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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
Agilent’s 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. We’ve
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 world’s best GC system. We give
you knowledge!

Maintaining Your Agilent GC System


Maximize your efficiency. Minimize your downtime.
3 Gas Management 37 Columns
4 Gas Types 38 Column Maintenance
5 Purities 38 Column Selection
POST ER ENCL
O UT OS 5 Purifiers 38 Installation/Setup
L-
ED

13 Regulators 39 Column
L
PU

14 Tubing Performance

oting
15 Leak Detection 43 Detectors

GC sho 16 Flow Rates 44 Thermal


ble
Trou Guide
Conductivity
19 Sample
Detector (TCD)
Introduction
& Inlets 45 Nitrogen-
Phosphorous
Sample Introduction
Detector (NPD)
20 Vials & Syringes
48 Electron-Capture
Inlet Types Detector (ECD)
26 Packed Column 50 Flame Photometric
28 Split/Splitless Detector (FPD)
31 Cool on-Column 52 Flame Ionization
34 PTV Detector (FID)
Inlet Accessories
55 Service & Support
36 Septa, Liners,
56 Expert Training,
Ferrules
Service & Support

This icon denotes a video that is available to view on our Don’t Miss…
web site. Just visit www.agilent.com/chem/supplies to GC Troubleshooting Guide (pullout poster)
view videos and obtain more information. GC Maintenance Schedule (inside back cover)

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

www.agilent.com/chem 3
GAS MANAGEMENT

Gas Types

Carrier Gases
The most frequently used carrier gases are and elevated column bleed, along with not it will make contact with the sample.
helium and hydrogen, although nitrogen column and/or detector damage. The Coolant gases (carbon dioxide) and
and argon can be used. Purity is essential following sections describe the gases pneumatic gases (air or nitrogen) generally
for these gases since they sweep the and purities that are necessary for gas do not come in contact with the sample or
sample through the column where it is chromatography carrier gases, as well detector. Therefore, these non-contact
separated into its component parts and as other support gases. gases do not have to be the highest purity
then through the detector for component available.
quantification. Carrier gas purity is also Support Gases For most applications, gases which are low
critical to prevent degradation of
Support gases may be specific for detectors in oils and particulates are desirable; thus,
chromatographic hardware.
or for applications. These gases include low-purity “specialty gas” grade products
Contaminants in carrier gases can have fuels, oxidants, coolants, detector gases, can be used. Fuels, oxidants and detector
a significant effect on column life and and pneumatic gases. The degree of purity gases, in most cases, do come in contact
subsequent analyte detection. Harmful required for support gases is dependent on with the sample and detector, and require
effects include contaminant peaks how that gas is being used, and whether or higher purity gases.

Carrier and Support Gases

Sample
Gas Type Function Contact Purity Required*

Air Pneumatics No Low Grade

Nitrogen Pneumatics No Low Grade

Limit of Detection required:

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

Hydrogen Carrier or fuel gas


for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero

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

Methane/Argon Carrier or make-up


or Nitrogen for ECD Yes Research Research Research N/A

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

Nitrogen, Helium, Carrier or


or Argon make-up gas Yes Research Ultra-Pure Ultra-Pure UHP/Zero

*Purities of gases 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%)

4 www.agilent.com/chem
GAS MANAGEMENT

Contaminants & Purities

Contaminants in gases are major ● can also cause baseline drift or wander, In some cases it may be difficult to
contributors to capillary column contaminant peaks, and noisy or high determine which contaminant presents
degradation and detector noise, and offsets of baselines the biggest problem in a given analysis. If
can interfere with chromatographic unsure, a call to your gas supplier may be
results. Concentration of these Moisture helpful. Once the problem contaminants
contaminants vary by the grade of gas. ● can be introduced by improper handling have been identified and a general
and/or installation of plumbing contaminant level is determined, the next
Analytical gases are available in many
step is to choose a gas purity level that
grades of quality, from high purity ● a common cause of column stationary comes closest to these requirements.
(99.995%) to chromatography grade purity phase degradation
(99.9995+%). The higher the purity, the Keep in mind that higher grades of gas
higher the cost.
● can damage instrument generally cost more. The greatest cost
savings can be achieved by using the
Oxygen
Identifying Contaminants lowest purity gas which will neither
● most common contaminant interfere with the analysis nor damage
To make a proper purity choice it is your equipment. Using the proper gas
● a common cause of column stationary
helpful to understand the contaminants purification equipment to remove common
phase and inlet liner degradation
most common in GC gases and how contaminants and achieve the desired
they can affect your analysis. Common ● can cause decomposition of labile purity level is essential.
contaminants are: analytes

Hydrocarbons and Halocarbons ● opportunity for introduction at every


fitting present in the gas line or during
● decrease detector sensitivity by
use of wrong tubing (i.e., gas permeable)
increasing detector background noise

Gas Purification Systems

Agilent brings the highest performance The illustration on the next page shows Other Considerations
and largest variety of gas purifiers (traps) the most common gas purification ● determine desired purity level
to gas chromatographers. Purifiers are configurations used in gas chromatography.
available in a variety of sizes and ● keep number of “breaks” in gas line
Regardless of which purification system to a minimum
configurations, to remove common
is employed, proper installation and
contaminants like oxygen, moisture, ● install purifiers in a convenient location
maintenance is required to achieve
and hydrocarbons. In-line gas purifiers, close to the GC
optimal performance from the purification
including refillable, indicating, S-shaped,
system(s). A purifier that is not maintained ● purifier log books are useful for
and metal body types, are made to remove
will eventually saturate and become determining maintenance schedule
specific contaminants. Agilent also offers
ineffective, or worse, a source of
gas purification systems with removable ● use indicating traps closest to the GC so
contamination.
cartridges. These systems provide the you can determine when to change the
ability to design the right combination traps that are upstream
of filters needed for your application to
achieve the proper gas purity.

www.agilent.com/chem 5
GAS MANAGEMENT

Carrier Gas Purification


Key:
1 = Moisture Trap
In-Line Gas Purifiers 2 = Hydrocarbon Trap
3 = Oxygen Trap
4 = Indicating Oxygen Trap
5 = Gas Purification System
6 = Combination Trap for
moisture, oxygen, and
hydrocarbon removal
-OR-

Gas Purification System Detector Gas Purification


Gas supply

FID make-up, air,


and H2

-OR-
Combination Trap ECD make-up
Gas supply Vent

ELCD reaction gas

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

Regulator = Brass dual stage regulator

Gas Traps
The purpose of gas traps is to remove Constant exposure of capillary columns to
detrimental impurities from the carrier oxygen and moisture, especially at high
and detector gases. Moisture (water), temperatures, results in rapid and severe
oxygen and hydrocarbon traps are the column damage. The use of oxygen and
most common traps used with GC moisture traps for the carrier gas may
systems. A few combination traps are extend column life and protect the
available which remove moisture, oxygen instrument. Traps may provide some
and/or organics with a single trap. The protection if there is a leak at or around
effectiveness of the traps depends on the the gas cylinder. Any moisture or oxygen
initial quality of the gas. Little enhancement introduced into the gas stream due to the
by traps to the GC system is obtained by leak will be removed by the trap until it
traps when using very high purity gases expires. This creates an opportunity to
(e.g., ultra-high purity or similar grades) detect and fix the leak before column or
while obvious improvement is obtained instrument damage occurs.
NEED MORE HELP? with lower grades of gas.
Tap Agilent’s 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.

6 www.agilent.com/chem
GAS MANAGEMENT

Moisture (Water) Traps


There are several different adsorbents Indicating moisture traps are available in
and indicating materials used in moisture plastic and glass bodies. Glass body traps
traps. Moisture traps can be easily are used when potential contaminants
refilled. Adsorbent refills are typically from plastic trap bodies are a concern.
1/4 to 1/2 the cost of a new trap making Glass traps are normally encased in a
refilling a more economical (and less protective, plastic shrink wrap or a high
wasteful) option. impact plastic shield (outer trap body).
Glass and plastic bodied traps are usually
pressure tested at 150 psi, thus they are
safe for use at the typical pressures
required by the GC.

Refillable Glass Moisture Trap

Moisture Removal Traps

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

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

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

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

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

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

Molecular Sieve Refill for GMT Series 250 GMSR GMSR

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

Moisture S-Trap – preconditioned 5060-9084

Big Moisture Traps – for the Ultimate Moisture Capacity

Big Moisture Trap 750 BMT-2 BMT-4

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

Refillable Moisture Trap Moisture S-Trap Big Moisture Trap

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 7
GAS MANAGEMENT

Oxygen Traps
Oxygen traps usually contain a metal- plastics are permeable to air and contain
containing inert support reagent. Most contaminants that can degrade gas quality.
Indicating Oxygen Trap oxygen traps reduce the oxygen In addition, many of the metal bodied
concentration to below 15-20 ppb. The oxygen traps can withstand high pressures
capacity of a standard oxygen trap is (up to 2000 psi). Some oxygen traps also
approximately 30mg of oxygen per 100cc remove moisture from the gas stream
of trap volume. Oxygen traps can remove without affecting the oxygen removal
some small organics and sulfur compounds capability.
from gas streams.
Big Oxygen Trap Indicating oxygen traps change color when
Metal (usually aluminum) trap bodies are oxygen is present in the gas at harmful
recommended for GC analyses. Some levels. Indicating traps are not intended to
Oxygen Traps be the primary oxygen removal trap, but
should be used in conjunction with a high
1/8 in. 1/4 in.
capacity non-indicating oxygen trap. They
Description Size (cc) Part No. Part No.
are installed after the high capacity oxygen
Indicating Oxygen Traps – glass body with plastic safety shield
trap in the gas line to indicate when the
high capacity trap is expired and needs to
Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP be changed. Expired oxygen traps need to
be immediately changed since they can
Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller size contaminate the gas, in addition to failing
available, see Agilent catalog) to remove oxygen.
Big Oxygen Trap 750 BOT-2 BOT-4

Hydrocarbon Traps Hydrocarbon Traps


Hydrocarbon traps remove organics, such
1/8 in. 1/4 in.
as hydrocarbons and halocarbons, from
Description Size (cc) Part No. Part No.
the gas stream. The adsorbent is usually
Hydrocarbon Traps – General Purpose activated carbon or an impregnated carbon
filter media. Carbon removes organic
Refillable Hydrocarbon Trap 200 HT200-2 HT200-4 solvents from the gas stream, including the
typical solvents used in nearly every lab.
Adsorbent Refill (1 pint, 2 refills) ACR ACR Hydrocarbon-moisture combination traps
are also available which remove water in
Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity

Big Hydrocarbon Trap 750 BHT-2 BHT-4

Refill for Big Hydrocarbon Trap (2 refills) BACR BACR

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

Hydrocarbon S-Trap 5060-9096

Capillary Grade Hydrocarbon Traps – for crucial capillary applications Hydrocarbon Trap

Capillary Grade Hydrocarbon Trap 100 HT3-2 HT3-4

Adsorbent Refill (1 pint, 3 refills) ACR ACR

8 www.agilent.com/chem
GAS MANAGEMENT

Hydrocarbon Traps continued


addition to organics as described in the next
section. Capillary grade hydrocarbon traps Big Hydrocarbon Trap
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.

