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Operate your lab at peak performance

Troubleshoot difficult problems


Select the right PerfectFit supplies
Plan preventive maintenance

Maintaining Your Agilent GC System


Maximize your efficiency. Minimize your downtime.

Introduction
With many labs today finding themselves
with reduced staff, our GC Maintenance
Guide was designed to put 35 years of
Agilents GC knowledge right in your lab.
We share everything from essential
maintenance schedules to keep you up
and running, to invaluable troubleshooting
tips and problem solving methods. Weve
even included an easy guide to help you
order the right Agilent PerfectFit parts
and supplies to keep your downtime to
a minimum.
At Agilent Technologies, we give you more
than the worlds best GC system. We give
you knowledge!

Maintaining Your Agilent GC System

UT

PU

O
L-

POST ER ENCL

OS
ED

Maximize your efficiency. Minimize your downtime.

oting
o
h
s
ble
Trou Guide
GC

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


web site. Just visit www.agilent.com/chem/supplies to
view videos and obtain more information.

3
4
5
5
13
14
15
16

Gas Management
Gas Types
Purities
Purifiers
Regulators
Tubing
Leak Detection
Flow Rates

19 Sample
Introduction
& Inlets
Sample Introduction
20 Vials & Syringes
Inlet Types
26 Packed Column
28 Split/Splitless
31 Cool on-Column
34 PTV
Inlet Accessories
36 Septa, Liners,
Ferrules

37
38
38
38
39

Columns
Column Maintenance
Column Selection
Installation/Setup
Column
Performance

43 Detectors
44 Thermal
Conductivity
Detector (TCD)
45 NitrogenPhosphorous
Detector (NPD)
48 Electron-Capture
Detector (ECD)
50 Flame Photometric
Detector (FPD)
52 Flame Ionization
Detector (FID)
55 Service & Support
56 Expert Training,
Service & Support

Dont Miss
GC Troubleshooting Guide (pullout poster)
GC Maintenance Schedule (inside back cover)

www.agilent.com/chem

GAS MANAGEMENT

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 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

www.agilent.com/chem

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 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.

not it will make contact with the sample.


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

Support Gases

For most applications, gases which are low


in oils and particulates are desirable; thus,
low-purity specialty gas grade products
can be used. Fuels, oxidants and detector
gases, in most cases, do come in contact
with the sample and detector, and require
higher purity gases.

Support gases may be specific for detectors


or for applications. These gases include
fuels, oxidants, coolants, detector gases,
and pneumatic gases. The degree of purity
required for support gases is dependent on
how that gas is being used, and whether or

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 depends 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%)

www.agilent.com/chem

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.

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
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

most common contaminant

a common cause of column stationary


phase and inlet liner degradation

can cause decomposition of labile


analytes

opportunity for introduction at every


fitting present in the gas line or during
use of wrong tubing (i.e., gas permeable)

decrease detector sensitivity by


increasing detector background noise

In some cases it may be difficult to


determine which contaminant presents
the biggest problem in a given analysis. If
unsure, a call to your gas supplier may be
helpful. Once the problem contaminants
have been identified and a general
contaminant level is determined, the next
step is to choose a gas purity level that
comes closest to these requirements.
Keep in mind that higher grades of gas
generally cost more. The greatest cost
savings can be achieved by using the
lowest purity gas which will neither
interfere with the analysis nor damage
your equipment. Using the proper gas
purification equipment to remove common
contaminants and achieve the desired
purity level is essential.

Gas Purification Systems


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

www.agilent.com/chem

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 saturate and become
ineffective, or worse, a source of
contamination.

Other Considerations

determine desired purity level

keep number of breaks 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

NEED MORE HELP?

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.

Tap Agilents GC knowledge


over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

www.agilent.com/chem

GAS MANAGEMENT

Moisture (Water) Traps


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

Indicating moisture traps are available in


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

Refillable Glass Moisture Trap

Moisture Removal Traps


Description

Size
(cc)

H2O Removal
Capacity (g)

Maximum Effluent H2O


Concentration (ppb)

1/8 in.
Part No.

1/4 in.
Part No.

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

MT200-2

MT200-4

MSR-1

MSR-1

GMT-2-HP

GMT-4-HP

GMSR

GMSR

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

Big Moisture Traps for the Ultimate Moisture Capacity

Big Moisture Trap

750

Refill for BMT Series (2 refills)

Refillable Moisture Trap

www.agilent.com/chem

Moisture S-Trap

BMT-2

BMT-4

BMSR-1

BMSR-1

Big Moisture Trap

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

GAS MANAGEMENT

Oxygen Traps
Oxygen traps usually contain 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 remove
some small organics and sulfur compounds
from gas streams.

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.

Indicating Oxygen Traps glass body with plastic safety shield

Indicating Oxygen Trap

30

IOT-2-HP

IOT-4-HP

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

Big Oxygen Trap

750

BOT-2

Hydrocarbon Traps
Size (cc)

1/8 in.
Part No.

1/4 in.
Part No.

200

HT200-2

HT200-4

ACR

ACR

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 is 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.

BOT-4

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)

BHT-2

BHT-4

BACR

BACR

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

Capillary Grade Hydrocarbon Traps for crucial capillary applications

Capillary Grade Hydrocarbon Trap


Adsorbent Refill (1 pint, 3 refills)

100

Hydrocarbon Trap

HT3-2

HT3-4

ACR

ACR

www.agilent.com/chem

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:

Leak-free, one-piece design to eliminate


potential leaks from using multiple traps

Efficient design which prevents


channeling and promotes efficient
scrubbing

The ultimate in purification with a single


trap (Big Universal Trap)

Optimized adsorbents for maximum


surface area and capacity

Description

Size (cc)

1/8 in.
Part No.

1/4 in.
Part No.

100

OT3-2

OT3-4

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

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

Big Universal Trap Helium


purged (also recommended
for GC Mass Spec)

750

RMSH-2

RMSH-4

Big Universal Trap Hydrogen purged

750

RMSHY-2

RMSHY-4

Big Universal Trap Nitrogen purged

750

RMSN-2

RMSN-4

UMC-5-2

UMC-5-2

Big Mounting Clip for


mounting Big Traps 2/pk

www.agilent.com/chem

Big Universal Trap

Hydrocarbon Moisture Trap

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

GAS MANAGEMENT

High Capacity
Gas Purification System

Single-Cartridge System

Contains a triple-combination cartridge


that offers the same highly efficient
contaminant removal properties from
eight cylinders of carrier gas but without
the visual indicator.

Other cartridges are also available for


detector gas supplies and as individual
filters for specialized requirements.

Three Cartridge System

Three Cartridge
High Capacity
Gas Purification
System

Agilents highest capacity and most


economical gas purification system.

Provides low-cost gas contaminant


removal for up to 18 cylinders of
carrier gas.

Includes a manifold with cartridge


mounts and three replaceable cartridges:
one moisture/hydrocarbon cartridge; one
oxygen cartridge; and one oxygen
indicating cartridge.

Consists of a permanent all-welded


stainless steel manifold to minimize
the potential for leaks.

Suitable for bench or wall mounting.

High Capacity Gas Purification System


Description

Part No.

