0.25

0.50

0.25

Price

121-1222

121-1232

128-1212

128-1222

122-1211

122-1212

122-1213

122-1231

122-1232

122-1236

122-1233

122-1262

123-1231

123-1232

123-1236

123-1262

Applications

PCB congeners, pesticides, chlorinated herbicides, phenoxy acid methyl esters, haloacetic acids

$412

$579

$261

$400

$295

$295

$295

$483

$483

$483

$483

$823

$521

$521

$521

$896

DB-35ms

• Equivalent to a (35%-Phenyl)methylpolysiloxane

• Midpolarity

• Very low bleed characteristics

• Extended temperature limit of 360°C

• Excellent inertness for active compounds

• Certified for MS

• Ideal for confirmational analyses

• Bonded and cross-linked

• Solvent rinsable

• Replaces HP-35ms

• Close equivalent to USP Phase G42

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

I.D.

0.20

0.20

0.25

0.25

0.25

0.25

0.32

0.32

Length

15

25

15

30

30

60

30

60

Film

0.33

0.33

0.25

0.15

0.25

0.25

0.25

0.25

Part No.

128-3812

128-3822

122-3812

122-3831

122-3832

122-3862

123-3832

123-3862

Similar Phases

Rtx-35, SPB-35, AT-35, Sup-Herb

Price

$261

$400

$295

$483

$483

$823

$521

$896

Applications

Aroclors, PCBs, amines, pesticides, chlorinated herbicides, haloacetic acids, pharmaceuticals, drugs of abuse www.agilent.com/chem • 800 227 9770

DB-17ms

• Equivalent to (50%-Phenyl)methylpolysiloxane

• 320/340°C Upper temperature limit

• Very low bleed midpolarity column

• Excellent inertness for active compounds

• Enhanced mass spectral integrity

• Bonded and cross-linked

• Solvent rinsable

• Best column for CLP pesticides

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

I.D.

Length Film Part No.

0.18

0.25

0.25

0.25

0.25

0.25

0.32

0.32

20

15

15

30

30

60

30

30

0.18

0.15

0.25

0.15

0.25

0.25

0.15

0.25

121-4722

122-4711

122-4712

122-4731

122-4732

122-4762

123-4731

123-4732

Similar Phases

DB-17, HP-50+, Rtx-50, 007-17, SP-2250,

SPB-50, BPX-50, SPB-17

Applications

Drugs, glycols, pesticides, steroids

Price

$412

$295

$295

$483

$483

$823

$521

$521

COLUMNS

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

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

I.D.

Length Film Part No.

0.25

0.25

0.25

0.32

15

30

60

30

0.25

0.25

0.25

0.25

122-2912

122-2932

122-2962

123-2932

Similar Phases

HP-225, SP-2330, CP-Sil 43CB, RSL-500,

Rtx-225, BP-225, CB-225, OV-225, 007-225

Applications

Price

$295

$483

$823

$521

Alditol acetates, FAMEs, neutral sterols www.agilent.com/chem • 800 227 9770

EASY ONLINE ORDERING

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

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

66

67

COLUMNS

HP-INNOWax

• Polyethylene glycol (PEG)

• High polarity

• Highest upper-temperature limits of the bonded PEG phases

• Column-to-column repeatability

• Bonded and cross-linked

• Solvent rinsable

• Close equivalent to USP Phase G16

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

I.D.

Length Film Part No.

Price

0.20

0.20

0.20

0.20

0.25

0.25

0.25

0.25

0.25

0.25

0.32

0.32

0.32

0.32

0.32

0.32

60

60

60

30

30

30

25

25

50

50

30

30

30

60

60

60

0.20

0.40

0.20

0.40

0.15

0.25

0.50

0.15

0.25

0.50

0.15

0.25

0.50

0.15

0.25

0.50

19091N-102

19091N-202

19091N-105

19091N-205

19091N-033

19091N-133

19091N-233

19091N-036

19091N-136

19091N-236

19091N-013

19091N-113

19091N-213

19091N-016

19091N-116

19091N-216

$379

$379

$636

$636

$413

$413

$413

$737

$737

$737

$447

$447

$447

$816

$816

$816

Similar Phases

HP-20M, SUPELCOWAX 10, CP-WAX 52CB,

SUPEROX II, CB-WAX, Stabilwax, BP-20,

007-CW, Carbowax, DB-WAXetr

Applications

Alcohols, aromatics, essential oils, solvents

GS-GasPro

• Unique bonded PLOT column technology

• Excellent choice for light hydrocarbons and sulfur gases

• Retention stability not affected by water

• Separates CO and CO2 on a single column

• Ideal PLOT column for GC/MS – no particles

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

I.D.

0.32

0.32

Length

30

60

Part No.

113-4332

113-4362

Similar Phase

CP-Silica PLOT

Price

$627

$942

Applications

C1 to C12 hydrocarbons, CO2, trace-level sulfurs, hydride gases, inorganic gases, halocarbons, SF6, oxygen/nitrogen separation at -80°C.

www.agilent.com/chem • 800 227 9770

Detectors

Most detectors require simple but periodic cleaning to maintain peak performance.

This is especially true for highly sensitive

GC detectors. Without routine detector maintenance, GC system performance will deteriorate and can cause detector failure.

Detailed procedures on how to clean, maintain and replace common detectors, including FID, TCD, NPD, ECD, and FPD are summarized in this section. Also included are special handling techniques and specific recommendations to maximize specific detector operations. For example, learn how to resolve flame ignition problems associated with your flame photometric detector and test electron capture detectors for radioactivity leaks. www.agilent.com/chem • 800 227 9770

“GC detectors are highly sensitive systems that are often compromised by various types of contamination. By implementing some recommended detector maintenance routines, you can minimize instrument downtime and keep your GC system working at peak efficiency.”

Bernhard Rothweiler

Applications Chemist

CATALOG

For a complete selection of Detector supplies, see Agilent’s 2005-2006

Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.

68

DETECTORS

Flame Ionization Detector (FID)

Flame Ionization Detectors require little maintenance to keep them performing at satisfactory levels. The primary task is to occasionally measure hydrogen, air and makeup gas flows. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be independently measured to obtain the most accurate values.

Condensation

Since the FID combustion process results in water formation, the detector temperature must be kept above 100˚C to prevent condensation. Such condensation, especially when combined with chlorinated solvents or samples, causes corrosion and sensitivity loss.

Hardware Problems

If the flame goes out or will not light:

• Check the column flow rate. It may be too high. Decrease the flow rate or pressure. Switch to a more restrictive column (longer or with a smaller id).

If you must use a large id column, first cool the GC oven to below 50˚C, then turn off the carrier flow long enough to allow the FID to light. Check for partially or completely plugged jet.

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

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

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

Cleaning & Replacement

Even with normal use, deposits develop in the jet and detector (usually white silica from column bleed or black carbonaceous soot). These deposits reduce sensitivity and cause chromatographic noise and spikes. Although you can clean the jet, it is usually more practical to replace dirty jets with new ones. If you do clean the jet, be careful not to scratch the jet internally; scratches will ruin the jet

Igniter Glow Plug Assembly

Collector Assembly

Collector Body

FID Jets

FID Ferrules

FID Cleaning Kit, P/N 9301-0985, $41

69

VIDEO

To view a video on FID column installation, jet replacement, collector maintenance, or ignitor replacement, visit

www.agilent.com/chem/techsupport.

www.agilent.com/chem • 800 227 9770

DETECTORS

Jet Cleaning Procedure

(using Agilent’s FID Cleaning Kit #9301-0985)

1. Run a cleaning wire through the top of the jet. Run it back and forth a few times until it moves smoothly. Be careful not to scratch the jet. (Do not force too large a wire or probe into the jet opening or the opening will become distorted. A loss of sensitivity, poor peak shape and/or lighting difficulties may result if the opening is deformed.)

2. Fill an ultrasonic cleaning bath with aqueous detergent, and place the jet in the bath. Sonicate for five minutes.

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

4. Sonicate again for five minutes.

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

5. Remove the jet from the bath and rinse it thoroughly, first with hot tap water and then with a small amount of GC-grade methanol.

6. Blow the jet dry with a burst of compressed air or nitrogen, and then place the jet on a paper towel and allow it to air dry.

6890/6850 Ionization Detector (FID) Supplies

Item Description Unit Part No.

Price

1 PTFE chimney (optional)**

2 Collector nut

3 Spring washer

4 Ignitor castle

Optional Hastelloy Ignitor Castle*

5 Ignitor glow plug assembly

6 Collector insulator

7 Collector body

Hastelloy Collector Body

10/pk

19231-21050

19231-20940

5181-3311

19231-20910

19231-21060

19231-60680

G1531-20700

G1531-20690

61531-21090

9 FID collector assembly 1

Detector insulation assembly

FID collector cleaning brush

Collector Housing

2/pk

G1531-60690

G1531-20700

8710-1346

G1531-20740

$194

$ 17

$ 8

$175

FID retainer nut wrench

(5880, 5890, 6890)

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

19301-00150 $ 8

8710-1561 $ 13

FID supplies kit-Includes: 5182-3450

Jet, packed standard 3 each 18710-20119

FID performance evaluation sample kit 2 each 18710-60170

Ignitor glow plug assembly

Jet, cap. series 530 µm

FID flow measuring insert

Cleaning wires for 0.03 in. ID jet

2 each

3 each

2 each

19231-60680

19244-80560

19301-60660

5180-4150

Cleaning wires: 0.018 in. ID/530 µm jet 1/pk

Wire, jet cleaning, 5 each

5180-4152

19301-20720

Capillary inlet cleaning wires

Detector cleaning kit

5180-4153

9301-0985

**Not included in assembly.

*Hastelloy components may be used when analyzing highly corrosive materials.

1 Does not include Hastelloy component.

$556

$ 49

$ 44

$ 42

$ 56

$ 53

$ 23

$ 23

$ 12

$ 8

$ 41

$ 14

$ 35

$ 9

$ 57

$184

$ 42

$ 17

$ 60

$260 www.agilent.com/chem • 800 227 9770

Plugged FID jet

EASY ONLINE ORDERING

Here’s another time-saving reason to place your order through our website: you can instantly view and edit the items in your shopping cart

– while keeping track of your total order price.