Hydrocarbon S-Trap

Combination Traps
Agilent carries several Combination Traps ● Leak-free, one-piece design to eliminate
that provide multiple contaminant removal potential leaks from using multiple traps
in a single trap. These traps offer: ● Efficient design which prevents
● Optimized adsorbents for maximum channeling and promotes efficient
surface area and capacity scrubbing
● The ultimate in purification with a single
trap (Big Universal Trap)

1/8 in. 1/4 in.


Description Size (cc) Part No. Part No.

Oxygen/Moisture Traps

Agilent OT3 Trap 100 OT3-2 OT3-4 Agilent OT3 Trap


Hydrocarbon/Moisture Traps

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

Refill for Hydrocarbon/


Moisture Trap (1 pint, 2 refills) HCRMS HCRMS

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

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


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

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 9
GAS MANAGEMENT

High Capacity Single-Cartridge System


Gas Purification System ● Contains a triple-combination cartridge
that offers the same highly efficient
Three Cartridge System contaminant removal properties from
● Agilent’s highest capacity and most eight cylinders of carrier gas but without
economical gas purification system. the visual indicator.
● Provides low-cost gas contaminant ● Other cartridges are also available for
removal for up to 18 cylinders of detector gas supplies and as individual
carrier gas. filters for specialized requirements.
Three Cartridge ● Includes a manifold with cartridge
High Capacity
Gas Purification mounts and three replaceable cartridges:
System 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 System—Includes manifold


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

With 1/8 in. fittings 5183-1907

With 1/4 in. fittings 5182-9776

Replacement Cartridge Kit—


Includes all three cartridges for 5182-9780
above system.

Single Cartridge System—Includes single


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

With 1/8 in. fittings 5183-4598

With 1/4 in. fittings 5183-4599

Triple combination replacement cartridge


for single cartridge system 5183-4600

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

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

Description Fitting (in.) Part No.

4-Head

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

Replacement Cartridges
NEED MORE HELP?
Description Part No. Tap Agilent’s GC knowledge
over the phone, on-line, in the
High capacity oxygen GC-1
classroom, even at your site.
High capacity moisture GC-2 See pages 56-58 for more
information about our expert
Indicating moisture GC-2-I training, service and support.
Hydrocarbon GC-3

Indicating oxygen GC-4

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem 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 Available with 1/8” fittings only
designed to provide the utmost in
convenience and contamination Description Part No.
reduction. The system is tested for
leak-tightness and the glass and metal Carrier Gas Purification System: Single
construction of the cartridges eliminates position system perfect for GC/MS,
diffusion of contaminants into the gas ECD and NPD detectors. Includes the
stream. During cartridge replacement, triple filter cartridge. 5182-9704
check valves close off the system to the
atmosphere, further minimizing the entry Super-Clean Gas Purification System:
of contaminants. For your most demanding GC application,
includes four position baseplate manifold
with four filter cartridges: oxygen,
moisture (both with indicator), and
two hydrocarbon cartridges. 5182-0816

Replacement Filter Cartridges

Triple Filter Cartridge: A single carrier gas


filter now with 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

Universal/External Split Vent Trap


Description Part No.
Split vent traps stop environmental
pollution. The split vent trap was designed
Universal/external split vent trap
to protect the lab environment from the
with 3 cartridges
contaminants released by split injection
(1/8 in. Swagelok fitting) RDT-1020
systems, which can vent up to 500 times
Replacement cartridges (3/pk) RDT-1023 the amount of sample reaching the
detector into the laboratory's air. A
replaceable, impregnated carbon filter
media traps and eliminates a broad range
of contaminants. The traps are also easy
to change and come with three packs of
replacement cartridges each. Replace
approximately every six months.
Split Vent Trap and Cartridges

Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
12 Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. www.agilent.com/chem
GAS MANAGEMENT

Regulators
Pressure regulators are an integral empties and the inlet pressure to the
component in any gas handling system. regulator decreases (inlet decay), the
Their function is to reduce the pressure pressure on the diaphragm is reduced.
from a high pressure source, such as a Without proper adjustment, the outlet
cylinder, to a suitable use pressure. pressure might slowly rise. Brass Body Regulator
Although regulators are very good at
A dual stage regulator overcomes this
controlling pressure, they do not control
problem by connecting two regulators
flow. They have a maximum flow rate
together. The first stage regulates the to purity considerations, then a stainless
which is dictated by the design. Basically,
pressure to the second stage thus creating steel regulator should be chosen for the
the flow is determined by the pressure
a constant pressure and allowing minimal same reasons. Unfortunately, use of high
drop across the regulator.
inlet decay. Agilent recommends using purity stainless steel regulators is often
two-stage regulators with our GC Systems cost-prohibitive.
Types of Regulators to provide the proper pressure control for
optimal use. No matter which material is chosen for the
There are primarily two types of
regulator body, be sure to specify one with
regulators: single stage and dual (or two)
stainless steel diaphragms for critical
stage. The difference is that a dual stage Regulator Materials applications such as use on carrier, fuel or
regulator is actually two regulators
Regulators are usually constructed of brass detector gases. Agilent recommends using
connected in a series.
or stainless steel. The choice of material our economical brass body, dual stainless
Dual stage regulators provide more precise follows the same guidelines as the choice steel diaphragm regulators for most GC
and consistent pressure control than single of tubing. Generally, it is not recommended applications. These regulators, combined
stage regulators. The reason is that in a that the materials be interchanged. If with the proper gas purification system,
single stage regulator, as the gas cylinder stainless steel tubing were chosen due provide proper gas pressure control and
purity for gas chromatography.
When ordering a regulator, be sure to
specify the proper connections. In the
Description Part No.
US, most gas manufacturers follow CGA
connection guidelines. In Europe, there
Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*
are a number of organizations designating
CGA 346, 125 psig max (8.6 bar), Air 5183-4641 cylinder connections that are specific to
individual countries. It is best to contact
CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642 your local supplier for the proper
connection designation.
CGA 540, 125 psig max (8.6 bar), O2 5183-4643

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

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

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

Regulator Outlet Adapters — Female NPT to Swagelok-style

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


(included with brass regulators) 0100-0118

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

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


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 used for non-critical applications, such as
delivery system for GC, choosing the proper pressurizing pneumatic lines; however, be
tubing material is very important and will aware of its pressure limitations.
help to eliminate potential problems and
In view of these problems, the list of
improve the overall quality of the gas
appropriate tubing materials has been
system. Although there are many common
narrowed down to two: copper and
tubing materials available, some pose
stainless steel. Agilent recommends using
safety or cleanliness problems.
copper tubing for most applications, since
Non-metallic types of tubing such as it is easy to bend and plumb and is less
polyethylene and Teflon are not expensive than stainless steel. Use
Spectra-Link Tubing Connecting System
recommended for GC applications due stainless steel tubing only for crucial
on a two-stage regulator to their gas permeability and difficulty applications that require very high purity.
in cleaning. This type of tubing can be
Cleaning Tubing
Determining Tubing Length Before any tubing is placed into service,
or if it becomes contaminated with use,
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig
it is essential that it be properly cleaned.
Tubing Type Diameter Recommended Pressure Drop
Unclean or improperly cleaned tubing can
(inches) Max. Length (feet) (psig)
lead to contamination of the system with
disastrous results.
Copper 1/8* 50 2
Cleaning tubing requires the use of suitable
Copper 1/4* 300 0.5 detergents and solvents along with
nitrogen and a purgeable oven for drying.
*Recommended when multiple instruments are connected to the same source 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
Tubing—Precleaned quality GC grade tubing for large systems
as an economical alternative.
Description 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 5183-1941


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

Leak Detection
Leaks allow oxygen and other and easy detection and measurement of
contaminants to enter the gas stream. gas leaks for 12 common gases. Based on a
Therefore, GC instrument maintenance dual cell micro volume thermal conductivity
should include checking fittings and system, this unit provides very high
connections with a gas leak detector. sensitivity and eliminates contamination
Agilent’s Gas Leak Detector enables quick 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 Selecting a Flowmeter
greatly affect the instrument accuracy Agilent manufactures the largest selection
and sensitivity. During maintenance, of volumetric and mass flowmeters for
verify carrier and support gas flows chromatography. We have developed
with the proper flowmeter. Choosing a flowmeters for measuring capillary column
flowmeter for your application depends flows, calibrating air pumps and flow
upon measurement speed, ease of use, controllers, and verifying instrument gas
accuracy, and flow rate range. flows. All flowmeters are calibrated to
NIST-traceable standards.

FlowTracker Flowmeters – volumetric, multimode flowmeters

Description Part No.

FlowTracker 1000 Flowmeter 5183-4779

FlowTracker 2000 Flowmeter and


FlowTracker 2000 Leak Detector 5183-4780

FlowTracker Universal AC Adapter (optional,


not supplied with FlowTracker units) 5183-4781

ADM 1000 features include: ADM 2000


● Accuracy ± 3% In addition to the features of the ADM
1000, the ADM 2000 includes:
● Operating temperature range—
0 to 45ºC for the instrument, -70 to ● Mass flow measurements—measure
135ºC for the tubing flow rate, independent of atmospheric
pressure and temperature (calculated)
● Calibration—traceable to NIST primary
ADM 1000
standards ● Data output through RS-232 port
● Real time, split ratio measurement ● 9V battery and AC power adapter
(120 or 220 VAC)
● CE mark certified
● Measures flow rates from 0.5 to
1000 mL/min
● Split ratios—compare the ratio from
one gas measurement to another
(i.e., injection port split ratios)
ADM 2000

16 www.agilent.com/chem
GAS MANAGEMENT

Flowmeters

Flow Rate (mL/min) Gases Accuracy Power RS-232 Data


Description Low High Measured (%) Supply Output Part No.

ADM Flowmeters – volumetric, measures all gases*


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

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

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

Electronic Mass Flowmeter – dedicated mass flowmeter, very accurate for specific gases*
Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery
(110 V) 5.0 500 N2, Air ±3 or 110 VAC Yes HVF-500

Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery


(220 V) 5.0 500 N2, Air ±3 or 220 VAC Yes HVF-500-2

Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters**


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

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

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

*non-corrosive gases only


**non-corrosive and mildly corrosive gases only

Veri-Flow 500
Optiflow 420

NEED MORE HELP?