Three Cartridge SystemIncludes manifold


for wall or bench mount and 3 cartridges
(H2O/hydrocarbon, oxygen, and indicating O2)
With 1/8 in. fittings

5183-1907

With 1/4 in. fittings

5182-9776

Replacement Cartridge Kit


Includes all three cartridges for
above system.

5182-9780

Single Cartridge SystemIncludes single


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

10

With 1/8 in. fittings

5183-4598

With 1/4 in. fittings

5183-4599

Triple combination replacement cartridge


for single cartridge system

5183-4600

www.agilent.com/chem

GAS MANAGEMENT

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.

1/8

RQC-P

4-Head

O2, indicating O2, HC, H2O

Replacement Cartridges
Description

NEED MORE HELP?


Part No.

High capacity oxygen

GC-1

High capacity moisture

GC-2

Indicating moisture

GC-2-I

Hydrocarbon

GC-3

Indicating oxygen

GC-4

www.agilent.com/chem

Tap Agilents GC knowledge


over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

11

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 close off the system to the
atmosphere, further minimizing the entry
of contaminants.

Available with 1/8 fittings only


Description

Part No.

Carrier Gas Purification System: Single


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

5182-9704

Super-Clean Gas Purification System:


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

5182-0816

Replacement Filter Cartridges

Description

Triple Filter Cartridge: A single carrier gas


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

5182-9705

Filter cartridge bundle of 4 (oxygen,


moisture, and 2 hydrocarbon)

5183-4770

Part No.

Universal/external split vent trap


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

RDT-1020

Replacement cartridges (3/pk)

RDT-1023

Split Vent Trap and Cartridges

12

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

Universal/External Split Vent Trap


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

www.agilent.com/chem

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

Description

Part No.

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

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

5183-4641

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

5183-4642

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

5183-4643

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

5183-4644

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

5183-4645

Brass Body Regulator

to purity considerations, then a stainless


steel regulator should be chosen for the
same reasons. Unfortunately, use of high
purity stainless steel regulators is often
cost-prohibitive.
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
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.

*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
Regulator Outlet Adapters Female NPT to Swagelok-style

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


(included with brass regulators)

0100-0118

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

0100-0119

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

HELPFUL HINT: Always depressurize


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

www.agilent.com/chem

13

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 as


pressurizing pneumatic lines; however, be
aware of its pressure limitations.
In view of these problems, the list of
appropriate tubing materials has been
narrowed down to two: copper and
stainless steel. Agilent recommends using
copper tubing for most applications, since
it is easy to bend and plumb and is less
expensive than stainless steel. Use
stainless steel tubing only for crucial
applications that require very high purity.

Cleaning Tubing
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

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 becomes unwieldy
sometimes, 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

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.

Part No.

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

5180-4196

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

5021-7107

HELPFUL HINT: 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.

14

www.agilent.com/chem

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.

Spectra-Link with 1/8 in. fittings


and 36 in. SS tubing

SL-8

Spectra-Link with 1/4 in. fittings


and 36 in. SS tubing

SL-4

Cylinder Bracket
Description

Part No.

Cylinder wall bracket with strap and chain


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

5183-1941
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.

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

Gas leak detector, 220 V

5182-9648

Gas Leak Detector


www.agilent.com/chem

15

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.

FlowTracker 1000 Flowmeter

5183-4779

FlowTracker 2000 Flowmeter and


Leak Detector

5183-4780

FlowTracker Universal AC Adapter (optional,


not supplied with FlowTracker units)
5183-4781

ADM 1000 features include:

Accuracy 3%

Operating temperature range


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

ADM 2000
In addition to the features of the ADM
1000, the ADM 2000 includes:

Calibrationtraceable to NIST primary


standards

Mass flow measurementsmeasure


flow rate, independent of atmospheric
pressure and temperature (calculated)

Data output through RS-232 port

Real time, split ratio measurement

CE mark certified

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 1000

ADM 2000

16

www.agilent.com/chem

GAS MANAGEMENT

Flowmeters
Description

Flow Rate (mL/min)


Low
High

Gases
Measured

Accuracy
(%)

Power
Supply

RS-232 Data
Output

Part No.

ADM Flowmeters volumetric, measures all gases*


ADM1000

0.5

1000

All

9V Battery

None

220-1170

ADM2000

0.5

1000

All

Battery or 120 VAC

Yes

220-1171-U

ADM2000E

0.5

1000

All

Battery or 220 VAC

Yes

220-1171-E

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

Veri-Flow 500
(220 V)

5.0

500

He, H2, Ar/CH4


N2, Air

Rechargeable Battery
or 220 VAC

Yes

HVF-500-2

Optiflow Flowmeters Gas Flowmeters versatile volumetric flowmeters**


Optiflow 420

0.1

50

All

+/- 3

9V Battery

None

HFM-420

Optiflow 570

0.5

700

All

+/- 3

9V Battery

None

HFM-570

Optiflow 650

5.0

5,000

All

+/- 2

9V Battery

None

HFM-650

*non-corrosive gases only


**non-corrosive and mildly corrosive gases only

Veri-Flow 500
Optiflow 420

NEED MORE HELP?


Tap Agilents GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

www.agilent.com/chem

Only a small sampling of flowmeters are shown here. For a complete selection of flowmeters, see the
Flowmeter Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

17

Theres More!
Agilent offers a series of free
Maintenance Guides for your GC System.

Successful chromatography depends on optimum


performance from every component of the GC system.
At Agilent, we want to help you keep your system running
at peak performance. We want to share our 35 years
experience in chromatography to help you maximize your
investment. This new GC System Maintenance Guide is just
one in a series of system support literature from Agilent,
designed to help you optimize the performance of your
GC system. Other Guides include:

GC Inlet Resource Guide

(publication # 5988-3466)

This 24-page Guide offers troubleshooting tips for all components


of the GC inlet, including septa, ferrules, and liners.

Maintaining Your GC/MS System

(publication # 5988-3960)

This 48-page Guide covers everything from maintaining a Mass


Selective Detector, to GC/MS columns and supplies, to GC/MS
support services.

Developed by Agilent GC and GC/MS experts, these Guides


are packed with system operation and maintenance
recommendations, repair tips, and easy ordering information
for PerfectFit parts and supplies. For a copy of these Guides,
visit www.agilent.com/chem, call 800-227-9770 (in US), or
contact your authorized Agilent distributor.

Sample Introduction
& Inlets
Agilent offers a wide range of GC sample
vials, septa, syringes, liners and inlets
for a broad range of gas-phase applications.
Our PerfectFit supplies have been designed
specifically for Agilent instruments so
they help to ensure GC results that are
reproducible and accurate. This section
reviews these critical components, and
helps you make the right choice. Also, look
for useful information from proper syringe
use and cleaning techniques to a detailed
discussion on optimized inlet settings. All
to make your GC analysis easier. All from
the GC experts.

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

www.agilent.com/chem

Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes, see the
Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

19

SAMPLE INTRODUCTION & INLETS

Sample Introduction
Vials

Vial Filling

Agilent wide opening vials are a perfect fit


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 Silanizedfor use with


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

Polypropylenefor use
with alcohols and aqueous
solvents

Amber Vialsfor use with Microvolume Inserts


light-sensitive samples
for use with very small
sample volumes

High Recovery Vials


for use with limited sample
volumes

Recommended fill volumes for sample vials


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

1 mL

50 L

3.6 mm*
*Needle position based on standard sampling depth.

