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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 todays labs face the challenge
of operating with a reduced staff. Thats why were committed to bringing you the
worlds 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.
Weve even included easy guides to help you order Agilent parts and supplies
which have 40 years of high quality and technical experience built right in. So you can
keep your downtime to a minimum, and get the results you need.

Maintaining Your Agilent GC and GC/MS Systems


Maximize your efficiency. Minimize your downtime.
Get the results you need.
2
3
4
4
12
13
14
15

Gas Management
Gas Types
Contaminants & Purities
Gas Purification Systems
Regulators
Tubing
Leak Detection
Flow Rates

18 Sample Introduction
Consumables & GC Inlets
Sample Introduction
19 Vials
21 Syringes

TIPS AND TOOLS


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

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.

26
28
31
34

36
42
47
52
54

Inlet Types
Packed-Column
Split/Splitless
Cool On-Column
Programmed Temperature
Vaporizer PTV
Inlet Accessories
Septa
Ferrules
Liners
Flip Top Inlet Sealing System
Parts & Supplies

56
57
57
58

Columns
Column Maintenance
Column Selection
Column Installation/Setup
& Conditioning
59 Column Performance
63 Columns Types and
Characteristics
68 Detectors
69 Flame Ionization Detector (FID)
Thermal Conductivity Detector
(TCD)
72 Electron-Capture Detector
(ECD)
74 Thermal Conductivity Detector
(TCD)
76 Flame Photometric Detector
(FPD)
78 Nitrogen-Phosphorus Detector
(NPD)
82 GC/MS Systems
83 Maintaining Mass Selective
Detectors (MSDs)
87 Mass Spectrometer Symptoms
88 Ion Source
93 Vacuum Systems & Pumps
96 Electron Multipliers &
Replacement Horn
97 Maintaining the MS Engine
99 Ion Source Parts & Supplies
100 General GC/MS Supplies
101 Test & Performance Samples
104 Services & Support
105 Expert Service, Training
& Support

Dont Miss
GC Maintenance Schedule (inside back cover)
1

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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. Its about selecting the
appropriate carrier gas for your needs,
and taking steps to prevent system
contamination. Agilent understands
this and provides products that make
gas management easy to implement
in your lab.
Kenji Yamaguchi
Applications Support Manager

CATALOG
For a complete selection of gas management supplies, see Agilents
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.

www.agilent.com/chem

800 227 9770

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.

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.

Support Gases

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
suppliers products, and to utilize the
appropriate Agilent gas purification
products (see next section).

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

Carrier and Support Gases


Sample
Contact

Purity Required*

Pneumatics

No

Low Grade

Pneumatics

No

Low Grade

Gas Type

Function

Air
Nitrogen

Limit of Detection required:

Hydrogen

Trace (0-1 ppm)

1-1000 ppm

1000 ppm-1%

1%-100%

Carrier or fuel gas


for detector

Yes

Research

Ultra-Pure

Ultra-Pure

UHP/Zero

Hydrogen/Helium Mix

Fuel gas for detector

Yes

Research

Ultra-Pure

Ultra-Pure

UHP/Zero

Methane/Argon
or Nitrogen

Carrier or make-up
for ECD

Yes

Research

Research

Research

N/A

Air

Oxidant for detector

No

Ultra-Pure

Ultra-Pure

UHP/Zero

UHP/Zero

Nitrogen, Helium,
or Argon

Carrier or
make-up gas

Yes

Research

Ultra-Pure

Ultra-Pure

UHP/Zero

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

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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

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.

opportunity for introduction at every


fitting present in the gas line or during
use of gas permeable tubing.

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.

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800 227 9770

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

GAS MANAGEMENT

Carrier Gas Purification


Key:
In-Line Gas Purifiers

-ORGas Purification System

Gas supply

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 H2

-ORCombination Trap
Gas supply

ECD make-up

Vent

ELCD reaction gas

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

MS carrier gas

Regulator = Brass dual stage regulator

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

Constant exposure of capillary columns to


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

TIPS AND TOOLS


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

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GAS MANAGEMENT

Moisture (Water) Traps


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

Indicating moisture traps are available in plastic and glass bodies.


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

Refillable Glass Moisture Trap

Moisture Removal Traps


Size
(cc)

Description

H2O Removal Maximum Effluent H2O


Capacity (g)
Concentration (ppb)

1/8 in.
Part No.

1/4 in.
Part No.

Price

MT200-2

MT200-4

$104

MSR-1

MSR-1

$ 55

GMT-2-HP

GMT-4-HP

$119

GMSR

GMSR

$ 63

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

Refillable Moisture Trap

200

36

18

Adsorbent Refill (1 pint) for MT Series


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

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

Moisture S-Trap preconditioned

5060-9084

$226

Big Moisture Traps for the Ultimate Moisture Capacity

Big Moisture Trap

750

Refill for BMT Series (2 refills)

Refillable Moisture Trap

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Moisture S-Trap

BMT-2

BMT-4

$235

BMSR-1

BMSR-1

$ 58

Big Moisture Trap

GAS MANAGEMENT

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.

Indicating Oxygen Trap

Big Oxygen Trap

Metal (usually aluminum) trap bodies are


recommended for GC analyses. Some

Oxygen Traps
Description

1/8 in.
Part No.

Size (cc)

1/4 in.
Part No.

Price

IOT-4-HP

$143

Indicating Oxygen Traps glass body with plastic safety shield

Indicating Oxygen Trap

30

IOT-2-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

Hydrocarbon Traps
Size (cc)

1/8 in.
Part No.

1/4 in.
Part No.

Price

200

HT200-2

HT200-4

$106

ACR

ACR

$ 63

BHT-2

BHT-4

$235

BACR

BACR

$ 52

Hydrocarbon Traps General Purpose

Refillable Hydrocarbon Trap


Adsorbent Refill (1 pint, 2 refills)

Big Hydrocarbon Traps for the Ultimate Hydrocarbon Capacity

Big Hydrocarbon Trap

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.

$235

Hydrocarbon Traps
Description

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.

750

Refill for Big Hydrocarbon Trap (2 refills)

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 Removal S-Trap can be reconditioned in the GC oven

Hydrocarbon S-Trap

5060-9096

$232

Capillary Grade Hydrocarbon Traps for crucial capillary applications

Capillary Grade Hydrocarbon Trap


Adsorbent Refill (1 pint, 3 refills)

100

HT3-2

HT3-4

$ 98

ACR

ACR

$ 63

Hydrocarbon Trap

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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:

Efficient design which prevents


channeling and promotes efficient
scrubbing

Optimized adsorbents for maximum


surface area and capacity

The ultimate in purification with a single


trap (Big Universal Trap)

Leak-free, one-piece design to eliminate


potential leaks from using multiple traps

Description

Size (cc)

1/8 in.
Part No.

1/4 in.
Part No.

Price

100

OT3-2

OT3-4

$104

Oxygen/Moisture Traps

Agilent OT3 Trap

Agilent OT3 Trap

Hydrocarbon/Moisture Traps

Refillable Hydro-Moisture Trap

200

Refill for Hydrocarbon/


Moisture Trap (1 pint, 2 refills)

HMT200-2 HMT200-4
HCRMS

HCRMS

$ 98
$ 63

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

Big Universal Trap Helium


purged (also recommended
for GC Mass Spec)

750

RMSH-2

RMSH-4

$261

Big Universal Trap Hydrogen purged 750

RMSHY-2

RMSHY-4

$261

Big Universal Trap Nitrogen purged

RMSN-2

RMSN-4

$261

UMC-5-2

UMC-5-2

$ 21

Big Mounting Clip for


mounting Big Traps 2/pk

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750

Big Universal Trap

Hydrocarbon Moisture Trap

GAS MANAGEMENT

High Capacity
Gas Purification System
Three Cartridge System

Single-Cartridge System

Agilents highest capacity and most


economical gas purification system.

Three Cartridge
High Capacity
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.

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.

Consists of a permanent all-welded


stainless steel manifold to minimize
the potential for leaks.
Suitable for bench or wall mounting.

High Capacity Gas Purification System


Description

Part No.

Price

With 1/8 in. fittings

5183-1907

$612

With 1/4 in. fittings

5182-9776

$567

Replacement Cartridge Kit


Includes all three cartridges for
above system

5182-9780

$393

With 1/8 in. fittings

5183-4598

$239

With 1/4 in. fittings

5183-4599

$255

Triple combination replacement cartridge


for single cartridge system

5183-4600

$136

Three Cartridge SystemIncludes manifold


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

Single Cartridge SystemIncludes single


cartridge manifold brackets for wall or bench
mount, and a triple combination cartridge
(H2O/hydrocarbon, and O2 )

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GAS MANAGEMENT

Quick Change Plus (QC+) Point of


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

Filter cartridges are of all metal or glass


construction, eliminating infusion and
resultant signal noise associated with
filters constructed from plastics. Cartridges
are quickly installed via a simple knurled
retaining nut, with no wrenches needed.
As many as four cartridges can be replaced
in a matter of seconds, and because there
is low dead volume, a minimal amount of
gas system purge is required after
installation.

RQC-P

Quick Change Plus (QC+) Point of Operation Panels


Description

Fitting (in.)

Part No.

Price

1/8

RQC-P

$1604

Part No.

Price

High capacity oxygen

GC-1

$ 64

High capacity moisture

GC-2

$ 64

Indicating moisture

GC-2-I

$106

Hydrocarbon

GC-3

$ 64

Indicating oxygen

GC-4

$155

4-Head

O2, indicating O2, HC, H2O

Replacement Cartridges
Description

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

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10

GAS MANAGEMENT

Super-Clean Gas Filter System

Super-Clean Gas Purification Systems

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.

Available with 1/8" fittings only


Description

Part No.

Price

Carrier Gas Purification System: Single


position system perfect for GC/MS,
ECD and NPD detectors. Includes the
triple filter cartridge.

5182-9704

$ 398

Super-Clean Gas Purification System:


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

5182-0816

$1291

Triple Filter Cartridge: A single carrier gas


filter now with hydrocarbon, moisture,
and oxygen trapping capability. Includes
moisture and oxygen indicator so you know
exactly when to replace the cartridge.

5182-9705

$ 186

Filter cartridge bundle of 4 (oxygen,


moisture, and 2 hydrocarbon)

5183-4770

$ 530

Replacement Filter Cartridges

Universal/External Split Vent Trap


Description

Part No.

Price

Universal/external split vent trap


with 3 cartridges
(1/8 in. Swagelok fitting)

RDT-1020

$ 94

Replacement cartridges (3/pk)

RDT-1023

$ 45

Split vent 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

11

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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.

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.

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

Description

Part No.

Price

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

5183-4641

$275

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

5183-4642

$275

CGA 540, 125 psig max (8.6 bar), O2

5183-4643

$275

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

5183-4644

$275

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

5183-4645

$275

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

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

TIPS AND TOOLS

Regulator Outlet Adapters Female NPT to Swagelok-style

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


(included with brass regulators)

0100-0118

$ 14

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

0100-0119

$ 15

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

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800 227 9770

Always depressurize a regulator before closing by


adjusting knob and removing the regulator from the
cylinder.

12

GAS MANAGEMENT

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.

Spectra-Link Tubing Connecting System


on a two-stage regulator

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: 70F; Pressure 30 psig
Tubing Type

Diameter
(inches)

Recommended
Max. Length (feet)

Pressure Drop
(psig)

Copper

1/8*

50

Copper

1/4*

300

0.5

*Recommended when multiple instruments are connected to the same source

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.

TubingPrecleaned
Description

as pressurizing pneumatic lines; however,


be aware of its pressure limitations.

Part No.

Price

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

5180-4196

$56

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

5021-7107

$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.

13

www.agilent.com/chem

800 227 9770

GAS MANAGEMENT

Spectra-Link is No Ordinary Flexible Tubing!


Stainless Steel: no outgassing or permeation through polymeric materials
Quick Connection: prevents air from entering gas lines during tank changeover
Tested: each system has leak rates lower than 1x10-5 cc/sec

Description

Part No.

Price

Spectra-Link with 1/8 in. fittings


and 36 in. SS tubing

SL-8

$496

Spectra-Link with 1/4 in. fittings


and 36 in. SS tubing

SL-4

$496

Part No.