Tap Agilent’s 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 flowmeters are shown here. For a complete selection of flowmeters, see the
www.agilent.com/chem Flowmeter Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 17
There’s 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. Agilent’s commitment to
offering the highest quality supplies
means accurate, reliable results.
Time after time.”
Bryan Bente, Ph.D.
Technology Development Manager

Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes, see the
www.agilent.com/chem 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 When filling sample vials, keep in mind:
for analyzing samples with your GC. They
● if you need to test a large amount of
have specially designed vial neck angles,
sample over repeated injections, divide
bottom design and height to ensure
the sample among several vials to obtain
compatibility with Agilent autosamplers
reliable results
with rotating or robotic arm trays. Agilent
offers a large variety of autosampler vials ● when sample volume in the vial is low,
in different closures, cap colors, septa contaminants from the previous sample
choices and package options. Agilent also injection or solvent washes may have a
offers convenience packs with 500 vials greater impact on the sample.
and caps in a reusable blue storage box.
The airspace in the vial is necessary to
For small sample sizes, Agilent offers a avoid forming a vacuum when sample is
variety of options. You can use microvolume withdrawn. This could affect
inserts with the wide opening vials or, for reproducibility.
added convenience, use vials with small
volume capacity.

Vial Options

Glass—for general purpose Silanized—for use with Polypropylene—for use Amber Vials—for use with Microvolume Inserts— High Recovery Vials—
use and for use with acids samples that bind to glass, with alcohols and aqueous light-sensitive samples for use with very small for use with limited sample
and for trace analyses solvents sample volumes 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 µL

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

20 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. Determining Your Quantity Needs
Red Rubber/Teflon To determine potential septa ordering
quantities, consider:
● Routine analysis
● Moderate resealing ● the number of samples run during a
● Excellent chemical inertness
day/week
● Not recommended for multiple ● if samples are run in small or large
injections or storage of samples batches
● Least expensive
HELPFUL HINT: Unattended autosampler
● if samples are run manually or with an runs require a precise fit for uninterrupted
autosampler
Silicone/Teflon operation. Typically, automated sample runs
● Excellent resealing ● if samples are run overnight, unattended use a higher quality and quantity of vials.
● Resists coring

● Good for multiple injections

Vials
Teflon/Silicone/Teflon
● Used in trace analysis applications Description Quantity Part No.
● Above average resealing
● Most resistant to coring Vials
● Least evaporation
2 mL Crimp top vial convenience
● Use with large diameter, blunt tip
pack with silver AI caps with
syringe needles Teflon/Red rubber septa 500/pk 5181-3400
Teflon Disc 2 mL Screw top vial convenience
● Good for MS and ECD analysis pack with blue screw caps and
● Chemically inert Teflon/Red rubber septa 500/pk 5182-0732
● No resealing
2 mL Snap top vial convenience pack
● Single injection
with clear polypropylene snap caps
● No long-term sampling storage and Teflon/Red rubber septa 500/pk 5182-0547

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


● Chlorinated solvents
300 µL Polypropylene vials 1000/pk 9301-0978
● Organic acids

● Limited resealing 100 µL Glass lined polypropylene vials 100/pk 9301-0977


● Not suitable for 32 gauge syringe
15 µL reservoir volume, Micro-V vial,
clear crimp top 100/pk 5184-3551

30 µL reservoir volume, High recovery


vial, crimp top 100/pk 5182-3454

www.agilent.com/chem 21
SAMPLE INTRODUCTION & INLETS

Syringes Selecting Syringes


Syringe type and design are important for 1. Select the syringe type based on the
chromatography to ensure reproducible inlet (injection port) you are using and
sample injections for consistent results. the volume of sample you want to inject.
The Agilent line of syringes are a perfect fit
2. Select a syringe. Refer to your automatic
with your autosamplers and come with a
liquid sampler operating documentation
variety of plunger and needle choices.
for available syringe sizes and
PerfectFit means they are designed: corresponding injection volumes.
● for reproducible sample volume delivery 3. Select the appropriate syringe
● specifically for the Agilent inlet or needle gauge.
autosampler
● to maximize inlet septum lifetime

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 µm

Cool on-column 26/32 gauge tapered 320 µm

Cool on-column 26/32 gauge tapered 250 µm

Needle Tip Needle Shape

Needle tips
Sharp tip Cone tip

Tapered needle

Use syringe needles with an Agilent dual-


taper needle or a conical tip. Sharp-tipped
NEED MORE HELP? needles tend to tear the inlet septum and
Tap Agilent’s GC knowledge cause leaks. Also, a sharp-tipped needle
over the phone, on-line, in the tends to leave residual amounts of sample
classroom, even at your site. on the septum as it exits, resulting in a
See pages 56-58 for more large solvent tail on the chromatogram.
information about our expert
training, service and support.

22 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS

Syringe Characteristics and Recommended Uses

Syringe Advantage Limitations Recommended Use

5 µL, fitted • Most accurate • Thinnest plunger, • 1 µL injections


plunger syringe for 1µL can bend • Clean samples
injection more easily • Routine analysis
• No hardware • Not ideal for higher
modification needed viscosity samples
for 0.5 µL injection • Plunger not
replaceable

10 µL, fitted • Most economical • Most accurate only • General purpose


plunger • Most reliable fitted for 2 µL and larger syringe
plunger syringe injections • Clean samples
• Less bending • Plunger not • Routine analysis
• Better for high replaceable
viscosity samples

10 µL, • Replaceable plunger • More expensive • Dirty samples


gas-tight for reduced than fitted plunger • Gases and volatile
repair cost • Not available in samples
• Less plunger binding 5 µL size • Reactive samples HELPFUL HINT: Failure to use an
than fitted plunger on-column syringe when injecting into
• Tight seal between an on-column inlet could damage the
plunger and barrel injector, syringe and column.

Replacing On-column Syringe Needles To insert a needle into a syringe barrel:


The stainless steel needles used for 1. Unscrew the syringe barrel cap and
250-µm and 320-µm injections must remove the spring.
be inserted into a glass syringe barrel.
2. Make sure the needle has the Teflon
Select the correct size needle for the
disk. If the syringe barrel does not
column you plan to use.
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 ● Remove a gas-tight plunger from the ● To maximize the lifetime of standard
size when setting up the injection section syringe for long-term storage to keep the plungers, rinse the syringe and wipe the
of your data handling device. Teflon tip leak-free. If a gas-tight plunger plunger with solvent (isopropanol or
does not fit properly, place it in hot water acetone) and a lint-free wipe, as specified
● Rinse syringes and clean their plungers
for about 10 minutes then press the tip in the syringe cleaning procedure
before use to maximize syringe lifetime.
uniformly on a clean, hard surface and let included with each syringe.
● Rinse the syringe 5-8 times between cool to room temperature. The plunger
injections to minimize sample carryover. should reseal correctly to provide 10-25%
more injections.
● Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
● A 26 gauge syringe can be used for on-
column injections into a 0.53mm id
column. Always check that on-column
syringe needles fit inside the capillary
column before installing the column and
syringe in the GC.
● For on-column injections, always use the
proper septum nut and stainless steel
insert for the column dimension you are
using. Use a septum with a molded
through-hole with injections onto 0.32mm
and 0.25mm columns.

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

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

Straight Needle Syringes


(use with Merlin Microseal)

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

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

Automatic Liquid Sampler Supplies

Description Unit Part No.

Miscellaneous Autosampler Supplies

4 mL wash vial with screw caps 144/pk 9301-0723

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

Septa for 4 mL vial 144/pk 9301-1031

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

Screw for mounting syringe 07673-20570

Quadrant kit (4 tray sections) 18596-40015

7673 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

Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 25
SAMPLE INTRODUCTION & INLETS

Packed-Column Inlets
Packed-column direct inlets are very Packed-Column Inlet Procedures/Practices
popular. Packed-column analysis is
frequently done when high efficiency Parameter Selection/Setting Rationale
separations are not needed or when gases
are analyzed by gas-solid chromatography. Inlet temperature BP of solvent +50˚C Ensures flash vaporization
Packed column inlets are simple in both BP of major solute(s) Use for neat samples
design and use. Few parameters need to be Insert type 1/8-inch stainless steel Use for ss column only
set, and all carrier gas flow flushes through 1/4-inch stainless steel Inserts permit connection of
the inlet into the column in the standard columns up to 1/4-inch od.
configuration.
Liner Glass Use to lower activity
(replaceable)
Initial column temperature programming Sharpens peaks and
temperature reduces run time
Column type 1/8-inch packed stainless Will not break
1/4-inch packed glass Better for polar or labile
compounds
Carrier gas flow 20-40 mL/min Use with N2 carrier gas
30-60 mL/min Use with He or
H2 carrier gas

Troubleshooting
Most problems with packed-column inlets The inherent activity of packed-column Leaks
involve sample decomposition, flashback, inlets is somewhat mediated by the fact Since packed-column inlets are usually
or leaks. that they usually have low internal volume. flow-controlled, septum and column leaks
When this is coupled with the relatively will have a direct impact on retention times
Decomposition fast flow rates used with packed columns, and peak areas. Sample can be lost through
Since packed-column inlets are active, the residence time of sample in the inlet is the leak holes, and air can diffuse back into
especially if glass liners are not used, polar short and decomposition is reduced in the inlet to cause column degradation.
sample components will often tail or comparison to the decomposition that Change the septum on a regular basis and
degrade in the inlet. Sample decomposition occurs with some capillary inlets (for check column connections at the first stage
caused by the inlet is easily diagnosed; the example, splitless inlets). of problems. To prevent stationary phase
decomposition products will have peaks at decomposition, make sure that the oven
the same retention times as standards for Flashback and inlet are at room temperature when not
the decomposition product. The negative side of low inlet volume, in use and when changing the septum.
however, means that excessively large
When inlet-caused decomposition is
sample injections will easily exceed the
suspected, try intracolumn direct injection,
capacity of the liner and will flash back into
deactivated glass liners, or lower inlet
gas supply lines and onto the septum. This
temperatures, and remove any column
can cause several maladies, including
packing in the inlet zone.
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.

26 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS

6890/6850/5890 Series GC Packed Port Supplies*

Item Description Unit Part No.

1
1 Septum nut 18740-60835 2
3
2 Septa Bleed temperature, 4
optimized, 11 mm** 50/pk 5183-4757

3 Top insert weldment 19243-80570

4 Viton O-rings 12/pk 5080-8898

5 Glass liner, disposable 25/pk 5080-8732

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

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

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


Liner
Adapters with glass liners

8 0.53 mm column adapter 19244-80540

1/8 in. column adapter 19243-80530


5
1/4 in. column adapter 19243-80540
6
9 Upper insulation‡ 19243-00067 7

10 Nut warmer cup with insulation 19234-60720 8 1/4 in. Vespel/


graphite ferrule

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


1/4 in. nut
Oven
1/8 in. or 1/4 in.
** For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals. 9 stainless steel liner
*‡ For Model 6890/6850 only
10
** For a complete selection of inlet supplies, refer to Agilent’s GC Inlet Resource Guide.

