Operate your lab at peak performance
Troubleshoot difficult problems
Select the right Agilent supplies
Plan preventative maintenance
Maintaining your Agilent
GC and GC/MS Systems
Maximize your efficiency. Minimize your downtime.
Get the results you need.
Our GC and GC/MS Maintenance Guide puts
nearly 40 years of Agilent knowledge at your fingertips.
At Agilent Technologies, we understand that many of today’s labs face the challenge
of operating with a reduced staff. That’s why we’re committed to bringing you the
world’s best GC and GC/MS systems — plus the critical information you need to keep
them running properly.
In this newly updated Maintenance Guide, we share everything from essential service
schedules … to invaluable troubleshooting tips and problem-solving methods.
We’ve even included easy guides to help you order Agilent parts and supplies —
which have 40 years of high quality and technical experience built right in. So you can
keep your downtime to a minimum, and get the results you need.
Maintaining Your Agilent GC and GC/MS Systems
Maximize your efficiency. Minimize your downtime.
Get the results you need.
2
3
4
4
12
13
14
15
Gas Management
Gas Types
Contaminants & Purities
Gas Purification Systems
Regulators
Tubing
Leak Detection
Flow Rates
18 Sample Introduction
Consumables & GC Inlets
Sample Introduction
19 Vials
21 Syringes
TIPS AND TOOLS
This icon denotes a helpful hint that provides useful information you
can find throughout this guide and online at www.agilent.com/chem.
VIDEO
This icon denotes a video that is available to view on our website.
Just visit www.agilent.com/chem/techsupport to view how-to
videos and obtain more information.
26
28
31
34
36
42
47
52
54
Inlet Types
Packed-Column
Split/Splitless
Cool On-Column
Programmed Temperature
Vaporizer PTV
Inlet Accessories
Septa
Ferrules
Liners
Flip Top Inlet Sealing System
Parts & Supplies
56
57
57
58
Columns
Column Maintenance
Column Selection
Column Installation/Setup
& Conditioning
59 Column Performance
63 Columns Types and
Characteristics
68 Detectors
69 Flame Ionization Detector (FID)
Thermal Conductivity Detector
(TCD)
72 Electron-Capture Detector
(ECD)
74 Thermal Conductivity Detector
(TCD)
76 Flame Photometric Detector
(FPD)
78 Nitrogen-Phosphorus Detector
(NPD)
82 GC/MS Systems
83 Maintaining Mass Selective
Detectors (MSDs)
87 Mass Spectrometer Symptoms
88 Ion Source
93 Vacuum Systems & Pumps
96 Electron Multipliers &
Replacement Horn
97 Maintaining the MS Engine
99 Ion Source Parts & Supplies
100 General GC/MS Supplies
101 Test & Performance Samples
104 Services & Support
105 Expert Service, Training
& Support
Don’t Miss…
GC Maintenance Schedule (inside back cover)
1
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Gas Management
The use of quality carrier gases is essential
for consistent and accurate GC analyses.
Proper gas management is key to achieving
this goal. Agilent provides a diverse line of
high quality gas management products —
gas purifiers, regulators, leak detectors
and flowmeters — all designed to prevent
column damage, improve detector life, and
improve the quality and consistency of your
GC separations. This section explains how
common contaminants like oxygen, moisture
and hydrocarbons can damage your GC
column, and helps you understand how to
prevent it. Also, look for practical information
about regulators, the importance of clean
GC-tubing, and minimizing the likelihood
of GC system contamination.
“Gas management is more than just
selecting the highest quality carrier
gas available. It’s about selecting the
appropriate carrier gas for your needs,
and taking steps to prevent system
contamination. Agilent understands
this and provides products that make
gas management easy to implement
in your lab.”
Kenji Yamaguchi
Applications Support Manager
CATALOG
For a complete selection of gas management supplies, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
•
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2
GAS MANAGEMENT
Gas Types
Carrier Gases
The most frequently used carrier gases are
helium and hydrogen, although nitrogen
and argon can be used. Purity is essential
for these gases since they sweep the
sample through the column where it is
separated into its component parts and
then through the detector for component
quantification. Carrier gas purity is also
critical to prevent degradation of
chromatographic hardware.
Contaminants in carrier gases can have
a significant effect on column life and
subsequent analyte detection. Harmful
effects of impure gases include
contaminant peaks and elevated column
bleed, along with column and/or detector
damage. The following sections describe
the gases and purities that are necessary
for gas chromatography carrier gases, as
well as other support gases.
dioxide) and pneumatic gases (air or
nitrogen) generally do not come in contact
with the sample or detector. Therefore,
these non-contact gases do not have to
be the highest purity available.
Support Gases
Fuels, oxidants and detector gases, in most
cases, do come in contact with the sample
and detector, and require higher purity
gases. Unfortunately, gas nomenclature as
it relates to purity is not consistent across
specialty gas suppliers. It is important to
recognize the impurities in your gas
supplier’s products, and to utilize the
appropriate Agilent gas purification
products (see next section).