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

70

DETECTORS

FID Jets

Description

Jets for capillary dedicated FID

Capillary jet (0.011 in./0.29 mm ID tip)

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

Adaptable FID

Capillary 0.53 mm jet (0.011 in. ID tip)

Packed (0.018 in. ID tip)

Packed (0.030 in. ID tip)

0.53 mm high temp (0.018 in. ID tip) for SimDIS

Length(mm) Part No.

48

48

61.5

63.5

63.5

61.5

G1531-80560

G1531-80620

19244-80560

18710-20119

18789-80070

19244-80620

Price

$43

$54

$56

$49

$55

$37

FID Consumables

Description Unit Part No.

Price

FID flow measuring insert

FID ignitor cable

19301-60660 $53

G1531-60680 $41

FID Performance evaluation sample kit, 0.03% C14,

C15, and C16 normal alkanes in hexane

O-rings

18710-60170 $44

Cleaning wire

Jet cleaning wire for 0.03 in. ID jet

Jet cleaning wire for Series 530 mm and 0.018 in. ID jet

12/pk 5080-4978

5/pk

5/pk

$ 7

19301-20720 $12

5180-4150 $23

5180-4152 $23

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

1

8

4

6

7

2

3

6

5

71

TIPS AND TOOLS

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

6890 Series GC FID Detector

Collector Body, P/N G1531-20690 www.agilent.com/chem • 800 227 9770

www.agilent.com/chem • 800 227 9770

DETECTORS

Electron-Capture Detector (ECD)

Agilent provides two types of electron capture detectors. The regular detector

(ECD) has a larger internal volume

(approximately 10 times) than the microcell detector (µ-ECD). These two types can be distinguished by the top cover of the detector – the ECD has a solid cover and the µ-ECD has a perforated cover.

Thermal Cleaning

If your baseline is noisy or the output value is abnormally high and you have determined that these problems are not being caused by leaks in the GC system, you may have contamination in the detector from column bleed and sample residues. To remove contamination, you should perform a thermal cleaning

(bakeout) of the detector.

Warning: Detector disassembly and/or cleaning procedures other than thermal should be performed only by personnel trained and licensed appropriately to handle radioactive materials. Trace amounts of radioactive 63 Ni may be removed during other procedures, causing possible hazardous exposure to ß and x-radiation.

Radioactivity Leak Test

Electron capture detectors must be tested for radioactive leakage at least every six months. Records of tests and results must be maintained for possible inspection by the Nuclear Regulatory Commission and/or the responsible local agency. More frequent tests may be conducted when necessary.

The procedure used is a “wipe test.” A wipe test kit is supplied with each new detector. Refer to the information card supplied in the Wipe Test Kit for instructions on performing the test.

Gas Purity

For successful EC detection, it’s important that the carrier and purge gases are very clean and dry (99.9995%). Moisture, oxygen, or other contaminants can improve sensitivity, but at a cost of linear range.

Always precondition the column before connection to the detector.

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.

72

DETECTORS

1

2

3

6890 Series GC ECD Detector

Electron-Capture Detector (ECD) Supplies

Item Description Part No.

Price

1 ECD makeup gas adapter*

2, 3 Nut warmer cup with insulation

ECD adapter replacement liner, fused silica

ECD end cap

G1533-80565

19234-60720

19233-20625

19233-20755

$198

$ 58

$ 15

$ 32

ECD chemical sample kit, 3 ampoules solution of 33 pg/mL (0.033 ppm) each of lindane and aldrin in isooctane

ECD wipe test kit

18713-60040 $ 46

18713-60050 $ 31

*Includes one each of P/N 19233-20625 and P/N 19233-20755

ECD Wipe Test:

A wipe test kit (P/N 18713-60050) is supplied with each new ECD. The kit includes an information card with instructions for performing the test. Records of tests and results must be maintained for possible inspection by the NRC (Nuclear Regulatory

Commission) and/or responsible state agency.

73

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.

www.agilent.com/chem • 800 227 9770

DETECTORS

Thermal Conductivity Detector (TCD)

The TCD compares the thermal conductivities of two gas flows – pure carrier gas (also called the reference gas) and carrier gas plus sample components

(also called column effluent).

Filament Maintenance

The primary maintenance for a TCD involves the filament. Most procedures involve improving filament life or keeping the filament from becoming damaged or contaminated.

A constant presence of oxygen can permanently damage filaments through oxidative processes. The most common source of oxygen is a leak(s) near the detector – or in the carrier or makeup gas line fittings. Oxygen traps are recommended for the carrier and makeup gases to reduce oxygen levels. Proper column installation techniques and regular leak checks (especially after column installation) help to keep leak problems to a minimum.

The damage caused by oxygen is more severe at high filament currents.

Chemically active sample components such as acids and halogenated compounds may attack and damage the filaments.

Avoiding these compounds when possible increases filament life. Turning off or substantially reducing the filament current when the TCD is not in use also prolongs filament life.

Increasing Filament Lifetime

Increased filament lifetime will result if the following startup process is used:

1. Purge the detector with carrier and makeup gas for 10-15 minutes before turning on the filaments. This prevents oxidation of the filaments due to the presence of oxygen that has diffused into the cell under no flow conditions.

2. Turn on the filaments at the lowest possible current setting, then increase the filament current in several increments to the desired value. This reduces the power surge upon current introduction and prolongs filament lifetime.

Thermal Conductivity Detector (TCD) Supplies

Description Unit

Cell Contamination

Cell contamination is a problem when a lower detector temperature is used to improve sensitivity. Also, low filament currents promote contamination since the filament is maintained at a lower temperature at lower currents. If the cell becomes contaminated, a solvent flush of the detector may help to remove the condensed material.

Part No.

6890/6850/5890 Common TCD Supplies

TCD replacement cell (6890/6850 only)

TCD cap column adapter seal

TCD cap column adapter

10/pk

Graphite ferrules, 1.0 mm id

Graphite ferrules, 0.5 mm id

Capillary column nut, for 6890

Capillary column nut, for 6850

10/pk

10/pk

2/pk

2/pk

TCD packed column adapter (6890/6850 only)

G1532-60675

18740-20950

18740-20960

5080-8773

5080-8853

5181-8830

5183-4732

G1532-20710

TCD chemical sample kit, 3 ampoules,

0.5 mL, 5 solution of 0.3% C14, C15, and C16, normal alkanes in hexane 18711-60060

5890 TCD Supplies

Makeup gas adapter, TCD

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

TCD replacement cartridge

19232-80550

19302-80020

19232-60676

Price

$ 45

$ 126

$ 138

$1625

$1030

$ 18

$ 33

$ 38

$ 47

$ 26

$ 47

$ 44 www.agilent.com/chem • 800 227 9770 74

75

DETECTORS

Solvent Flush Procedure

1. Cool the cell to room temperature and remove the column.

2. Place a septum in a nut or fitting assembly that fits onto the detector entrance.

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

4. Inject 20-100 µL volumes of toluene or benzene into the detector through the septum. Inject a total volume of at least 1mL of solvent. Do not inject halogenated solvents such as methylene chloride and chloroform into the detector.

5. After the final injection, allow makeup gas to flow for 10 minutes or more.

Slowly raise the temperature of the cell to 20-30˚C above the normal operating temperature.

6. After 30 minutes, decrease the temperature to the normal value and install the column as usual.

Thermal Cleaning

The TCD can become contaminated with deposits from such things as column bleed or dirty samples. A wandering baseline, increased noise level, or changes in response on a checkout chromatogram all indicate contamination. Thermal cleaning, or bakeout (heating the detector block to evaporate the contaminant), should be performed only after you have confirmed that the carrier gas and the flow system components are leak-free and contaminant-free.

Watch out for decreased sensitivity caused by samples that react with the filament, originating from oxygen-contaminated carrier gas, leaks in plumbing, or column bleeding. Samples with active components, such as acids and halogenated compounds can chemically attack the filament as well. Also, sample condensation will contaminate the detector cell if the temperature is too low.

Some types of contaminants can be removed by temperature bakeout. Also, in non-modulated designs, wandering baselines due to temperature variation can be corrected by making sure the detector temperature remains constant.

www.agilent.com/chem • 800 227 9770

DETECTORS

Flame Photometric Detector (FPD)

Maintenance

Flame Photometric Detectors require minimal maintenance to keep them performing at satisfactory levels. The hydrogen, air and makeup gas flows should be measured occasionally. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be measured independently to obtain the most accurate values.

Cleaning & Parts Replacement

The FPD requires periodic cleaning. In most cases, this only involves the jet, and less frequently, the filter. Agilent provides brushes and wires that simplify the cleaning of all detector parts (see FPD

Supplies on page 77). The brushes are used to dislodge particulates clinging to the metal surfaces. A fine wire is used to clean the jet opening of particulates. Do not force too large a wire or probe into the jet opening or the opening may become distorted. A loss of sensitivity, poor peak shape, and/or lighting difficulties may result if the opening is deformed. The filter or any of the window parts should be handled gently. Scratches or other surface deformities reduce the amount of light passing through the filter, thus reducing response. The filter and related parts should be clean and free from fingerprints.

The Photo Multiplier Tube (PMT) needs periodic replacement. The PMT is defective and needs to be rebuilt or replaced if:

• high voltage is on and the flame is lit

• low or no signal and/or noise not attributed to any other source such as bad cables are observed

• light leaks occur

• high temperatures are used

• defective signal boards are present

High detector temperatures reduce the

PMT life. When not in use, turn off the

PMT to maximize its usable lifetime. Some

PMTs may have a shelf life and should not be stored for prolonged periods before use.

Column bleed and/or effluent can contaminate the first quartz window (heat shield) nearest the detector module. Dust, fingerprints, and atmospheric contaminants can dirty both quartz windows, the filter, and/or the photomultiplier tube window.

Contamination anywhere along the light path between flame and PMT can reduce detector sensitivity.

If a response problem is encountered

(sensitivity, noise, selectivity) the FPD jet should be inspected for deposits and, if necessary, cleaned or replaced. To properly service the jet, the detector module should be removed from the instrument, and followed by appropriate service (see jet cleaning procedure on page 70).

Occasionally, the transfer line fused silica liner between the column and FPD module must be inspected, cleaned and/or replaced.