11

5890 Packed Column Inlet Supplies

Description Unit Part No.

Nonpurging septum nut assembly


for manual flow control only, not EPC 19243-60570

Adapters without glass liners

1/8 in. column adapter 19243-80510 NEED MORE HELP?


Tap Agilent’s GC knowledge
1/4 in. column adapter 19243-80520
over the phone, on-line, in the
Universal Packed Column Inlet (non-purged) classroom, even at your site.
See pages 56-58 for more
Septum retainer nut for
information about our expert
headspace sampling, nonpurging 19243-60505
training, service and support.
Brass nut, 1/4 in. 10/pk 5180-4105

www.agilent.com/chem 27
SAMPLE INTRODUCTION & INLETS

Split/Splitless Inlets
The combined “split/splitless” inlet is the Troubleshooting results to the lower temperature analysis.
most popular inlet for capillary column gas Repeat if results are positive until no
Split inlets are spared from most band-
chromatography. Because it can be used in further improvement is seen.
broadening phenomena, since narrow
either split or splitless mode, it provides a
peaks are generated as part of the A majority of the problems encountered
very effective combination that can cover
splitting process. Therefore, any peak with split inlets are related to
most analysis requirements.
broadening or tailing observed with split discrimination and decomposition. Both
injection is usually due to improper analytical accuracy and reproducibility
Split Mode column installation, low split flow, or decrease with the increases in
Split injection is an effective way to low inlet temperature. If you suspect that discrimination and decomposition.
introduce small amounts of sample without the inlet temperature may be too low, Split inlets suffer from both needle
overloading the column. Split injection is increase it by 50˚C and compare the discrimination and inlet discrimination.
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 Split Mode Procedures/Practices
directly before the solvent peak (as in
solvent analysis) Parameter Selection/Setting Rationale

Split injection is also good for screening Inlet temperature BP last eluting compound Ensures flash vaporization
samples of which little is known or for Minimizes inlet discrimination
those that have widely differing Inlet liner Large volume, deactivated Minimizes flashback
concentrations, since the split ratio Minimizes degradation
can be adjusted easily. Split inlets are
also a good choice for dirty samples. Inlet packing Silanized glass wool Retains non-volatiles
Stops flow of droplets
Glass beads or frit Less active than wool
None Least active
Injection volume 0.5-3 µL liquid Split easily adjusted
0.10-10 mL gas Split adjusted accordingly
Injection technique Fast autoinjection Less needle discrimination
Hot-needle fast manual Reproducible discrimination
injection
Split ratio 50:1 to 500:1 Depends on sample and
injection volume
Initial column Not critical Narrow initial peaks
temperatures
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


For splitless injection, a conventional split
Parameter Selection/Setting Rationale
injector is operated in a nonsplitting mode
Inlet temperature Just above highest Ensures flash vaporization by closing the split valve during injection.
boiling point of Reduce if degradation occurs The sample is flash-vaporized in the liner,
solutes (+20˚C) Use higher for dirty samples and sample vapors are carried into the
and higher-boiling solutes column by the carrier gas where they are
recondensed at temperatures below the
Inlet liner Large volume >0.8mL Use with autoinjector boiling point of the solvent. After most of
Small volume <0.2mL Use only for slow manual the sample has been transferred into the
injections column, vapors remaining in the liner are
cleared by opening the split vent which
Inlet packing None Use only with slow injection
remains open for the duration of the run.
Decreases degradation
The most important benefit of splitless
Silanized glass wool Use for fast autoinjection injection is that a majority of the injected
& dirty samples sample is introduced into the column. This
Injection volume 0.5-2 µL liquid Depends on solvent, liner, results in much higher sensitivity than that
& conditions achieved using split injection.

Injection technique Fast autoinjection Most reproducible Solvent Effect


Less needle discrimination
Hot-needle slow manual Inject 1-2µL.sec if narrow liner One requirement of splitless injections is
is used and >1µL injection that the initial column temperature should
Hot-needle fast manual Use for <1µL injections be kept at least 10˚C below the boiling
point of the sample solvent. This allows the
Purge flow 20-50 mL/min Not critical sample solvent to condense at the front of
the column trapping the solvent molecules
Purge delay time 20-80 sec Adjust according to column
into a tight, narrow band.
flow rate/liner type
& sample conditions

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

Column flow >2mL/min when possible Clears inlet fast


Reduces backflash and
decomposition

Septum purge 2-3mL/min Reduces ghosting

Quantification Internal standard Maximizes reproducibility


Standard addition Use only with constant
injection volume

Retention gap 1-3m, deactivated Reduces peak distortion


(1-2m per µL injected) Promotes solvent and NEED MORE HELP?
stationary phase focusing
Tap Agilent’s 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 29
SAMPLE INTRODUCTION & INLETS

Splitless injection is routinely used in on the solvent tail may be focused by the volume), leading to irreproducibility and
areas such as: solvent to yield more sensitive analyses. nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
● environmental analysis
Troubleshooting volume carefully to avoid backflash.
● pesticide monitoring of foods
Most problems encountered with splitless Decomposition
● drug screening injection are related to incorrect purge Loss of peak area or generation of new
In these applications, sample preparation time, degradation, improper focusing, and peaks, can sometimes be dramatically
requirements are significant, and it is not flashback. reduced by changing liner type or by
always possible or economically justifiable Appropriate initial column temperature is deactivating the liner and inlet with
to clean up a sample extensively. So critical. Sample vapors can be lost through silanizing reagents. Removing or reducing
column protection becomes as important the septum purge line if the insert is the amount of liner packing can also
as sensitivity. Also, samples with trace overfilled with sample vapor (either too decrease inlet activity.
quantities of important solutes that elute large injection volume or too small liner

HELPFUL HINT: A guard column or


retention gap is often beneficial for
splitless injections (see page 41). 6890/6850/5890 Split/Splitless Inlet Supplies*

Item Description Unit Part No.

1
1 Septum retainer nut 18740-60835
2
2 Septa**
3
4
3 Insert Weldment**
6
5
4 Liner O-ring**

5 Liner**

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

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


Retaining nut (5890 only) 19251-20620

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

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

10 Reducing nut 18740-20800


7
11 Insulation (requires 3) 19243-00067
8
9
12 Lower insulation cover 19243-00070
10
13 Ferrule**

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

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


11
Angled wrench for split/splitless inlet 19251-00100
12
**For a complete parts breakdown, see the 6890/6850/5890 Series GC Instrument User and/or Service Manuals.
13 **For a complete selection of inlet supplies, refer to Agilent’s GC Inlet Resource Guide.
14

30 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS

Cool On-Column Inlets


Cool on-column injection is superior in If done properly, cool on-column injection apparent that cool on-column injection
many ways to other sample introduction provides the most accurate and precise should be considered whenever high
techniques. results of the available inlets. Syringe precision and accurate results are required.
discrimination is completely eliminated.
Advantages: Moreover, inlet-related discrimination does Limitations:
● elimination of sample discrimination not occur, since the liquid is introduced ● maximum sample volumes are smaller
directly into the column. Automated on- compared with other inlets (0.5 µL
● elimination of sample alteration
column injection provides even higher to 2.0 µL)
● solvent focusing of early eluting solutes analytical precision. Add to this the
● solute peaks eluting just before the
elimination of thermal decomposition and
● high analytical precision solvent cannot be focused and are
rearrangement reactions, and it becomes
difficult to determine
● capillary columns (especially those with a
Cool On-Column Inlet Procedures/Practices large phase ratio or small inner diameter)
can be easily overloaded with sample
Parameter Selection/Setting Rationale ● parameters such as initial column
Initial inlet = or 3˚C above column Ensures sample focusing temperature, solvent nature, and injection
temperature oven temperature in solvent front rate must often be optimized

Initial inlet Same as oven (oven track) Simple and effective Sample Considerations
temperature ramp Faster than oven Narrows initial peak width
Sample preparation is important for
Injection volume 0.1-2.0 µL liquid Use smaller injections for on-column injection because of:
small id columns;
Depends on column capacity ● the potential for column overload,
column contamination,
Injection technique Fast autoinjection Projects droplets away from
syringe tip
● the incompatibility of some solvents
Fused silica needle Use for manual injection into with the stationary phase,
small id columns ● dependence of the initial column
temperature on the boiling point of
Oven temperature Inlet temperature or Prevents backflash
the solvent.
slightly lower
Many of the problems associated
Column flow 50-80cm/sec Use for H2 carrier gas
with these variables can be resolved
30-50cm/sec Use for He carrier gas
by using a retention gap ahead of the
Septum purge 12-15mL/min Use if installed to prevent analytical column.
ghosting
Quantification All methods Inherently reproducible
technique
Lack of discrimination
Retention gap 1-3m, deactivated Corrects peak distortion
requirements Protects column from non-
volatile components
Permits autoinjection with
narrow-bore columns

HELPFUL HINT: Since the sample is directly deposited into the column, nonvolatile sample
To view a video on cool on-column installation and
components can accumulate at the head of the column and will degrade efficiency and/or septum replacement, visit www.agilent.com/chem/supplies,
interact with subsequent injections. click on “How-to Video” under the Reference Library.

www.agilent.com/chem 31
SAMPLE INTRODUCTION & INLETS

Troubleshooting
The major problems found with cool on- prevent displacement of the stationary
column injection are associated with phase by solvents.
column overload, solvent/stationary phase
Immobilized stationary phases can be
incompatibility, and column contamination.
washed to remove contaminants and
If the flooded zone after injection is too renew performance. If column performance
long (large injections, poor wettability), does not improve after washing, cut 0.5m
peaks will be broad or split. A retention gap off the inlet side of the column. If that does
usually will resolve this problem. Loss of not return column performance, the column
column efficiency with on-column injection must be replaced and a retention gap
usually is caused by contamination or should be used for all further injections of
degradation of the stationary phase at the dirty samples.
head of the column. Only columns with an
immobilized stationary phase should be
used with cool on-column injection to

Column/Retention Gap Installation Consumables

Item Description Unit Part No.

Column nut 2/pk 5181-8830

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

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

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

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

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

Quartz deactivated column connector


fits 0.18-0.53 mm 5/pk 5181-3396

NEED MORE HELP?


Tap Agilent’s GC knowledge
HELPFUL HINT: Sample degradation can
over the phone, on-line, in the
occur with cool on-column injection if
classroom, even at your site.
column or retention gap activity is high.
See pages 56-58 for more
Use only well-deactivated retention gaps
information about our expert
and high quality capillary columns from
training, service and support.
Agilent.