Support gases may be specific for
detectors or for applications. These gases
include fuels, oxidants, coolants, detector
gases, and pneumatic gases. The degree
of purity required for support gases is
dependent on how that gas is being used,
and whether or not it will make contact
with the sample. Coolant gases (carbon
Carrier and Support Gases
Sample
Contact
Purity Required*
Pneumatics
No
Low Grade
Pneumatics
No
Low Grade
Gas Type
Function
Air
Nitrogen
Limit of Detection required:
Hydrogen
Trace (0-1 ppm)
1-1000 ppm
1000 ppm-1%
1%-100%
Carrier or fuel gas
for detector
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
Hydrogen/Helium Mix
Fuel gas for detector
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
Methane/Argon
or Nitrogen
Carrier or make-up
for ECD
Yes
Research
Research
Research
N/A
Air
Oxidant for detector
No
Ultra-Pure
Ultra-Pure
UHP/Zero
UHP/Zero
Nitrogen, Helium,
or Argon
Carrier or
make-up gas
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
*Purities of gases depend upon the type of detector that is used. Use this table as a general guide only and refer to
your detector manual for specific gas purities that are needed.
Low Grade = Specialty or industrial gases (≤99.998%)
UHP/Zero Grade (99.999%)
Ultra-Pure Grade (99.9995%)
Research Grade (99.9999%)
3
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GAS MANAGEMENT
Contaminants & Purities
Contaminants in gases are major
contributors to capillary column
degradation and detector noise, and
can interfere with chromatographic
results. Concentration of these
contaminants vary by the grade of gas.
Analytical gases are available in many
grades of quality, from high purity
(99.995%) to chromatography grade purity
(99.9995+%). The higher the purity, the
higher the cost.
Identifying Contaminants
To make a proper purity choice it is
helpful to understand the contaminants
most common in GC gases and how
they can affect your analysis. Common
contaminants are:
Hydrocarbons and Halocarbons
• decrease detector sensitivity by
increasing detector background noise
• can also cause baseline drift or wander,
contaminant peaks, and noisy or high
offsets of baselines
Moisture
• can be introduced by improper handling
and/or installation of plumbing
• a common cause of column stationary
phase degradation
• can damage instrument
Oxygen
• most common contaminant
• a common cause of column stationary
phase and inlet liner degradation
• can cause decomposition of labile
analytes
In some cases it may be difficult to
determine which contaminant presents
the biggest problem in a given analysis. If
unsure, a call to your gas supplier may be
helpful. Once the problem contaminants
have been identified and a general
contaminant level is determined, the next
step is to choose a gas purity level that
comes closest to these requirements.
Keep in mind that higher grades of gas
generally cost more. The greatest cost
savings can be achieved by using the
lowest purity gas which will neither
interfere with the analysis nor damage
your equipment. Using the proper gas
purification equipment to remove common
contaminants and achieve the desired
purity level is essential.
• opportunity for introduction at every
fitting present in the gas line or during
use of gas permeable tubing.
Gas Purification Systems
Agilent brings the highest performance
and largest variety of gas purifiers (traps)
to gas chromatographers. Purifiers are
available in a variety of sizes and
configurations to remove common
contaminants like oxygen, moisture,
and hydrocarbons. In-line gas purifiers,
including refillable, indicating, S-shaped,
and metal body types, are made to remove
specific contaminants. Agilent also offers
gas purification systems with removable
cartridges. These systems provide the
ability to design the right combination
of filters needed for your application to
achieve the proper gas purity.
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•
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The illustration on the next page shows
the most common gas purification
configurations used in gas chromatography.
Regardless of which purification system
is employed, proper installation and
maintenance is required to achieve
optimal performance from the purification
system(s). A purifier that is not maintained
will eventually expire and become
ineffective, or worse, a source of
contamination.
Other Considerations
• determine desired purity level
• keep number of fittings in gas line
to a minimum
• install purifiers in a convenient location
close to the GC
• purifier log books are useful for
determining maintenance schedule
• use indicating traps closest to the GC so
you can determine when to change the
traps that are upstream
4
GAS MANAGEMENT
Carrier Gas Purification
Key:
In-Line Gas Purifiers
-ORGas Purification System
Gas supply
1 = Moisture Trap
2 = Hydrocarbon Trap
3 = Oxygen Trap
4 = Indicating Oxygen Trap
5 = Gas Purification System
6 = Combination Trap for
moisture, oxygen, and
hydrocarbon removal
Detector Gas Purification
FID make-up, air,
and H2
-ORCombination Trap
Gas supply
ECD make-up
Vent
ELCD reaction gas
Gas supply = cylinder, in-house line, or gas generator
MS carrier gas
Regulator = Brass dual stage regulator
Gas Traps
The purpose of gas traps is to remove
detrimental impurities from the carrier
and detector gases. Moisture (water),
oxygen and hydrocarbon traps are the
most common traps used with GC
systems. A few combination traps are
available which remove moisture, oxygen
and/or organics with a single trap. The
effectiveness of the traps depends on the
initial quality of the gas. Little
enhancement by traps to the GC system is
obtained by traps when using very high
purity gases (e.g., ultra-high purity or
similar grades) while obvious improvement
is obtained with lower grades of gas.