Flame Ignition Problems

If the FPD flame won’t light or stay lit:

• Be sure there is a problem. Ignition is best confirmed by holding a mirror or shiny surface near the aluminum exhaust tube, with the rubber drip tube removed, and observe condensation if the flame is lit.

• Check Lit Offset. If it is zero, autoignition is turned off. If it is too large, the GC will not know that the flame is lit and will shut down the detector.

• Increase the air supply pressure to the pneumatics module. This makes the flame easier to light but does not affect the air flow rate setpoint.

• If the flame doesn’t light at all, check the glow plug circuit. Observe the visual display, which will momentarily go to greater than 65500 counts when the flame lights. If the display doesn’t change, check the pin connections at the printed circuit board, the lead connection on the glow plug and the appropriate 5A fuse on the GC main circuit board.

• The flame is easier to light at higher detector temperatures.

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

• If the flame still won’t light, there could be a large leak in the system. This results in measured flow rates being different from actual flow rates, causing non-ideal ignition conditions. Thoroughly leak check the whole system.

Flame Conditions & Gas Flows

The flame conditions are critical to successful operation. Since the detection zone is above the flame, the gas flows and jet diameter must be optimized so that components burned (activated) in the flame will emit in the detection zone.

Gas flows are also critical for optimized selectivity and sensitivity. The most critical parameters are the hydrogen/air or hydrogen/oxygen ratio, and the total gas flow, which effects flame temperature.

www.agilent.com/chem • 800 227 9770 76

77

DETECTORS

6890/5890 FPD Supplies

Item Description Unit Part No.

1 Exit tube assembly

2 Nut, brass, 1/4 in.

4 Weldment, block

5 O-ring, ignitor, Kalrez

6 Spacer, ignitor

7 FPD Ignitor Replacement Kit

8 Ignitor cable assembly (6890 only)

9 Gasket, heat shield

10 Window, first heat shield

11 Disk, heat shield

12 Coupling, SS

10/pk

14 Screw, M3 x 12 (4 required)

15 Clamp

16 O-ring, inner window

17 Window, second heat shield

18 O-ring, outer window

19 Flange adapter

12/pk

12/pk

20 Flange ring

21 O-ring, Viton, 1.239 in. id

Adapter weldment, 1/8 in. columns

12/pk

Adapter weldment, capillary

Start-up kit (5890 only)

FPD O-ring (5890 only)

Liner/ferrule kit

19256-80570

19256-60500

12/pk 5061-5867

19256-60590

19256-80000

19256-80010

Sulfur filter

Phosphorus filter

Kalrez O-ring, size 2-002

Kalrez O-ring, size 2-011

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

FPD Performance Evaluation Sample: Solution of

20 ng/mL (20 ppm) dodecanethiol and tributylphosphate in isooctane, 3 ampoules

0905-1609

0905-1608

5061-5889

19305-60580

19256-60700

5180-4105

19256-80560

0905-1610

19256-20590

19256-60800

G1535-60600

19256-80045

19256-80030

19256-20580

19256-20550

0515-0911

19256-00090

5061-5886

19256-80060

5061-5891

19256-20510

19256-00200

5061-5890

19256-80590

Price

$ 19

$ 40

$ 22

$ 21

$141

$114

$434

$ 17

$ 89

$378

$378

$ 42

$ 42

$ 1

$ 59

$ 24

$ 40

$ 24

$131

$ 68

$ 22

$ 83

$ 38

$ 80

$165

$ 72

$ 13

$536

$ 42

$ 15

8

7

6

5

1

4

3

2

16

17

18

19

20

9

10

11

12

13

14

15

21

Install the correct optical filter, depending on the choice of Sulfur or

Phosphorus mode.

For Sulfur Mode, use the 393 nanometer filter.

For Phosphorus Mode, use the 525 nanometer filter.

www.agilent.com/chem • 800 227 9770

DETECTORS

Nitrogen-Phosphorus Detector (NPD)

Bead Maintenance

NPDs are temperamental and require frequent maintenance. Small changes in any of a number of parameters can significantly change the performance characteristics of an NPD. The bead requires the most maintenance. It needs to be changed frequently, thus a spare is a necessity.

Bead Life

To extend the life of the bead:

• Use the lowest practical adjust offset or bead voltage.

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

• Turn off the bead when not in use.

The beads have to be kept dry which limits their storage life to about six months. When a new bead is installed, slowly raise the detector temperature and bead current.

Rapid heating can crack or break the bead especially if it has been stored under humid conditions. It has been observed that higher hydrogen flows and bead currents decrease bead life. If the NPD is not in use, the hydrogen flow and bead current should be reduced or turned off to increase bead life.

Make sure there is some type of gas flow in a heated detector or when there is current to the bead.

• Keep the detector temperature high

(320 – 335˚C).

• Turn off the hydrogen flow during solvent peaks 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 detector temperature to 100˚C and maintain it for 30 minutes. Then set the detector temperature to 150˚C and maintain it for another 30 minutes.

Gas Flow

The hydrogen, air and makeup gas flows should be measured frequently. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be measured independently to obtain the most accurate values. NPDs are very sensitive to changes in the gas flows and consistent flows are necessary to maintain performance levels.

Gas Purity

Because of its high sensitivity, the NPD requires very pure gases (99.999% or better).

We strongly recommend that moisture and hydrocarbon traps be used on the carrier gas and all detector gases, including the detector hydrogen, air, and makeup gases.

Dirty gases will not only give poor chromatographic performance, but will shorten the bead life as well.

www.agilent.com/chem • 800 227 9770 78

79

DETECTORS

Cleaning & Replacement

The NPD requires periodic cleaning. In most cases, this only involves the collector and the jet. Agilent provides brushes and wires that simplify the cleaning of all detector parts (see NPD Supplies on page 79). The brushes are used to dislodge particulates clinging to the metal surfaces. A fine wire is used to clean the jet opening of particulates.

Do not force too large a wire or probe into the jet opening or the opening will become distorted. A loss of sensitivity or poor peak shape may result if the opening is deformed.

The various parts can be ultrasonicated after cleaning with a brush. Eventually the jet needs to be replaced, so it is strongly recommended to have spare jets on hand.

Over time, residue from the bead or sample can build up in the collector and cause baseline problems. You should clean the collector after you have changed the bead two or three times.

The metal C-rings wear slightly with each assembly and disassembly. After several assemblies and disassemblies (five or more), the rings may not seal effectively, causing an erratic baseline. A ceramic insulator and seal kit is available. Always cool the detector to near-ambient when changing seals and insulators.

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

NPD Jets

Description

Contaminants

Some chemical problems can also arise when using the NPD. Because it is a trace detector, be careful not to contaminate the analytical system.

Glassware

Glassware must be very clean. Phosphate detergents should be avoided, so acid washing of glassware followed by distilled water and solvent rinsing is recommended.

Solvents

Solvents should be checked for purity.

Chlorinated solvents and silanizing reagents can decrease the useful lifetime of the alkali source; excess reagent should be removed prior to injection, if possible.

Other Contamination Sources

Phosphate-containing leak detectors, phosphoric acid-treated columns or glass wool, polyimide-coated columns, or nitrogen-containing liquid phases can add noise to the system and should be avoided.

Capillary jet (0.011 in./0.29 mm id tip)

(6890 only, dedicated)

6890/5890 Adaptable

Capillary 0.53 mm jet (0.011 in. id tip)

Packed (0.018 in. id tip)

Length (mm) Part No.

48

61.5

63.5

G1531-80560

19244-80560

18710-20119

Price

$ 43

$ 56

$ 49 www.agilent.com/chem • 800 227 9770

Nitrogen-Phosphorous Detector (NPD) Supplies

Item Description Part No.

12

13

14

15

8

9

10

11

6

7

6890 NPD Supplies

1 Screws, M3 x 0.5 x 8 mm (Pozidriv)

2 NPD white ceramic bead assembly*

NPD black ceramic bead assembly**

3

4

5

Lid weldment

Metal C-ring, top

Alumina insulator, upper

Collector funnel

Alumina insulator, lower

Metal C-ring bottom and top

Screw, M4 x 10 mm

J-Clamp

Screw, M4 x 10 mm

NPD interconnect assembly

Mounting pallet

Jets (see page 79)

Base weldment, Capillary NPD

Base Weldment, Packed NPD

16

17

18

Lid stop

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

Column adapters for packed NPD

Nut warmer cup with insulation

5890 NPD Supplies

NPD collector (NPD bead)

Recoating kit, sufficient for 10 collectors

Detector Trap Replacement Kit

G1534-80500

G1534-80540

G1534-20590

5182-9722

19234-60720

19234-60540

5080-8872

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.

0515-0655

G1534-60570

5183-2007

G1534-80510

0905-2580

G1534-40020

G1534-20530

G1534-40030

0905-1284

0515-2495

1400-0015

0515-2495

G1534-60610

G1531-40020

Price

$ 58

$289

$216

$284

$ 64

$ 42

$ 53

$ 1

$ 1

$ 1

$ 1

$368

$379

$160

$ 53

$ 72

$160

$ 29

$501

$532

$ 36

$175

13

14

16

15

17

18

2

1

3

6

5

4

8 7

9

10

12

11

DETECTORS

www.agilent.com/chem • 800 227 9770 80

You asked … we listened!

Our new e-Catalog makes online ordering easier than ever.

We’ve streamlined our online store to complement the design and content of our

2005-2006 Essential

Chromatography 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

GC/MS Systems

Your mass spectrometer is a sensitive, highly specialized device that offers more functionality – and requires more maintenance – than other GC detectors.

Therefore, we have devoted an entire section of this guide to MSDs.

www.agilent.com/chem • 800 227 9770

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

Jim McCurry

Senior Applications Chemist

CATALOG

For a complete selection of gas management supplies, see Agilent’s

2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.

82

GC/MS SYSTEMS

Maintaining Mass Selective Detectors (MSDs)

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 book of system performance, Autotune, and maintenance operations performed. This makes it easier to identify variations from normal performance and to take corrective action. Subtle differences may exist between MSD models. Consult your hardware manual for specific instruction.

TASK EVERY EVERY EVERY AS

WEEK 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

•*

Every day

Check, and if necessary, replace the septum. Check the injection port liners.

Check the tightness of the column nuts.

Hint: With Agilent’s new Flip Top Inlet

Sealing System, you don’t have to check or change liners. So you save time and effort.