20

100 L vial

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

Selecting Vial Septa Materials


Vial cap septa are critically important
to optimal analysis. Each septum
complements the overall system and
enhances chemical performance.
Agilent vial cap septa are specifically
formulated and constructed for optimum
system performance, with minimal coring
and superior chemical inertness.

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

Determining Your Quantity Needs


To determine potential septa ordering
quantities, consider:

the number of samples run during a


day/week

if samples are run in small or large


batches

if samples are run manually or with an


autosampler

if samples are run overnight, unattended

Silicone/Teflon
Excellent resealing
Resists coring
Good for multiple injections

Teflon/Silicone/Teflon
Used in trace analysis applications
Above average resealing
Most resistant to coring
Least evaporation
Use with large diameter, blunt tip
syringe needles

HELPFUL HINT: Unattended autosampler


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

Vials
Description

Quantity

Part No.

2 mL Crimp top vial convenience


pack with silver AI caps with
Teflon/Red rubber septa

500/pk

5181-3400

2 mL Screw top vial convenience


pack with blue screw caps and
Teflon/Red rubber septa

500/pk

5182-0732

2 mL Snap top vial convenience pack


with clear polypropylene snap caps
and Teflon/Red rubber septa

500/pk

5182-0547

100 L Insert for wide opening vials

100/pk

5181-1270

1000/pk

9301-0978

100 L Glass lined polypropylene vials

100/pk

9301-0977

15 L reservoir volume, Micro-V vial,


clear crimp top

100/pk

5184-3551

30 L reservoir volume, High recovery


vial, crimp top

100/pk

5182-3454

Teflon Disc
Good for MS and ECD analysis
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

Vials

300 L Polypropylene vials

21

SAMPLE INTRODUCTION & 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 are a perfect fit
with your autosamplers and come with a
variety of plunger and needle choices.

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.

PerfectFit means they 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 applicable

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

NEED MORE HELP?


Tap Agilents GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

22

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.

www.agilent.com/chem

SAMPLE INTRODUCTION & 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 2 L and larger syringe
injections
Clean samples
Plunger not
Routine analysis
replaceable

Replacing On-column Syringe Needles

To insert a needle into a syringe barrel:

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.

1. Unscrew the syringe barrel cap and


remove the spring.

HELPFUL HINT: Failure to use an


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

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.

To view a video on syringe installation, visit


www.agilent.com/chem/supplies, click on
How-to Video under the Reference Library.
www.agilent.com/chem

23

SAMPLE INTRODUCTION & INLETS

Syringe Tips

Make sure to input the proper syringe


size when setting up the injection section
of your data handling device.

Rinse syringes and clean their plungers


before use to maximize syringe lifetime.

Rinse the syringe 5-8 times between


injections to minimize sample carryover.

Pump sample in and out of the syringe at


least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.

A 26 gauge syringe can be used for oncolumn 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.

24

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.

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

Syringes
Description

Gauge

Quantity

Part No.

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

5 L

Tapered

Fixed Needle

23-26s/42

6/pk

5181-8810

10 L

Straight

Fixed Needle

23/42

6/pk

9301-0725

5 L

Straight

Fixed Needle

23/42

6/pk

5182-0875

Straight Needle Syringes


(use with Merlin Microseal)

Automatic Liquid Sampler Supplies


Description

Unit

Part No.

144/pk

9301-0723

12/pk

07673-40180

144/pk

9301-1031

25/pk

5182-0551

Miscellaneous Autosampler Supplies


4 mL wash vial with screw caps
Diffusion caps for 4 mL vials
Septa for 4 mL vial
4 mL wash vial with fill marking, caps
Screw for mounting syringe

07673-20570

Quadrant kit (4 tray sections)

18596-40015

7673 Basic Supply Kit contains:


10 mL syringes (6/ea), 23/26 gauge
needles, 4 mL vials with diffusion caps
(144/pk), 2 mL automatic sampler
vials with screw caps (1,000/pk),
GC septa (25/pk), Vial racks (5/pk)

07673-60840

www.agilent.com/chem

Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

25

SAMPLE INTRODUCTION & 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.

26

The inherent activity of packed-column


inlets is somewhat mediated by the fact
that they usually have low internal volume.
When this is coupled with the relatively
fast flow rates used with packed columns,
the residence time of sample in the inlet is
short and decomposition is reduced in
comparison to the decomposition that
occurs with some capillary inlets (for
example, splitless inlets).

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

Leaks
Since packed-column inlets are usually
flow-controlled, septum and column leaks
will have a direct impact on retention times
and peak areas. Sample can be lost through
the leak holes, and air can diffuse back into
the inlet to cause column degradation.
Change the septum on a regular basis and
check column connections at the first stage
of problems. To prevent stationary phase
decomposition, make sure that the oven
and inlet are at room temperature when not
in use and when changing the septum.

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

6890/6850/5890 Series GC Packed Port Supplies*


Item

Description

Septum nut

Septa Bleed temperature,


optimized, 11 mm**

Unit

Part No.
1

18740-60835
50/pk

2
3
4

5183-4757

Top insert weldment

19243-80570

Viton O-rings

12/pk

5080-8898

Glass liner, disposable

25/pk

5080-8732

Glass liner, disposable/deactivated

5/pk

5181-3382

Vespel/graphite ferrules, 1/4 in. id

10/pk

5080-8774

Tubing nut, 1/4 in. brass

10/pk

5180-4105
Liner

Adapters with glass liners


8

0.53 mm column adapter

19244-80540

1/8 in. column adapter

19243-80530

1/4 in. column adapter

19243-80540

Upper insulation

19243-00067

10

Nut warmer cup with insulation

19234-60720

11

Column nut for 0.53 mm column

2/pk

5181-8830

** For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
* For Model 6890/6850 only
** For a complete selection of inlet supplies, refer to Agilents GC Inlet Resource Guide.

Inside of
Oven
9

1/4 in. Vespel/


graphite ferrule
1/4 in. nut
1/8 in. or 1/4 in.
stainless steel liner

10

11

5890 Packed Column Inlet Supplies


Description

Unit

Nonpurging septum nut assembly


for manual flow control only, not EPC

Part No.

19243-60570

Adapters without glass liners


1/8 in. column adapter

19243-80510

1/4 in. column adapter

19243-80520

Universal Packed Column Inlet (non-purged)


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

www.agilent.com/chem

19243-60505
10/pk

NEED MORE HELP?


Tap Agilents GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

5180-4105

27

SAMPLE INTRODUCTION & INLETS

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

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

cannot be diluted for analysis (for


example, solvents)

are gases that cannot be focused, or


that have long injection times (valve
injections)

have important minor peaks eluting


directly before the solvent peak (as in
solvent analysis)

Split injection is also good for screening


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

Troubleshooting
Split inlets are spared from most bandbroadening phenomena, since narrow
peaks are generated as part of the
splitting process. Therefore, any peak
broadening or tailing observed with split
injection is usually due to improper
column installation, low split flow, 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.

Split Mode Procedures/Practices


Parameter

Selection/Setting

Rationale

Inlet temperature

BP 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
Stops flow of droplets
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

Initial column
temperatures

Not critical

Narrow initial peaks

Septum purge

2-3 mL/min

Minimizes ghosting

To view a video on liner and gold seal replacement,


visit www.agilent.com/chem/supplies, click on
How-to Video under the Reference Library.