Constant exposure of capillary columns to
oxygen and moisture, especially at high
temperatures, results in rapid and severe
column damage. The use of oxygen and
moisture traps for the carrier gas may
extend column life and protect the
instrument. Traps may provide some
protection if there is a leak at or around
the gas cylinder. Any moisture or oxygen
introduced into the gas stream due to the
leak will be removed by the trap until it
expires. This creates an opportunity to
detect and fix the leak before column or
instrument damage occurs.
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom,
even at your site. See pages 104-115 for more information about our
services and support.
5
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•
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GAS MANAGEMENT
Moisture (Water) Traps
There are several different adsorbents and indicating materials
used in moisture traps. Moisture traps can be easily refilled.
Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap
making refilling a more economical (and less wasteful) option.
Indicating moisture traps are available in plastic and glass bodies.
Glass body traps are used when potential contaminants from
plastic trap bodies are a concern. Glass traps are normally
encased in a protective, plastic shrink wrap or a high impact
plastic shield (outer trap body). Glass and plastic bodied traps are
usually pressure tested at 150 psi, thus they are safe for use at the
typical pressures required by the GC.
Refillable Glass Moisture Trap
Moisture Removal Traps
Size
(cc)
Description
H2O Removal Maximum Effluent H2O
Capacity (g)
Concentration (ppb)
1/8 in.
Part No.
1/4 in.
Part No.
Price
MT200-2
MT200-4
$104
MSR-1
MSR-1
$ 55
GMT-2-HP
GMT-4-HP
$119
GMSR
GMSR
$ 63
Molecular Sieve 13X and Indicating 4Å – Economy, with plastic Lexan body (other packings available, see Agilent catalog)
Refillable Moisture Trap
200
36
18
Adsorbent Refill (1 pint) for MT Series
Glass Indicating Moisture Traps (larger size is available, see Agilent catalog)
Glass Indicating Moisture Traps
100
Molecular Sieve Refill for GMT Series
250
16.3
6
Moisture Removal S-Trap – can be reconditioned in the GC oven
Moisture S-Trap – preconditioned
5060-9084
$226
Big Moisture Traps – for the Ultimate Moisture Capacity
Big Moisture Trap
750
Refill for BMT Series (2 refills)
Refillable Moisture Trap
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•
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Moisture S-Trap
BMT-2
BMT-4
$235
BMSR-1
BMSR-1
$ 58
Big Moisture Trap
6
GAS MANAGEMENT
Oxygen Traps
Oxygen traps usually include a metalcontaining inert support reagent. Most
oxygen traps reduce the oxygen
concentration to below 15-20 ppb. The
capacity of a standard oxygen trap is
approximately 30mg of oxygen per 100cc
of trap volume. Oxygen traps can also
remove some small organic and sulfur
compounds from gas streams, but this is
not their primary application.
Indicating Oxygen Trap
Big Oxygen Trap
Metal (usually aluminum) trap bodies are
recommended for GC analyses. Some
Oxygen Traps
Description
1/8 in.
Part No.
Size (cc)
1/4 in.
Part No.
Price
IOT-4-HP
$143
Indicating Oxygen Traps – glass body with plastic safety shield
Indicating Oxygen Trap
30
IOT-2-HP
Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller size
available, see Agilent catalog)
Big Oxygen Trap
750
BOT-2
BOT-4
Hydrocarbon Traps
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
Price
200
HT200-2
HT200-4
$106
ACR
ACR
$ 63
BHT-2
BHT-4
$235
BACR
BACR
$ 52
Hydrocarbon Traps – General Purpose
Refillable Hydrocarbon Trap
Adsorbent Refill (1 pint, 2 refills)
Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity
Big Hydrocarbon Trap
Indicating oxygen traps change color when
oxygen is present in the gas at harmful
levels. Indicating traps are not intended to
be the primary oxygen removal trap, but
should be used in conjunction with a high
capacity non-indicating oxygen trap. They
are installed after the high capacity oxygen
trap in the gas line to indicate when the
high capacity trap has expired and needs
to be changed. Expired oxygen traps need
to be immediately changed since they can
contaminate the gas, in addition to failing
to remove oxygen.
$235
Hydrocarbon Traps
Description
plastics are permeable to air and contain
contaminants that can degrade gas quality.
In addition, many of the metal bodied
oxygen traps can withstand high pressures
(up to 2000 psi). Some oxygen traps also
remove moisture from the gas stream
without affecting the oxygen removal
capability.
750
Refill for Big Hydrocarbon Trap (2 refills)
Hydrocarbon traps remove organics, such
as hydrocarbons and halocarbons, from
the gas stream. The adsorbent is usually
activated carbon or an impregnated carbon
filter media. Carbon removes organic
solvents from the gas stream, including the
typical solvents used in nearly every lab.