See page 52 for ordering information.

Every week

Check the foreline pump oil level and diffusion pump fluid. Change the injection port liners and O-rings. Gas ballast the foreline pump.

Every month

Clean the split/splitless inlet vent line trap. Check for leaks (inlet and column connections).

Every three months

Replace gas cylinders (when below

500 psig).

Every six months

Replace the foreline pump oil. Check, and if necessary, refill the calibration vial.

Every year

Replace the diffusion pump fluid.

Recondition or replace internal and external traps and chemical filters on the GC.

As needed

Tune 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 electron multiplier and ion source parameters in a log book to monitor instrument performance. In addition note the high vacuum and foreline vacuum pressures.

83

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

www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

Contamination

Contamination is usually identified by excessive background in the mass spectra. It can come from the GC or from the MSD. The source of the contamination can sometimes be determined by identifying the contaminants. Some contaminants are much more likely to originate in the GC, others are 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 of contamination and the level of contamination. Minor contamination by water or solvents can usually be removed by allowing the system to pump (with a flow of clean carrier gas) overnight. Serious contamination by rough pump oil, diffusion pump fluid or fingerprints is much more difficult to remove; it may require extensive cleaning. For further details contact your Agilent

Customer Engineer (CE).

Air Leaks

Air leaks are a problem for any instrument that requires a vacuum to operate. Leaks are generally caused by vacuum seals that are damaged or not fastened correctly.

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) www.agilent.com/chem • 800 227 9770 84

GC/MS SYSTEMS

85

Leaks can occur in many more places in the MSD:

• GC/MSD interface column nut

• side/top plate O-ring (all the way around)

• vent valve O-ring

• calibration valve

• high vacuum gauge tube fitting

• cracked ion gauge tube

• front and rear end plate O-rings

• GC/MSD interface O-ring (where the interface attaches to the vacuum manifold)

• diffusion pump co-seal and/or baffle adapter O-ring

• turbomolecular pump O-ring

• new Vespel/graphite ferrules contract when heated

Corrective Action

• Check interface nut for tightness.

Replace if necessary.

• Check leak/test the GC injection port.

Description

MS interface column nut

Column nut for GC/MS and two-hole ferrules

Universal Column Nut (2/pk)

Part No.

05988-20066

05921-21170

5181-8830

TIPS AND TOOLS

The most likely point for an air leak is a seal you recently opened.

Price

$13

$16

$26

Cleaning Solvents

It is common to see cleaning solvent peaks in the mass spectra shortly after the ion source is cleaned.

Corrective Action

• Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them. Refer to specific cleaning procedures in your MSD Hardware

Manual.

• Use a temperature that’s just above the boiling point of the solvent.

Fingerprints

Fingerprints contain hydrocarbons that can appear in mass spectra. Hydrocarbon contamination is characterized by a series of mass peaks 14 amu apart. The abundances of these peaks decrease as peak mass increases. Fingerprint contamination is usually caused by the failure to wear lint-free, nylon gloves during ion source cleaning, GC inlet maintenance, or from installing the column. Use special care to avoid recontamination of parts after you clean them. This typically occurs after some maintenance or part replacement.

Corrective Action

• Reclean using clean, nylon gloves and proper cleaning techniques.

Description

Nylon gloves, lint-free, Large

Nylon gloves, lint-free, Small

Part No.

8650-0030

8650-0029

Price

$16

$16

Diffusion Pump Fluid

If the diffusion pump is allowed to operate with no column (carrier gas) flow into the vacuum system, vapor from the diffusion pump fluid can drift up into the vacuum manifold. A more serious problem is when fluid is back streamed into the vacuum manifold by sudden or improper venting of the vacuum system. If a diffusion pump has back streamed, a prominent peak will often be seen at m/z 446 and the spectral baseline will exhibit increased background noise.

Corrective Action

• If m/z 446 appears please call Agilent for assistance.

www.agilent.com/chem • 800 227 9770

Foreline Pump Oil

Foreline pump oil contamination is characterized by peaks spaced 14 amu apart (hydrocarbons). Contamination with foreline pump oil is less common than contamination with diffusion pump fluid.

Corrective Action

• Call Agilent for assistance.

GC/MS SYSTEMS

Contamination Identification

The following table lists some of the more common contaminants, the ion characteristic of those contaminants, and the likely sources of those contaminants.

Common Contaminants

Ions (m/z) Compound

13,14,15,16

18, 28, 32, 44 or 14, 16

Methane

H

2

O, N

2

, O

2

, CO

2 or N, O

31, 51, 69, 100, 119, 131, 169,

181, 214, 219, 264, 376, 414,

426, 464, 502, 576, 614

31

43, 58

PFTBA and related ions

Methanol

Acetone

78 Benzene

91, 92 Toluene or xylene

105, 106

151, 153

69

Xylene

Trichloroethane

Foreline pump fluid or

PFTBA

Dimethylpolysiloxane 73, 147, 207, 221, 281,

295, 355, 429

77, 94, 115, 141, 168, 170,

262, 354, 446

149

Diffusion pump fluid

Plasticizer (phthalates)

Peaks spaced 14 amu apart Hydrocarbons

Possible Source

CI gas

Residual air and water, air leaks, outgassing from

Vespel™ ferrules

PFTBA (tuning compound)

Cleaning solvent

Cleaning solvent

Cleaning solvent

Cleaning solvent

Cleaning solvent

Foreline pump oil vapor or calibration valve leak

Septum bleed or methyl silicone column coating

Diffusion pump fluid and related ions

Vacuum seals (O-rings) damaged by high temperatures, use of vinyl or plastic gloves

Fingerprints, foreline pump oil www.agilent.com/chem • 800 227 9770 86

87

GC/MS SYSTEMS

Mass Spectrometer Symptoms

Sensitivity

Symptoms

This section describes some of the symptoms you might observe – either in the spectra of samples or in a tune report.

Typically, these symptoms fall into two broad classes:

1. those that affect the system sensitivity.

2. those that affect the repeatability of a measurement.

Some symptoms can be corrected by following the suggested corrective actions.

Others require the services of an Agilent

Customer Engineer.

Corrective Action

Wrong retention time

Low signal

Leaking injection port

Check GC, method, application and carrier gas velocity

Check GC, tune vacuum system

Clean the injection port

Replace the injection port liner and septa

Air leak

Peak widths

Check and tighten interface nut, leak test GC injection port

Do Autotune, check flow rate and temperature stability

Interfering peaks

Excessive background

Check time parameters, coeluting peaks, column type

Do Autotune and compare to background specifications

Check time parameters

Incorrect mass assignment Retune

Abnormal spectra – excessive background contamination

Incorrect tuning

Check for contamination

Check tune file, retune, check sample

Repeller voltage is too low Raise voltage to test for response

Dirty ion source Clean source

Repeatability

Symptoms Corrective Action

Dirty syringe needle

Wrong syringe needle

Leaking injection port

Injection is too large

Clean or replace the syringe

Replace syringe and septa

Perform injection port maintenance

Replace the injection port liner, septa, and liner o-ring

Check method and injection volume, split ratio and/or splitless purge time

Loose column connections Tighten column nuts on injection port or transfer line

Replace column nuts and ferrule

Variations in pressure, column flow, and temperature

Ensure the MSD is located in an environment where the temperature is stable

– Keep MSD out of drafts and direct sunlight

– Check that the carrier gas is steady and well regulated

– Service the foreline pump and/or diffusion pump

Clean source Dirty ion source

Loose connections in the analyzer

Ground loops

Check internal and external analyzer wiring connections, make sure all are secure

Check main electrical lines www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

Ion Source

The ion source operates by electron ionization (EI) or chemical ionization (CI).

The sample enters the ion source from the

GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting them. The positive voltage on the repeller pushes the positive ions into the lens stack, where they pass through several electrostatic lenses. These lenses concentrate the ions into a tight beam, which is directed into the mass filter.

5973 Ion Source Assembly (EI)

Maintaining the Ion Source

Cleaning procedures for MSDs vary. Refer to your MSD Hardware Manual for specific ion source cleaning procedures.

Common measures of instrument performance:

• abundance of certain ions (e.g.

percentage of the 502 ion from the

Autotune report)

• shape of lens ramps and the chosen voltages, especially Repeller Ramp

• sensitivity obtainable for a given analysis

• ability to tune to a given reference compound (e.g. DFTPP)

When to Clean:

The ion source should be cleaned:

• according to a customer’s predefined schedule

• based on instrument performance (e.g.

deteriorated performance over time)

Frequency of Cleaning

The cleaning frequency is determined by:

• the number of samples run (throughput)

• the type of samples

• unique, established laboratory protocol

Selecting a Cleaning Method

The primary action of any cleaning procedure is to remove contamination from surfaces. Removing this contamination restores the electrostatic properties of the ion source lensing system. Numerous cleaning methods have been developed for restoring ion source performance. The cleaning methods include abrasive, sonic, and electropolish.

Abrasive methods offer several advantages:

• provide adequate energy to remove contamination from surfaces

• require minimal equipment

• pose minimal risks to the user

A popular material used to abrasively clean stainless steel ion source parts is aluminum oxide. It is available in either powder form or an abrasive film. After the critical surfaces have been abrasively cleaned, the loose particles must be removed. One method of removing particles is swabbing with a cotton swab or a clean cloth dipped in acetone. A clean swab should be used for each element followed by a sonication. These cleaning supplies are listed on page 89.

Preparing to Clean

Prior to cleaning, the mass spectrometer must be vented and the ion source must be removed. Before venting the system, the following conditions must be met:

• heated zones are less than 100°C

• the diffusion pump is off and cool

• the turbo pump is off and not spinning

• the rough pump is off

Always allow the automatic venting routine to run its full course. Improper venting may cause diffusion pump fluid to be deposited into the analyzer (backstreaming). It can also reduce the life of the multiplier, or other sensitive MS parts.