28

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

Splitless Mode Procedures/Practices

Splitless Mode

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

Inlet packing

None

Use only with slow injection


Decreases degradation

Silanized glass wool

Use for fast autoinjection


& dirty samples

Injection volume

0.5-2 L liquid

Depends on solvent, liner,


& conditions

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

Not critical

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

Septum purge

2-3mL/min

Reduces ghosting

Quantification

Internal standard
Standard addition

Maximizes reproducibility
Use only with constant
injection volume

Retention gap

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

Reduces peak distortion


Promotes solvent and
stationary phase focusing

www.agilent.com/chem

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.

NEED MORE HELP?


Tap Agilents GC knowledge
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29

SAMPLE INTRODUCTION & INLETS

Splitless injection is routinely used in


areas such as:

environmental analysis

pesticide monitoring of foods

drug screening

In these applications, sample preparation


requirements are significant, and it is not
always possible or economically justifiable
to clean up a sample extensively. So
column protection becomes as important
as sensitivity. Also, samples with trace
quantities of important solutes that elute

HELPFUL HINT: A guard column or


retention gap is often beneficial for
splitless injections (see page 41).

on the solvent tail may be focused by the


solvent to yield more sensitive analyses.

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

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.

6890/6850/5890 Split/Splitless Inlet Supplies*


Item

volume), leading to irreproducibility and


nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
volume carefully to avoid backflash.

Description

Septum retainer nut

Unit

Part No.

18740-60835

Septa**

Insert Weldment**

Liner O-ring**

Liner**

Split vent trap assembly (6890/6850 only)

G1544-80550

Retaining nut (6890/6850 only)


Retaining nut (5890 only)

G1544-20590
19251-20620

SS seal
Gold-plated seal

18740-20880
18740-20885

Washer, 0.375 in. od

7
8
9

12/pk

5061-5869

10

Reducing nut

18740-20800

11

Insulation (requires 3)

19243-00067

12

Lower insulation cover

19243-00070

13

Ferrule**

14

Column nut (6890/5890 only)

2/pk

5181-8830

Column nut (6850 only)

2/pk

5183-4732

10

11

Angled wrench for split/splitless inlet

19251-00100

12
13
14

30

**For a complete parts breakdown, see the 6890/6850/5890 Series GC Instrument User and/or Service Manuals.
**For a complete selection of inlet supplies, refer to Agilents GC Inlet Resource Guide.

www.agilent.com/chem

SAMPLE INTRODUCTION & 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 nonvolatile components
Permits autoinjection with
narrow-bore columns

HELPFUL HINT: Since the sample is directly deposited into the column, nonvolatile sample
components can accumulate at the head of the column and will degrade efficiency and/or
interact with subsequent injections.
www.agilent.com/chem

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

the potential for column overload,


column contamination,

the incompatibility of some solvents


with the stationary phase,

dependence of the initial column


temperature on the boiling point of
the solvent.

Many of the problems associated


with these variables can be resolved
by using a retention gap ahead of the
analytical column.

To view a video on cool on-column installation and


septum replacement, visit www.agilent.com/chem/supplies,
click on How-to Video under the Reference Library.

31

SAMPLE INTRODUCTION & INLETS

Troubleshooting
The major problems found with cool oncolumn injection are associated with
column overload, solvent/stationary phase
incompatibility, and column contamination.
If the flooded zone after injection is too
long (large injections, poor wettability),
peaks will be broad or split. A retention gap
usually will resolve this problem. Loss of
column efficiency with on-column injection
usually is caused by contamination or
degradation of the stationary phase at the
head of the column. Only columns with an
immobilized stationary phase should be
used with cool on-column injection to

prevent displacement of the stationary


phase by solvents.
Immobilized stationary phases can be
washed to remove contaminants and
renew performance. If column performance
does not improve after washing, cut 0.5m
off the inlet side of the column. If that does
not return column performance, the column
must be replaced and a retention gap
should be used for all further injections of
dirty samples.

Column/Retention Gap Installation Consumables


Item Description

Unit

Part No.

Column nut

2/pk

5181-8830

250 m graphite/Vespel ferrule

10/pk

5181-3323

320 m 0.5 mm graphite/Vespel ferrule

10/pk

5062-3514

250 m retention gap (one 5 m piece)

160-2255-5

320 m retention gap (one 5 m piece)

160-2325-5

530 m retention gap (one 5 m piece)

160-2535-5

Quartz deactivated column connector


fits 0.18-0.53 mm

5/pk

5181-3396

NEED MORE HELP?


Tap Agilents GC knowledge
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classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

32

HELPFUL HINT: Sample degradation can


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

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

6890/5890 Series Cool On-Column Inlet Supplies


Item Description

Unit

Part No.
1a

1b

Manual injection
1c

Cooling tower assembly

1d

Duckbill septum

10/pk

19245-40050

Fused silica syringe needles

6/pk

19091-63000

1c
1d

19320-80625

Syringe barrel for use with


fused-silica needles,10 L

2
3

9301-0658

Common Supplies
3

Spring

Inserts for capillary columns

19245-60760

For 200 m columns (one ring)

19245-20510

For 250 m columns (six rings)

19245-20515

For 320 m columns (five rings)

19245-20525

For 530 m columns (no rings)

19245-20580

For 530 m Al clad columns (four rings)

19245-20780

Ferrule

5080-8853

Column nut

2/pk

5
6

5181-8830

6890 Series GC Cool On-Column Inlet Supplies


Automatic Injection
1a

Septum nut base for 320 mm assembly

19245-80521

1b

Septum nut base for 530 mm assembly

G1545-80520

Advanced green 5 mm through hole septa


BTO 5 mm through hole septa

50/pk
50/pk

5183-4760
5183-4758

5890 Series Cool On-Column Inlet Supplies


Automatic Injection
1a
Septum nut (5890 Series II GC)

19245-80520

1b

19245-20670

Needle guide (for 7673A only)

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

www.agilent.com/chem

Only a small sampling of inlet supplies are shown here. For a complete selection of inlet supplies,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

33

SAMPLE INTRODUCTION & 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
minimal inlet discrimination
no special syringe needed
use of large injection volumes
removal of solvent and low boiling
components
trapping of nonvolatile components in liner
split or splitless operation
retention time and area reproducibility
approaching cool on-column injection

Ballistic

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 ramps rates to
shorten splitless purge delay time
Simpler, less expensive
instrumentation

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

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

To view a video on PTV column installation,


liner installation and silver seal replacement,
visit www.agilent.com/chem/supplies,
click on How-to Video under the Reference Library.

34

www.agilent.com/chem

SAMPLE INTRODUCTION & INLETS

6890 PTV Inlet


Item

Description

Column ID

Unit

Part No.