32 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS

6890/5890 Series Cool On-Column Inlet Supplies

Item Description Unit Part No.


1a
1b 1c
Manual injection
1d
1c Cooling tower assembly 19320-80625
1d Duckbill septum 10/pk 19245-40050
Fused silica syringe needles 6/pk 19091-63000 2
3
4
Syringe barrel for use with
fused-silica needles,10 µL 9301-0658
Common Supplies
3 Spring 19245-60760
4 Inserts for capillary columns
For 200 µm columns (one ring) 19245-20510
For 250 µm columns (six rings) 19245-20515
For 320 µm columns (five rings) 19245-20525
For 530 µm columns (no rings) 19245-20580
5
For 530 µm Al clad columns (four rings) 19245-20780
6
5 Ferrule 5080-8853
6 Column nut 2/pk 5181-8830

6890 Series GC Cool On-Column Inlet Supplies


Automatic Injection
1a Septum nut base for 320 mm assembly 19245-80521
1b Septum nut base for 530 mm assembly G1545-80520
2 Advanced green 5 mm through hole septa 50/pk 5183-4760
BTO 5 mm through hole septa 50/pk 5183-4758

5890 Series Cool On-Column Inlet Supplies


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

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

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

Only a small sampling of inlet supplies are shown here. For a complete selection of inlet supplies,
www.agilent.com/chem 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, PTV Inlet Procedures/Practices (cold split/splitless modes)
splitless and on-column inlets. The sample is
usually injected into a cool liner, so syringe Parameter Selection/Setting Rationale
needle discrimination does not occur. Then
the inlet temperature is increased to vaporize Injection mode Cold split For general use
the sample. The user programs vent times and sample screening
and temperature to achieve the equivalent of Cold splitless For trace analysis
split or splitless transfer of sample vapors to Inlet temperature Adjustable (i.e., 2˚C/sec Use slower ramp rates for
the column. PTV injection is considered the ramp rate to 12˚C/sec) labile, complex, or large
most universal sample introduction system volume samples
because of its flexibility. Use faster ramp rates for
most samples
Advantages Use faster ramps rates to
● no syringe-needle discrimination shorten splitless purge delay time
● minimal inlet discrimination Ballistic Simpler, less expensive
● no special syringe needed
instrumentation
● use of large injection volumes Inlet liner Straight with silanized wool For general use
● removal of solvent and low boiling Baffled For labile samples
components Packed with an adsorbent For focusing gaseous
● trapping of nonvolatile components in liner
injections from auxiliary
sampling devices
● split or splitless operation

● retention time and area reproducibility Injection volume 0.1-1.5µL Use lower volumes for
approaching cool on-column injection volatile solvents and fast
ramp rates
PTV inlets are actively cooled before and Use volumes larger than
during injection by Peltier devices or by 1.5µL only in solvent-
forced gases (air, liquid N2, or liquid CO2). elimination mode
Cryogenic cooling of the inlet can reduce
inlet temperature enough to thermally Sample Injection Autosampler or manual, Not critical for cold split
focus gas injections from other sampling technique fast or slow & splitless modes
devices in the liner. This is a distinct Oven temperature 10-25˚C below solvent BP For proper solvent effect in
advantage of using PTV inlets in splitless mode
comparison to conventional inlets for Sample dependent For split mode
coupling auxiliary sampling devices to
capillary columns. Column flow 30-50 cm/sec Clears inlet faster
Less backflash
Post-injection, PTV inlets are heated
using electrical heaters or preheated Septum purge 1-5mL/min Minimizes ghosting
compressed air. Depending on design,
inlet temperature ramps are either Quantification Any method Inherently reproducible
ballistic (i.e., ramped to the maximum Low discrimination in cold
injection modes
temperature at an uncontrolled maximum
rate) or programmable. Retention gap 1-3m, deactivated Compensates for extended
flooded zone and solvent-
column 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. 1


3
1 Septumless head G2617-60507
2
2 Septum head G2618-80500
3 Septum nut 18740-60835
4 PTV inlet assy G2617-60506
5 PTV LCO2 cooling jacket G2617-60508
6 PTV LN2 cooling jacket G2619-60501 4

7 Silver seal 5/pk 5182-9763


8 Graphpak inlet adapter 0.20 mm 5182-9754
0.25-0.33 mm 5182-9761
0.53 mm 5182-9762
9 Ferrules for 0.20 mm 10/pk 5182-9756 5, 6

Graphpak inlet 0.25 mm 10/pk 5182-9768 7


8
0.32 mm 10/pk 5182-9769 9
10
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 11

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 HELPFUL HINT: There are few
CO2 Cryo inline filter 3150-0602 choices in liner design for PTV inlets.
Service kit for septumless head 5182-9747 However, liner volume and activity are still
contains Kalrez seal, valve body, key issues to be considered when selecting
and pressure spring among the few available PTV liners. PTV
Graphpak 3D ferrules 5/pk 5182-9749 liners require packing or a modified
Installation tool for 3D ferrules G2617-80540 surface to hold the liquid sample in place
before and during the vaporizing process.

PTV Liners

Description Part No.

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


PTV Liner Single Baffle, 2 mm id 200 µL volume, deactivated 5183-2036
PTV Liner Multi Baffle, 1.5 mm id 150 µL volume, deactivated 5183-2037
PTV Liner Fritted Glass, 1.5 mm id 150 µL volume, deactivated 5183-2041

www.agilent.com/chem 35
SAMPLE INTRODUCTION & INLETS

Septa Ferrules
The septum isolates the sample flow path Ferrules seal the connection of the column Installation
from the outside world. It must provide a or liner to the system. The ideal ferrule Be sure to install ferrules correctly to avoid
barrier that is readily penetrated by the provides a leak-free seal, accommodates problems:
injector needle while maintaining internal various column outer diameters, seals with
pressure without contaminating the minimum torque, will not stick to the ● don’t overtighten – finger-tighten column
analysis. Septa are generally made of column or fittings, and will tolerate nut, then use wrench to tighten 1/4 turn
special high temperature, low-bleed temperature cycling. ● maintain cleanliness
silicone rubber formulations. Septa should
Signals that a ferrule is damaged include: ● bake out ferrules prior to use
be replaced regularly to avoid leaks,
decomposition, sample loss, reduced ● background noise from oxygen diffusing ● avoid contamination (i.e., fingerprints,
column or split vent flow, ghost peaks, into the system oils)
and column degradation. ● column bleed catalyzed by oxygen ● inspect used ferrules with magnifier for
To minimize problems: ● sample degradation cracks, chips, or other damage before
● use septa with the recommended reusing them
● loss of sample
temperature range ● change ferrules when new columns or
● change septa regularly
● increase in detector signal/noise injector/detector parts are installed
● install the retainer nut “hand tight” ● poor retention time reproducibility
● use septum purge when available

● use autoinjectors

● use Agilent dual-taper, conical point

syringe needles

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 For a complete selection of inlet
discrimination, poor reproducibility, sample supplies, refer to Agilent’s
decomposition, and ghost peaks. Change
liners on a regular basis, as determined by: GC Inlet Resource Guide.
● previous use pattern (publication # 5988-3466)
● sample cleanliness
● chromatographic abnormalities such as
peak shape changes, peak discrimination,
poor reproducibility, sample pyrolysis

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

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

Column Selection Description Part No.

Choose the Column that offers the best DB-1ms, 0.25mm i.d., 30m, 0.25µm 122-0132
longevity:
● Use low-bleed columns whenever HP-5ms, 0.25mm i.d., 30m, 0.25µm 19091S-433
possible.
DB-XLB, 0.25mm i.d., 30m, 0.25µm 122-1232
● Choose the least polar column that
provides the best resolution for the most DB-35ms, 0.25mm i.d., 30m, 0.25µm 122-3832
difficult separation.
HP-INNOWax, 0.25mm i.d.,
● Use more polar phases when difficult 30m, 0.25µm 19091N-133
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.

Column Installation & Setup


The first step in obtaining optimal ● Make sure column ends are
column performance and lifetime is cleanly cut and free of particulate
proper installation: matter before installing into the
injector and detector.
● Choose the appropriate size and
material ferrule for the column, ● Install the column the appropriate
NEED MORE HELP? injector and detector type. distance into the injector and detector
as specified by the GC manufacturer.
Tap Agilent’s GC knowledge ● Avoid re-using ferrules.
over the phone, on-line, in the ● The column should be placed on
● Use an appropriate column cutting
classroom, even at your site. a column hanger and no portion of
tool such as a ceramic wafer or
See pages 56-58 for more the capillary tubing should touch the
diamond tipped scribe.
information about our expert oven walls.
training, service and support. ● Verify that all fittings are leak-free and
the carrier gas is oxygen-free before
heating the oven.

38 www.agilent.com/chem
COLUMNS

Column Installation & Setup continued


Description Part No.

Ceramic wafer (4/pk) 5181-8836


Bad 20x Magnifier 430-1020

General Purpose Graphite ferrule


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

General Purpose Graphite ferrule


Good (1.0mm ID, for 0.45-0.53mm
ID columns) 10/pk 5080-8773
Example of column cuts
Gas leak detector 115V 5182-9646
Gas leak detector 220V (US only) 5182-9648
● 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.

Causes of Performance Degradation


Column Breakage Prevention
Description Part No.
Fused silica columns can break wherever ● Avoid scratches and abrasions by not
there are small scratches or abrasions in exposing the column to sharp edges such Fused Silica Union,
the protective polyimide coating. as column hangers and tags, metal edges Universal 2-way
Continuous heating and cooling of the in the GC oven, column cutters and other (5/pk) 705-0905
oven, vibrations caused by the oven miscellaneous items on the lab bench.
fan as well as being wound on a circular Quartz deactivated
● Avoid winding or bending the column column connector
cage all place stress on the tubing. too tightly. (5/pk) 5181-3396
While under these stresses, flaws
will propagate until breakage occurs. Recovery Polyimide Sealing
● If a broken column has been heated, resin (5 grams) 500-1200
NOTE: Larger diameter columns
damage to the stationary phase is very
(0.45- 0.53mm id) are more prone
likely. Discard the back of the column
to breakage.
(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.