TIPS AND TOOLS

Agilent’s new MS Inert Ion Source improves inertness – and maintains it over multiple cleanings . For more information see page 90.

www.agilent.com/chem • 800 227 9770 88

GC/MS SYSTEMS

Cleaning and Maintenance Supplies

89

Description

Cleaning and Maintenance

Nylon gloves, lint-free, Large

Nylon gloves, lint-free, Small

Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk)

Generic ion source cleaning kit for all GC/MS types

Includes: Cloths, lint-free (15/pk), Abrasive sheets (5/pk), Cotton swabs

(100/pk), Nylon gloves, lint-free, Alumina powder, abrasive

Cloths, lint-free (15/pk)

Abrasive Sheets, aluminum oxide green lapping paper for ion source cleaning, 600 mesh (5 sheets)

Alumina powder, abrasive

PFTBA sample, certified (10 g)

PFTBA sample kit, 1 mL

Activated alumina, absorbent pellets for Edwards rough pump traps, non-LC/MS (1 lb can)

PFTBA glass vial

Cotton swabs (100/pk)

Tools

Screwdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws

Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws

Wrench, open-end, 1/4 x 5/16 in.

Screwdriver, TORX, T15

Screwdriver, TORX, T10

Ferrules and O-rings

Teflon 1/4 in. ferrule (back)

Teflon 1/4 in. ferrule (front)

Retainer rings (10/pk)

5973 One Year Maintenance Kit (for diffusion pump systems)

Includes: Big Universal Trap for He, Abrasive sheets (5/pk),

Cloths, lint-free (15/pk), Cotton swabs (100/pk), SantoVac Ultra,

18.5 mL (2 ea.), Rough pump oil, 1 liter, Filament assembly,

Octafluoronapthalene (OFN)

MSD Tool Kit

Includes: Small cleaning rod, Large cleaning rod, Source hold tool,

Cotton swabs (100/pk), Nylon gloves, lint-free, Abrasive sheet,

30 mm (5/pk), Tool kit (wrenches, driving tools)

Price

$ 16

$ 16

$185

$124

$ 16

$ 25

$ 24

$ 38

$ 24

$ 8

$ 8

$ 10

$657

$ 64

$ 27

$ 29

$168

$ 85

$115

$ 14

$ 10

$510

Part No.

8650-0030

8650-0029

9310-4828

5181-8863

05980-60051

5061-5896

8660-0791

8500-0656

05971-60571

8500-1233

05980-20018

5080-5400

8710-0899

8710-0900

8710-0510

8710-1622

5182-3466

0100-0160

0100-0787

5181-1258

5183-2096

05971-60561 www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

5973 MSD Ion Source Parts (EI)

Item Description

(A) Ion source body

(B) Repeller

(J) Washer, M3 (1/pk)

(K) Nut, 5.5 mm

(L) Ion Source Sensor

(M) Lens insulator, (2/pk)

Ion source assembly

Source heater assembly

Repeller assembly

Screw (for filament on the source)

5973 Part No.

G1099-20130

G1099-20132

G1099-20136

05971-20134

G1072-20008

05971-20143

05971-20126

G1099-20133

0515-1446

3050-0891

0535-0071

G1099-60104

05971-20130

G1099-60106

G1099-60177

G1099-60170

0515-1046

Price

$ 3

$ 1

$ 1

$ 200

$ 270

$ 270

$ 408

$ 481

$ 2

$ 198

$ 112

$ 29

$ 69

$ 190

$ 263

$ 105

$ 82

H

D

E

F

M

5973 Ion Source Parts (EI).

G

M

A

C

L

MS Inert Ion Source Parts

Description 5973A 5973N 5973 inert** Price

Drawout plate – 3 mm Inert

Drawout plate – 6 mm Inert** G2589-20045 G2589-20045

EI High Temp Filament

Repeller assembly, Inert source G1099-60170 G1099-60170

Screws for filament High Temp 0515-1046

Source body, Inert G1099-20130

0515-1046

G1099-20130

Source Washer, Inert

G2589-20100 $ 99

G2589-20045 $ 225

G2590-60053 $ 97

G2589-60102 $ 499

G1999-20021 $ 3

G2589-20043 $ 563

G2589-20101 $ 12

I

I

K

J

H

5973 Repeller Assembly (EI).

L

H

B

**used in G2860A and G2860B extended linearity kits www.agilent.com/chem • 800 227 9770 90

GC/MS SYSTEMS

91

B

A

D

F

C

E

B

G

5972/5971/GCD Ion Source (EI)

5972/5971/GCD MSD Ion Source Parts (EI)

Description

(A) Entrance lens

(B) Lens insulator, (2/pk)

(C) Ion focus lens

(D) Drawout cylinder

(E) Drawout plate

(F) Ion source body

(G) Set screw

(H) Repeller assembly

(I) Screw (for filament on the source)

H

I

5972/5971/GCD Part No.

05971-20126

05971-20130

05971-20143

G1072-20008

05971-20134

05971-20128

0515-1446

05971-60170

0515-1046

TIPS AND TOOLS

It is good practice to replace scratched lenses and other ion source parts.

Scratched source parts lead to poor performance.

Price

$ 108

$ 278

$ 271

$ 190

$ 71

$ 531

$ 3

$ 593

$ 2

Ion source assembly

Transfer line tip, gold-plated

5972 Part No.

Price

05972-60226 $3554

5972/5971 Part No.

05971-20305

Price

$ 242

GCD Part No.

G1800-20305

Price

$259

MSD Flowrates (ml/min)

Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates below for flow limitations.

5973

5972

5971

GCD

Min

0.1

0.1

0.1

0.1

Max Diff Pump

2.0

2.0

1.5

1.0

Max Turbo Pump

4.0

NA

NA

NA

Tuning Max

2.0

2.0

1.0

1.0

www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

Filaments

Two filaments are located on opposite sides outside of the ion source. The active filament carries an adjustable ac emission current. The emission current heats the filament, causing it to emit electrons; these electrons ionize the sample molecules. In addition, for the 5973 and 5972, both filaments have an adjustable dc bias voltage. The bias voltage determines the energy on the electrons, usually -70 eV.

Maintaining the Filaments

Like the filament in an incandescent light bulb, the ion source filaments will eventually burn out. Certain practices will reduce the chance of early failure:

Tips to increase filament life

• When setting up data acquisition parameters, set the solvent delay so that the analyzer will not turn on while the solvent peak is eluting.

• When the software prompts Override

solvent delay at the beginning of a run, always select “No.”

• Higher emission current will reduce filament life.

• If you are controlling your MSD from the

Edit Parameters screen, always select

MS Off before changing any of the filament parameters.

It is very useful to switch from one filament to the other every three months so that when one filament fails, you know the other will fail soon. This will allow you to change both filaments at the same time, which helps to maximize your instrument uptime.

Filament Assembly

Description Unit

Filament, 5973 (EI)

Filament, 5973 (CI)

Filament, EI High Temperature for the 5973 inert

Filament, 5972 (EI/CI)

Filament, 5971 (EI/CI) / GCD (EI)

2/pk

Part No.

05972-60053

G1099-80053

G2590-60053

05972-60053

05971-60140

Price

$ 90

$282

$ 97

$ 90

$159

Quadrupole Mass Filter

The mass filter does not require periodic maintenance. It should not be removed from the radiator or distributed in any way.

• Never put the quadrupole in an ultrasonic cleaner.

• Never change the physical orientation of the quadrupole mass filter.

• The fused-quartz quadrupole is fragile and will break if dropped or handled roughly.

• The material in the cusps of the quadrupole is very hygroscopic. If exposed to water, the quadrupole must be dried very slowly to prevent damage.

• Cleaning techniques appropriate for other manufacturers’ instruments are not suitable for Agilent MSDs – and may actually harm the mass filter.

• To save time and effort, use only Agilent

MSD mass filters, which do not require periodic cleaning or maintenance.

• In case of extreme contamination, contact a trained Agilent service representative to perform the mass filter cleaning.

www.agilent.com/chem • 800 227 9770 92

GC/MS SYSTEMS

Vacuum Systems and Pumps

Vacuum System Operation

The vacuum system creates the high vacuum (low pressure) required for the

MSD to operate. Without this vacuum, the molecular mean free path is too short.

Ions cannot travel from the ion source through the mass filter to the electron multiplier (detector) without colliding with other molecules.

The major components of the vacuum system are:

• Vacuum manifold

• Foreline gauge

• Calibration valve

• Gauge controller (optional)

• Vacuum seals

• Foreline pump and/or trap

• Diffusion/turbo pump and fan

• High vacuum gauge tube

A properly maintained vacuum system will:

• Prevent premature filament failure

• Provide better sensitivity

• Require less frequent source cleaning

• Extend quadrupole lifetime

• Prevent premature EM Horn failure

MAINTENANCE MINDER

Keeping a pan under the vacuum pump helps to detect and identify the origin of oil leaks.

93

Calibration

The calibration valve is an electromechanical valve with a vial that contains a tuning compound. Perfluorotribuylamine (PFTBA) is the most commonly used tuning compound. It is required for automatic tuning of the MSD in EI mode. The tuning compound is usually a liquid but can be volatile or semi-volatile solid.

How to Refill

The calibration vial can be refilled without venting the system. Fill the vial to 0.5 cm from the top. DO NOT overfill. Air is trapped in the vial when it is refilled.

Description

PFTBA sample, certified (10 g) (EI)

PFDTD sample (10 g) (CI)

Part No.

8500-0656

8500-8130

Price

$168

$ 43

This sometimes causes an “Excess source pressure” error message during the first tune after refilling. This is more likely if the vial is overfilled. Be sure to purge the air upon refilling the vial.

MAINTENANCE MINDER

If using the 5973 with a CI source, use Perfluorodimethyltrioxadodecane

(PFDTD) sample.

www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

Pressure Symptoms

This section describes unusual pressure readings and their possible causes. The symptoms in this section are based on typical pressures. At typical column flow rates (0.5 – 2.0 ml/minute), the foreline pressure will be approximately 20 to 100 mTorr. The vacuum manifold pressure will be approximately 1 x 10-6 to 1.4 x 10-4 Torr.

These pressures can vary widely from instrument to instrument so it is important that you are familiar with the pressures that are typical for your instrument at a given carrier gas flow and oven temperature.

The foreline pressures listed can only be measured on diffusion pump-equipped systems. Turbomolecular pumps are controlled according to their speed and do not have foreline pressure gauges.

The vacuum manifold pressures can only be measured if your system is equipped with the optional gauge controller.

Foreline pressure is too high

Symptom • Pressure is above 100 mTorr.