Hydrocarbon-moisture combination traps
are also available which remove water in
Hydrocarbon Removal S-Trap – can be reconditioned in the GC oven
Hydrocarbon S-Trap
5060-9096
$232
Capillary Grade Hydrocarbon Traps – for crucial capillary applications
Capillary Grade Hydrocarbon Trap
Adsorbent Refill (1 pint, 3 refills)
7
100
HT3-2
HT3-4
$ 98
ACR
ACR
$ 63
Hydrocarbon Trap
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•
800 227 9770
GAS MANAGEMENT
Hydrocarbon Traps continued
addition to organics as described in the next
section. Capillary grade hydrocarbon traps
are purged with ultra-high purity helium
and packed with a very efficient activated
carbon material. Metal trap bodies are used
to prevent any contaminants in plastic trap
bodies from contaminating the carbon
adsorbent. Most hydrocarbon traps can
be refilled by the end user.
Big Hydrocarbon Trap
Hydrocarbon S-Trap
Combination Traps
Agilent carries several Combination Traps
that provide multiple contaminant removal
in a single trap. These traps offer:
• Efficient design which prevents
channeling and promotes efficient
scrubbing
• Optimized adsorbents for maximum
surface area and capacity
• The ultimate in purification with a single
trap (Big Universal Trap)
• Leak-free, one-piece design to eliminate
potential leaks from using multiple traps
Description
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
Price
100
OT3-2
OT3-4
$104
Oxygen/Moisture Traps
Agilent OT3 Trap
Agilent OT3 Trap
Hydrocarbon/Moisture Traps
Refillable Hydro-Moisture Trap
200
Refill for Hydrocarbon/
Moisture Trap (1 pint, 2 refills)
HMT200-2 HMT200-4
HCRMS
HCRMS
$ 98
$ 63
Big Universal Traps – for the Ultimate in Gas Purification, removes oxygen, moisture,
hydrocarbons, CO, and CO2
Big Universal Trap – Helium
purged (also recommended
for GC Mass Spec)
750
RMSH-2
RMSH-4
$261
Big Universal Trap – Hydrogen purged 750
RMSHY-2
RMSHY-4
$261
Big Universal Trap – Nitrogen purged
RMSN-2
RMSN-4
$261
UMC-5-2
UMC-5-2
$ 21
Big Mounting Clip for
mounting Big Traps 2/pk
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•
800 227 9770
750
Big Universal Trap
Hydrocarbon Moisture Trap
8
GAS MANAGEMENT
High Capacity
Gas Purification System
Three Cartridge System
Single-Cartridge System
• Agilent’s highest capacity and most
economical gas purification system.
Three Cartridge
High Capacity
Gas Purification
System
• Provides low-cost gas contaminant
removal for up to 18 cylinders of
carrier gas.
• Includes a manifold with cartridge
mounts and three replaceable cartridges:
one moisture/hydrocarbon cartridge; one
oxygen cartridge; and one oxygen
indicating cartridge.
• Contains a triple-combination cartridge
that offers the same highly efficient
contaminant removal properties from
eight cylinders of carrier gas but without
the visual indicator.
• Other cartridges are also available for
detector gas supplies and as individual
filters for specialized requirements.
• Consists of a permanent all-welded
stainless steel manifold to minimize
the potential for leaks.
• Suitable for bench or wall mounting.
High Capacity Gas Purification System
Description
Part No.
Price
With 1/8 in. fittings
5183-1907
$612
With 1/4 in. fittings
5182-9776
$567
Replacement Cartridge Kit–
Includes all three cartridges for
above system
5182-9780
$393
With 1/8 in. fittings
5183-4598
$239
With 1/4 in. fittings
5183-4599
$255
Triple combination replacement cartridge
for single cartridge system
5183-4600
$136
Three Cartridge System–Includes manifold
for wall or bench mount and 3 cartridges
(H2O/hydrocarbon, oxygen, and indicating O2)
Single Cartridge System–Includes single
cartridge manifold brackets for wall or bench
mount, and a triple combination cartridge
(H2O/hydrocarbon, and O2 )
9
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GAS MANAGEMENT
Quick Change Plus (QC+) Point of
Operation Panel
The QC+ Point of Operation Panel contains
purifier cartridges that can be quickly
changed. The cartridges are removed from
the panel without interruption of gas flow
to the system, drastically minimizing costly
instrument downtime.
Filter cartridges are of all metal or glass
construction, eliminating infusion and
resultant signal noise associated with
filters constructed from plastics. Cartridges
are quickly installed via a simple knurled
retaining nut, with no wrenches needed.
As many as four cartridges can be replaced
in a matter of seconds, and because there
is low dead volume, a minimal amount of
gas system purge is required after
installation.
RQC-P
Quick Change Plus (QC+) – Point of Operation Panels
Description
Fitting (in.)
Part No.
Price
1/8
RQC-P
$1604
Part No.
Price
High capacity oxygen
GC-1
$ 64
High capacity moisture
GC-2
$ 64
Indicating moisture
GC-2-I
$106
Hydrocarbon
GC-3
$ 64
Indicating oxygen
GC-4
$155
4-Head
O2, indicating O2, HC, H2O
Replacement Cartridges
Description
EASY ONLINE ORDERING
From oxygen traps to purification systems, you can find all your
gas management supplies … all in one place.