Price

5183-1941

$ 60

Cylinder Bracket
Description
Cylinder wall bracket with strap and chain
(cylinder size up to 14 in., 35 cm)

Cylinder Wall Bracket

Leak Detection
Leaks allow oxygen and other
contaminants to enter the gas stream.
Therefore, GC instrument maintenance
should include checking fittings and
connections with a gas leak detector.
Agilents 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

5182-9646

$1915

Gas leak detector, 220 V

5182-9648

$1915

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.

FlowTracker Flowmeters volumetric, multimode flowmeters


Description

FlowTracker 2000

Part No.

Price

FlowTracker 1000 Flowmeter

5183-4779

$ 816

FlowTracker 2000 Flowmeter and


Leak Detector

5183-4780

$1143

FlowTracker Universal AC Adapter (optional,


not supplied with FlowTracker units)
5183-4781

$ 43

ADM 1000 features include:

ADM 2000

Accuracy 3%

In addition to the features of the ADM


1000, the ADM 2000 includes:

Operating temperature range


0 to 45C for the instrument, -70 to
135C for the tubing
ADM 1000

Calibrationtraceable to NIST primary


standards
Real time, split ratio measurement
CE mark certified

Mass flow measurementsmeasure 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)

Measures flow rates from 0.5 to


1000 mL/min
Split ratioscompare the ratio from
one gas measurement to another
(i.e., injection port split ratios)
ADM 2000

15

www.agilent.com/chem

800 227 9770

GAS MANAGEMENT

Flowmeters
Flow Rate (mL/min)
Low
High

Description

Gases
Measured

Accuracy
(%)

Power
Supply

RS-232 Data
Output

Part No.

Price

220-1170

$620

ADM Flowmeters volumetric, measures all gases*


ADM1000

0.5

1000

All

9V Battery

None

ADM2000

0.5

1000

All

Battery or 120 VAC

Yes

220-1171-U

$725

ADM2000E

0.5

1000

All

Battery or 220 VAC

Yes

220-1171-E

$725

Electronic Mass Flowmeter dedicated mass flowmeter, very accurate for specific gases*
Veri-Flow 500
(110 V)

5.0

500

He, H2, Ar/CH4


N2, Air

Rechargeable Battery
or 110 VAC

Yes

HVF-500

$681

Veri-Flow 500
(220 V)

5.0

500

He, H2, Ar/CH4


N2, Air

Rechargeable Battery
or 220 VAC

Yes

HVF-500-2

$681

Optiflow Flowmeters Gas Flowmeters versatile volumetric flowmeters**


Optiflow 420

0.1

50

All

+/- 3

9V Battery

None

HFM-420

$573

Optiflow 570

0.5

700

All

+/- 3

9V Battery

None

HFM-570

$573

Optiflow 650

5.0

5,000

All

+/- 2

9V Battery

None

HFM-650

$677

*non-corrosive gases only


**non-corrosive and mildly corrosive gases only

Veri-Flow 500
Optiflow 420

TIPS AND TOOLS


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

www.agilent.com/chem

800 227 9770

16

You asked we listened!

Announcing the launch of


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

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.

Sample
Introduction
Gas
Management
Consumables &
GC Inlets

The use of quality carrier gases is essential


for consistent and accurate GC analyses.
Proper
management
is key
to achieving
Agilentgas
offers
a wide range
of high-quality
this
goal.vials,
Agilent
provides
a diverse
sample
septa,
syringes,
liners line
and of
high
quality
gas
management
products
inlets for a broad range of gas-phase gas
purifiers,
regulators,
applications.
Just asleak
youdetectors
depend on our
and
flowmeters
all designed
to prevent
meticulously
engineered
GC and
GC/MS
column
damage,
detector
life, and
instruments,
youimprove
can count
on Agilent
improve
the
quality
and
consistency
of your
consumables. This section reviews these
GC
separations.
This section
explains
how
critical
components.
Also, look
for useful
common
moisture
infofrom contaminants
proper syringelike
useoxygen,
and cleaning
and
hydrocarbons
can damage
your GC
techniques
to a detailed
discussion
on
column,
and
helps
you
understand
how to
optimized inlet settings.
prevent it. Also, look for practical information
about regulators, the importance of clean
GC-tubing, and minimizing the likelihood
of GC system contamination.

Good sample introduction helps ensure


good reproducibility, optimal peak shape,
and accurate sample delivery. Agilents
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 Agilents
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.

www.agilent.com/chem

800 227 9770

18

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Introduction
Vials

Vial Filling

Agilents 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.

When filling sample vials, keep in mind:

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.

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

Glassfor general purpose


use and for use with acids

Silanizedfor use with


samples that bind to glass,
and for trace analyses

Polypropylene for use


with alcohols and aqueous
solvents

Amber Vialsfor use with


light-sensitive samples

Microvolume Insertsfor High Recovery Vials


use with very small sample for use with limited sample
volumes
volumes

Recommended fill volumes for sample vials

1 mL

50 L

3.6 mm*
100 L vial
*Needle position based on standard sampling depth.

TIPS AND TOOLS


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

19

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

Red Rubber/Teflon
Determining Your Quantity Needs
To determine potential septa ordering
quantities, consider:
the number of samples run during a
day/week

Silicone/Teflon

if samples are run in small or large


batches

Excellent resealing
Resists coring
Good for multiple injections

if samples are run manually or with an


autosampler
if samples are run overnight, unattended

Unattended autosampler
runs require a precise fit for
uninterrupted operation.
Typically, automated sample
runs use a higher quality and
quantity of vials.

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

www.agilent.com/chem

800 227 9770

TIPS AND TOOLS

Routine analysis
Moderate resealing
Excellent chemical inertness
Not recommended for multiple
injections or storage of samples
Least expensive

Vials
Description

Quantity

Part No.

Price

2 mL Crimp top vial convenience


pack with silver AI caps with
Teflon/Red rubber septa

500/pk

5181-3400

$115

2 mL Screw top vial convenience


pack with blue screw caps and
Teflon/Red rubber septa

500/pk

5182-0732

$183

2 mL Snap top vial convenience pack


with clear polypropylene snap caps
and Teflon/Red rubber septa

500/pk

5182-0547

$154

100 L Insert for wide opening vials

100/pk

5181-1270

$ 88

250 L Polypropylene flat bottom inserts 500/pk

5183-2087

$ 57

100 L Glass lined polypropylene vials

100/pk

9301-0977

$158

Less than 5 L dead volume,


Micro-V vial, clear crimp top

100/pk

5184-3551

$ 69

30 L reservoir volume, High recovery


vial, crimp top

100/pk

5182-3454

$109

Vials

20

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringes

Selecting 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.

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.

Agilent syringes are designed:


for reproducible sample volume delivery
specifically for the Agilent inlet or
autosampler
to maximize inlet septum lifetime

3. Select the appropriate syringe


needle gauge.

Needle Gauge Selection


Inlet

Needle Gauge

Column Type

Packed, split or
splitless (including PTV)

23 gauge or 23/26 gauge tapered

any

Cool on-column

23/26 gauge tapered or 26 gauge

530 m

Cool on-column

26/32 gauge tapered

320 m

Cool on-column

26/32 gauge tapered

250 m

Needle Tip

Needle Shape

Needle tips
Sharp tip

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.

TIPS AND TOOLS


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

21

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800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Characteristics and Recommended Uses


Syringe

Advantage

Limitations

Recommended Use

5 L, fitted
plunger

Most accurate
Thinnest plunger, 1 L injections
syringe for 1L
can bend
Clean samples
injection
more easily
Routine analysis
No hardware
Not ideal for higher
modification needed
viscosity samples
for 0.5 L injection
Plunger not
replaceable

10 L, fitted
plunger

Most economical
Most reliable fitted
plunger syringe
Less bending
Better for high
viscosity samples

10 L,
gas-tight

Replaceable plunger More expensive


Dirty samples
for reduced
than fitted plunger Gases and volatile
repair cost
Not available in
samples
Less plunger binding 5 L size
Reactive samples
than fitted plunger
Tight seal between
plunger and barrel

Most accurate only General purpose


for 1 L and larger syringe
injections
Clean samples
Plunger not
Routine analysis
replaceable

Replacing On-column Syringe Needles


The stainless steel needles used for
250-m and 320-m injections must
be inserted into a glass syringe barrel.
Select the correct size needle for 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.

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.

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.

NEW! Agilent Gold Standard


GC Autosampler Syringes
see page 25

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

23

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

Possible Cause(s)

Suggested Action(s)

Bent plungers or stuck syringes

Particles such as dust, leftover samples, salts,


metal, or glass can fill the narrow gap between
the plunger shaft and the inside wall of the
barrel.

If the plungers 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

Narrow-gauge needles (26 gauge) bend more


easily than larger (23 gauge) needles.

Use only Agilent autosamplers. They are


precision-designed to ensure proper
alignment with the syringe needle.

Needles tend to bend when inserted into the


sample vial not the inlet port. This can be
caused by septa that are too tough.

Use 23 to 26-gauge tapered needles to get


the combined benefits of greater septa life
and fewer bent needles.

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.

Only use Agilent vials and septa.

Sample material or contaminants may be


trapped inside the needle.

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.

Improper needle alignment.

Blocked needles

The needle may not have been properly cleaned.

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

During normal use, the shaft rubs against the


glass walls of the barrel. This gradually wears
away the rust-resistant metal on the shafts
surface.
Rusting happens most rapidly when using water
or solvents that may contain (or absorb) water.

Ring around the neck (A dark ring between


the top of the barrel and the end of the
volume scale.)

Skin oils and other organic material.

Loose plungers accompanied by syringe


leaks and area count reproducibility problems.

The syringe is nearing the end of its useful life.

www.agilent.com/chem

800 227 9770

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.

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.
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.

24

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Gold Standard GC Autosampler Syringes


Description

Gauge/Length

Quantity

Part No.

Price

Tapered Needle Syringes


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

Tapered

Fixed Needle

23-26s/42

6/pk

5181-3360

$198

5 L

Tapered

Fixed Needle

23-26s/42

6/pk

5181-8810

$303

10 L

Straight

Fixed Needle

23/42

6/pk

9301-0725

$191

5 L

Straight

Fixed Needle

23/42

6/pk

5182-0875

$292

Straight Needle Syringes


(use with Merlin Microseal)

GC Automatic Liquid Sampler Supplies


Description

Unit

Part No.

Price

4 mL Clear screw top wash vials


with screw caps (no Septa)

144/pk

9301 0723

$ 64

Gold Standard GC
ALS Syringe Features

Septa for 4 mL vial

144/pk

9301-1031

$ 21

Lot Numbers ensure certified


performance to all specifications

Diffusion caps for 4 mL vials

12/pk

07673-40180

$ 19

4 mL wash vial with fill marking, caps

25/pk

5182-0551

$ 26

Screw for mounting syringe

07673-20570

$ 13

Quadrant kit (4 tray sections)

18596-40015

$ 75

Miscellaneous Autosampler Supplies

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)

25

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

07673-60840

$755

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 +50C
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

Glass

Use to lower activity


(replaceable)

Initial column
temperature

temperature programming

Sharpens peaks and


reduces run time

Column type

1/8-inch packed stainless


1/4-inch packed glass

Will not break


Better for polar or labile
compounds

Carrier gas flow

20-40 mL/min
30-60 mL/min

Use with N2 carrier gas


Use with He or
H2 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.

www.agilent.com/chem

800 227 9770

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.

26

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890/6850 Series GC Packed Port Supplies*


Item

Description

Septum nut

Septa Bleed temperature,


optimized, 11 mm

Unit

Part No.

Price

18740-60835

$ 37

1
2
3
4

50/pk

5183-4757

$ 67

19243-80570

$132

Top insert weldment

Viton O-rings

12/pk

5080-8898

$ 12

Glass liner, disposable

25/pk

5080-8732

$ 37

Glass liner, disposable/deactivated

5/pk

5181-3382

$ 14

Vespel/graphite ferrules, 1/4 in. id

10/pk

5080-8774

$ 42

Tubing nut, 1/4 in. brass

10/pk

5180-4105

$ 13
Liner

Adapters with glass liners


8

0.53 mm column adapter

19244-80540

$119

1/8 in. column adapter

19243-80530

$ 99

1/4 in. column adapter

19243-80540

$141

Upper insulation

19243-00067

$ 5

10

Nut warmer cup with insulation

19234-60720

$ 54

11

Column nut for 0.53 mm column

5181-8830

$ 25

2/pk

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

Inside ofof
Inside
OvenOven

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

1/8 in.
1/8
in.oror1/4
1/4in.in.
stainless steel
linerliner
stainless
steel

9
10

11

5890 Packed-Column Inlet Supplies


Description

Unit

Part No.