• 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.

www.agilent.com/chem • 800 227 9770 94

GC/MS SYSTEMS

Diffusion Pump

It is not necessary to change the diffusion pump fluid more than once a year, unless you observe symptoms that suggest a problem with the diffusion pump fluid. The

MSD must be vented in order to check the diffusion pump fluid (except for the 5973).

Therefore, the best time to check the fluid is when the instrument is already vented for other maintenance.

Importance of the Fluid Level

The amount of fluid in the pump affects the amount of vapor and the temperature of the base plate. Too little fluid will cause the pump to run at a higher temperature because there is less fluid to carry away the heat resulting in fluid cracking or degradation and loss of high vacuum. It will also lower the pumping speed because there is less fluid vapor available to pump away gases which can especially affect operation in

CI Mode due to higher flow rates.

How to Check the Fluid Level

1. If it is not vented already, shut down and vent the MSD according to instrument manual.

2. Unplug the MSD power cord.

3. Remove the pump and cover the top with 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 particulate material, the fluid must be changed.

6a. Use a metal ruler to determine the depth of the fluid. A pump that has been in operation should have a pool

9 mm plus or minus 1 mm deep. Fluid in freshly charged pumps will be 12 mm deep. It is normal that up to 2 ml of oil may be in the rear portion of the vacuum manifold. The recommended total fluid charge for the 5971/5972 is

18 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

Diffusion pump fluid: SantoVac Ultra 5P,

18.5 ml (5973, 5972 or 5971/GCD)

Ion gauge controller (5973/5972A)

Ion gauge tube for measuring vacuum (5971/5972)

Triode gauge tube for measuring vacuum (5972/5973)

Part No.

Price

6040-0809

59864B

0960-0376

0960-0897

$ 82

$1399

$ 195

$ 358

95

Foreline Pump

The oil in the foreline or rough pump should be replaced on average once every six months, but can vary depending upon applications. After oil replacement, if the foreline trap is present, the molecular sieves should be replaced.

Avoid contact with the pump oil. The residue from some samples may be toxic.

Dispose of used oil properly.

Description

Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD)

Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD)

Molecular sieve (5973, 5972 or 5971/GCD)

Oil mist filter RV3/E1M18/E2M18/E2M2

Oil mist filter E2M1.5

Oil mist filter E2M18

Part No.

6040-0798

6040-0834

9301-1104

3162-1056

G1099-80037

5063-5224

Price

$122

$ 39

$ 57

$430

$173

$417 www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

General Instructions on How to Replace the

Pump Oil

1. Shutdown and vent the MSD.

2. Place a container under the drain plug on the foreline pump.

3. Remove the fill cap from the top of the pump to expose the fill hole.

4. Remove the drain plug from the pump.

5. Reconnect the MSD to its power source. Switch on for 2 or 3 seconds, and then switch it off again. This displaces old oil from the internal pump cavities. Disconnect the power cord again.

6. Reinstall the drain plug and pour pump oil into the fill hole.

7. Reinstall the fill cap.

8. Reconnect the MSD power cord.

9. Start up and pump down the MSD according to the Instrument Manual procedure.

TIPS AND TOOLS

Use chemical-resistant gloves and safety glasses when replacing pump fluid. Avoid contact with the fluid. Always dispose of used oil properly.

Electron Multipliers and Replacement Horn

Description

Electron multiplier replacement horn

(5973, 5972, 5971/GCD)

High energy dynode (5973 only)

Electron multiplier kit (5972, 5971/GCD only)

Part No.

05971-80103

G1099-80001

05971-80102

Price

$1004

$2131

$1136

Maximize Lifetime

The lifetime of an EM is directly related to the current that flows through it and the extent of contamination or condensation that it experiences. To maximize electron multiplier life:

• Maintain the best possible vacuum, especially in the analyzer manifold.

• Use extreme caution and be conservative with venting, pumpdown, and all vacuum system procedures to keep pump fluid background to a minimum.

• After venting, allow four hours for pumpdown and thermal equilibration before scanning.

• Actively look for background contamination and leaks and repair them immediately.

• Don’t tune excessively. PFTBA can result in higher background over an extended period of time.

Symptom

• Voltage is over 2500 volts

• Poor vacuum

Corrective Action

• Replace electron multiplier www.agilent.com/chem • 800 227 9770

TIPS AND TOOLS

Use only Agilent replacement multipliers and horns for Agilent MSDs.

Other manufacturers’ products can increase noise, while reducing sensitivity and linearity.

96

97

GC/MS SYSTEMS

Maintaining the MS Engine

Maintenance Schedule

• Always wear clean, lint-free, nylon gloves when handling parts which will come in contact with the sample stream. Oil from your fingers is a particularly difficult contaminant to remove.

• If you must set parts down, place them on clean, lint-free cloths or clean aluminum foil, not directly onto a laboratory bench.

• Keep parts covered so that dust does not accumulate on them.

• Do not leave the interior of the vacuum system open to the atmosphere. For example, if you are removing the ion source for cleaning, put the vacuum manifold cover back in its normal position after you have removed the source. Re-establish a low vacuum in the vacuum manifold until you need to reinstall the ion source.

Common maintenance tasks are listed on page 83. Performing these tasks on a regular basis can reduce overall operating costs.

Keep a record (logbook) of system performance characteristics and maintenance operations performed.

This makes it easier to detect variances from normal operation and to take corrective action.

Cleaning the Ion Source

There is not a regular interval for ion source cleaning. The ion source should be cleaned when symptoms indicate. Symptoms of a dirty ion source include poor sensitivity and inadequate abundances at high masses.

See the Troubleshooting chapter in your hardware manual for more information about these symptoms.

MS Engine Pump Lubricants and Oils

5989 or Thermo or 5985 or 5999x, 5993x

5988 Electro Spray 5987 or 5995x Part No.

Lubricant Oil

Turbo pump lubricant:

Balzers turbo pump lubricant, 0.25 liter

Diffusion pump oil:

SantoVac 5, 1 liter

SantoVac 5, 128 ml

Rough pump oil:

Rough pump oil, 1 gal Inland 45

Rough pump oil, 1 liter Inland 45

Particle Beam pump oil, Fomblin

6040-0468

6040-0370

6040-0819

6040-0798

6040-0834

6040-0730

Price

$ 134

$2553

$ 283

$ 133

$ 40

$ 760 www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

We strongly recommend keeping a log of all system performance and routine maintenance operations. That way, problems that might impact performance can be identified and resolved quickly.

The most common maintenance tasks are listed in the table below.

Task

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

Every Every Every As

Week 3 Months 6 Months Needed

We recommend keeping a separate set of tools that have been thoroughly cleaned for working with the MS engine.

These tools are needed to prevent contamination when reassembling or installing clean assemblies such as the ion source.

www.agilent.com/chem • 800 227 9770 98

GC/MS SYSTEMS

Ion Source Parts and Supplies

Many of the tools and supplies needed to service the 5989 MS Engine are included in the installation kit supplied with the instrument. The following tables list common consumable parts and supplies used in the maintenance of the MS Engine.

A

5989 Lens Stack

C

B

Description

(A) Clamp insulator, ion source

(B) Entrance lens

(C) Lens insulator, ion source

(D) Plate insulator, ion source

(E) EI/CI repeller

(F) Repeller insulator

Filament block

Filament assembly

Heater cartridge

Part No.

05989-20110

05989-67002

05989-20111

05989-20109

05989-20145

05989-20119

05989-20165

05985-60179

05989-60098

Price

$108

$990

$ 62

$ 88

$318

$580

$448

$ 58

$926

D

E

F

5989 Repeller Assembly

99

Replacement Parts and Supplies

The electron multiplier lifetime on the 5989 may be 6 to 9 months or shorter, especially with the following applications:

• Thermospray

• Particle Beam

• Purge and trap, with no jet separator

• Extensive CI

• High sensitivity work with high EM voltage

Description

5989

Electron multiplier kit

Electron multiplier replacement horn

Parts and Supplies

Ion gauge tube, K-25 flange

O-rings and Seals

Insulating ring

O-ring, detector flange (5/pk)

Diffusion pump fluid fitting fill and drain cap O-ring (12/pk)

KF 25 centering ring and O-ring

O-ring, manifold window

Part No.

05989-80043

05971-80103

0960-0799

05989-20705

5181-3367

0905-1145

3162-0110

0905-1189

Price

$2012

$1004

$ 448

$ 18

$ 47

$ 19

$ 39

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

GC/MS SYSTEMS

General GC/MS Supplies

Contents:

• Start-Up Guide, pub. No. 5988-3073EN

• Application Note, “Improvements in the

Agilent 6890/5973 GC/MSD System for use 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 0.5um

HP-5 MS, part no. 19091S – 139

• Single-taper splitless liner, 4mm i.d., deactivated, part no. 5181-3316

• Direct Connect Liner, single taper, 4mm i.d., deactivated, part no. G1544-80730

• Direct Connect Liner, dual taper, 4mm i.d., deactivated, part no. G1544-80700

• Floppy Disk with tuning macros

Description

8270 Semi-Volatiles Applications Kit

Part No.

G2860A

G2860A 8270 Semi-Volatiles

Applications Kit

The G2860A 8270 Semi-Volatiles

Applications Kit is designed for use in

Agilent 6890/5973A and 6890/5973N

GC/MSD Systems. The kit provides modified and/or pretested components to improve system performance for USEPA

Method 8270. With the kit, system linearity is maximized and activity is minimized.

Price

$2333

LIBRARY

There are many ways to perform semi-volatile analysis. For another option that also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem and do a library search for 5989-1510EN.

www.agilent.com/chem • 800 227 97700 100

GC/MS SYSTEMS

Test and Performance Samples

Each GC/MS has a specific test and performance sample. Refer to the chart below for the exact sample.