Just visit www.agilent.com/chem/4ecatalog
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•
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10
GAS MANAGEMENT
Super-Clean Gas Filter System
Super-Clean Gas Purification Systems
Super-Clean gas filter systems are
designed to provide the utmost in
convenience and contamination
reduction. The system is tested for
leak-tightness and the glass and metal
construction of the cartridges eliminates
diffusion of contaminants into the gas
stream. During cartridge replacement,
check valves and close off the system to
the atmosphere, further minimizing the
entry of contaminants.
Available with 1/8" fittings only
Description
Part No.
Price
Carrier Gas Purification System: Single
position system perfect for GC/MS,
ECD and NPD detectors. Includes the
triple filter cartridge.
5182-9704
$ 398
Super-Clean Gas Purification System:
For your most demanding GC application,
includes four position baseplate manifold
with four filter cartridges: oxygen,
moisture (both with indicator), and
two hydrocarbon cartridges.
5182-0816
$1291
Triple Filter Cartridge: A single carrier gas
filter now with hydrocarbon, moisture,
and oxygen trapping capability. Includes
moisture and oxygen indicator so you know
exactly when to replace the cartridge.
5182-9705
$ 186
Filter cartridge bundle of 4 (oxygen,
moisture, and 2 hydrocarbon)
5183-4770
$ 530
Replacement Filter Cartridges
Universal/External Split Vent Trap
Description
Part No.
Price
Universal/external split vent trap
with 3 cartridges
(1/8 in. Swagelok fitting)
RDT-1020
$ 94
Replacement cartridges (3/pk)
RDT-1023
$ 45
Split vent traps stop environmental
pollution. The split vent trap was designed
to protect the lab environment from the
contaminants released by split injection
systems, which can vent up to 500 times
the amount of sample reaching the
detector into the laboratory's air. A
replaceable, impregnated carbon filter
media traps and eliminates a broad range
of contaminants. The traps are also easy
to change and come with three packs of
replacement cartridges each. Replace
approximately every six months.
Split Vent Trap and Cartridges
11
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GAS MANAGEMENT
Regulators
Pressure regulators are an integral
component in any gas handling system.
Their function is to reduce the pressure
from a high pressure source, such as a
cylinder, to a suitable use pressure.
Although regulators are very good at
controlling pressure, they do not control
flow. They have a maximum flow rate
which is dictated by the design. Basically,
the flow is determined by the pressure
drop across the regulator.
Types of Regulators
There are primarily two types of regulators:
single stage and dual (or two) stage.
The difference is that a dual stage
regulator is actually two regulators
connected in a series.
Dual stage regulators provide more precise
and consistent pressure control than single
stage regulators. The reason is that in a
single stage regulator, as the gas cylinder
empties and the inlet pressure to the
regulator decreases (inlet decay), the
pressure on the diaphragm is reduced.
Without proper adjustment, the outlet
pressure might slowly rise.
A dual stage regulator overcomes this
problem by connecting two regulators
together. The first stage regulates the
pressure to the second stage, thus creating
a constant pressure and allowing minimal
inlet decay. Agilent recommends using
two-stage regulators with our GC Systems
to provide the proper pressure control for
optimal use.
Regulator Materials
Regulators are usually constructed of brass
or stainless steel. The choice of material
follows the same guidelines as the choice
of tubing. Generally, it is not recommended
that the materials be interchanged. If
stainless steel tubing were chosen due
to purity considerations, then a stainless
steel regulator should be chosen for the
same reasons. Steel regulators are more
expensive, which is why Agilent offers
brass regulators for less demanding
applications.
Brass Body Regulator
steel diaphragm regulators for most GC
applications. These regulators, combined
with the proper gas purification system,
provide proper gas pressure control and
purity for gas chromatography.
When ordering a regulator, be sure to
specify the proper connections. In the
US, most gas manufacturers follow CGA
connection guidelines. In Europe, there
are a number of organizations designating
cylinder connections that are specific to
individual countries. It is best to contact
your local supplier for the proper
connection designation.
No matter which material is chosen for the
regulator body, be sure to specify one with
stainless steel diaphragms for critical
applications such as use on carrier, fuel or
detector gases. Agilent recommends using
our economical brass body, dual stainless
Description
Part No.
Price
CGA 346, 125 psig max (8.6 bar), Air
5183-4641
$275
CGA 350, 125 psig max (8.6 bar), H2, Ar/Me
5183-4642
$275
CGA 540, 125 psig max (8.6 bar), O2
5183-4643
$275
CGA 580, 125 psig max (8.6 bar), He, Ar, N2
5183-4644
$275
CGA 590, 125 psig max (8.6 bar), Air
5183-4645
$275
Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
TIPS AND TOOLS
Regulator Outlet Adapters – Female NPT to Swagelok-style
1/4 in. to 1/8 in. brass
(included with brass regulators)
0100-0118
$ 14
1/4 in. to 1/4 in. brass**
0100-0119
$ 15
** Required for plumbing 1/4 in. tubing to regulators above
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•
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Always depressurize a regulator before closing by
adjusting knob and removing the regulator from the
cylinder.