Septumless head

G2617-60507

Septum head

G2618-80500

Septum nut

18740-60835

PTV inlet assy

G2617-60506

PTV LCO2 cooling jacket

G2617-60508

PTV LN2 cooling jacket

G2619-60501

Silver seal

Graphpak inlet adapter

5/pk

3
2

5182-9763

0.20 mm

5182-9754

0.25-0.33 mm

5182-9761

0.53 mm
9

5182-9762

Ferrules for

0.20 mm

10/pk

5182-9756

5, 6

Graphpak inlet

0.25 mm

10/pk

5182-9768

0.32 mm

10/pk

5182-9769

7
8

0.53 mm

10/pk

5182-9770

10

Split nut for inlet adapters

5062-3525

11

PTV insulation block

G2617-20510

PTV cryo insulator (not shown)

G2617-60510

Teflon ferrule (needle seal)

5182-9748

Kalrez seal

5182-9759

Valve body

5182-9757

Pressure spring

5182-9758

Viton seal

5182-9775

Sealing element

5182-9760

CO2 Cryo inline filter

3150-0602

Service kit for septumless head


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

5182-9747

Installation tool for 3D ferrules

5/pk

9
10

11

HELPFUL HINT: 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.

5182-9749
G2617-80540

PTV Liners
Description

Part No.

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

5183-2038

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

5183-2036

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

5183-2037

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

5183-2041

www.agilent.com/chem

35

SAMPLE INTRODUCTION & INLETS

Septa
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. Septa 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,
and column degradation.
To minimize problems:
use septa with the recommended
temperature range
change septa regularly
install the retainer nut hand tight
use septum purge when available
use autoinjectors
use Agilent dual-taper, conical point
syringe needles

Ferrules
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.

Installation

Signals that a ferrule is damaged include:

Be sure to install ferrules correctly to avoid


problems:

dont overtighten finger-tighten column


nut, then use wrench to tighten 1/4 turn

maintain cleanliness

bake out ferrules prior to use

background noise from oxygen diffusing


into the system

avoid contamination (i.e., fingerprints,


oils)

column bleed catalyzed by oxygen

sample degradation

loss of sample

inspect used ferrules with magnifier for


cracks, chips, or other damage before
reusing them

increase in detector signal/noise

change ferrules when new columns or


injector/detector parts are installed

poor retention time reproducibility

Liners
Liners are the centerpiece of the inlet
system in which the sample is vaporized
and brought into the gas phase.
The liner should be changed on a regular
basis, and the correct liner must be used
to avoid peak shape degradation, solute
discrimination, poor reproducibility, sample
decomposition, and ghost peaks. Change
liners on a regular basis, as determined by:

previous use pattern

sample cleanliness

chromatographic abnormalities such as


peak shape changes, peak discrimination,
poor reproducibility, sample pyrolysis

36

For a complete selection of inlet


supplies, refer to Agilents
GC Inlet Resource Guide.
(publication # 5988-3466)

www.agilent.com/chem

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 nonvolatile and semi-volatile contamination,
as well as appropriate recovery measures.

With our expertise in GC columns and


applications we can quickly assist you
with choosing the right column for your
application, and save you time and money
by helping you protect your GC column
from permanent damage and common
sources of contamination.
Eberhardt Kuhn, Ph.D.
Technical Support Engineer

www.agilent.com/chem

37

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

Column Selection
Choose the Column that offers the best
longevity:

Use low-bleed columns whenever


possible.

Choose the least polar column that


provides the best resolution for the most
difficult separation.

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.)

Use most favorable dimensions to enable


required separation while optimizing
temperature ranges.

installation/system setup, and avoiding


the primary factors that cause column
performance degradation (breakage,
thermal damage, oxygen damage, chemical
damage and contamination).

Description

Part No.

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

122-0132

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

19091S-433

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

122-1232

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

122-3832

HP-INNOWax, 0.25mm i.d.,


30m, 0.25m

19091N-133

Column Installation & Setup


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

NEED MORE HELP?


Tap Agilents GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

38

Choose the appropriate size and


material ferrule for the column,
injector and detector type.

Avoid re-using ferrules.

Use an appropriate column cutting


tool such as a ceramic wafer or
diamond tipped scribe.

Make sure column ends are


cleanly cut and free of particulate
matter before installing into the
injector and detector.

Install the column the appropriate


distance into the injector and detector
as specified by the GC manufacturer.

The column should be placed on


a column hanger and no portion of
the capillary tubing should touch the
oven walls.

Verify that all fittings are leak-free and


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

www.agilent.com/chem

COLUMNS

Column Installation & Setup continued

Bad

Good

Example of column cuts

Check the installation and set the


linear velocity by injecting a non-retained
compound.

Condition the column as specified in the


literature provided with each column.

Description

Part No.

Ceramic wafer (4/pk)

5181-8836

20x Magnifier

430-1020

General Purpose Graphite ferrule


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

5080-8853

General Purpose Graphite ferrule


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

5080-8773

Gas leak detector 115V


Gas leak detector 220V (US only)

5182-9646
5182-9648

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.

NOTE: Larger diameter columns


(0.45- 0.53mm id) are more prone
to breakage.

www.agilent.com/chem

Avoid scratches and abrasions by not


exposing the column to sharp edges such
as column hangers and tags, metal edges
in the GC oven, column cutters and other
miscellaneous items on the lab bench.
Avoid winding or bending the column
too tightly.

Recovery

If a broken column has been heated,


damage to the stationary phase is very
likely. Discard the back of the column
(the column half without carrier gas).
Trim 6 inches off of the end of the
column and reinstall.

If the broken column has not been


heated, connect the two pieces with
a low volume union. No more than
2-3 unions should be installed for
one column.

Description

Part No.

Fused Silica Union,


Universal 2-way
(5/pk)
705-0905
Quartz deactivated
column connector
(5/pk)
5181-3396
Polyimide Sealing
resin (5 grams) 500-1200

This is a small sampling of the many GC columns and parts. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

39

COLUMNS

Thermal Damage

Oxygen Damage

Prevention

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).

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).

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

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.

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.

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.

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.

40

HELPFUL HINT: Install a moisture trap


upstream of the oxygen trap to increase
the oxygen trap lifetime.

Description

Part No.

FlowTracker 2000 Flowmeter and Leak Detector

5183-4780

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

BOT-2

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

BMT-2

Big Universal Trap (Combination Trap)


(750cc, 1/8 fitting, He)

RMSH-2

Advanced Green Septa (11mm, 50/pk)

5183-4759

www.agilent.com/chem

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 should be the same as the column. Guard columns


with larger ids can be used.

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

Recovery

Guard Column
INJECTOR

DETECTOR

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.

www.agilent.com/chem

Union

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


on Consumer Products.

This is a small sampling of the many GC columns and parts. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

41

COLUMNS

Nonvolatile Contaminants
Nonvolatile contaminants or residues do
not elute and accumulate in the column
(most often confined to the first few
meters). The column becomes coated with
these residues which interfere with the
proper partitioning of solutes in and out
of the stationary phase. Also, the residues
may interact with active solutes resulting
in peak adsorption problems (evident as
peak tailing or loss of peak size). Active
solutes are those containing a hydroxyl
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes.

Prevention

Perform sample cleanup to remove


nonvolatile materials from the sample

Use injection port liners packed with


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

Description

Part No.

SPE product guide

Pub#5988-2685EN

Split/Splitless Inlet liner: glass wool,


taper, deactivated (5/pk)

5183-4712

Splitless Inlet liner: single-taper,


no glass wool, deactivated (5/pk)

5183-4695

Quartz deactivated column


connector (5/pk)

5181-3396

Polyimide sealing resin (5 grams)

500-1200

Deactivated Fused silica,


10m, 0.53mm i.d.