MSD

Tuning Samples

EI CI

Tune Tune EI

Verification Samples Performance Checkout Samples

Negative Positive

Mode CI Mode CI Semi-Volatile Volatile

5973

5972

5971

GCD

PFTBA PFDTD

PFTBA PFTBA

OFN 1 pg/µL

HCB 10 pg/µL

PFTBA PFTBA HCB 10 pg/µL

PFTBA NA Sample A (10 ng/µL)

OFN 1 pg/µL Benzophenone 100 pg/µL

NA

NA

NA

Benzophenone 100 pg/µL

Benzophenone 100 pg/µL

NA

DFTPP

DFTPP

DFTPP

DFTPP

BFB

BFB

BFB

BFB

MS Engine

5989A

5989B

PFTBA PFTBA HCB 50 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL

PFTBA PFTBA HCB 20 pg/µL OFN 500 fg/µL Benzophenone 100 pg/µL

DFTPP

DFTPP

BFB

BFB

101

EASY ONLINE ORDERING

Visit the Agilent website at www.agilent.com/chem/4ecatalog for one-click access to:

• Product pricing links (when available)

• Local sales contact information

• Online quote requests

• Order status updates … and more www.agilent.com/chem • 800 227 9770

GC/MS SYSTEMS

Description

Evaluation Sample for GC/MS Systems

Contains 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

GC/MS Tuning Standard contains:

DFTPP, Benzidine, Pentachlorophenol, and p,p’-DDT 1 mg/mL in methylene chloride

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

Extended Mass Performance Sample

PFTBA certified

PFTBA Sample Kit

PFDTD

Benzophenone

Hexachlorobenzene

Hexachlorobenzene

Methyl stearate (in methanol);

PFTBA not certified

Octafluoronapthalene (OFN)

Octafluoronapthalene (OFN) p-Bromofluorobenzene (BFB)

Quantity

1 ng/µL (2 ea)

1 pg/µL,

5 ampoules

500 fg/µL

25 µg/mL

Part No.

Price

05970-60045 $ 46

8500-5995 $ 62

0.5 g, fomblin oil

1 bottle, 10 g

0.5 mL

10 g

8500-6406

8500-5500

8500-0656

05971-60571

8500-8130

100 pg/µL,

5 ampoules 8500-5440

10 pg/µL, 4 ampoules 8500-5808

1 ng/µL, 2 ampoules

20 pg/µL 8500-6405

$ 38

$141

$168

$ 85

$ 44

$ 74

$ 39

$ 32

05990-60075 $ 67

8500-5441

8500-6572

8500-5851

$ 67

$ 30

$ 39 www.agilent.com/chem • 800 227 9770 102

You asked … we listened!

Announcing the launch of our new Life Sciences and

Chemical Analysis website.

Based on customer feedback, we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.

The new site features:

• A coherent page design – that Automatically detects

screen resolution and optimizes the page size for less scrolling.

• An expanded navigation – that includes links to

product literature, technical support, education, events, and news.

• A newly designed online store – with fast access to

pricing, order status, quotes, and local sales information.

• Direct links – to the services, parts, and consumables that

keep your instruments running in top condition.

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

www.agilent.com/chem • 800 227 9770

Services & Support

Every Agilent GC and GC/MS system is backed by our nearly 40 years of experience with instrument design, lab operations, business processes, and regulatory requirements.

We stand behind our products with …

• Immediate technical assistance by phone or online.

• Prompt onsite service from Agilent-certified

Engineers.

• A variety of service options, including maintenance, repair, compliance, and consultation.

• Industry-leading training courses to help increase your lab’s overall knowledge base.

Our professionals are standing by to help you solve problems and optimize your resources.

So you can spend more time running samples, developing methods and meeting production deadlines – and less time arranging for instrument services.

“Our customers know they can rely on Agilent's expertise and resources to keep their instruments running at top performance."

Yukiko Sameshima

Customer Engineer

104

SERVICES & SUPPORT

Our focus is on keeping your lab running at peak performance.

105

A Total Commitment to Your Lab for One Fixed Cost.

Agilent service agreements operate under a yearly fixed cost, which includes preventative maintenance, compliance, telephone support, repairs, parts, and labor. No matter how many service visits or replacement parts you need, this fixed cost covers it all – at no additional charge.

If you choose, you can also consolidate instrument maintenance and repair services into multi-year agreements for administrative ease and greater cost savings.

The Unmatched Expertise of Fully Trained Engineers.

You can rest assured that the engineer who arrives at your site will perform the requested 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-approved replacement parts, columns, and supplies to ensure peak instrument reliability.

• Carry calibrated, traceable tools and testing equipment, as well as Agilent hardware and software qualification protocols.

What’s more, most Agilent engineers are part of the Agilent product development team. So you can be certain that ease of repair, maintenance, and compliance are built into your GC and GC/MS systems right from the start.

The Flexibility to Select The

Solution That’s Right for You.

Our team will work with you to help your laboratory achieve …

• Maximum uptime

• High productivity

• Total compliance

• Extended instrument life

• Fast problem resolution

• Verified system performance

• The skills and knowledge you need for efficient operation and maintenance

• Consistent, in-depth documentation

• Reduced administrative burdens www.agilent.com/chem • 800 227 9770

SERVICES & SUPPORT

Agilent Services

Telephone Service

Software Service

Features Advantages to You

• Telephone access to skilled Agilent service professionals.

• Available parts option.

• Fast identification and resolution of hardware problems.

• Low cost.

• Telephone access to trained technical professionals.

• Enhancements to the original application software purchase.

• Software bulletins that identify discovered defects and recommend workarounds.

• Fast identification and resolution of software problems.

• A fixed annual cost for software upgrades makes budget management more predictable.

• A single cost-effective source for telephone support and software updates.

• A convenient way to keep up with the latest software enhancements.

Onsite Instrument Repair • Hardware telephone support with access to skilled, factory-trained Agilent service professionals.

• Travel expenses and labor.

• Optional coverage for consumables used during repair.

• A fixed annual cost for parts makes budget management more predictable.

• You can choose the response method that fits your business needs and budget.

Offsite Instrument Repair

For selected Agilent analysis instruments

• Option 1: Replacement with an identical instrument (your fastest choice).

• Option 2: Return to Agilent for repair.

Preventative Maintenance

For selected Agilent analysis instruments

• Expert cleaning, adjustment, lubrication, and inspection of your instrument.

• Travel expenses and labor.

• Coverage for consumables used.

• Less expensive than onsite repair.

• Fast and easy.

• Includes extensive diagnostics and testing that are not feasible with onsite maintenance or repair.

• Maximum uptime.

• Extended instrument life.

• Confidence in the integrity of your measurements.

www.agilent.com/chem • 800 227 9770 106

SERVICES & SUPPORT

Agilent Services

Installation Qualification (IQ)

Advantages to You

• Supplies the evidence you need to satisfy regulatory agencies.

• Helps fulfill the master validation plan – and change-control SOP requirements – for the IQ phase.

Operational Qualification/Performance

Verification (OQ/PV)

For selected Agilent analysis instruments

Note: We recommend Preventative

Maintenance before OQ/PV.

• Verification and documentation of an instrument’s ability to meet specified criteria.

• Procedures and documentation that fit the requirements of GLP, ISO 9000, and other regulatory agencies.

• Full automation to increase the qualification scope without excess time requirements.

• Measuring equipment that is traceable to national and international standards.

• Supplies the evidence you need to satisfy regulatory agencies.

• No need to write your own SOPs to qualify Agilent instruments – or to train your staff.

• Consistent, traceable results among all your laboratories – and improved method transfer.

• Confidence in the integrity of your measurements, with traceable, documented chains from sample introduction to reporting.

• Less risk of financial loss due to noncompliance.

• Meaningful, relevant, and understandable system tests.

Requalification (RQ) After Repair

For instruments that have their operational performance verified by an annual OQ/PV.

Features

• Qualification and documentation of shipment completeness.

• Comprehensive system and application software verification tests.

• Delivered by professionals with training certification.

• Verification that a system is performing at operation specifications after repair.

• Complete system operation testing.

Note: only a subset of the Operational

Qualification test is performed, based on the type and extent of the repair.

• A comprehensive test of the repaired module using established conditions and known sample characteristics to ensure the basic accuracy and precision of your module.

• Measuring equipment is traceable to national and international standards.

• Minimal system downtime after completion of instrument repair.

• Efficient system requalification by performing the appropriate tests based on the components repaired.

• Assurance that all instrument subsystems are performing within specifications.

• All procedures and documentation meet regulatory agency requirements.

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

SERVICES & SUPPORT

Agilent Services

Network Qualification

Features Advantages to You

Mass Spectrometer Ion Source Cleaning

For selected Agilent analysis instruments

• Network definition and performance testing using established Agilent Design,

Installation Qualification, and Operational

Qualification protocols.

• Documentation of the definition, integrity, supportability, and health of high-risk network segments.

• Completed protocols, created using hardware and software network testing tools. 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, and evaluates its operation over a controlled range of traffic conditions. We’ll also provide the following reports:

- Long Duration Network Characterization, which analyzes each function in its operating environment.

- Performance Predictability Analysis, which documents reserve capacity and stability over a range of operating demands.

• Significant time savings.

• Increased uptime – issues that might impact application performance are quickly identified and resolved.

• Improved consistency – network qualification protocols are developed according to a quality lifecycle, and are maintained under version and revision control.

• Increased control – Agilent will verify known elements and identify unknown network contingency states that may impact application performance.

• Reduced regulatory exposure – audit-ready documentation establishes evidence of network system control.

• Onsite disassembling

• Cleaning

• Reassembling

• Testing

• Your staff can devote more time to chemistry, not instrument maintenance.

• Efficient cleaning with minimal downtime.

www.agilent.com/chem • 800 227 9770 108

SERVICES & SUPPORT

Agilent Services

Software Backup

Features

• Telephone or onsite factory support to facilitate restoration.

• Captures the unique system settings for all software components needed to reconstruct 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

Advantages to You

• Fast and easy – you simply insert a disk

… reboot … and you’ll be back in operation in as little as two hours.

Normally, you would have to reload and reconfigure your software – a process that can take days.

• A complete solution – the initial configuration 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

109

TIPS AND TOOLS

To learn more about Agilent’s complete portfolio of services, please visit www.agilent.com/chem/service.

www.agilent.com/chem • 800 227 9770

SERVICES & SUPPORT

Education & Training Services

Highly trained lab professionals can boost your productivity, minimize errors and reruns, and expand your chromatography capabilities. And that’s why Agilent offers several training options that cover everything from troubleshooting and maintenance to the most advanced operational techniques. eLearning

Agilent’s e-Learning program features a series of focused, economical and individualized instrument training modules designed to enhance and simplify your learning experience. From theory and operations... to common problems with your instruments... eLearning is available when you want it, where you want it, and how often you want it. All you need is Internet access!