12
GAS MANAGEMENT
Tubing
When constructing or maintaining a gas
delivery system for GC, choosing the
proper tubing material is very important
and will help to eliminate potential
problems and improve the overall quality of
the gas system. Although there are many
common tubing materials available, some
pose safety or cleanliness problems.
Spectra-Link Tubing Connecting System
on a two-stage regulator
Non-metallic types of tubing such as
polyethylene and Teflon are not
recommended for GC applications due
to their gas permeability and difficulty
in cleaning. This type of tubing can be
used for non-critical applications, such
Determining Tubing Length
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig
Tubing Type
Diameter
(inches)
Recommended
Max. Length (feet)
Pressure Drop
(psig)
Copper
1/8*
50
2
Copper
1/4*
300
0.5
*Recommended when multiple instruments are connected to the same source
In view of these problems, the list of
appropriate tubing materials has been
narrowed down to two: copper and
stainless steel. Agilent recommends using
copper tubing for most applications, since
it is easy to bend and plumb and is less
expensive than stainless steel. Use
stainless steel tubing only for crucial
applications that require very high purity,
or where building codes mandate its use.
Cleaning Tubing
Before any tubing is placed into service,
or if it becomes contaminated with use,
it is essential that it be properly cleaned.
Unclean or improperly cleaned tubing can
lead to contamination of the system with
disastrous results.
Cleaning tubing requires the use of
suitable detergents and solvents along
with nitrogen and a purgeable oven for
drying. This may be done easily for small
lengths of tubing, but in larger systems the
cleaning procedure sometimes becomes
unwieldy, leaving behind a large quantity
of solvent requiring proper disposal.
Fortunately, Agilent provides clean, high
quality GC grade tubing for large systems
as an economical alternative.
Tubing–Precleaned
Description
as pressurizing pneumatic lines; however,
be aware of its pressure limitations.
Part No.
Price
Copper tubing, 1/8 in., 50 ft.
5180-4196
$56
Copper tubing, 1/8 in., 12 ft.
5021-7107
$28
MAINTENANCE MINDER
Always replace cylinders at around 500 psi, to reduce the risk of having
a drastic pressure drop right in the middle of an important analysis.
13
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•
800 227 9770
GAS MANAGEMENT
Spectra-Link is No Ordinary Flexible Tubing!
• Stainless Steel: no outgassing or permeation through polymeric materials
• Quick Connection: prevents air from entering gas lines during tank changeover
• Tested: each system has leak rates lower than 1x10-5 cc/sec
Description
Part No.
Price
Spectra-Link with 1/8 in. fittings
and 36 in. SS tubing
SL-8
$496
Spectra-Link with 1/4 in. fittings
and 36 in. SS tubing
SL-4
$496
Part No.
Price
5183-1941
$ 60
Cylinder Bracket
Description
Cylinder wall bracket with strap and chain
(cylinder size up to 14 in., 35 cm)
Cylinder Wall Bracket
Leak Detection
Leaks allow oxygen and other
contaminants to enter the gas stream.
Therefore, GC instrument maintenance
should include checking fittings and
connections with a gas leak detector.
Agilent’s Gas Leak Detector enables quick
and easy detection and measurement of
gas leaks for 12 common gases. Based on a
dual cell micro volume thermal conductivity
system, this unit provides very high
sensitivity and eliminates contamination
caused by soap solution methods.
Gas Leak Detector Kit
Description
Part No.
Price
Leak detector includes probe, extended flexible probe, range extension nozzle,
probe clip and template, cable, AC power adapter/battery charger, battery, user
manual, cleaning wipe, and carrying case (available in 115 V or 220 V).
Gas leak detector, 115 V
5182-9646
$1915
Gas leak detector, 220 V
5182-9648
$1915
Gas Leak Detector
www.agilent.com/chem
•
800 227 9770
14
GAS MANAGEMENT
Flow Rates
Setting and maintaining GC flow rates
greatly affect the instrument accuracy
and sensitivity. During maintenance,
verify carrier and support gas flows
with the proper flowmeter. Choosing a
flowmeter for your application depends
upon measurement speed, ease of use,
accuracy, and flow rate range.
Selecting a Flowmeter
Agilent manufactures the largest selection
of volumetric and mass flowmeters for
chromatography. We have developed
flowmeters for measuring capillary column
flows, calibrating air pumps and flow
controllers, and verifying instrument gas
flows. All flowmeters are calibrated to
NIST-traceable standards.
FlowTracker Flowmeters – volumetric, multimode flowmeters
Description
FlowTracker 2000
Part No.
Price
FlowTracker 1000 Flowmeter
5183-4779
$ 816
FlowTracker 2000 Flowmeter and
Leak Detector
5183-4780
$1143
FlowTracker Universal AC Adapter (optional,
not supplied with FlowTracker units)
5183-4781
$ 43
ADM 1000 features include:
ADM 2000
• Accuracy ± 3%
In addition to the features of the ADM
1000, the ADM 2000 includes:
• Operating temperature range–
0 to 45ºC for the instrument, -70 to
135ºC for the tubing
ADM 1000
• Calibration–traceable to NIST primary
standards
• Real time, split ratio measurement
• CE mark certified
• Mass flow measurements–measure flow
rate, independent of atmospheric
pressure and temperature (calculated)
• Data output through RS-232 port
• 9V battery and AC power adapter
(120 or 220 VAC)
• 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
15
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•
800 227 9770
GAS MANAGEMENT
Flowmeters
Flow Rate (mL/min)
Low
High
Description
Gases
Measured
Accuracy
(%)
Power
Supply
RS-232 Data
Output
Part No.