This is a small sampling of the many GC columns and parts. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 39
COLUMNS

Thermal Damage Oxygen Damage Prevention


Exceeding a column’s upper temperature Oxygen is an enemy to all capillary GC ● Maintain an oxygen and leak free
limit results in accelerated degradation of columns. Constant exposure to oxygen system by:
the stationary phase and tubing surface. does not damage the column at or near – performing periodic leak checks
This results in the premature onset of ambient temperatures; however, severe
excessive column bleed, peak tailing for damage occurs as the column temperature – changing septa regularly
active compounds and/or loss of efficiency increases. A leak in the carrier gas flow – using high quality carrier gases
(resolution). path (e.g., gas lines, fittings, injector, septa)
is the most common source of oxygen – installing and maintaining oxygen traps
Prevention exposure. As the column is heated, very – changing gas cylinders before they are
● Do not exceed the columns specified rapid degradation of the stationary phase completely empty
upper temperature limits: occurs. This results in the premature onset
of excessive column bleed, peak tailing for Recovery
– Isothermal limit: temperature that
active compounds and/or loss of efficiency Perform column “bakeout” as described
the column can be held at for an
(resolution). under thermal damage recovery.
indefinite time
– Programmed limit: maximum column NOTE: Momentary exposure to oxygen
NOTE: Oxygen damage occurs very rapidly.
temperature; column should only be such as an injection of air or removing In less severe cases, the column may still
held there for about 5-10 minutes the septum nut for a short period of be functional but at a reduced performance
time is not a problem. level. In more severe cases, the column is
● Set the GC maximum oven temperature
irreversibly damaged.
function at or a few degrees above the
temperature limit of the column. With two
columns in the oven be sure to set the
maximum temperature to the temperature
limit of the column with the lowest value.

Recovery
● Disconnect column from detector
● Heat the column 8-16 hours at the
isothermal limit HELPFUL HINT: Install a moisture trap
upstream of the oxygen trap to increase
● Remove 10-15 cm from the column end
the oxygen trap lifetime.
● Reinstall into the detector and condition
as usual
Description Part No.
NOTE: Thermal damage cannot be reversed.
The column usually does not return to its
original performance; however, it is often FlowTracker 2000 Flowmeter and Leak Detector 5183-4780
still functional. The life of the column will
be reduced after thermal damage. 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

40 www.agilent.com/chem
COLUMNS

Chemical Damage GUARD COLUMN


Inorganic or mineral acids and bases are A guard column is a piece of fused silica tubing attached with a union to
the primary sources of chemical damage the front of the analytical column with the following characteristics:
to stationary phases. Most of these acids
● Material should be deactivated fused silica tubing to minimize solute
and bases have low volatility and
interactions.
accumulate at the front of the column. If
allowed to remain, the acids or bases ● Length should be from 1-10 meters. Typical lengths of 5-10 meters allow
damage the stationary phase. The only substantial trimming before the entire guard column has to replaced.
organic compounds that have been
● Internal diameter should be the same as the column. Guard columns
reported to chemically damage stationary
with larger ids can be used.
phases are perfluoroacids and these need
to be present at high levels (e.g., 1% or ● A low volume union should be used to attach the tubing to the column.
higher). This results in the premature onset Glass pressfit unions are inexpensive and easy to install. DuraGuard
of excessive column bleed, peak tailing for columns offer the guard column built into the analytical column as a
active compounds and/or loss of efficiency single piece of fused silica, eliminating the need for unions.
(resolution).
Guard columns are used to minimize the effect of non-volatile residues
NOTE: Hydrochloric acid and ammonium on the analysis. The non-volatile residues deposit in the guard column and
hydroxide are the least harmful of the group not in the analytical column. This greatly reduces the interaction between
as both tend to follow any water that is the residues and the sample. Periodic cutting or trimming of the guard
present in the sample. Thus, if HCl or NH4OH column is usually required upon a build-up of residues. The onset of peak
are present in a sample, minimizing water shape problems is the usual indicator that the guard column needs
retention will render these compounds trimming or changing.
relatively harmless to the column.

Prevention
● Perform sample preparation to remove
inorganic acids and bases from the
sample
● Install guard column and trim frequently

● If acids or bases must be used choose an

organic alternative or HCl or NH4OH Guard Column


INJECTOR DETECTOR
Recovery
● Remove 0.5 to 1 meter from the front
of the column
● Severe cases may require the removal

of 5 or more meters
Column
Guard Column

Column Contamination
Column contamination is the most common
Union
problem encountered in capillary GC.
Unfortunately, it mimics most other
chromatographic problems and is often Guard column installation instructions are available at www.agilent.com/chem. Click
misdiagnosed. A contaminated column is on “Consumer Products.”
usually not damaged, but it may be
rendered unusable. There are two basic
types of contaminants: nonvolatile and
semivolatile.

This is a small sampling of the many GC columns and parts. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 41
COLUMNS

Nonvolatile Contaminants
Description Part No.
Nonvolatile contaminants or residues do
not elute and accumulate in the column
(most often confined to the first few SPE product guide Pub#5988-2685EN
meters). The column becomes coated with
Split/Splitless Inlet liner: glass wool,
these residues which interfere with the
taper, deactivated (5/pk) 5183-4712
proper partitioning of solutes in and out
of the stationary phase. Also, the residues Splitless Inlet liner: single-taper,
may interact with active solutes resulting no glass wool, deactivated (5/pk) 5183-4695
in peak adsorption problems (evident as
peak tailing or loss of peak size). Active Quartz deactivated column
solutes are those containing a hydroxyl connector (5/pk) 5181-3396
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes. Polyimide sealing resin (5 grams) 500-1200

Prevention Deactivated Fused silica,


● Perform sample cleanup to remove 10m, 0.53mm i.d. 160-2535-10
nonvolatile materials from the sample Deactivated Fused silica,
● Use injection port liners packed with 10m, 0.25mm i.d. 160-2255-10
glass wool (may not be feasible when
analyzing active compounds) Capillary column rinse kit 430-3000

● Install a guard column and trim regularly

Recovery
● Do not bakeout the column
● Front End Maintenance: are usually responsible for many baseline Column Storage
problems (instability, wander, drift, ghost
– Clean or change the injection port liner Capillary columns should be stored in their
peaks, etc.).
– Clean out the injector original box when removed from the GC.
Prevention Place GC septa over the ends to prevent
– Cut off typically 0.5 to 1 meter of the debris from entering the tubing. Upon
front of the column
● Perform sample cleanup to remove
reinstallation of the column, the column
semi-volatile materials from the sample
● Turn the column around (install detector ends need to be trimmed by 2-4 cm to
end into injector)
● Increase the final temperature of the ensure that a small piece of septa is not
GC run (not to exceed the temperature lodged in the column.
● Solvent rinse the column limit of the column)
If a column is left in a heated GC, there
● Cut the column in half and use the back ● Change septa regularly should always be carrier gas flow through
half (detector side). the column. The carrier gas flow can be
Recovery turned off only if the oven, injector, detector
Semivolatile Contaminants ● Bakeout the column: limit 1-2 hours and transfer lines are turned off (i.e., not
Semivolatile contaminants or residues (excess baking may polymerize some heated). Without carrier gas flow, damage
accumulate in the column, but eventually contamination and reduce column to the heated portion of the column occurs.
elute. Hours to days may elapse before they lifetime)
completely leave the column. Like ● Solvent rinse the column
nonvolatile residues, they may cause peak
shape and size problems and, in addition,

42 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

Only a small sampling of FID supplies are shown here. For a complete selection of FID supplies,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 43
DETECTORS

Thermal Conductivity Detector (TCD)


The TCD compares the thermal Increasing Filament Lifetime introduction and prolongs filament
conductivities of two gas flows — pure lifetime.
Increased filament lifetime will result if the
carrier gas (also called the reference gas)
following startup process is used:
and carrier gas plus sample components
(also called column effluent). 1. Purge the detector with carrier and Cell Contamination
makeup gas for 10-15 minutes before Cell contamination is a problem when a
turning on the filaments. This prevents lower detector temperature is used to
Filament Maintenance oxidation of the filaments due to the improve sensitivity. Also, low filament
The primary maintenance for a TCD presence of oxygen that has diffused into currents promote contamination since
involves the filament. Most procedures the cell under no flow conditions. the filament is maintained at a lower
involve improving filament life or keep the 2. Turn on the filaments at the lowest temperature at lower currents. If the cell
filament from becoming damaged or possible current setting, then increase becomes contaminated, a solvent flush
contaminated. the filament current in several of the detector may help to remove the
increments to the desired value. This condensed material.
A constant presence of oxygen can
permanently damage filaments through reduces the power surge upon current
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 Thermal Conductivity Detector (TCD) Supplies
oxygen levels. Proper column installation
techniques and regular leak checks Description Unit Part No.
(especially after column installation) help
to keep leak problems to a minimum. 6890/6850/5890 Common TCD Supplies
The damage caused by oxygen is more
TCD replacement cell (6890/6850 only) G1532-60675
severe at high filament currents.
Chemically active sample components TCD cap column adapter seal 10/pk 18740-20950
such as acids and halogenated compounds
may attack and damage the filaments. TCD cap column adapter 18740-20960
Avoiding these compounds when possible
increases filament life. Turning off or Graphite ferrules, 1.0 mm id 10/pk 5080-8773
substantially reducing the filament current Graphite ferrules, 0.5 mm id 10/pk 5080-8853
when the TCD is not in use also prolongs
filament life. 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

Makeup gas adapter, TCD 19232-80550

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

TCD replacement cartridge 19232-60676

44 www.agilent.com/chem
DETECTORS

Solvent Flush Procedure 5. After the final injection, allow makeup that the carrier gas and the flow system
gas to flow for 10 minutes or more. components are leak-free and contaminant-
1. Cool the cell to room temperature and
Slowly raise the temperature of the cell free.
remove the column.
to 20-30˚C above the normal operating
Watch out for decreased sensitivity caused
2. Place a septum in a nut or fitting temperature.
by samples that react with the filament,
assembly that fits onto the detector
6. After 30 minutes, decrease the originating from oxygen-contaminated
entrance.
temperature to the normal value and carrier gas, leaks in plumbing, or column
3. Place the nut or assembly on the install the column as usual. bleeding. Samples with active components,
detector fitting and tighten. Verify such as acids and halogenated compounds
the presence of makeup gas flow. can chemically attack the filament as
Thermal Cleaning well. Also, sample condensation will
4. Inject 20-100 µL volumes of toluene or contaminate the detector cell if the
benzene into the detector through the The TCD can become contaminated with
deposits from such things as column bleed temperature is too low.
septum. Inject a total volume of at
least 1mL of solvent. Do not inject or dirty samples. A wandering baseline, Some types of contaminants can be
halogenated solvents such as methylene increased noise level, or changes in removed by temperature bakeout. Also,
chloride and chloroform into the detector. response on a checkout chromatogram all in non-modulated designs, wandering
indicate contamination. Thermal cleaning, baselines due to temperature variation can
or bakeout (heating the detector block to be corrected by making sure the detector
evaporate the contaminant), should be temperature remains constant.
performed only after you have confirmed

Nitrogen-Phosphorus Detector (NPD)