Price

19243-60570

$100

1/8 in. column adapter

19243-80510

$ 88

1/4 in. column adapter

19243-80520

$128

19243-60505

$ 70

5180-4105

$ 13

Nonpurging septum nut assembly


for manual flow control only, not EPC

TIPS AND TOOLS

Adapters without glass liners

27

Tap Agilents GC knowledge over the phone,


online, in the classroom, even at your site.
See pages 104-115 for more information
about our services and support.

Universal Packed-Column Inlet (non-purged)


Septum retainer nut for
headspace sampling, nonpurging
Brass nut, 1/4 in.

10/pk

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)

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 50C 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.

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.

Split Mode Variables, Practices, and Rationales


Parameter

Selection/Setting

Rationale

Inlet temperature

Try 250C or BP of
last eluting compound

Ensures flash vaporization


Minimizes inlet discrimination

Inlet liner

Large volume, deactivated

Minimizes flashback
Minimizes degradation

Inlet packing

Silanized glass wool


Glass beads or frit
None

Retains non-volatiles
Minimizes inlet discrimination
Less active than wool
Least active

0.5-3 L liquid
0.10-10 mL gas

Split easily adjusted


Split adjusted accordingly

Injection volume

Injection technique Fast autoinjection


Hot-needle fast manual
injection

Less needle discrimination


Reproducible discrimination

Split ratio

50:1 to 500:1

Depends on sample and


injection volume, and column ID

Initial column
temperatures

Not critical

Narrow initial peaks

Septum purge

2-3 mL/min

Minimizes ghosting

TIPS AND TOOLS


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

www.agilent.com/chem

800 227 9770

28

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Split Mode Variables, Practices, and Rationales


Parameter

Selection/Setting

Rationale

Inlet temperature

Just above highest


boiling point of
solutes (+20C)

Ensures flash vaporization


Reduce if degradation occurs
Use higher for dirty samples
and higher-boiling solutes

Inlet liner

Large volume >0.8mL


Small volume <0.2mL

Use with autoinjector


Use only for slow manual
injections, and gas injections

Inlet packing

None

Use only with slow injection


Decreases degradation

Silanized glass wool

Use for fast autoinjection


& dirty samples

0.5-2 L liquid

Depends on solvent, liner,


& conditions

Injection volume

Injection technique Fast autoinjection

Most reproducible
Less needle discrimination
Hot-needle slow manual Inject 1-2L.sec if narrow liner
is used and >1L injection
Hot-needle fast manual Use for <1L injections

Purge flow

20-50 mL/min

Higher if using constant flow

Purge delay time

20-80 sec

Adjust according to column


flow rate/liner type
& sample conditions

Oven temperature

10-25C below solvent BP Necessary for solvent focusing

Column flow

>2mL/min when possible Clears inlet fast


Reduces backflash and
decomposition

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 10C 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

Septum purge

2-3mL/min

Reduces ghosting

pesticide monitoring of foods

Quantification

Internal standard
Standard addition

Maximizes reproducibility
Use only with constant
injection volume

drug screening

1-3m, deactivated
(1-2m per L injected)

Reduces peak distortion


Promotes solvent and
stationary phase focusing

Retention gap

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.

29

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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.

6890/6850 Split/Splitless Inlet Supplies*


Item

1
2
3
4
6

Description

Unit

Price
$ 39

Septum retainer nut

18740-60835

Septa

See page 36

Insert Weldment

G1544-60575

Liner O-ring

See page 52

Liner

See page 47

Split vent trap assembly (6890/6850 only)

G1544-80550

$128

Retaining nut (6890/6850 only)


Retaining nut (5890 only)

G1544-20590
19251-20620

$ 26
$ 31

SS seal
Gold-plated seal

18740-20880
18740-20885

$ 26
$ 33

Washer, 0.375 in. od

5061-5869

$ 8

12/pk

$216

10

Reducing nut

18740-20800

$ 34

11

Insulation (requires 3)

19243-00067

$ 5

12

Lower insulation cover

19243-00070

$ 15

13

Ferrule

14

Column nut (6890/5890 only)

2/pk

5181-8830

$ 26

Column nut (6850 only)

2/pk

5183-4732

$ 47

19251-00100

$ 29

Angled wrench for split/splitless inlet

Part No.

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

8
9
10

TIPS AND TOOLS


11
12

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).

13
14

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800 227 9770

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 L to 2.0 L)
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 3C above column oven temperature

Ensures sample focusing in solvent front

Initial inlet temperature ramp

Same as oven (oven track) Faster than oven

Simple and effective


Narrows initial peak width

Injection volume

0.1-2.0 L liquid

Use smaller injections for small id columns;


Depends on column capacity

Injection technique

Fast autoinjection
Fused silica needle

Projects droplets away from syringe tip


Use for manual injection into small id columns

Oven temperature

Inlet temperature or slightly lower

Prevents backflash

Column flow

50-80cm/sec
30-50cm/sec

Use for H2 carrier gas


Use for He carrier gas

Septum purge

12-15mL/min

Use if installed to prevent ghosting

Quantification

All methods

Inherently reproducible technique


Lack of discrimination

Retention gap requirements

1-3m, deactivated

Corrects peak distortion


Protects column from non-volatile components
Permits autoinjection with narrow-bore columns

TIPS AND TOOLS


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

31

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800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Considerations

Troubleshooting

Sample preparation is important for


on-column injection because of:

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

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.

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

Unit

Part No.

Price

Column nut

2/pk

5181-8830

$ 26

250 m graphite/Vespel ferrule

10/pk

5181-3323

$ 55

320 m 0.5 mm graphite/Vespel ferrule

10/pk

5062-3514

$ 51

250 m retention gap (one 5 m piece)

160-2255-5

$ 39

320 m retention gap (one 5 m piece)

160-2325-5

$ 42

530 m retention gap (one 5 m piece)

160-2535-5

$ 59

5181-3396

$ 94

Quartz deactivated column connector fits 0.18-0.53 mm

5/pk

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.

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

www.agilent.com/chem

800 227 9770

32

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 Series Cool On-Column Inlet Supplies*


Item Description

Unit

Part No.

Price
1a

Manual injection
1c

Cooling tower assembly

1d

Duckbill septum
Fused silica syringe needles

19320-80625

$175

10/pk

19245-40050

$ 29

6/pk

19091-63000

$ 41

Syringe barrel for use with


fused-silica needles,10 L

9301-0658

$ 90

19245-60760

$ 9

For 200 m columns (one ring)

19245-20510

$ 89

For 250 m columns (six rings)

19245-20515

$114

For 320 m columns (five rings)

19245-20525

$ 78

For 530 m columns (no rings)

19245-20580

$ 55

For 530 m Al clad columns (four rings)

19245-20780

$ 54

Ferrule

5080-8853

$ 47

Column nut

5181-8830

$ 26

1b

2
3

1c
1d

Common Supplies
3

Spring

Inserts for capillary columns

2/pk

5
6

6890 Series GC Cool On-Column Inlet Supplies


Automatic Injection
1a

Septum nut base for 320 mm assembly

19245-80521

$ 62

1b

Septum nut base for 530 mm assembly

G1545-80520

$ 63

Advanced green 5 mm through hole septa


BTO 5 mm through hole septa

5183-4760
5183-4758

$ 62
$ 72

50/pk
50/pk

5890 Series Cool On-Column Inlet Supplies


Automatic Injection
1a

Septum nut (5890 Series II GC)

19245-80520

$ 91

1b

Needle guide (for 7673A only)

19245-20670

$ 35

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

33

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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.

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


Parameter

Selection/Setting

Rationale

Injection mode

Cold split

For general use


and sample screening
For trace analysis

Cold splitless
Inlet temperature
ramp rate

Adjustable (i.e., 2C/sec


to 12C/sec)

Advantages
no syringe-needle discrimination
Ballistic

minimal inlet discrimination


no special syringe needed
use of large injection volumes

Inlet liner

Straight with silanized wool


Baffled
Packed with an adsorbent

For general use


For labile samples
For focusing gaseous
injections from auxiliary
sampling devices

Injection volume

0.1-1.5L

Use lower volumes for


volatile solvents and fast
ramp rates
Use volumes larger than
1.5L only in solventelimination mode

Sample Injection
technique

Autosampler or manual,
fast or slow

Not critical for cold split


& splitless modes

Oven temperature

10-25C below solvent BP

For proper solvent effect in


splitless mode
For split mode

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 N2, or liquid CO2).
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.

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

Sample dependent
Column flow

30-50 cm/sec

Clears inlet faster


Less backflash

Septum purge

1-5mL/min

Minimizes ghosting

Quantification

Any method

Inherently reproducible
Low discrimination in cold
injection modes

Retention gap

1-3m, deactivated

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

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 PTV Inlet

1
3

Description

Column ID Unit

Part No.

Price

Septumless head

G2617-60507

$2661

Septum head

G2618-80500

$1078

Septum nut

18740-60835

$ 39

PTV inlet assy

G2617-60506

$4850

PTV LCO2 cooling jacket

G2617-60508

$ 544

PTV LN2 cooling jacket

G2619-60501

$ 473

Silver seal

5182-9763

$ 62

Graphpak inlet adapter

0.20 mm

5182-9754

$ 173

0.25-0.33 mm

5182-9761

$ 152

5, 6

0.53 mm

5182-9762

$ 146

7
8

5/pk

Ferrules for

0.20 mm

10/pk

5182-9756

$ 158

Graphpak inlet

0.25 mm

10/pk

5182-9768

$ 166

0.32 mm

10/pk

5182-9769

$ 166

0.53 mm

10/pk

5182-9770

$ 146

10

Split nut for inlet adapters

5062-3525

$ 159

11

PTV insulation block

G2617-20510

$ 61

PTV cryo insulator (not shown)

G2617-60510

$ 53

Teflon ferrule (needle seal)

5182-9748

$ 137

Kalrez seal

5182-9759

$ 110

Valve body

5182-9757

$ 91

Pressure spring

5182-9758

5182-9775

$ 24

Sealing element

5182-9760

$ 73

CO2 Cryo inline filter

3150-0602

$ 137

Service kit for septumless head


contains Kalrez seal, valve body,
and pressure spring
Graphpak 3D ferrules

5182-9747

$ 224

5182-9749

$ 143

G2617-80540

$ 208

Installation tool for 3D ferrules

9
10

11

Viton seal

5/pk

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.

TIPS AND TOOLS

Item

PTV Liners

35

Description

Part No.

Price

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

5183-2038

$ 25

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

5183-2036

$ 20

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

5183-2037

$ 29

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

5183-2041

$ 55

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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.

What is the Function

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.

Why Replace

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800 227 9770

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.
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
dont 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

36

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Troubleshooting
Symptom

Possible Cause

Remedy

Extra Peaks/Humps

Septum bleed.

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.

Large leak at septum during injection and


for a short time thereafter (common with
large diameter needles).

Replace septum and use smaller diameter


needles.

Carrier gas leaks at septum or column


connection.

Check for leaks. Replace septum or tighten


connections if necessary.

Normal

Problem

Baseline Change After Large Peak

Normal

Problem

Problem

(flow increase)

(flow decrease)

Retention Times Prolonged

Normal

Problem

Problem

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

37

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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

Introducing Agilent Premium Non-Stick Septa


featuring a proprietary plasma coating that wont
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.
Agilents plasma-treated non-stick septa

But Agilents 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

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.
Agilents premium GC inlet septa are not garden-variety septa
stamped out in large sheets, creating variations in geometry. Rather,
each Agilent premium septum is molded to a perfectly uniform size
and shape.

Figure 1. Comparison of Coring, With and Without CenterGuide


(30x magnification)
High-Temperature Septa Without CenterGuide: Major Coring Before 1
00 Autoinjections

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.
1 autoinjection

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

100 autoinjections

700 autoinjections

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

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.