Price
220-1170
$620
ADM Flowmeters – volumetric, measures all gases*
ADM1000
0.5
1000
All
±3
9V Battery
None
ADM2000
0.5
1000
All
±3
Battery or 120 VAC
Yes
220-1171-U
$725
ADM2000E
0.5
1000
All
±3
Battery or 220 VAC
Yes
220-1171-E
$725
Electronic Mass Flowmeter – dedicated mass flowmeter, very accurate for specific gases*
Veri-Flow 500
(110 V)
5.0
500
He, H2, Ar/CH4
N2, Air
±3
Rechargeable Battery
or 110 VAC
Yes
HVF-500
$681
Veri-Flow 500
(220 V)
5.0
500
He, H2, Ar/CH4
N2, Air
±3
Rechargeable Battery
or 220 VAC
Yes
HVF-500-2
$681
Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters**
Optiflow 420
0.1
50
All
+/- 3
9V Battery
None
HFM-420
$573
Optiflow 570
0.5
700
All
+/- 3
9V Battery
None
HFM-570
$573
Optiflow 650
5.0
5,000
All
+/- 2
9V Battery
None
HFM-650
$677
*non-corrosive gases only
**non-corrosive and mildly corrosive gases only
Veri-Flow 500
Optiflow 420
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom,
even at your site. See pages 104-115 for more information about our
services and support.
www.agilent.com/chem
•
800 227 9770
16
You asked … we listened!
Announcing the launch of
our new Life Sciences and
Chemical Analysis website.
Based on customer feedback, we’ve rebuilt our site navigation
and layout to help you more quickly find the information you
need about Agilent products and services.
The new site features:
• A coherent page design – that automatically detects
screen resolution and optimizes the page size for
less scrolling.
• An expanded navigation – that includes links to
product literature, technical support, education,
events, and news.
• A newly designed online store – with fast access to
pricing, order status, quotes, and local sales information.
• Direct links – to the services, parts, and consumables that
keep your instruments running in top condition.
To experience these exciting new changes for yourself, go to www.agilent.com/chem.
Sample
Introduction
Gas
Management
Consumables &
GC Inlets
The use of quality carrier gases is essential
for consistent and accurate GC analyses.
Proper
management
is key
to achieving
Agilentgas
offers
a wide range
of high-quality
this
goal.vials,
Agilent
provides
a diverse
sample
septa,
syringes,
liners line
and of
high
quality
gas
management
products
inlets for a broad range of gas-phase – gas
purifiers,
regulators,
applications.
Just asleak
youdetectors
depend on our
and
flowmeters
– all designed
to prevent
meticulously
engineered
GC and
GC/MS
column
damage,
detector
life, and
instruments,
youimprove
can count
on Agilent
improve
the
quality
and
consistency
of your
consumables. This section reviews these
GC
separations.
This section
explains
how
critical
components.
Also, look
for useful
common
moisture
infofrom contaminants
proper syringelike
useoxygen,
and cleaning
and
hydrocarbons
can damage
your GC
techniques
to a detailed
discussion
on
column,
and
helps
you
understand
how to
optimized inlet settings.
prevent it. Also, look for practical information
about regulators, the importance of clean
GC-tubing, and minimizing the likelihood
of GC system contamination.
“Good sample introduction helps ensure
good reproducibility, optimal peak shape,
and accurate sample delivery. Agilent’s
commitment to offering the highest quality
supplies means accurate, reliable results.
Time after time.”
Bryan Bente, Ph.D.
Technology Development Manager
CATALOG
For a complete selection of vials, syringes, and inlets, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
•
800 227 9770
18
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Sample Introduction
Vials
Vial Filling
Agilent’s wide opening vials are designed
specifically for analyzing samples with your
GC. They have specially designed vial neck
angles, bottom design and height to ensure
compatibility with Agilent autosamplers
with rotating or robotic arm trays. Agilent
offers a large variety of autosampler vials
in different closures, cap colors, septa
choices and package options. Agilent also
offers convenience packs with 500 vials
and caps in a reusable blue storage box.
When filling sample vials, keep in mind:
For small sample sizes, Agilent offers a
variety of options. You can use microvolume
inserts with the wide opening vials or, for
added convenience, use vials with small
volume capacity.
• if you need to test a large amount of
sample over repeated injections, divide
the sample among several vials to obtain
reliable results
• when sample volume in the vial is low,
contaminants from the previous sample
injection or solvent washes may have a
greater impact on the sample.
The airspace in the vial is necessary to
avoid forming a vacuum when sample
is withdrawn. This could affect
reproducibility.