Bead Maintenance higher hydrogen flows and bead currents ● Turn off the bead when not in use.
decrease bead life. If the NPD is not in use,
NPDs are temperamental and require ● Keep the detector temperature high
the hydrogen flow and bead current should
frequent maintenance. Small changes (320 – 335˚C).
be reduced or turned off to increase bead
in any of a number of parameters can
life. Make sure there is some type of gas ● Turn off the hydrogen flow during solvent
significantly change the performance
flow in a heated detector or when there is peaks and between runs.
characteristics of an NPD. The bead
current to the bead.
requires the most maintenance. It needs ● If the NPD is off for an extended period
to be changed frequently, thus a spare is of time in a high humidity environment,
a necessity. Bead Life water may accumulate in the detector.
To evaporate this water, set the detector
The beads have to be kept dry which limits To extend the life of the bead: temperature to 100˚C and maintain it
their storage life to about six months.
● Use the lowest practical adjust offset or for 30 minutes. Then set the detector
When a new bead is installed, slowly raise
bead voltage. temperature to 150˚C and maintain it
the detector temperature and bead current.
for another 30 minutes.
Rapid heating can crack or break the bead ● Run clean samples and keep the
especially if it has been stored under humid inlet/liner clean to minimize
conditions. It has been observed that contamination.

www.agilent.com/chem 45
DETECTORS

Gas Flow Cleaning & Replacement the FID jet. Although you can clean the jet,
it is usually more practical to simply replace
The hydrogen, air and makeup gas flows The NPD requires periodic cleaning. In
dirty jets with new ones. If you do clean the
should be measured frequently. They can most cases, this only involves the collector
jet, use the cleaning wire, taking care not
drift over time or be changed unintentionally and the jet. Agilent provides brushes and
to damage the inside of the jet. You can
without knowledge of it occurring. Each gas wires that simplify the cleaning of all
also use a sonicator bath to clean the jet.
flow should be measured independently to detector parts (see FID Supplies on page
obtain the most accurate values. NPDs are 53). The brushes are used to dislodge
very sensitive to changes in the gas flows particulates clinging to the metal surfaces. Contaminants
and consistent flows are necessary to A fine wire is used to clean the jet opening
maintain performance levels. of particulates. Do not force too large a Some chemical problems can also arise
wire or probe into the jet opening or the when using the NPD. Because it is a trace
opening will become distorted. A loss of detector, be careful not to contaminate the
Gas Purity sensitivity or poor peak shape may result if analytical system.
Because of its high sensitivity, the NPD the opening is deformed. The various parts
Glassware
requires very pure gases (99.999% or can be ultrasonicated after cleaning with
a brush. Eventually the jet needs to be Glassware must be very clean. Phosphate
better). We strongly recommend that
replaced, so it is strongly recommended detergents should be avoided, so acid
moisture and hydrocarbon traps be used
to have spare jets on hand. washing of glassware followed by distilled
on the carrier gas and all detector gases,
water and solvent rinsing is recommended.
including the detector hydrogen, air, and Over time, residue from the bead or sample
makeup gases. Dirty gases will not only can build up in the collector and cause Solvents
give poor chromatographic performance, baseline problems. You should clean the Solvents should be checked for purity.
but will shorten the bead life as well. collector after you have changed the bead Chlorinated solvents and silanizing
two or three times. reagents can decrease the useful lifetime
The metal C-rings wear slightly with each of the alkali source; excess reagent should
assembly and disassembly. After several be removed prior to injection, if possible.
assemblies and disassemblies (five or
more), the rings may not seal effectively, Other Contamination Sources
causing an erratic baseline. A ceramic Phosphate-containing leak detectors,
insulator and seal kit is available. Always phosphoric acid-treated columns or glass
cool the detector to near-ambient when wool, polyimide-coated columns, or
changing seals and insulators. nitrogen-containing liquid phases can add
noise to the system and should be avoided.
Because there is no flame in the NPD, the
jet does not collect silica and soot as does

NPD Jets

Description Length (mm) Part No.

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


(6890 only, dedicated) 48 G1531-80560

6890/5890 Adaptable

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

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

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

2 NPD white ceramic bead assembly* G1534-60570


2
1
NPD black ceramic bead assembly** 5183-2007

3 Lid weldment G1534-80510


3
4 Metal C-ring, top 0905-2580
9
5 Alumina insulator, upper G1534-40020 10
11

4 12
6 Collector funnel G1534-20530
5
7 Alumina insulator, lower G1534-40030 6

8 Metal C-ring bottom and top 0905-1284 8 7

9 Screw, M4 x 10 mm 0515-2495

10 J-Clamp 1400-0015

11 Screw, M4 x 10 mm 0515-2495

12 NPD interconnect assembly G1534-60610 13


14
13 Mounting pallet G1531-40020

14 Jets (see page 54)

15 Base weldment, Capillary NPD G1534-80500 15


16
Base Weldment, Packed NPD G1534-80540

16 Lid stop G1534-20590 17

NPD Ceramic Insulator Kit


includes items 4, 5, 7, and 8 5182-9722
18
17 Column adapters for packed NPD

18 Nut warmer cup with insulation 19234-60720

5890 NPD Supplies

NPD collector (NPD bead) 19234-60540

Recoating kit, sufficient for 10 collectors 5080-8872

Detector Trap Replacement Kit 19231-60790

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

For a complete selection of NPD supplies,


www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 47
DETECTORS

Electron-Capture Detector (ECD)


Agilent provides two types of electron Radioactivity Leak Test
capture detectors. The regular detector
Electron capture detectors must be tested
(ECD) has a larger internal volume
for radioactive leakage at least every six
(approximately 10 times) than the micro-
months. Records of tests and results must
cell detector (µ-ECD). These two types can
be maintained for possible inspection by
be distinguished by the top cover of the
the Nuclear Regulatory Commission and/or
detector — the ECD has a solid cover and
the responsible local agency. More frequent
the µ-ECD has a perforated cover.
tests may be conducted when necessary.
The procedure used is a “wipe test.” A
Thermal Cleaning wipe test kit is supplied with each new
If your baseline is noisy or the output detector. Refer to the information card
value is abnormally high and you have supplied in the Wipe Test Kit for
determined that these problems are not instructions on performing the test.
being caused by leaks in the GC system,
you may have contamination in the
detector from column bleed. To remove
Gas Purity
contamination, you should perform a For successful EC detection, it’s important
thermal cleaning (bakeout) of the detector. that the carrier and purge gases are very
clean and dry (99.9995%). Moisture, oxygen,
Warning: Detector disassembly and/or
or other contaminants can be responsible
cleaning procedures other than thermal
for improved sensitivity, but at a cost of
should be performed only by personnel
linear range. Always precondition the
trained and licensed appropriately to
column before connection to the detector.
handle radioactive materials. Trace
amounts of radioactive 63Ni may be
removed during other procedures,
causing possible hazardous exposure
to ß and x-radiation.

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 1

5890 ECD Supplies 2

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


3
Vespel/graphite 85%/15%
ferrule, 1/4 in. id 10/pk 0100-1331
ECD Packed for 1/4 in. Glass Columns
2 Tubing nut, 1/4 in. brass 10/pk 5180-4105

3 ECD column adapter, 1/4 to 1/8 in. metal 19301-80530


7
4 Makeup gas adapter for micro ECD adapter G2397-80520
6
5 Makeup gas adapter, ECD, new style 19233-80565

6890/5890 Common ECD Supplies 5, 4

6 ECD fused silica liner (new style) 19233-20625

ECD adapter fused silica liner micro ECD G2397-20540 ECD Make up Gas Adapter

7 Stainless steel cap for ECD makeup gas adapter 19233-20755


(new style and micro ECD)

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 Agilent’s 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 ● Increase the air supply pressure to the
pneumatics module. This makes the
Flame Photometric Detectors require ● defective signal boards are present
flame easier to light but does not affect
minimal maintenance to keep them
High detector temperatures reduce the the air flow rate setpoint.
performing at satisfactory levels. The
PMT life. When not in use, turn off the PMT
hydrogen, air and makeup gas flows should ● If the flame doesn’t light at all, check the
to maximize its usable lifetime. Some PMTs
be measured occasionally. They can drift glow plug circuit. Observe the visual
may have a shelf life and should not be
over time or be changed unintentionally display, which will momentarily go to
stored for prolonged periods before use.
without knowledge of it occurring. Each gas greater than 65500 counts when the
flow should be measured independently to Column bleed and/or effluent can flame lights. If the display doesn’t
obtain the most accurate values. contaminate the first quartz window (heat change, check the pin connections at the
shield) nearest the detector module. Dust, printed circuit board, the lead connection
fingerprints, and atmospheric contaminants on the glow plug and the appropriate 5A
Cleaning & Parts Replacement can dirty both quartz windows, the filter, fuse on the GC main circuit board.
The FPD requires periodic cleaning. In and/or the photomultiplier tube window. ● The flame is easier to light at higher
most cases, this only involves the jet, and Contamination anywhere along the light
detector temperatures.
less frequently, the filter. Agilent provides path between flame and PMT can reduce
brushes and wires that simplify the detector sensitivity. ● Under some operating conditions, the
cleaning of all detector parts (see FID flame may be more easily lit with the
If a response problem is encountered
Supplies on page 53). The brushes are used rubber drip tube removed. After lighting
(sensitivity, noise, selectivity) the FPD jet
to dislodge particulates clinging to the the flame, reinstall the drip tube.
should be inspected for deposits and, if
metal surfaces. A fine wire is used to clean necessary, cleaned or replaced. To properly ● If the flame still won’t light, there could
the jet opening of particulates. Do not force service the jet, the detector module should be a large leak in the system. This results
too large a wire or probe into the jet be removed from the instrument, and in measured flow rates being different
opening or the opening may become followed by appropriate service (see jet from actual flow rates, causing non-ideal
distorted. A loss of sensitivity, poor peak cleaning procedure on page 53). ignition conditions. Thoroughly leak
shape, and/or lighting difficulties may check the whole system.
result if the opening is deformed. The filter Occasionally, the transfer line fused silica
or any of the window parts should be liner between the column and FPD module
handled gently. Scratches or other surface must be inspected, cleaned and/or replaced.
deformities reduce the amount of light
passing through the filter, thus reducing
Flame Conditions & Gas Flows
response. The filter and related parts
Flame Ignition Problems
The flame conditions are critical to
should be clean and free from fingerprints. If the FPD flame won’t light or stay lit: successful operation. Since the detection
zone is above the flame, the gas flows and
The Photo Multiplier Tube needs periodic ● Be sure there is a problem. Ignition is best
jet diameter must be optimized so that
replacement. The PMT is defective and confirmed by holding a mirror or shiny
components burned (activated) in the flame
needs to be rebuilt or replaced if: surface near the aluminum exhaust tube,
will emit in the detection zone.
with the rubber drip tube removed, and
● high voltage is on and the flame is lit
observe condensation if the flame is lit. Gas flows are also critical for optimized
● low or no signal and/or noise not selectivity and sensitivity. The most critical
● Check Lit Offset. If it is zero, autoignition
attributed to any other source such as parameters are the hydrogen/air or
is turned off. If it is too large, the GC will
bad cables are observed hydrogen/oxygen ratio, and the total gas
not know that the flame is lit and will
flow, which effects flame temperature.
● light leaks occur shut down the detector.