Summary of Inlet Septum Characteristics


SEPTUM TYPE
BTO
(Bleed and
Temperature
Optimized)
Long Life
Advanced Green
= best

39

BLEED

LIFETIME

TEMPERATURE
LIMIT

(optimized for
high temperature)

to 400C

to 350C

to 350C

= very good

= good

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800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

p/n 5183-4757

p/n 5183-4761

p/n 5183-4759

Agilent Bleed and Temperature


Optimized Non-Stick Septa (BTO)

Agilent Long-Life Non-Stick Septa

Agilent Advance Green


Non-Stick Septa

Extended temperature range, low-bleed

Pre-pierced for extended life and


reduced coring

Maximum Injection Port Temperature


400C

The preferred Septum for Autosamplers

True Long-Life, High Temperature


Green Septum

Ideal for Overnight Runs

More Injections per Septum

Virtually eliminates injection-port


sticking

Up to 400 Injections Per Septum injection

Reduced Injection Port Sticking

Maximum Injection Port Temperature


350C

Maximum Injection Port Temperature


350C

Soft, 45 Durometer, Easy On


Autosampler Needles

Packaged in glass vials for high purity

Pre-conditioned; packaged in glass


to prevent contamination
Ideal for use with low-bleed,
Mass Spec capillary columns

Economical alternative to competitors


Green Septa

General Purpose Septa


Agilents 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
350C. 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.

www.agilent.com/chem

800 227 9770

Agilents 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

40

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Ordering Information


Part No.

Price

5183-4757
5183-4757-100
5183-4758

$72
$134
$72

5183-4759
5183-4759-100
5183-4760

$62
$107
$62

5183-4761
5183-4761-100
5183-4762

$84
$150
$84

5080-8896-50
5080-8894-100
5080-8728-50
5080-8728-100

$52
$93
$52
$93

5181-1263-50
5181-1263-100
5181-3383-50

$52
$93
$52

5181-3383-100

$93

5181-1283-50
5181-1283-100
5181-1260

$52
$93
$29

5181-1261

$29

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

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

41

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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 450C, and Vespel and Vespelgraphite ferrules are rated to 280C and
350C, respectively.

Column Ferrule Types


Graphite

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.

Advantages

Limitations

Easy-to-use, stable seal

Soft, easily deformed or destroyed

Higher temperature limit

possible system contamination


not for use with GC/MS
transfer-lines

Vespel or

Mechanically robust

Flows at elevated temperature

Vespel-graphite

Long lifetime

must retighten frequently


prone to leakage
Polymer bleed problematic with
some detectors (NPD and ECD)

Why Replace
Signals that a ferrule is damaged include:
background noise from oxygen diffusing
into the system
column bleed catalyzed by oxygen
sample degradation
loss of sample
increase in detector signal/noise
poor retention time reproducibility

www.agilent.com/chem

800 227 9770

How to Minimize Problems


General technique for installing ferrules:
dont 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

42

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Troubleshooting
Problems possible after changing ferrules

Normal Peaks

Tailing Solvent Peaks

Wrong Peak Ratios

Normal Peaks

Tailing Solvent Peaks

Wrong Peak Ratios

Correct column positioning in both


injection port and FID

Column positioned incorrectly in the


injection port, 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. Thats
because youll 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 51818830) has a hexagonal head requiring the
use of a wrench to tighten it completely.
The finger-tight column nut (p/n 50208293 for 530um columns and p/n 50208292 for columns 320m or less) does
not require a wrench to tighten.
It can only be used with the 100%
graphite ferrules.

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.

43

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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

5181-8830

Vespel/Graphite Ferrules
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
05988-20066

Vespel/Graphite Ferrules
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.

Agilent Ferrule Selection Recommendations


Ferrule/Seal
Type

Upper
Temperature
Limit

Usages

Limitations

-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Graphite
450C
General purpose
Not for MS or
(100%)
for capillary columns.
oxygen sensitive
Suitable for FID and NPD.
detectors.
Recommended for high
temperature and cool
on-column applications.
Can be removed easily.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel/Graphite
350C
General purpose for
Not reusable.
(85%/15%)
capillary columns.
Recommended for
MS or oxygen sensitive
detectors. Most reliable
leak-free connection.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel
280C
Isothermal operation.
Leaks after
(100%)
temperature cycle.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------SilTite
N/A
Use only with SilTite Nut Kits
Not Reusable
(100% metal)

45

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800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Ordering Information


Ferrule Id
(mm)

Column Id
(mm)

Quantity

Part No.

Price

0.1, 0.2, 0.25, 0.32


0.53
0.05-0.25
0.45, 0.53

10/pk
10/pk
10/pk
10/pk

5080-8853
5080-8773
500-2114
500-2118

$
$
$
$

47
38
26
26

0.1, 0.2
0.1, 0.2, 0.25
0.32
0.45, 0.53

10/pk
10/pk
10/pk
10/pk

5062-3516
5181-3323
5062-3514
5062-3512

$
$
$
$

51
55
51
53

0.1
0.1, 0.2, 0.25
0.32
0.53

10/pk
10/pk
10/pk
10/pk

5062-3507
5062-3508
5062-3506
5062-3538

$
$
$
$

62
62
56
48

0.1, 0.2, 0.25


0.32
0.45, 0.53

10/pk
10/pk
10/pk

5181-3322
5062-3513
5062-3511

$ 55
$ 51
$ 51

0.1, 0.2, 0.25


0.32

10/pk
10/pk
10/pk

5062-3580
5062-3581
5181-3308

$ 79
$ 79
$ 47

0.4

10/pk

5184-3569

$ 87

0.5

10/pk

5184-3570

$ 87

10/pk

5184-3571

$ 85

10/pk

5188-2789

$135

2/pk
1 ea
1 ea
1 ea
2/pk

5181-8830
5020-8293
5020-8292
5020-8294
5183-4732

$
$
$
$
$

1 ea
1 ea
1 ea

05988-20066
05921-21170
8710-0510

$ 13
$ 16
$ 24

General Purpose Graphite Ferrules (Short Ferrules)

0.5
1.0
0.4
0.8
85% Vespel, 15% Graphite Ferrules (Short Ferrules)

0.80.3
0.80.4
0.80.5
0.80.8
Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)

0.3
0.4
0.5
0.8
These ferrules are recommended for use with GC/MS.

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

0.8

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

26
18
18
12
47

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.

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800 227 9770a

46

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 manufacturers liners,
Agilent liners are built to Agilents 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.

47

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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 L) are
characterized by larger inside diameters
(ID) and are typically used with injection
sizes of 1 L or more. The small volume
liners have a smaller ID and are usually
used with small injection sizes (< 1 L),
fast 100 m 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.

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.

www.agilent.com/chem

800 227 9770

48

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.

49

Packing
Glass Wool

Glass Cups

Many liner designs use deactivated


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

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.

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.

Figure 1.

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

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800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Troubleshooting
Symptom

Possible Cause

Remedy

Tailing Peaks

Sample components adsorbed by column,


inlet liner or contaminated gold inlet seal.

Use new, deactivated liner or clean old


liner and replace glass wool.

Needle hitting and breaking packing in


inlet liner.

Partially remove packing from liner or use


without packing.

Column end poorly cut


(sample absorption).
Broken or chipped inlet liner.

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.

Inlet flow too low.

Make sure total flow in inlet is above


40 mL/min.

Sample decomposing.

Remove inlet liner and check cleanliness.


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

Column and inlet liner misaligned.


See alsoSeptum Troubleshooting,
page 37

Check installation of column end and inlet


liner; adjust if necessary.

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

Baseline Rise Before or After Peak

Normal

Problem

Problem

Baseline Change After Large Peak

Normal

Problem

Problem

Unresolved Peaks

Normal

www.agilent.com/chem

Problem

800 227 9770

Problem

50

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:

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.

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. 51834647, but with an outer diameter that
compromises for both split and splitless
injections, Agilent Part No. 5183-4711.

51

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 350C.

www.agilent.com/chem

800 227 9770

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Flip Top Inlet Sealing System


Agilents NEW Flip Top Inlet Sealing System is the faster, smarter way to change
inlet liners on Agilent GCs
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!
Agilents 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.

VIDEO
Description

Part No.

Price

Flip Top Inlet Sealing System

5188-2717

$514

Liner O-rings (10/pk)

5188-2741

$19

www.agilent.com/chem

800 227 9770

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
Volume(l)

Single
Liner

For split injection

870

5183-4647
$35

5183-4701
$157

5183-4702
$700

Liner, splitless, single-taper,


no glass wool, deactivated

For splitless injection

900

5181-3316
$29

5183-4695
$124

5183-4696
$533

NEW! Liner, Splitless,


Single-taper, no glass wool,
polymerically deactivated

For trace pesticide


analysis

900

5181-3316EN
$32

Liner, direct, 2 mm ID,


deactivated

For direct injection


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

250

5181-8818
$24

5183-4703
$95

5183-4704
$414

Liner, general purpose


split/splitless, glass wool,
taper, deactivated

For split/splitless
injection

870

5183-4711
$27

5183-4712
$112

5183-4713
$476

Splitless Inlet Liners


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

900

5062-3587
$30

5183-4693
$129

5183-4694
$560

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

800

5181-3315
$36

5183-4705
$163

5183-4706
$751

NEW! Liner, Splitless,


double-taper, no glass wool,
polymerically deactivated

800

5181-3315EN
$43

250

18740-80220
$28

5183-4707
$124

5183-4708
$533

140

18740-80200
$17

5183-4709
$73

5183-4710
$308

990
$19

210-3003
$84

210-3003-5

Agilent Choice Liners


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

For trace pesticide


analysis

Direct Inlet Liners


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

5/pk

25/pk

Split Inlet Liner


Liner, split, glass wool, non-deactivated

990

19251-60540
$19

5183-4691
$78

5183-4692
$336

Split Inlet Liners For Manual Injection


Liner, split, with cup, no glass wool

800

18740-80190
$40

5183-4699
$179

5183-4700
$784

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


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

800

18740-60840
$43

5183-4697
$191

5183-4698
$840

Direct Connect Liners


Part No.
G1544-80730
G1544-80700

Price
$62
$62

Dimensions
6.3 mm X 78.5 mm
6.3 mm X 78.5 mm

Part No.
210-4004-5
210-4022-5

Price
$98
$108

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)

Part No.
5180-4182
5180-4173
5180-4168

Price
$13
$52
$52
5188-2741 $19

Single taper direct connect liner, 4 mm ID, deactivated


Dual taper direct connect liner, 4 mm ID, deactivated
Focus Liners
Focus liner
Focus liner

53

ID
4.0 mm
4.0 mm

Wool
Yes
Yes

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, dont
settle for imitations; choose only genuine Agilent parts.
Our inlets are backed by the same 40 years of design experience that
youve come to expect from our instruments. So you get optimal
performance, plus the reproducible results that your lab demands.
Whats 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.

Gold-Plated Seal (Splitless)


See page 55

Retaining Nut
Part No. G1544-20590
Washer
Part No. 5061-5869, 12/pk
Reducing Nut
Part No. 18740-20800,
1 each

Ferrules (85% Vespel, 15% Graphite)


Part No. 5062-3516, 0.37 mm I.D.,
for 100-200 m Columns, 10/pk
Part No. 5181-3323, 0.40 mm I.D.,
for 250 m Columns, 10/pk
Part No. 5062-3514, 0.50 mm I.D.,
for 320 m Columns, 10/pk
Part No. 5062-3512, 0.74 mm I.D.,
for 530 m Columns, 10/pk
Column Nut for 6890 GC
Part No. 5181-8830, 2/pk

www.agilent.com/chem

800 227 9770

54

SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

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.

Part No.

Price

19251-60575
G1544-60575
G1544-80580

$230
$216
$73

G1544-60585

$330

G1580-60575

$261

G1580-60585

$236

5890 Split/Splitless Multimode Inlet Supplies


Septum retainer nut
18740-60835
Retainer nut for headspace sampling
18740-60830
Retaining nut
19251-20620
Reducing nut
18740-20800
For a complete parts breakdown, 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

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

55

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 Agilents 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, weve also
included a detailed discussion about the
prevention of non-volatile and semi-volatile
contamination, as well as appropriate
recovery measures.