160-2535-10

Deactivated Fused silica,


10m, 0.25mm i.d.

160-2255-10

Capillary column rinse kit

430-3000

Install a guard column and trim regularly

Recovery

Do not bakeout the column

Front End Maintenance:


Clean or change the injection port liner

are usually responsible for many baseline


problems (instability, wander, drift, ghost
peaks, etc.).

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)

Solvent rinse the column

Cut the column in half and use the back


half (detector side).

Prevention

Perform sample cleanup to remove


semi-volatile materials from the sample

Increase the final temperature of the


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

Change septa regularly

Recovery
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,

42

Bakeout the column: limit 1-2 hours


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

Solvent rinse the column

Column Storage
Capillary columns should be stored in their
original box when removed from the GC.
Place GC septa over the ends to prevent
debris from entering the tubing. Upon
reinstallation of the column, the column
ends need to be trimmed by 2-4 cm to
ensure that a small piece of septa is not
lodged in the column.
If a column is left in a heated GC, there
should always be carrier gas flow through
the column. The carrier gas flow can be
turned off only if the oven, injector, detector
and transfer lines are turned off (i.e., not
heated). Without carrier gas flow, damage
to the heated portion of the column occurs.

www.agilent.com/chem

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

www.agilent.com/chem

Only a small sampling of FID supplies are shown here. For a complete selection of FID supplies,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

43

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 keep 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 elevated levels in the
carrier or makeup gas or a leak near the
detector. Oxygen traps are recommended
for the carrier and makeup gases to reduce
oxygen levels. Proper column installation
techniques and regular leak checks
(especially after column installation) help
to keep leak problems to a minimum.
The damage caused by oxygen is more
severe at high filament currents.
Chemically active sample components
such as acids and halogenated compounds
may attack and damage the filaments.
Avoiding these compounds when possible
increases filament life. Turning off or
substantially reducing the filament current
when the TCD is not in use also prolongs
filament life.

Increasing Filament Lifetime


Increased filament lifetime will result if the
following startup process is used:
1. Purge the detector with carrier and
makeup gas for 10-15 minutes before
turning on the filaments. This prevents
oxidation of the filaments due to the
presence of oxygen that has diffused into
the cell under no flow conditions.
2. Turn on the filaments at the lowest
possible current setting, then increase
the filament current in several
increments to the desired value. This
reduces the power surge upon current

introduction and prolongs filament


lifetime.

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

Thermal Conductivity Detector (TCD) Supplies


Description

Unit

Part No.

6890/6850/5890 Common TCD Supplies


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

G1532-60675
10/pk

TCD cap column adapter

18740-20950
18740-20960

Graphite ferrules, 1.0 mm id

10/pk

5080-8773

Graphite ferrules, 0.5 mm id

10/pk

5080-8853

Capillary column nut, for 6890

2/pk

5181-8830

Capillary column nut, for 6850

2/pk

5183-4732

TCD packed column adapter (6890/6850 only)

G1532-20710

TCD chemical sample kit, 3 ampoules,


0.5 mL, 5 solution of 0.3% C14, C15, and C16, normal
alkanes in hexane
18711-60060
5890 TCD Supplies

44

Makeup gas adapter, TCD

19232-80550

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

19302-80020

TCD replacement cartridge

19232-60676

www.agilent.com/chem

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.

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 contaminantfree.
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.

Nitrogen-Phosphorus Detector (NPD)


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

www.agilent.com/chem

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.

Bead Life
To extend the life of the bead:

Use the lowest practical adjust offset or


bead voltage.

Run clean samples and keep the


inlet/liner clean to minimize
contamination.

Turn off the bead when not in use.

Keep the detector temperature high


(320 335C).

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.

45

DETECTORS

Gas Flow

Cleaning & Replacement

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.

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 FID Supplies on page
53). 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.

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.

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

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


(6890 only, dedicated)

Length (mm)

Part No.

48

G1531-80560

Capillary 0.53 mm jet (0.011 in. id tip)

61.5

19244-80560

Packed (0.018 in. id tip)

63.5

18710-20119

6890/5890 Adaptable

46

www.agilent.com/chem

DETECTORS

Nitrogen-Phosphorous Detector (NPD) Supplies


Item

Description

Part No.

6890 NPD Supplies


1

Screws, M3 x 0.5 x 8 mm (Pozidriv)

0515-0655

NPD white ceramic bead assembly*

G1534-60570

NPD black ceramic bead assembly**

5183-2007

Lid weldment

G1534-80510

Metal C-ring, top

0905-2580

Alumina insulator, upper

G1534-40020

Collector funnel

G1534-20530

Alumina insulator, lower

G1534-40030

Metal C-ring bottom and top

0905-1284

Screw, M4 x 10 mm

0515-2495

10

J-Clamp

1400-0015

11

Screw, M4 x 10 mm

0515-2495

12

NPD interconnect assembly

G1534-60610

13

Mounting pallet

G1531-40020

14

Jets (see page 54)

15

Base weldment, Capillary NPD

G1534-80500

Base Weldment, Packed NPD

G1534-80540

Lid stop

G1534-20590

NPD Ceramic Insulator Kit


includes items 4, 5, 7, and 8

5182-9722

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

19234-60720

5890 NPD Supplies


NPD collector (NPD bead)

19234-60540

Recoating kit, sufficient for 10 collectors

5080-8872

Detector Trap Replacement Kit

19231-60790

*This bead is more sensitive but exhibits some tailing for phosphorous compounds.
Quantity discounts available.
**The black bead is potentially a little less sensitive but does not exhibit peak tailing and
typically has longer lifetime.

www.agilent.com/chem

For a complete selection of NPD supplies,


see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

47

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.

Thermal Cleaning
If your baseline is noisy or the output
value is abnormally high and you have
determined that these problems are not
being caused by leaks in the GC system,
you may have contamination in the
detector from column bleed. 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.

Radioactivity Leak Test


Electron capture detectors must be tested
for radioactive leakage at least every six
months. Records of tests and results must
be maintained for possible inspection by
the Nuclear Regulatory Commission and/or
the responsible local agency. More frequent
tests may be conducted when necessary.
The procedure used is a wipe test. A
wipe test kit is supplied with each new
detector. Refer to the information card
supplied in the Wipe Test Kit for
instructions on performing the test.

Gas Purity
For successful EC detection, its important
that the carrier and purge gases are very
clean and dry (99.9995%). Moisture, oxygen,
or other contaminants can be responsible
for improved 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.

48

www.agilent.com/chem

DETECTORS

Electron-Capture Detector (ECD) Supplies


Item Description

Unit

Part No.