50 www.agilent.com/chem
DETECTORS

6890/5890 FPD Supplies

Item Description Unit Part No.

1 Exit tube assembly 19256-60700


1
2 Nut, brass, 1/4 in. 10/pk 5180-4105 2
3
4 Weldment, block 19256-80560
4

5 O-ring, ignitor, Kalrez 0905-1102 5


9
6 10
7 11
6 Spacer, ignitor 19256-20590
12
7 Glow plug 0854-0141 8 13
14
8 Ignitor cable assembly (6890 only) G1535-60600
15

9 Gasket, heat shield 19256-80040


16
10 Window, first heat shield 19256-80030 17
18
11 Disk, heat shield 19256-20580 19

12 Coupling, SS 19256-20550 20

14 Screw, M3 x 12 (4 required) 0515-0911 21

15 Clamp 19256-00090
16 O-ring, inner window 12/pk 5061-5886
17 Window, second heat shield 19256-80060
18 O-ring, outer window 12/pk 5061-5891
19 Flange adapter 19256-20510
20 Flange ring 19256-00200
21 O-ring, Viton, 1.239 in. id 12/pk 5061-5890
Adapter weldment, 1/8 in. columns 19256-80590
Adapter weldment, capillary 19256-80570
Start-up kit (5890 only) 19256-60500
FPD O-ring (5890 only) 12/pk 5061-5867
HELPFUL HINT: Install the correct optical
Liner/ferrule kit 19256-60590 filter, depending on the choice of Sulfur or
Sulfur filter 19256-80000 Phosphorus mode. For Sulfur Mode, use
the 393 nanometer filter. For Phosphorus
Phosphorus filter 19256-80010
Mode, use the 525 nanometer filter.
Kalrez O-ring, size 2-002 0905-1101
Kalrez O-ring, size 2-011 0905-1103
Fluorocarbon Elastomer O-ring,
brown, 0.926 in. id 12/pk 5061-5889
FPD Performance Evaluation Sample: Solution of
20 ng/mL (20 ppm) dodecanethiol and
tributylphosphate in isooctane, 3 ampoules 19305-60580

www.agilent.com/chem 51
DETECTORS

Flame Ionization Detector (FID)


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

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

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
Cleaning & Replacement
use a large id column, turn off the carrier
flow long enough to allow the FID to light. Even with normal use, deposits develop in
Check for partially or completely the jet and detector (usually white silica
plugged jet. from column bleed or black carbonaceous
soot). These deposits reduce sensitivity
● Check that the right type of jet is installed
and cause chromatographic noise and
for the column you are using.
spikes. Although you can clean the jet, it is
● Injecting large volumes of aromatic usually more practical to replace dirty jets
FID Cleaning Kit
solvent can cause the flame to go out. with new ones. If you do clean the jet, be
Switch to a nonaromatic solvent. careful not to scratch the jet internally;
scratches will ruin the jet.
● The lit offset value may be too low or too
high. Adjust the value.

Plugged FID jet

52 www.agilent.com/chem
DETECTORS

Flame Ionization Detector (FID) Supplies

Description Unit Part No.


Jet Cleaning Procedure
(using Agilent’s FID Cleaning Kit #9301-0985)
6890/6850 Supplies
1. Run a cleaning wire through the top of
the jet. Run it back and forth a few times Collector insulator G1531-20700
until it moves smoothly. Be careful not to
Collector body G1531-20690
scratch the jet. (Do not force too large a
wire or probe into the jet opening or the FID collector assembly* G1531-60690
opening will become distorted. A loss of Detector insulation assembly G1531-20700
sensitivity, poor peak shape and/or
lighting difficulties may result if the FID ignitor cable G1531-60680
opening is deformed.) Collector Housing G1531-20740
2. Fill an ultrasonic cleaning bath with 5890 Supplies
aqueous detergent, and place the jet in
Collector assembly* 19231-60690
the bath. Sonicate for five minutes.
Upper collector insulator 19231-20970
3. Use a jet reamer to clean the inside of
the jet. Collector body 19231-20960
4. Sonicate again for five minutes. Hastelloy collector 19231-21080
Lower collector insulator 19231-20950
NOTE: From this point on, handle the parts
only with forceps! 6890/6850/5890 Common Supplies
5. Remove the jet from the bath and rinse it PTFE chimney (optional) 19231-21050
thoroughly, first with hot tap water and Collector nut 19231-20940
then with a small amount of GC-grade
methanol. Spring washer 10/pk 5181-3311

6. Blow the jet dry with a burst of the Ignitor castle 19231-20910
compressed air or nitrogen, and then Hastelloy Ignitor Castle 19231-21060
place the jet on a paper towel and allow
it to air dry. Ignitor glow plug assembly 19231-60680
FID collector cleaning brush 2/pk 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 5080-4978
FID Performance evaluation sample kit,
0.03% C14, C15, and C16 normal
alkanes in hexane 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)

Only a small sampling of FID supplies are shown here. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 53
DETECTORS

FID Jets

Description Length (mm) Part No.

Jets for capillary dedicated FID (6890 only)

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

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

Adaptable FID (6890/6850/5890)

Capillary 0.53 mm jet (0.011 in. id tip) 61.5 19244-80560 Agilent FID Jets (from top to bottom): Dedicated
capillary, Adaptable capillary, Adaptable packed
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

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
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wealth of knowledge, all at your fingertips.
Tap our 35 years of instrument expertise
and applications knowledge by phone, in
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telephone support, on-site repair, even
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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
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doesn’t stop there. We want to
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And our technical support.”
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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 Course #H5308A introduces the
productivity high, minimize the number fundamental concepts of gas
of errors and reruns, and expand chromatography and the operation of
chromatography capabilities. With expert the Agilent 6890 GC using the Agilent
training that gives you on-site expertise ChemStation for GC and capillary columns.
for troubleshooting and maintenance, This five-day hands-on course is designed
your lab will run at peak performance. for the new GC operator who is responsible
for routine sample analysis. It covers
GC Training everything from inlets, columns, and
Agilent’s training courses for gas detectors to data analysis and reporting.
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proper and efficient ways to use select “Education.”
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These ISO-registered courses also target
Maintenance Training
those who want to broaden or sharpen
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Agilent GC system. For more information
on all Agilent Training offerings, visit
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● Course #H5308A (for Series 6890)
Technical Support Consultation
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Have a technical GC column, method, or
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56 www.agilent.com/chem
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www.agilent.com/chem 57
SERVICE & SUPPORT

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highly trained experts. We’ll provide all Open inside cover for:
enhancements to the original chemical
analysis software purchased. We’ll even GC System
send you Software Bulletins to let you Recommended
know about ongoing issues and
recommended workarounds. Contact
Maintenance
Agilent today for more information about Schedule
these and other Support Services. ● Technical Support Assistance (a logical,
Hardware Support step-by-step approach to help you solve
common problems)
Agilent’s highly trained technical staff is
just a phone call away to offer you basic ● Technical Document Library (a searchable
hardware troubleshooting, operation collection of service and support
assistance, instrument and system documents)
configuration, and remote diagnostics. Call ● Chromatogram Library (a searchable
us toll-free today, or submit your question collection of GC, LC, and CE
on-line at www.agilent.com/chem. chromatograms – nearly a thousand
Stay on Top with “Separation Times” chemical compounds)

Tap into Agilent’s chromatography ● Product Support Literature (including


expertise all year long with a free Operating Manuals and Installation
subscription to Separation Times magazine. Guides)
For knowledge, tips, and insight, go to ● Illustrated Parts Breakdowns (instrument
www.agilent.com/chem/supplies, click diagrams to help you identify parts or part
on “What’s New,” then select “Tap into numbers)
Agilent’s Expertise” to sign up today and
stay ahead of the information curve. ● Software Status Bulletins (updates on
recommended software workarounds)
Visit Agilent on-line
Plus, a host of information and features to
For a wealth of GC knowledge any time, make ordering easier and faster.
visit www.agilent.com/chem. You’ll 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 www.agilent.com/chem
GC System Recommended Maintenance

Gas Management
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Gas purifiers Every 6-12 months Replacement schedule is based on capacity and grade of gases.
(carrier gas & In general, replace non-indicating traps every 6-12 months or when
detector gas) indicating traps start to change color. Replace indicating traps when
indicating material is spent.
Split vent trap Every 6 months* Replace.
Flowmeter Every 1-2 years Re-calibrate electronic flowmeters – follow recommended schedule for
calibration the unit (shown on calibration certificate).

Sample Introduction and Inlets


ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Syringes Every 3 months* Replace syringe if dirt is noticeable in the syringe, if it cannot be
and/or syringe cleaned, if the plunger doesn’t slide easily, or if clogged. Replace
needles needle if septa wear is abnormal or the needle becomes clogged.
Inlet liner Weekly* Check often. Replace when dirt is visible in the liner or if
chromatography is degraded.
Liner O-rings Monthly* Replace with liner or with signs of wear.
Inlet septum Daily* Check often. Replace when signs of deterioration are visible
(gaping holes, fragments in inlet liner, poor chromatography,
low column pressure, etc.).
Inlet Hardware Every 6 months Check for leaks and clean.
Every year Check parts and replace when parts are worn, scratched, or broken.

Remember, the downtime for scheduled


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

Columns
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

Front-end Weekly – monthly* Remove 1⁄2 -1 meter from the front of the column when experiencing
Maintenance chromatographic problems (peak tailing, decreased sensitivity, retention
time changes, etc.). Replace inlet liner, septum and clean inlet as
necessary. Guard column may be useful for increasing column lifetime.
Solvent rinse As needed When chromatography degradation is due to column contamination.
Only for bonded and cross-linked phases.
Replacement As needed When trimming and/or solvent rinsing no longer return chromatographic
performance.
Ferrules Replace ferrules when changing columns and inlet/detector parts.

Detectors
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

FID/NPD Jets As needed Clean when deposits are present. Replace when they become scratched,
& Collector bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead As needed Replace when signal drifts or there is a dramatic change in sensitivity.
FID Every 6 months Measure hydrogen, air, and makeup gas flows.
TCD As needed Thermally clean by “baking-out” when a wandering baseline, increased
noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.
ECD Every 6 months Wipe test.
As needed Thermally clean by “baking-out” when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD Every 6 months Measure hydrogen, air, and makeup gas flows.
As needed Clean/replace FPD windows, and seals when detector sensitivity
is reduced.

*Schedule is an approximation of average usage requirements.


Frequency may vary widely based upon application and sample type.

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