Agilent lets you choose from over 1,000


different columns. Its 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 Agilents 20052006 Essential Chromatography Catalog. Or, visit our online catalog at
www.agilent.com/chem/4ecatalog.

www.agilent.com/chem

800 227 9770

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).

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 columns 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)

57

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

COLUMNS

Popular Column Choices


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.

Description

Part No.

Price

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

122-0132

$483

HP-5ms, 0.25mm i.d., 30m, 0.25m

19091S-433

$483

DB-XLB, 0.25mm i.d., 30m, 0.25m

122-1232

$483

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

122-3832

$483

HP-INNOWax, 0.25mm i.d.,


30m, 0.25m

19091N-133

$413

Column Installation, Setup, & Conditioning


The first step in obtaining optimal
column performance and lifetime is
proper installation:

Verify that all fittings are leak-free and


the carrier gas is oxygen-free before
heating the oven.

Choose the appropriate size and


material ferrule for the column,
injector and detector type.

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.

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.

TIPS AND TOOLS


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

www.agilent.com/chem

800 227 9770

58

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.

Description

Part No.

Price

Ceramic wafer (4/pk)

5181-8836

$ 15

20x Magnifier

430-1020

$ 42

General Purpose Graphite ferrule


(0.5mm ID, for column IDs 0.32mm)
10/pk

5080-8853

$ 47

General Purpose Graphite ferrule


(1.0mm ID, for 0.45-0.53mm
ID columns) 10/pk

5080-8773

$ 38

Gas leak detector 115V


Gas leak detector 220V

5182-9646
5182-9648

$1859
$1859

Condition the column as specified in the


literature provided with each column.

Causes of Performance Degradation


Column Breakage

Prevention

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.

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.

NOTE: Larger diameter columns

(0.45- 0.53mm id) are more prone


to breakage.

Avoid winding or bending the column


too tightly.

Recovery

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

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.

59

www.agilent.com/chem

800 227 9770

COLUMNS

Thermal Damage
Exceeding a columns 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).

Description

Part No.

Price

FlowTracker 2000 Flowmeter and Leak Detector

5183-4780

$1143

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

BOT-2

$ 235

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

BMT-2

$ 235

Big Universal Trap (Combination Trap)


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

RMSH-2

$ 261

Advanced Green Septa (11mm, 50/pk)

5183-4759

$ 62

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.

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

COLUMNS

Chemical Damage

GUARD COLUMN

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).

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:

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 NH4OH are present in a sample,
minimizing water retention will render
these compounds relatively harmless
to the column.

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.

Prevention
Perform sample preparation to remove
inorganic acids and bases from the
sample
Install guard column and trim frequently
If acids or bases must be used choose an
organic alternative or HCl or NH4OH

Guard Column
INJECTOR

DETECTOR

Recovery
Remove 0.5 to 1 meter from the front
of the column
Severe cases may require the removal
of 5 or more meters

Column

Guard Column

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.

61

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
Description

Part No.

Price

Split/Splitless Inlet liner: glass wool,


taper, deactivated (5/pk)

5183-4712

$112

Splitless Inlet liner: single-taper,


no glass wool, deactivated (5/pk)

5183-4695

$124

Quartz deactivated column


connector (5/pk)

5181-3396

$ 94

Polyimide sealing resin (5 grams)

500-1200

$ 24

Deactivated Fused silica,


10m, 0.53mm i.d.

160-2535-10

$110

Perform sample cleanup to remove


nonvolatile materials from the sample

Deactivated Fused silica,


10m, 0.25mm i.d.

160-2255-10

$ 73

Use injection port liners packed with


glass wool (may not be feasible when
analyzing active compounds)

Capillary column rinse kit

430-3000

$ 78

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

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.).

Prevention

Column Storage

Perform sample cleanup to remove


semi-volatile materials from the sample

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.

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.

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.

1. Place 20-30 L 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.

www.agilent.com/chem

800 227 9770

62

COLUMNS

Column Types and Characteristics

DB-1ms
100% Dimethylpolysiloxane
Identical selectivity to DB-1
Nonpolar
Very low bleed characteristics
Improved acid performance compared to
standard 100% Dimethylpolysiloxane
columns
Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
Excellent general purpose column
Bonded and cross-linked
Solvent rinsable

63

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


I.D.

Length

Film

Part No.

Price

0.10
0.10
0.10
0.10

10
10
20
20

0.10
0.40
0.10
0.40

127-0112
127-0113
127-0122
127-0123

$343
$343
$495
$495

0.20
0.20

12
25

0.33
0.33

128-0112
128-0122

$261
$400

0.25
0.25
0.25

30
30
60

0.10
0.25
0.25

122-0131
122-0132
122-0162

$483
$483
$823

0.32
0.32
0.32

30
30
60

0.10
0.25
0.25

123-0131
123-0132
123-0162

$521
$521
$896

Similar Phases

Applications

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

General purpose: Amines, hydrocarbons,


pesticides, PCBs, phenols, sulfur
compounds, flavors and fragrances.

www.agilent.com/chem

800 227 9770

COLUMNS

DB-5ms

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

Phenyl Arylene polymer equivalent to a


(5%-Phenyl)-methylpolysiloxane
Nonpolar
Very low bleed characteristics
Excellent inertness for active compounds
Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
Bonded and cross-linked
Solvent rinsable
Certified for MS
Exact replacement of HP-5TA
Close equivalent to USP Phase G27

HP-5ms

I.D.

Length

Film

Part No.

Price

0.18
0.18

20
40

0.18
0.18

121-5522
121-5542

$412
$740

0.20
0.20

25
50

0.33
0.33

128-5522
128-5552

$400
$674

0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25

25
25
30
30
30
50
60
60

0.25
0.40
0.10
0.25
0.50
0.25
0.10
0.25

122-5522
122-552A
122-5531
122-5532
122-5536
122-5552
122-5561
122-5562

$421
$421
$483
$483
$483
$753
$823
$823

0.32
0.32
0.32
0.32
0.32
0.32

30
30
30
50
60
60

0.10
0.25
0.50
0.25
0.10
0.25

123-5531
123-5532
123-5536
123-5552
123-5561
123-5562

$521
$521
$521
$804
$896
$896

Similar Phases

Applications

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


BPX-5

Semivolatiles, alkaloids, drugs, FAMEs,


halogenated compounds, pesticides,
herbicides

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

(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

I.D.

Length

Film

Part No.

Price

0.20
0.20
0.20

12
25
50

0.33
0.33
0.33

19091S-101
19091S-102
19091S-105

$261
$400
$674

0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25

15
15
15
30
30
30
60
60

0.10
0.25
1.00
0.10
0.25
0.50
0.10
0.25

19091S-331
19091S-431
19091S-231
19091S-333
19091S-433*
19091S-133
19091S-336
19091S-436

$295
$295
$295
$483
$483
$483
$823
$823

0.32
0.32
0.32
0.32
0.32
0.32
0.32

15
25
30
30
30
60
60

1.00
0.52
0.10
0.25
0.50
0.10
0.25

19091S-211
19091S-112
19091S-313
19091S-413
19091S-113
19091S-316
19091S-416

$319
$448
$521
$521
$521
$896
$896

* This column is shipped with the 5973 MSD.

www.agilent.com/chem

800 227 9770

64

COLUMNS

DB-XLB
Exceptionally low bleed
Low polarity
Extended temperature limit of 360C
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

DB-35ms
Equivalent to a (35%-Phenyl)methylpolysiloxane
Midpolarity
Very low bleed characteristics
Extended temperature limit of 360C
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

65

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


I.D.

Length

Film

Part No.

Price

0.18
0.18

20
30

0.18
0.18

121-1222
121-1232

$412
$579

0.20
0.20

12
25

0.33
0.33

128-1212
128-1222

$261
$400

0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25

15
15
15
30
30
30
30
60

0.10
0.25
1.00
0.10
0.25
0.50
1.00
0.25

122-1211
122-1212
122-1213
122-1231
122-1232
122-1236
122-1233
122-1262

$295
$295
$295
$483
$483
$483
$483
$823

0.32
0.32
0.32
0.32

30
30
30
60

0.10
0.25
0.50
0.25

123-1231
123-1232
123-1236
123-1262

$521
$521
$521
$896

Similar Phase

Applications

MDN-12

PCB congeners, pesticides, chlorinated


herbicides, phenoxy acid methyl esters,
haloacetic acids

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


I.D.

Length

Film

Part No.

Price

0.20
0.20

15
25

0.33
0.33

128-3812
128-3822

$261
$400

0.25
0.25
0.25
0.25

15
30
30
60

0.25
0.15
0.25
0.25

122-3812
122-3831
122-3832
122-3862

$295
$483
$483
$823

0.32
0.32

30
60

0.25
0.25

123-3832
123-3862

$521
$896

Similar Phases

Applications

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

Aroclors, PCBs, amines, pesticides,


chlorinated herbicides, haloacetic acids,
pharmaceuticals, drugs of abuse

www.agilent.com/chem

800 227 9770

COLUMNS

DB-17ms

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

Equivalent to (50%-Phenyl)methylpolysiloxane
320/340C Upper temperature limit
Very low bleed midpolarity column
Excellent inertness for active compounds
Enhanced mass spectral integrity
Bonded and cross-linked
Solvent rinsable
Best column for CLP pesticides

DB-225ms

I.D.

Length

Film

Part No.

Price

0.18

20

0.18

121-4722

$412

0.25
0.25
0.25
0.25
0.25

15
15
30
30
60

0.15
0.25
0.15
0.25
0.25

122-4711
122-4712
122-4731
122-4732
122-4762

$295
$295
$483
$483
$823

0.32
0.32

30
30

0.15
0.25

123-4731
123-4732

$521
$521

Similar Phases

Applications

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


SPB-50, BPX-50, SPB-17

Drugs, glycols, pesticides, steroids

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

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

I.D.

Length

Film

Part No.

Price

0.25
0.25
0.25

15
30
60

0.25
0.25
0.25

122-2912
122-2932
122-2962

$295
$483
$823

0.32

30

0.25

123-2932

$521

Similar Phases

Applications

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


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

Alditol acetates, FAMEs, neutral sterols

EASY ONLINE ORDERING


Need a column thats custom-designed for your lab?
Just visit www.agilent.com/chem/4ecatalog

www.agilent.com/chem

800 227 9770

66

COLUMNS

HP-INNOWax
Polyethylene glycol (PEG)
High polarity
Highest upper-temperature limits of the
bonded PEG phases
Column-to-column repeatability
Bonded and cross-linked
Solvent rinsable
Close equivalent to USP Phase G16

GS-GasPro
Unique bonded PLOT column technology
Excellent choice for light hydrocarbons
and sulfur gases
Retention stability not affected by water
Separates CO and CO2 on a single
column
Ideal PLOT column for GC/MS
no particles

67

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


I.D.

Length

Film

Part No.

Price

0.20
0.20
0.20
0.20

25
25
50
50

0.20
0.40
0.20
0.40

19091N-102
19091N-202
19091N-105
19091N-205

$379
$379
$636
$636

0.25
0.25
0.25
0.25
0.25
0.25

30
30
30
60
60
60

0.15
0.25
0.50
0.15
0.25
0.50

19091N-033
19091N-133
19091N-233
19091N-036
19091N-136
19091N-236

$413
$413
$413
$737
$737
$737

0.32
0.32
0.32
0.32
0.32
0.32

30
30
30
60
60
60

0.15
0.25
0.50
0.15
0.25
0.50

19091N-013
19091N-113
19091N-213
19091N-016
19091N-116
19091N-216

$447
$447
$447
$816
$816
$816

Similar Phases

Applications

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


SUPEROX II, CB-WAX, Stabilwax, BP-20,
007-CW, Carbowax, DB-WAXetr

Alcohols, aromatics, essential oils, solvents

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


I.D.

Length

Part No.

Price

0.32
0.32

30
60

113-4332
113-4362

$627
$942

Similar Phase

Applications

CP-Silica PLOT

C1 to C12 hydrocarbons, CO2, trace-level


sulfurs, hydride gases, inorganic gases,
halocarbons, SF6, oxygen/nitrogen
separation at -80C.