6890 ECD Supplies


ECD makeup gas adapter*

G1533-80565

Nut warmer cup with insulation

19234-60720

5890 ECD Supplies


1

Vespel graphite ferrule, 1/4 in. id

10/pk

5080-8774

Vespel/graphite 85%/15%
ferrule, 1/4 in. id

10/pk

0100-1331

Tubing nut, 1/4 in. brass

10/pk

5180-4105

ECD column adapter, 1/4 to 1/8 in. metal

19301-80530

Makeup gas adapter for micro ECD adapter

G2397-80520

Makeup gas adapter, ECD, new style

19233-80565

ECD Packed for 1/4 in. Glass Columns

7
6

6890/5890 Common ECD Supplies


6

5, 4

ECD fused silica liner (new style)

19233-20625

ECD adapter fused silica liner micro ECD

G2397-20540

Stainless steel cap for ECD makeup gas adapter


(new style and micro ECD)

19233-20755

ECD Make up Gas Adapter

ECD Performance evaluation sample lindane and


aldrin (0.033 ppm) in Isooctane 3 ampoules, 0.5 mL 18713-60040
ECD wipe test kit

18713-60050

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

NEED MORE HELP?


Tap Agilents GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.

www.agilent.com/chem

49

DETECTORS

Flame Photometric Detector (FPD)


Maintenance

high temperatures are used

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.

defective signal boards are present

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 FID
Supplies on page 53). 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 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

50

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 53).
Occasionally, the transfer line fused silica
liner between the column and FPD module
must be inspected, cleaned and/or replaced.

Increase the air supply pressure to the


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

If the flame 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


Flame Ignition Problems
If the FPD flame wont light or stay lit:

Be sure there is a problem. Ignition is best


confirmed by holding a mirror or shiny
surface near the aluminum exhaust tube,
with the rubber drip tube removed, and
observe condensation if the flame is lit.
Check Lit Offset. If it is zero, autoignition
is turned off. If it is too large, the GC will
not know that the flame is lit and will
shut down the detector.

The flame conditions are critical to


successful operation. Since the detection
zone is above the flame, the gas flows and
jet diameter must be optimized so that
components burned (activated) in the flame
will emit in the detection zone.
Gas flows are also critical for optimized
selectivity and sensitivity. The most critical
parameters are the hydrogen/air or
hydrogen/oxygen ratio, and the total gas
flow, which effects flame temperature.

www.agilent.com/chem

DETECTORS

6890/5890 FPD Supplies


Item Description

Exit tube assembly

Nut, brass, 1/4 in.

Unit

Part No.

19256-60700
10/pk

5180-4105

2
3

Weldment, block

19256-80560

O-ring, ignitor, Kalrez

0905-1102

Spacer, ignitor

19256-20590

Glow plug

0854-0141

Ignitor cable assembly (6890 only)

G1535-60600

Gasket, heat shield

19256-80040

10

Window, first heat shield

19256-80030

11

Disk, heat shield

19256-20580

12

Coupling, SS

19256-20550

14

Screw, M3 x 12 (4 required)

0515-0911

15

Clamp

19256-00090

16

O-ring, inner window

17

Window, second heat shield

18

O-ring, outer window

19

Flange adapter

19256-20510

20

Flange ring

19256-00200

21

O-ring, Viton, 1.239 in. id

10

11

12
8

13

14

15

16
17
18

12/pk

12/pk

12/pk

5061-5891

5061-5890

Adapter weldment, capillary

19256-80570

Start-up kit (5890 only)

19256-60500
12/pk

5061-5867

Liner/ferrule kit

19256-60590

Sulfur filter

19256-80000

Phosphorus filter

19256-80010

Kalrez O-ring, size 2-002

0905-1101

Kalrez O-ring, size 2-011

0905-1103
12/pk

FPD Performance Evaluation Sample: Solution of


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

www.agilent.com/chem

21

19256-80060

19256-80590

Fluorocarbon Elastomer O-ring,


brown, 0.926 in. id

20

5061-5886

Adapter weldment, 1/8 in. columns

FPD O-ring (5890 only)

19

HELPFUL HINT: 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.

5061-5889

19305-60580

51

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

FID Ferrules

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, 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 can cause the flame to go out.
Switch to a nonaromatic solvent.

The lit offset value may be too low or too


high. Adjust the value.

Cleaning & Replacement


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

FID Cleaning Kit

Plugged FID jet

52

www.agilent.com/chem

DETECTORS

Flame Ionization Detector (FID) Supplies


Jet Cleaning Procedure

Description

Unit

Part No.

(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

6890/6850 Supplies
Collector insulator

G1531-20700

Collector body

G1531-20690

FID collector assembly*

G1531-60690

Detector insulation assembly

G1531-20700

FID ignitor cable

G1531-60680

Collector Housing

G1531-20740

5890 Supplies
Collector assembly*

19231-60690

Upper collector insulator

19231-20970

Collector body

19231-20960

Hastelloy collector

19231-21080

Lower collector insulator

19231-20950

only with forceps!

6890/6850/5890 Common Supplies

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.

PTFE chimney (optional)

19231-21050

Collector nut

19231-20940

6. Blow the jet dry with a burst of the


compressed air or nitrogen, and then
place the jet on a paper towel and allow
it to air dry.

Ignitor castle

19231-20910

Hastelloy Ignitor Castle

19231-21060

Ignitor glow plug assembly

19231-60680

Spring washer

FID collector cleaning brush

10/pk

2/pk

5181-3311

8710-1346

FID retainer nut wrench


(5880, 5890, 6890)

19301-00150

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

8710-1561

FID flow measuring insert

19301-60660

O-rings for flow measuring insert

12/pk

FID Performance evaluation sample kit,


0.03% C14, C15, and C16 normal
alkanes in hexane

5080-4978

18710-60170

Jet cleaning wire for 0.03 in. id jet

5/pk

5180-4150

Jet cleaning wire for Series 530 mm


and 0.018 in. id jet

5/pk

5180-4152

FID cleaning kit

9301-0985

*Assembly Contains: Gasket, Ignitor Castle, Ignitor Glow Plug Assembly, Spring Washer-Wavy
Collector, Housing, Mount, Nut, Body, Spanner Nut, Insulator (upper and lower)

www.agilent.com/chem

Only a small sampling of FID supplies are shown here. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.

53

DETECTORS

FID Jets
Description

Length (mm)

Part No.

48

G1531-80560

High-temperature jet (SimDIS 0.018 in. id tip) 48

G1531-80620

Jets for capillary dedicated FID (6890 only)


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

Adaptable FID (6890/6850/5890)


Capillary 0.53 mm jet (0.011 in. id tip)

61.5

19244-80560

Packed (0.018 in. id tip)

63.5

18710-20119

Packed (0.030 in. id tip)

63.5

18789-80070

0.53 mm high temp (0.018 in. id tip) for SimDIS 61.5

19244-80620

Agilent FID Jets (from top to bottom): Dedicated


capillary, Adaptable capillary, Adaptable packed

HELPFUL HINT: Different size jets are available to optimize flame shape for capillary
columns, or reduce contamination build-up for high molecular weight eluates. 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.

To view a video on FID column installation, jet replacement,


collector maintenance, or ignitor replacement,
visit www.agilent.com/chem/supplies,
click on How-to Video under the Reference Library.

54

www.agilent.com/chem

Service & Support


Every Agilent GC system is backed by a
wealth of knowledge, all at your fingertips.
Tap our 35 years of instrument expertise
and applications knowledge by phone, in
person, in print, or on-line. Contact us for
a variety of service and repair options from
telephone support, on-site repair, even
product exchange. Take advantage
of our industry leading training courses
to help increase the overall knowledge in
your lab.
Any way you want, you get the full support
of Agilent expertise and service with every
GC system.