You can review and register for our e-Learning offerings by visiting www.agilent.com/chem/elearning

Course Title

6890 GC Split Inlet Mode Operation

Duration

Self-paced;

Four hours access

6890 GC Splitless Inlet Mode Operation Self-paced;

Four hours access

6890 GC Purged Packed Inlet Operation Self-paced;

Four hours access

Description

Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in split mode.

Clarifies flow paths, so you can gain the maximum benefit from this inlet operational mode.

Discusses typical problems and routine maintenance procedures.

Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in splitless mode.

Clarifies flow paths, so you can gain the maximum benefit from this inlet operational mode.

Discusses typical problems and routine maintenance 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 routine maintenance procedures.

www.agilent.com/chem • 800 227 9770 110

SERVICES & SUPPORT

Course Title

6890 GC Keyboard Operation

6890 GC FID Theory and Operation

Duration

Self-paced;

Four hours access

Self-paced;

Four hours access

6890 GC ECD Theory and Operation Self-paced;

Four hours access

6890 GC TCD Theory and Operation Self-paced;

Four hours access

GC Automatic Liquid Sampler Operation Instructor-led;

60-90 minutes

Description

Reviews the basic operation of the 6890

GC keyboard.

Thoroughly describes all keys, so you can gain 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 routine maintenance procedures.

Reviews the basic theory and operation of the ECD.

Covers proper column installation, keyboard setup, and flow optimization.

Discusses typical problems and routine maintenance procedures.

Reviews the basic theory and operation of the TCD.

Covers proper column installation, keyboard setup, and flow optimization.

Discusses typical problems and routine maintenance procedures.

Reviews the basic operation of the 7683A automatic liquid sampler system (ALS).

Shows you how to gain maximum productivity from the ALS.

Discusses routine maintenance procedures, and how to return an ALS to Agilent for repair or exchange.

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

Course Title

Logical GC Troubleshooting

Duration

Instructor-led;

60-90 minutes

Using the GC/MSD

Security ChemStation to Achieve

FDA CFR Part 11 Compliance

Managing and Administering the

GC/MSD Security ChemStation to Meet FDA CFR Part 11

Compliance Requirements

Designed for systems administrators

Instructor-led;

60-90 minutes

Instructor-led;

60-90 minutes

SERVICES & SUPPORT

Description

Teaches a methodical process for troubleshooting GC system problems.

Helps you identify the source of problems quickly, making troubleshooting less daunting.

Note: This course does not discuss hardwarespecific problems or solutions.

Describes in detail how to operate the

GC/MSD Security ChemStation software in accordance with FDA CFR Part 11 requirements.

Shows you how to manage the GC/MSD

Security ChemStation software in accordance with FDA CFR Part 11 requirements.

www.agilent.com/chem • 800 227 9770 112

SERVICES & SUPPORT

Classroom Training

Agilent’s training courses for gas chromatography and mass spectrometry help new and experienced lab professionals learn proper and efficient ways to use analytical instruments and software. 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 information about our training and services. Or visit

www.agilent.com/chem and select

“Education.”

Course Title

Technique

Introduction to Capillary GC

Techniques of GC

Introduction to GC-MS

Techniques of GC-MS

Hardware/Software Operation

ChemStation Operation for the 6890 GC/ALS

Operation of the GC-MSD System

Using the ChemStation for GC-MSD

GC-MSD System for Environmental Applications

Course No.

No. of Days Description

H2615A

H4002A

H2609A

H4040A

H5926A

H4043A

H4050A

1

5

1

3

5

5

5

Provides an overview of capillary gas chromatography in a lecture format.

Presents the fundamental concepts of gas chromatography.

Introduces the technique of GC-MS in a lecture format that includes worksheet exercises.

Reviews the key concepts of the GC-MS analysis process, as well as qualitative and quantitative GC-MS techniques.

Explains how to operate the Agilent 6890 GC using GC

ChemStation software.

Enhances an operator’s efficiency and productivity when using the Agilent GC-MSD system.

Provides experience in data acquisition and analysis, library searching, reporting, and customizing the system to meet specific laboratory or customer needs.

Increases an operator’s skill in using a mass selective detector with mass spectrometer EnviroQuant software.

Troubleshooting and Maintenance

6890 GC Maintenance

5890 GC Maintenance

6890 GC Troubleshooting and

Preventative Maintenance

H5308A

H4001A

H5309A

4

4

1

Addresses preventative maintenance and first-level repair for the Agilent 6890 GC.

Addresses preventative maintenance and first-level repair for the Agilent 5890 GC.

Introduces troubleshooting of the Agilent 6890 GC in a lecture format.

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

SERVICES & SUPPORT

Course Title

Introduction to 5973 GC-MSD Troubleshooting and Preventative Maintenance

Course No.

No. of Days

H5947A 1

Description

5973 GC-MSD Troubleshooting and Preventative Maintenance H2294A 3

Demonstrates how to perform preventative maintenance and troubleshooting to keep the

Agilent 5973 GC-MSD system working properly.

Includes a discussion of typical vs. problem

Auto-Tunes.

Offers class exercises that enhance understanding of troubleshooting and maintenance principles.

Covers tuning and diagnostics, the vacuum system, the 5973 MSD ion source, the quadrupole mass filter, and the 5973 MSD.

Includes hands-on laboratory exercises to demonstrate and practice the principles conveyed.

Data Analysis and Reporting

ChemStation for GC Data Analysis and Reporting H2606A 3

Data Analysis and Reporting Using the

ChemStation for GC-MSD

Data Analysis and Reporting Using the EnviroQuant ChemStation for GC-MSD

H4076A

H4053A

3

3

Teaches the operation of the Agilent GC

ChemStation software through instructor explanations, combined with extensive hands-on and laboratory exercises.

Specifically focuses on data analysis and reporting.

Enhances skills in using the Agilent ChemStation for GC-MSD.

Makes users more efficient and productive, while expanding their ability to use ChemStation features.

Describes how to customize the software for laboratory and customer needs.

Improves proficiency in using the Agilent

EnviroQuant software.

Covers data analysis and reporting, including completion of EPA-like forms.

Describes how to customize the software for laboratory and customer needs.

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115

SERVICES & SUPPORT

Support

Tap Agilent’s GC and GC/MS expertise anytime.

Just give us a call to discuss hardware, software, application concerns, or basic operation techniques.

Visit Agilent online

For a wealth of knowledge, tips, and insights, go to www.agilent.com/chem.

You’ll find:

• Frequently Asked Questions about Agilent instruments and supplies.

• Interactive Troubleshooter A step-by-step approach to help you solve common problems.

• Find a Part Includes parts information, pricing, and availability, plus an illustrated parts breakdown.

• Software Downloads and Utilities Feature patches and status bulletins, tools and utilities, firmware, and revision tables.

• How-to Videos Show you how to perform common installation and maintenance procedures for Agilent products.

• Chromatogram Library A searchable collection of GC, LC, and CE chromatograms for nearly a thousand chemical compounds.

• Instrument and Software Demos Such as product videos, 3D animations and interactive software demos.

a

Technical Support Consultation

Have a technical GC column, method, or troubleshooting question? Agilent’s technical GC and GC/MS experts are available to answer your questions by phone, fax or e-mail for free. With years of experience in running samples, developing methods and troubleshooting GC systems, our chemists are promptly able to help you consistently achieve excellent performance and high productivity in your lab.

GC Technical Support in the United States:

Phone: 1-800-227-9770, press #4, then #1

Fax: 1-916-608-1964

Online: go to www.agilent.com/chem/techsupport and click on “Interactive Troubleshooter.” www.agilent.com/chem • 800 227 9770

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We’ve streamlined our online store to complement the design and content of our

2005-2006 Essential

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Visit www.agilent.com/chem/4ecatalog for one-click access to:

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GC System Recommended Maintenance Schedule

Gas Management

ITEM TYPICAL SCHEDULE

Gas purifiers

(carrier gas & detector gas)

Split vent trap

Flowmeter calibration

Every 6-12 months

Every 6 months*

Every 1-2 years

ACTIONS/COMMENTS

Replacement schedule is based on capacity and grade of gases.

In general, replace non-indicating traps every 6-12 months or when indicating traps start to change color. Replace indicating traps when indicating material is spent.

Replace.

Re-calibrate electronic flowmeters – follow recommended schedule for the unit (shown on calibration certificate).

Sample Introduction Consumables and GC Inlets

ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Every 3 months* Syringes and/or syringe needles

Inlet liner

Liner O-rings

Inlet septum

Inlet Hardware

Weekly*

Monthly*

Daily*

Every 6 months

Every year

Replace syringe if dirt is noticeable in the syringe, if it cannot be cleaned, if the plunger doesn’t slide easily, or if clogged. Replace needle if septa wear is abnormal or the needle becomes clogged.

Check often. Replace when dirt is visible in the liner or if chromatography is degraded.

Replace with liner or with signs of wear.

Check often. Replace when signs of deterioration are visible

(gaping holes, fragments in inlet liner, poor chromatography, low column pressure, etc.).

Check for leaks and clean.

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!

Columns

ITEM

Front-end

Maintenance

Solvent rinse

Replacement

Ferrules

TYPICAL SCHEDULE

Weekly – monthly*

As needed

As needed

ACTIONS/COMMENTS

Remove

1

2

-1 meter from the front of the column when experiencing 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.

When chromatography degradation is due to column contamination.

Only for bonded and cross-linked phases.

When trimming and/or solvent rinsing no longer return chromatographic performance.

Replace ferrules when changing columns and inlet/detector parts.

Detectors

ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

FID/NPD Jets

& Collector

NPD Bead

FID

As needed

As needed

Every 6 months

Clean when deposits are present. Replace when they become scratched, bent or damaged, or when having difficulty lighting FID or keeping flame lit.

Replace when signal drifts or there is a dramatic change in sensitivity.

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

As needed

Wipe test.

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

As needed

Measure hydrogen, air, and makeup gas flows.

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.

www.agilent.com/chem

800 227 9770

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800 227 9770

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 Series

HPLC System

• Essential Chromatography Catalog

• Online Library and Tech Support

The information and pricing in this guide are subject to change without notice.

© Agilent Technologies, Inc. 2005

Printed in USA February 15, 2005

5989-1925ENUS

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