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.

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

www.agilent.com/chem

800 227 9770

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.

Igniter Glow Plug Assembly

Collector Assembly

Collector Body

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

FID Jets

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 50C, 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.

FID Ferrules

Cleaning & Replacement


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

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

VIDEO
To view a video on FID column installation, jet replacement,
collector maintenance, or ignitor replacement, visit
www.agilent.com/chem/techsupport.
69

www.agilent.com/chem

800 227 9770

DETECTORS

Jet Cleaning Procedure

6890/6850 Ionization Detector (FID) Supplies

(using Agilents 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

Item Description

Unit

Part No.

Price

PTFE chimney (optional)**

19231-21050

$ 14

Collector nut

19231-20940

$ 35

Spring washer

5181-3311

$ 9

Ignitor castle

19231-20910

$ 57

Optional Hastelloy Ignitor Castle*

19231-21060

$184

Ignitor glow plug assembly

19231-60680

$ 42

Collector insulator

G1531-20700

$ 17

Collector body
Hastelloy Collector Body

G1531-20690
61531-21090

$ 60
$260

FID collector assembly 1

G1531-60690

$194

Detector insulation assembly

G1531-20700

$ 17

8710-1346

$ 8

10/pk

FID collector cleaning brush

2/pk

only with forceps!

Collector Housing

G1531-20740

$175

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.

FID retainer nut wrench


(5880, 5890, 6890)

19301-00150

$ 8

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

8710-1561

$ 13

5182-3450
18710-20119
18710-60170
19231-60680
19244-80560
19301-60660
5180-4150
5180-4152
19301-20720
5180-4153
9301-0985

$556
$ 49
$ 44
$ 42
$ 56
$ 53
$ 23
$ 23
$ 12
$ 8
$ 41

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.

FID supplies kit-Includes:


Jet, packed standard
FID performance evaluation sample kit
Ignitor glow plug assembly
Jet, cap. series 530 m
FID flow measuring insert
Cleaning wires for 0.03 in. ID jet
Cleaning wires: 0.018 in. ID/530 m jet
Wire, jet cleaning,
Capillary inlet cleaning wires
Detector cleaning kit

3 each
2 each
2 each
3 each
2 each
1/pk
5 each

**Not included in assembly.


*Hastelloy components may be used when analyzing highly corrosive materials.
1 Does not include Hastelloy component.

Plugged FID jet

EASY ONLINE ORDERING


Heres 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
www.agilent.com/chem

800 227 9770

70

DETECTORS

FID Jets
Description

Length(mm)

Part No.

Price

Jets for capillary dedicated FID

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

48

G1531-80560

$43

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

48

G1531-80620

$54

Capillary 0.53 mm jet (0.011 in. ID tip)

61.5

19244-80560

$56

Packed (0.018 in. ID tip)

63.5

18710-20119

$49

Packed (0.030 in. ID tip)

63.5

18789-80070

$55

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

61.5

19244-80620

$37

Adaptable FID

Agilent FID Jets (from top to bottom): Dedicated


capillary, Adaptable capillary, Adaptable packed

2
3

FID Consumables
4

Description

Unit

Part No.

Price

FID flow measuring insert

19301-60660

$53

FID ignitor cable

G1531-60680

$41

FID Performance evaluation sample kit, 0.03% C14,


C15, and C16 normal alkanes in hexane

18710-60170

$44

5080-4978

$ 7

19301-20720

$12

O-rings

12/pk

Cleaning wire
Jet cleaning wire for 0.03 in. ID jet

5/pk

5180-4150

$23

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

5/pk

5180-4152

$23

8
6
7

6890 Series GC FID Detector

TIPS AND TOOLS

Collector Body, P/N G1531-20690

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.

71

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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 (-ECD). These two types can
be distinguished by the top cover of the
detector the ECD has a solid cover and
the -ECD has a perforated cover.

Radioactivity Leak Test

Thermal Cleaning

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.

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 63Ni may be
removed during other procedures,
causing possible hazardous exposure
to and x-radiation.

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.

Gas Purity
For successful EC detection, its 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.

www.agilent.com/chem

800 227 9770

72

DETECTORS

Electron-Capture Detector (ECD) Supplies


Item Description

Part No.

Price

ECD makeup gas adapter*

G1533-80565

$198

2, 3 Nut warmer cup with insulation

19234-60720

$ 58

ECD adapter replacement liner, fused silica

19233-20625

$ 15

ECD end cap

19233-20755

$ 32

ECD chemical sample kit, 3 ampoules


solution of 33 pg/mL (0.033 ppm)
each of lindane and aldrin in isooctane

18713-60040

$ 46

ECD wipe test kit

18713-60050

$ 31

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


1

6890 Series GC ECD Detector

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.

TIPS AND TOOLS


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

73

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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

Cell Contamination

Increased filament lifetime will result if the


following startup process is used:

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.

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

Part No.

Price

G1532-60675

$1030

18740-20950

$ 18

18740-20960

$ 33

6890/6850/5890 Common TCD Supplies


TCD replacement cell (6890/6850 only)
TCD cap column adapter seal

10/pk

TCD cap column adapter


Graphite ferrules, 1.0 mm id

10/pk

5080-8773

$ 38

Graphite ferrules, 0.5 mm id

10/pk

5080-8853

$ 47

Capillary column nut, for 6890

2/pk

5181-8830

$ 26

Capillary column nut, for 6850

2/pk

5183-4732

$ 47

G1532-20710

$ 44

TCD chemical sample kit, 3 ampoules,


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

$ 45

TCD packed column adapter (6890/6850 only)

5890 TCD Supplies

www.agilent.com/chem

800 227 9770

Makeup gas adapter, TCD

19232-80550

$ 126

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

19302-80020

$ 138

TCD replacement cartridge

19232-60676

$1625

74

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 L 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.

75

5. After the final injection, allow makeup


gas to flow for 10 minutes or more.
Slowly raise the temperature of the cell
to 20-30C 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

www.agilent.com/chem

800 227 9770

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).

If the flame doesnt 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 doesnt
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 wont 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

If the FPD flame wont light or stay lit:

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.

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.

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.

Occasionally, the transfer line fused silica


liner between the column and FPD module
must be inspected, cleaned and/or replaced.

Flame Ignition Problems

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.

76

DETECTORS

6890/5890 FPD Supplies


Item Description
1

Exit tube assembly

Nut, brass, 1/4 in.

Unit

Part No.

Price

19256-60700

$ 72

5180-4105

$ 13

10/pk

2
3

Weldment, block

19256-80560

$536

O-ring, ignitor, Kalrez

0905-1610

$ 42

Spacer, ignitor

19256-20590

$ 15

FPD Ignitor Replacement Kit

19256-60800

$ 68

Ignitor cable assembly (6890 only)

G1535-60600

$ 22

Gasket, heat shield

19256-80045

$ 83

10

Window, first heat shield

19256-80030

$ 38

11

Disk, heat shield

19256-20580

$ 80

12

Coupling, SS

19256-20550

$165

14

Screw, M3 x 12 (4 required)

0515-0911

$ 1

15

Clamp

19256-00090

$ 59

16

O-ring, inner window

5061-5886

$ 24

17

Window, second heat shield

19256-80060

$ 40

18

O-ring, outer window

5061-5891

$ 24

19

Flange adapter

19256-20510

$131

20

Flange ring

19256-00200

$ 22

21

O-ring, Viton, 1.239 in. id

5061-5890

$ 21

Adapter weldment, 1/8 in. columns

19256-80590

$141

Adapter weldment, capillary

19256-80570

$114

Start-up kit (5890 only)

19256-60500

$434

5061-5867

$ 17

Liner/ferrule kit

19256-60590

$ 89

Sulfur filter

19256-80000

$378

Phosphorus filter

19256-80010

$378

Kalrez O-ring, size 2-002

0905-1609

$ 42

Kalrez O-ring, size 2-011

0905-1608

$ 42

5061-5889

$ 19

19305-60580

$ 40

10

11

12
8

13

14

15

16
17
18

Fluorocarbon Elastomer O-ring,


brown, 0.926 in. id

12/pk

12/pk

12/pk

12/pk

FPD Performance Evaluation Sample: Solution of


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

77

20
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

MAINTENANCE MINDER

FPD O-ring (5890 only)

12/pk

19

800 227 9770

DETECTORS

Nitrogen-Phosphorus Detector (NPD)


Bead Maintenance

Bead Life

Gas Flow

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.

To extend the life of the bead:


Use the lowest practical adjust offset or
bead voltage.

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 335C).

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.

www.agilent.com/chem

800 227 9770

Run clean samples and keep the inlet/liner


clean to minimize contamination.
Turn off the bead when not in use.

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 100C and maintain it
for 30 minutes. Then set the detector
temperature to 150C and maintain it
for another 30 minutes.

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.

78

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.

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.

NPD Jets
Description

Part No.

Price

48

G1531-80560

$ 43

Capillary 0.53 mm jet (0.011 in. id tip)

61.5

19244-80560

$ 56

Packed (0.018 in. id tip)

63.5

18710-20119

$ 49

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


(6890 only, dedicated)

Length (mm)

6890/5890 Adaptable

79

www.agilent.com/chem

800 227 9770

DETECTORS

Nitrogen-Phosphorous Detector (NPD) Supplies


Item

Description

Part No.

Price

6890 NPD Supplies


1

Screws, M3 x 0.5 x 8 mm (Pozidriv)

0515-0655

$ 1

NPD white ceramic bead assembly*

G1534-60570

$368

NPD black ceramic bead assembly**

5183-2007

$379

Lid weldment

G1534-80510

$160

Metal C-ring, top

0905-2580

$ 53

Alumina insulator, upper

G1534-40020

$ 72

Collector funnel

G1534-20530

$ 64

Alumina insulator, lower

G1534-40030

$ 42

Metal C-ring bottom and top

0905-1284

$ 53

Screw, M4 x 10 mm

0515-2495

$ 1

10

J-Clamp

1400-0015

$ 1

11

Screw, M4 x 10 mm

0515-2495

$ 1

12

NPD interconnect assembly

G1534-60610

$160

13

Mounting pallet

G1531-40020

$ 29

14

Jets (see page 79)

15

Base weldment, Capillary NPD

G1534-80500

$501

Base Weldment, Packed NPD

G1534-80540

$532

Lid stop

G1534-20590

$ 36

NPD Ceramic Insulator Kit


includes items 4, 5, 7, and 8

5182-9722

$175

19234-60720

$ 58

NPD collector (NPD bead)

19234-60540

$289

Recoating kit, sufficient for 10 collectors

5080-8872

$216

Detector Trap Replacement Kit

19231-60790

$284

16

17

Column adapters for packed NPD

18

Nut warmer cup with insulation

9
10

11

12

4
5
6

13
14

15
16

17

18

5890 NPD Supplies

*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.

www.agilent.com/chem

800 227 9770

80

You asked we listened!

Our new e-Catalog makes online


ordering easier than ever.
Weve 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.

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

www.agilent.com/chem

800 227 9770

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.

Every day
Check, and if necessary, replace the
septum. Check the injection port liners.
Check the tightness of the column nuts.
Hint: With Agilents new Flip Top Inlet
Sealing System, you dont 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).
TASK

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
WEEK

EVERY
6 MONTHS

EVERY
YEAR

AS
NEEDED

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.

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


83

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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

Air Leaks

Symptoms of leaks include:

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.

www.agilent.com/chem

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).

800 227 9770

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)

84

GC/MS SYSTEMS

Leaks can occur in many more places


in the MSD:
GC/MSD interface column nut
side/top plate O-ring (all the way around)
vent valve O-ring
calibration valve
high vacuum gauge tube fitting
cracked ion gauge tube
front and rear end plate O-rings
GC/MSD interface O-ring (where the
interface attaches to the vacuum
manifold)
diffusion pump co-seal and/or baffle
adapter O-ring
turbomolecular pump O-ring
new Vespel/graphite ferrules contract
when heated

Description

Part No.

Price

MS interface column nut

05988-20066

$13

Column nut for GC/MS and two-hole ferrules

05921-21170

$16

Universal Column Nut (2/pk)

5181-8830

$26

TIPS AND TOOLS

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

Corrective Action
Check interface nut for tightness.
Replace if necessary.
Check leak/test the GC injection port.