Of course we have all the right


consumables and supplies you need
to keep your Agilent GC system
running at peak performance. But it
doesnt stop there. We want to
extend our knowledge. Our expertise.
And our technical support.
Hwee-Sian Tan
Application Manager

www.agilent.com/chem

55

SERVICE & SUPPORT

Expert Training, Service & Support


Expert Training from the GC Experts

GC System Operation Training

Well trained lab professionals keep


productivity high, minimize the number
of errors and reruns, and expand
chromatography capabilities. With expert
training that gives you on-site expertise
for troubleshooting and maintenance,
your lab will run at peak performance.

Course #H5308A introduces the


fundamental concepts of gas
chromatography and the operation of
the Agilent 6890 GC using the Agilent
ChemStation for GC and capillary columns.
This five-day hands-on course is designed
for the new GC operator who is responsible
for routine sample analysis. It covers
everything from inlets, columns, and
detectors to data analysis and reporting.
For more information on all Agilent Training
offerings, visit www.agilent.com/chem and
select Education.

GC Training
Agilents training courses for gas
chromatography helps 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 and maintenance,
and system operation skills. Contact
Agilent today for more information about
our training and other Support Services.
Or visit www.agilent.com/chem and
select Education.

Technical Support Consultation


Have a technical GC column, method, or
troubleshooting question? Agilents Technical
GC Column 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 Troubleshooting/
Maintenance Training
Agilent offers a four-day hands-on course
providing practical information for
troubleshooting and maintenance for the
complete Agilent Gas Chromatography
System. Its designed for the professional
with a fundamental GC knowledge and
who is responsible for troubleshooting
and maintenance. Learn how preventive
maintenance can ensure the long-term
reliability and proper operation of your
Agilent GC system. For more information
on all Agilent Training offerings, visit
www.agilent.com/chem and select
Education.

Course #H5308A (for Series 6890)

Course #H4001A (for Series 5890)

On-line: www.agilent.com/chem, choose Technical Support, then select


Ask our Technical Support Specialist.

56

www.agilent.com/chem

SERVICE & SUPPORT

Your Choice for Instrument


Maintenance & Repair
Contact the Agilent experts for GC
maintenance and repair. We can bring our
technical experts to your facility, or you can
ship your instrument to us. Well even send
an exchange instrument* to keep you up
and running.

Service Contracts Offer Big Rewards


Sign up for Agilents Chemical Analysis
Service Contract** today and youll enjoy
industry-leading product support and
service. Youll also get regular special
offers, including:

exclusive introductory offers on new


products and services

* for select instruments only

Preventive Maintenance &


Repair At Your Site

incentives for PerfectFit supplies to keep


your lab running at peak performance

notification and advice on replacement


strategies for older instrumentation

discounts on selected Agilent training


courses

With an Agilent Support Service Contract,


an Agilent service professional will come
to your site for repair. You even get a
choice of response times to keep repairs
cost-efficient. Well even come to your
site to conduct a thorough preventive
maintenance, to keep your instruments
running at peak performance.
Contact Agilent today, or visit
www.agilent.com/chem, for more
information about these and other
Support Services.

Expert Instrument Repair


You can keep your repair costs low and
maintain productivity with a choice of
off-site repair options. Just ship your
instrument to an Agilent Analytical
Customer Service Center. Well diagnose
the problem, repair the unit and return it
to you (usually within five days). Or if
maximum uptime is critical, ask about our
Instrument Exchange program. Agilent will
ship you a replacement instrument to keep
until your unit is repaired and returned.

www.agilent.com/chem

Sign up today and get access to exclusive


areas of the Agilent web site providing
valuable instrument and application
information, instructional videos for
instrument maintenance, and easy on-line
ordering. Well also e-mail regular
reminders about product development, and
upcoming exclusive rewards. Sign up today
at www.agilent.com/chem/rewards.
** Contract covers travel, parts, labor for Agilent
service professional plus expert telephone assistance
to isolate and resolve hardware problems.

Bundled Service to Save You Money


Agilent offers industry-specific Service
Bundles for the Petrochemical and
Pharmaceutical industries. Service Bundles
contain essential services to keep your
chemical analysis instruments in top
condition for dependable operation. Youll
get telephone support, on-site and off-site
instrument repair including exchange
instruments, as well as on-site preventive
maintenance services, all for less than the
cost of purchasing each service separately.
Contact Agilent today for more information
about these and other Support Services.

Create Your Own Service Bundle


Contact Agilent today to configure a
package of support services to meet your
labs needs hardware maintenance,
troubleshooting, repair, support, and
preventive maintenance. Just let us know
what you need and well configure a
package for you. Contact Agilent today
for more information about our Support
Services and Contracts.

Operational Re-Qualification
After Repair
For instruments that require qualification,
Agilents Re-qualification After Repair
service verifies that a system is still
performing to Agilents operational
specifications after a repair, including
documentation that meets audit
requirements. Contact Agilent today for
more information about this and other
service contracts.

57

SERVICE & SUPPORT

Tap Agilent Expertise


Tap Agilents extensive GC knowledge
any time. Just give us a call to discuss
hardware, software, applications concerns
or just basic GC operation techniques. And
be sure to subscribe to our informationpacked magazine.

Software Support
Only Agilent can provide expert assistance
to isolate and resolve software problems.
Well provide telephone assistance from
highly trained experts. Well provide all
enhancements to the original chemical
analysis software purchased. Well even
send you Software Bulletins to let you
know about ongoing issues and
recommended workarounds. Contact
Agilent today for more information about
these and other Support Services.

GC System
Recommended
Maintenance
Schedule

Technical Support Assistance (a logical,


step-by-step approach to help you solve
common problems)

Technical Document Library (a searchable


collection of service and support
documents)

Chromatogram Library (a searchable


collection of GC, LC, and CE
chromatograms nearly a thousand
chemical compounds)

Product Support Literature (including


Operating Manuals and Installation
Guides)

Illustrated Parts Breakdowns (instrument


diagrams to help you identify parts or part
numbers)

Software Status Bulletins (updates on


recommended software workarounds)

Hardware Support
Agilents highly trained technical staff is
just a phone call away to offer you basic
hardware troubleshooting, operation
assistance, instrument and system
configuration, and remote diagnostics. Call
us toll-free today, or submit your question
on-line at www.agilent.com/chem.

Stay on Top with Separation Times


Tap into Agilents chromatography
expertise all year long with a free
subscription to Separation Times magazine.
For knowledge, tips, and insight, go to
www.agilent.com/chem/supplies, click
on Whats New, then select Tap into
Agilents Expertise to sign up today and
stay ahead of the information curve.

Visit Agilent on-line


For a wealth of GC knowledge any time,
visit www.agilent.com/chem. Youll find:

Ask our Technical Support Specialists


(send an on-line question to a technical
Support Chemist)

Frequently Asked Questions (answers


to the most commonly asked technical
questions about Agilent instruments
and supplies)

58


Open inside cover for:

Plus, a host of information and features to


make ordering easier and faster.

www.agilent.com/chem

GC System Recommended Maintenance


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 and 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/troubleshooting!

Schedule
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.

*Schedule is an approximation of average usage requirements.


Frequency may vary widely based upon application and sample type.

www.agilent.com/chem

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