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 thats 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

Part No.

Price

Nylon gloves, lint-free, Large


Nylon gloves, lint-free, Small

8650-0030
8650-0029

$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

85

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

GC/MS SYSTEMS

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.

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

Possible Source

13,14,15,16

Methane

CI gas

18, 28, 32, 44 or 14, 16

H2O, N2, O2, CO2 or N, O

Residual air and water, air leaks, outgassing from


Vespel ferrules

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


181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614

PFTBA and related ions

PFTBA (tuning compound)

31

Methanol

Cleaning solvent

43, 58

Acetone

Cleaning solvent

78

Benzene

Cleaning solvent

91, 92

Toluene or xylene

Cleaning solvent

105, 106

Xylene

Cleaning solvent

151, 153

Trichloroethane

Cleaning solvent

69

Foreline pump fluid or


PFTBA

Foreline pump oil vapor or calibration valve leak

73, 147, 207, 221, 281,


295, 355, 429

Dimethylpolysiloxane

Septum bleed or methyl silicone column coating

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


262, 354, 446

Diffusion pump fluid

Diffusion pump fluid and related ions

149

Plasticizer (phthalates)

Vacuum seals (O-rings) damaged by high temperatures,


use of vinyl or plastic gloves

Peaks spaced 14 amu apart

Hydrocarbons

Fingerprints, foreline pump oil

www.agilent.com/chem

800 227 9770

86

GC/MS SYSTEMS

Mass Spectrometer Symptoms


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

Symptoms

Corrective Action

Wrong retention time

Check GC, method, application and carrier gas velocity

Low signal

Check GC, tune vacuum system

Leaking injection port

Clean the injection port


Replace the injection port liner and septa

Air leak

Check and tighten interface nut, leak test GC injection port

Peak widths

Do Autotune, check flow rate and temperature stability

Interfering peaks

Check time parameters, coeluting peaks, column type

Excessive background

Do Autotune and compare to background specifications


Check time parameters

Incorrect mass assignment

Retune

Abnormal spectra
excessive background
contamination

Check for contamination

Incorrect tuning

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

Clean or replace the syringe

Wrong syringe needle

Replace syringe and septa

Leaking injection port

Perform injection port maintenance


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

Injection is too large

Check method and injection volume, split ratio


and/or splitless purge time

Loose column connections Tighten column nuts on injection port or transfer line
Replace column nuts and ferrule

87

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

Dirty ion source

Clean source

Loose connections
in the analyzer

Check internal and external analyzer wiring connections,


make sure all are secure

Ground loops

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 mole-

cules, 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.

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.

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:

Abrasive methods offer several advantages:


provide adequate energy to remove
contamination from surfaces
require minimal equipment
pose minimal risks to the user

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.

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 customers 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

heated zones are less than 100C


the diffusion pump is off and cool
the turbo pump is off and not spinning
the rough pump is off

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.

TIPS AND TOOLS


Agilents 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

Description

Part No.

Price

8650-0030
8650-0029
9310-4828
5181-8863

$ 16
$ 16
$185
$124

05980-60051
5061-5896

$ 64
$ 27

8660-0791
8500-0656
05971-60571
8500-1233

$ 29
$168
$ 85
$115

05980-20018
5080-5400

$ 14
$ 10

8710-0899
8710-0900
8710-0510

$ 16
$ 25
$ 24

Screwdriver, TORX, T15


Screwdriver, TORX, T10

8710-1622
5182-3466

$ 38
$ 24

Ferrules and O-rings


Teflon 1/4 in. ferrule (back)
Teflon 1/4 in. ferrule (front)
Retainer rings (10/pk)

0100-0160
0100-0787
5181-1258

$ 8
$ 8
$ 10

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)

5183-2096

$657

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)

05971-60561

$510

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.

89

www.agilent.com/chem

800 227 9770

GC/MS SYSTEMS

5973 MSD Ion Source Parts (EI)


Item

Description

5973 Part No.

Price

(A) Ion source body

G1099-20130

$ 198

(B) Repeller

G1099-20132

$ 112

(C) Interface socket

G1099-20136

$ 29

(D) Drawout plate

05971-20134

$ 69

(E)

Drawout cylinder

G1072-20008

$ 190

(F)

Ion focus lens

05971-20143

$ 263

(G) Entrance lens

05971-20126

$ 105

(H) Repeller insulator

G1099-20133

$ 82

(I)

Set screw

0515-1446

(J)

Washer, M3 (1/pk)

3050-0891

(K) Nut, 5.5 mm

0535-0071

(L)

G1099-60104

$ 200

05971-20130

$ 270

Ion source assembly

G1099-60106

$ 270

Source heater assembly

G1099-60177

$ 408

Ion Source Sensor

(M) Lens insulator, (2/pk)

Repeller assembly

G1099-60170

$ 481

Screw (for filament on the source)

0515-1046

H
L

E
D
M

5973 Ion Source Parts (EI).

MS Inert Ion Source Parts


Description

5973A

5973N

5973 inert**

Price

B
I

Drawout plate 3 mm Inert


Drawout plate 6 mm Inert** G2589-20045

G2589-20045

EI High Temp Filament

G2589-20100

$ 99

G2589-20045

$ 225

G2590-60053

$ 97

Repeller assembly, Inert source G1099-60170

G1099-60170

G2589-60102

$ 499

Screws for filament High Temp 0515-1046

0515-1046

G1999-20021

G1099-20130

G2589-20043

$ 563

G2589-20101

$ 12

Source body, Inert


Source Washer, Inert

G1099-20130

H
I

5973 Repeller Assembly (EI).

**used in G2860A and G2860B extended linearity kits

www.agilent.com/chem

800 227 9770

90

GC/MS SYSTEMS

TIPS AND TOOLS

It is good practice to replace scratched lenses and other ion source parts.
Scratched source parts lead to poor performance.

G
5972/5971/GCD Ion Source (EI)

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


Description
(A) Entrance lens

5972/5971/GCD Part No.

Price

05971-20126

$ 108

(B) Lens insulator, (2/pk)

05971-20130

$ 278

(C) Ion focus lens

05971-20143

$ 271

(D) Drawout cylinder

G1072-20008

$ 190

(E) Drawout plate

05971-20134

$ 71

(F) Ion source body

05971-20128

$ 531

(G) Set screw

0515-1446

(H) Repeller assembly

05971-60170

(I) Screw (for filament on the source)

Ion source assembly

Transfer line tip, gold-plated

$ 593

0515-1046

5972 Part No.

Price

05972-60226

$3554

5972/5971 Part No.

Price

GCD Part No.

Price

05971-20305

$ 242

G1800-20305

$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

91

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

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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.

TIPS AND TOOLS

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:

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.

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.

Filament Assembly
Description

Unit

Part No.

Price

05972-60053

$ 90

G1099-80053

$282

Filament, EI High Temperature for the 5973 inert

G2590-60053

$ 97

Filament, 5972 (EI/CI)

05972-60053

$ 90

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

05971-60140

$159

Filament, 5973 (EI)


Filament, 5973 (CI)

2/pk

Quadrupole Mass Filter


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

www.agilent.com/chem

800 227 9770

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.

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.

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

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

MAINTENANCE MINDER

Keeping a pan under the vacuum pump helps to


detect and identify the origin of oil leaks.

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

Part No.

Price

PFTBA sample, certified (10 g) (EI)


PFDTD sample (10 g) (CI)

8500-0656
8500-8130

$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.

93

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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 vacuum manifold pressures can only be


measured if your system is equipped with
the optional gauge controller.

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.

Foreline pressure is too high

Vacuum manifold pressure is too high

Symptom

Pressure is above 100 mTorr.


Pressure for a given column flow has
increased over time.

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 (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

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

Vacuum manifold pressure is too low

Symptom

Pressure is below 20 mTorr.

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*
Foreline gauge is not working correctly

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

* These could create a fault condition in the


GC that would prevent the GC from operating.

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 60C 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.

Description

Part No.

Price

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)

6040-0809
59864B
0960-0376
0960-0897

$ 82
$1399
$ 195
$ 358

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.

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.

95

Avoid contact with the pump oil. The


residue from some samples may be toxic.
Dispose of used oil properly.

Description

Part No.

Price

Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD)

6040-0798

$122

Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD)

6040-0834

$ 39

Molecular sieve (5973, 5972 or 5971/GCD)

9301-1104

$ 57

Oil mist filter RV3/E1M18/E2M18/E2M2

3162-1056

$430

Oil mist filter E2M1.5

G1099-80037

$173

Oil mist filter E2M18

5063-5224

$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.

8. Reconnect the MSD power cord.


9. Start up and pump down the MSD
according to the Instrument Manual
procedure.

3. Remove the fill cap from the top of the pump to


expose the fill hole.
4. Remove the drain plug from the pump.

TIPS AND TOOLS

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.

Use chemical-resistant gloves and safety glasses when replacing pump


fluid. Avoid contact with the fluid. Always dispose of used oil properly.

6. Reinstall the drain plug and pour pump oil into


the fill hole.
7. Reinstall the fill cap.

Electron Multipliers and Replacement Horn


Maximize Lifetime
The lifetime of an EM is directly related to the current that
flows through it and the extent of contamination or
condensation that it experiences. 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.
Dont tune excessively. PFTBA can result in higher
background over an extended period of time.

Description

Part No.

Price

Electron multiplier replacement horn


(5973, 5972, 5971/GCD)
High energy dynode (5973 only)
Electron multiplier kit (5972, 5971/GCD only)

05971-80103

$1004

G1099-80001
05971-80102

$2131
$1136

Symptom
Voltage is over 2500 volts
Poor vacuum
Corrective Action
Replace electron multiplier

TIPS AND TOOLS


Use only Agilent replacement multipliers and horns for Agilent MSDs.
Other manufacturers products can increase noise, while reducing
sensitivity and linearity.

www.agilent.com/chem

800 227 9770

96

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

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

97

5989 or
5988

Thermo or
Electro Spray

5985 or
5987

5999x, 5993x
or 5995x

Part No.

Price

6040-0468

$ 134

6040-0370
6040-0819

$2553
$ 283

6040-0798
6040-0834
6040-0730

$ 133
$ 40
$ 760

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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

Every
Week

Every
3 Months

Every
6 Months

As
Needed

Autotune or manual tune (save results)

Cabinet Maintenance

Clean the cabinet

Inspect hoses and cords

Vacuum the fan filter

Vacuum System Maintenance


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

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.

TIPS AND TOOLS

Check mech. pump oil

GC/MS Interface Maintenance


Refill EI calibration vial
Refill CI calibration vial
Replace interface heater

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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.

C
D

5989 Lens Stack

Description

Part No.

Price

(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

05989-20110
05989-67002
05989-20111
05989-20109
05989-20145
05989-20119
05989-20165
05985-60179
05989-60098

$108
$990
$ 62
$ 88
$318
$580
$448
$ 58
$926

E
F

5989 Repeller Assembly

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

Part No.

Price

05989-80043
05971-80103

$2012
$1004

0960-0799

$ 448

05989-20705
5181-3367

$ 18
$ 47

0905-1145
3162-0110
0905-1189

$ 19
$ 39
$ 38

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

99

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GC/MS SYSTEMS

General GC/MS Supplies


G2860A 8270 Semi-Volatiles
Applications Kit
The G2860A 8270 Semi-Volatiles
Applications Kit is designed for use in
Agilent 6890/5973A and 6890/5973N
GC/MSD Systems. 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.

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

Part No.

Price

8270 Semi-Volatiles Applications Kit

G2860A

$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.

Tuning Samples

Verification Samples Performance

Checkout Samples
Semi-Volatile Volatile

MSD

EI
Tune

CI
Tune

EI

Negative
Mode CI

Positive
Mode CI

5973

PFTBA

PFDTD

OFN 1 pg/L

OFN 1 pg/L

Benzophenone 100 pg/L

DFTPP

BFB

5972

PFTBA

PFTBA

HCB 10 pg/L

NA

Benzophenone 100 pg/L

DFTPP

BFB

5971

PFTBA

PFTBA

HCB 10 pg/L

NA

Benzophenone 100 pg/L

DFTPP

BFB

GCD

PFTBA

NA

Sample A (10 ng/L)

NA

NA

DFTPP

BFB

5989A

PFTBA

PFTBA

HCB 50 pg/L

OFN 1 pg/L

Benzophenone 100 pg/L

DFTPP

BFB

5989B

PFTBA

PFTBA

HCB 20 pg/L

OFN 500 fg/L

Benzophenone 100 pg/L

DFTPP

BFB

MS Engine

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

101

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GC/MS SYSTEMS

Description

Quantity

Part No.

Price

05970-60045

$ 46

8500-5995

$ 62

8500-6406

$ 38

Evaluation Sample for GC/MS Systems


Contains 6 vials: 4 vials (Sample A, 10 ng/L), 1 vial (Sample B, 100 pg/L),
and 1 vial (Sample C, 100 ng/L) 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/L, HCB 20 pg/mL, Benzophenone 100 pg/L,
OFN 1 pg/L, mix of HCB, OFN and Benzophenone 5 ng/L
Extended Mass Performance Sample

0.5 g, fomblin oil

8500-5500

$141

PFTBA certified

1 bottle, 10 g

8500-0656

$168

PFTBA Sample Kit

0.5 mL

05971-60571

$ 85

PFDTD

10 g

8500-8130

$ 44

Benzophenone

100 pg/L,
5 ampoules

8500-5440

$ 74

Hexachlorobenzene

10 pg/L, 4 ampoules
1 ng/L, 2 ampoules

8500-5808

$ 39

Hexachlorobenzene

20 pg/L

8500-6405

$ 32

PFTBA not certified

1 ng/L (2 ea)

05990-60075

$ 67

Octafluoronapthalene (OFN)

1 pg/L,
5 ampoules

8500-5441

$ 67

Octafluoronapthalene (OFN)

500 fg/L

8500-6572

$ 30

p-Bromofluorobenzene (BFB)

25 g/mL

8500-5851

$ 39

Methyl stearate (in methanol);

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You asked we listened!

Announcing the launch of


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

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.

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 labs 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

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SERVICES & SUPPORT

Our focus is on keeping your lab running at peak performance.

A Total Commitment
to Your Lab for One Fixed Cost.

The Unmatched Expertise


of Fully Trained Engineers.

The Flexibility to Select The


Solution Thats Right for You.

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.

You can rest assured that the engineer


who arrives at your site will perform the
requested service with optimum skill.
Thats because Agilent engineers

Our team will work with you to help your


laboratory achieve

If you choose, you can also consolidate


instrument maintenance and repair
services into multi-year agreements
for administrative ease and greater
cost savings.

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.

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

Whats 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.

105

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SERVICES & SUPPORT

Agilent Services

Features

Advantages to You

Telephone Service

Telephone access to skilled Agilent service


professionals.

Fast identification and resolution


of hardware problems.

Available parts option.

Low cost.

Telephone access to trained technical


professionals.

Fast identification and resolution


of software problems.

Enhancements to the original application


software purchase.

A fixed annual cost for software


upgrades makes budget management
more predictable.

Software Service

Software bulletins that identify discovered


defects and recommend workarounds.

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.

A fixed annual cost for parts makes


budget management more predictable.
You can choose the response
method that fits your business
needs and budget.

Optional coverage for consumables


used during repair.
Offsite Instrument Repair
For selected Agilent analysis instruments

Option 1: Replacement with an identical


instrument (your fastest choice).

Less expensive than onsite repair.


Fast and easy.

Option 2: Return to Agilent for repair.


Includes extensive diagnostics and
testing that are not feasible with onsite
maintenance or repair.
Preventative Maintenance
For selected Agilent analysis instruments

Expert cleaning, adjustment, lubrication,


and inspection of your instrument.

Maximum uptime.
Extended instrument life.

Travel expenses and labor.


Coverage for consumables used.

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Confidence in the integrity


of your measurements.

106

SERVICES & SUPPORT

Agilent Services

Features

Advantages to You

Installation Qualification (IQ)

Qualification and documentation of


shipment completeness.

Supplies the evidence you need to


satisfy regulatory agencies.

Comprehensive system and application


software verification tests.

Helps fulfill the master validation plan


and change-control SOP requirements
for the IQ phase.

Delivered by professionals with training


certification.
Operational Qualification/Performance
Verification (OQ/PV)
For selected Agilent analysis instruments

Verification and documentation of an


instruments ability to meet specified
criteria.

Note: We recommend Preventative


Maintenance before OQ/PV.

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.

Verification that a system is performing


at operation specifications after repair.

Minimal system downtime after


completion of instrument repair.

Complete system operation testing.

Efficient system requalification by


performing the appropriate tests based
on the components repaired.

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.

Assurance that all instrument


subsystems are performing within
specifications.
All procedures and documentation meet
regulatory agency requirements.

Measuring equipment is traceable to


national and international standards.

107

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SERVICES & SUPPORT

Agilent Services

Features

Advantages to You

Network Qualification

Network definition and performance


testing using established Agilent Design,
Installation Qualification, and Operational
Qualification protocols.

Significant time savings.

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. Well also
provide the following reports:
- Long Duration Network Characterization,
which analyzes each function in its
operating environment.

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.

- Performance Predictability Analysis,


which documents reserve capacity and
stability over a range of operating
demands.
Mass Spectrometer Ion Source Cleaning
For selected Agilent analysis instruments

Onsite disassembling
Cleaning

Your staff can devote more time to


chemistry, not instrument maintenance.
Efficient cleaning with minimal
downtime.

Reassembling
Testing

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108

SERVICES & SUPPORT

Agilent Services

Features

Advantages to You

Software Backup

Telephone or onsite factory support to


facilitate restoration.

Fast and easy you simply insert a disk


reboot and youll 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.

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

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

TIPS AND TOOLS


To learn more about Agilents complete portfolio of services, please
visit www.agilent.com/chem/service.

109

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SERVICES & SUPPORT

Education & Training Services


Highly trained lab professionals can boost your productivity, minimize errors and
reruns, and expand your chromatography capabilities. And thats why Agilent offers
several training options that cover everything from troubleshooting and maintenance
to the most advanced operational techniques.
eLearning
Agilents 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

Duration

Description

6890 GC Split Inlet Mode Operation

Self-paced;
Four hours access

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.

6890 GC Splitless Inlet Mode Operation

Self-paced;
Four hours access

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.

6890 GC Purged Packed Inlet Operation

Self-paced;
Four hours access

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.

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110

SERVICES & SUPPORT

Course Title

Duration

Description

6890 GC Keyboard Operation

Self-paced;
Four hours access

Reviews the basic operation of the 6890


GC keyboard.
Thoroughly describes all keys, so you can
gain the maximum benefit from your GC.

6890 GC FID Theory and Operation

Self-paced;
Four hours access

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.

6890 GC ECD Theory and Operation

Self-paced;
Four hours access

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.

6890 GC TCD Theory and Operation

Self-paced;
Four hours access

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.

GC Automatic Liquid Sampler Operation

Instructor-led;
60-90 minutes

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

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SERVICES & SUPPORT

Course Title

Duration

Description

Logical GC Troubleshooting

Instructor-led;
60-90 minutes

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.

Using the GC/MSD


Security ChemStation to Achieve
FDA CFR Part 11 Compliance

Instructor-led;
60-90 minutes

Describes in detail how to operate the


GC/MSD Security ChemStation software
in accordance with FDA CFR Part 11
requirements.

Managing and Administering the


GC/MSD Security ChemStation
to Meet FDA CFR Part 11
Compliance Requirements

Instructor-led;
60-90 minutes

Shows you how to manage the GC/MSD


Security ChemStation software in
accordance with FDA CFR Part 11
requirements.

Designed for systems administrators

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112

SERVICES & SUPPORT

Classroom Training
Agilents 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

113

Course No.

No. of Days

Description

Technique
Introduction to Capillary GC

H2615A

Provides an overview of capillary gas chromatography in a


lecture format.

Techniques of GC

H4002A

Presents the fundamental concepts of gas


chromatography.

Introduction to GC-MS

H2609A

Introduces the technique of GC-MS in a lecture format that


includes worksheet exercises.

Techniques of GC-MS

H4040A

Reviews the key concepts of the GC-MS analysis process,


as well as qualitative and quantitative GC-MS techniques.

Hardware/Software Operation
ChemStation Operation for the 6890 GC/ALS

H5926A

Explains how to operate the Agilent 6890 GC using GC


ChemStation software.

Operation of the GC-MSD System


Using the ChemStation for GC-MSD

H4043A

Enhances an operators 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.

GC-MSD System for Environmental Applications

H4050A

Increases an operators skill in using a mass selective


detector with mass spectrometer EnviroQuant software.

Troubleshooting and Maintenance


6890 GC Maintenance

H5308A

Addresses preventative maintenance and first-level repair


for the Agilent 6890 GC.

5890 GC Maintenance

H4001A

Addresses preventative maintenance and first-level repair


for the Agilent 5890 GC.

6890 GC Troubleshooting and


Preventative Maintenance

H5309A

Introduces troubleshooting of the Agilent 6890 GC in a


lecture format.

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SERVICES & SUPPORT

Course Title

Course No.

No. of Days

Description

Introduction to 5973 GC-MSD Troubleshooting


and Preventative Maintenance

H5947A

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.

5973 GC-MSD Troubleshooting


and Preventative Maintenance

H2294A

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

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.

Data Analysis and Reporting Using the


ChemStation for GC-MSD

H4076A

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.

Data Analysis and Reporting Using


the EnviroQuant ChemStation for GC-MSD

H4053A

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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114

SERVICES & SUPPORT

Support
Tap Agilents 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.
Youll 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.

aTechnical Support Consultation


Have a technical GC column, method, or troubleshooting question? Agilents 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.

115

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You asked we listened!

Our new e-Catalog makes online


ordering easier than ever.
Weve 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

Receive a years worth of current chromatography insights with a

FREE subscription to Separation Times.

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been one of the scientific communitys most
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analysis. And now, its available online!
Each issue is packed with
Application details geared toward specific
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and well automatically e-mail it to you
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GC System Recommended Maintenance Schedule

Gas Management
ITEM

TYPICAL SCHEDULE

ACTIONS/COMMENTS

Gas purifiers
(carrier gas &
detector gas)

Every 6-12 months

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.

Split vent trap

Every 6 months*

Replace.

Flowmeter
calibration

Every 1-2 years

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

Syringes
and/or syringe
needles

Every 3 months*

Replace syringe if dirt is noticeable in the syringe, if it cannot be


cleaned, if the plunger doesnt slide easily, or if clogged. Replace
needle if septa wear is abnormal or the needle becomes clogged.

Inlet liner

Weekly*

Check often. Replace when dirt is visible in the liner or if


chromatography is degraded.

Liner O-rings

Monthly*

Replace with liner or with signs of wear.

Inlet septum

Daily*

Check often. Replace when signs of deterioration are visible


(gaping holes, fragments in inlet liner, poor chromatography,
low column pressure, etc.).

Inlet Hardware

Every 6 months

Check for leaks and clean.

Every year

Check parts and replace when parts are worn, scratched, or broken.

Remember, the downtime for scheduled


maintenance is always less disruptive
than the downtime for unscheduled
maintenance and troubleshooting!

Columns
ITEM

TYPICAL SCHEDULE

ACTIONS/COMMENTS

Front-end
Maintenance

Weekly monthly*

Remove 12 -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.

Solvent rinse

As needed

When chromatography degradation is due to column contamination.


Only for bonded and cross-linked phases.

Replacement

As needed

When trimming and/or solvent rinsing no longer return chromatographic


performance.

Ferrules

Replace ferrules when changing columns and inlet/detector parts.

Detectors
ITEM

TYPICAL SCHEDULE

ACTIONS/COMMENTS

FID/NPD Jets
& Collector

As needed

Clean when deposits are present. Replace when they become scratched,
bent or damaged, or when having difficulty lighting FID or keeping flame lit.

NPD Bead

As needed

Replace when signal drifts or there is a dramatic change in sensitivity.

FID

Every 6 months

Measure hydrogen, air, and makeup gas flows.

TCD

As needed

Thermally clean by baking-out when a wandering baseline, increased


noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.

ECD

Every 6 months
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

www.agilent.com/chem
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 Agilents 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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