Vial Options
Glass–for general purpose
use and for use with acids
Silanized–for use with
samples that bind to glass,
and for trace analyses
Polypropylene –for use
with alcohols and aqueous
solvents
Amber Vials–for use with
light-sensitive samples
Microvolume Inserts–for High Recovery Vials–
use with very small sample for use with limited sample
volumes
volumes
Recommended fill volumes for sample vials
1 mL
50 µL
3.6 mm*
100 µL vial
*Needle position based on standard sampling depth.
TIPS AND TOOLS
Do not inject air into the vials to prevent the vacuum.
This often damages the cap seal.
19
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Selecting Vial Septa Materials
Vial cap septa are critically important
to optimal analysis. Each septum
complements the overall system and
enhances chemical performance.
Agilent’s vial cap septa are specifically
formulated and constructed for optimum
system performance, with minimal coring
and superior chemical inertness.
Red Rubber/Teflon
Determining Your Quantity Needs
To determine potential septa ordering
quantities, consider:
• the number of samples run during a
day/week
Silicone/Teflon
• if samples are run in small or large
batches
• Excellent resealing
• Resists coring
• Good for multiple injections
• if samples are run manually or with an
autosampler
• if samples are run overnight, unattended
Unattended autosampler
runs require a precise fit for
uninterrupted operation.
Typically, automated sample
runs use a higher quality and
quantity of vials.
Teflon/Silicone/Teflon
• Used in trace analysis applications
• Above average resealing
• Most resistant to coring
• Least evaporation
• Use with large diameter, blunt tip
syringe needles
Teflon Disc
• Good for MS and ECD analysis
• Good for large-volume injections
• Chemically inert
• No resealing
• Single injection
• No long-term sampling storage
Viton
• Chlorinated solvents
• Organic acids
• Limited resealing
• Not suitable for 32 gauge syringe
www.agilent.com/chem
•
800 227 9770
TIPS AND TOOLS
• Routine analysis
• Moderate resealing
• Excellent chemical inertness
• Not recommended for multiple
injections or storage of samples
• Least expensive
Vials
Description
Quantity
Part No.
Price
2 mL Crimp top vial convenience
pack with silver AI caps with
Teflon/Red rubber septa
500/pk
5181-3400
$115
2 mL Screw top vial convenience
pack with blue screw caps and
Teflon/Red rubber septa
500/pk
5182-0732
$183
2 mL Snap top vial convenience pack
with clear polypropylene snap caps
and Teflon/Red rubber septa
500/pk
5182-0547
$154
100 µL Insert for wide opening vials
100/pk
5181-1270
$ 88
250 µL Polypropylene flat bottom inserts 500/pk
5183-2087
$ 57
100 µL Glass lined polypropylene vials
100/pk
9301-0977
$158
Less than 5 µL dead volume,
Micro-V vial, clear crimp top
100/pk
5184-3551
$ 69
30 µL reservoir volume, High recovery
vial, crimp top
100/pk
5182-3454
$109
Vials
20
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Syringes
Selecting Syringes
Syringe type and design are important for
chromatography to ensure reproducible
sample injections for consistent results.
The Agilent line of syringes include a
variety of plunger and needle choices
to use with your autosamplers.
1. Select the syringe type based on the
inlet (injection port) you are using and
the volume of sample you want to inject.
2. Select a syringe. Refer to your automatic
liquid sampler operating documentation
for available syringe sizes and
corresponding injection volumes.
Agilent syringes are designed:
• for reproducible sample volume delivery
• specifically for the Agilent inlet or
autosampler
• to maximize inlet septum lifetime
3. Select the appropriate syringe
needle gauge.
Needle Gauge Selection
Inlet
Needle Gauge
Column Type
Packed, split or
splitless (including PTV)
23 gauge or 23/26 gauge tapered
any
Cool on-column
23/26 gauge tapered or 26 gauge
530 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 dualtaper needle or a conical tip. Sharp-tipped
needles tend to tear the inlet septum and
cause leaks. Also, a sharp-tipped needle
tends to leave residual amounts of sample
on the septum as it exits, resulting in a
large solvent tail on the chromatogram.
TIPS AND TOOLS
For best results, use the Agilent Cone Tip (HP Point Style) with
Agilent’s Centerguide Septa, page 38.
21
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Syringe Characteristics and Recommended Uses
Syringe
Advantage
Limitations
Recommended Use
5 µL, fitted
plunger
• Most accurate
• Thinnest plunger, • 1 µL injections
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
plunger
• Most economical
• Most reliable fitted
plunger syringe
• Less bending
• Better for high
viscosity samples
10 µL,
gas-tight
• Replaceable plunger • More expensive
• Dirty samples
for reduced
than fitted plunger • Gases and volatile
repair cost
• Not available in
samples
• Less plunger binding 5 µL size
• Reactive samples
than fitted plunger
• Tight seal between
plunger and barrel
• Most accurate only • General purpose
for 1 µL and larger syringe
injections
• Clean samples
• Plunger not
• Routine analysis
replaceable
Replacing On-column Syringe Needles
The stainless steel needles used for
250-µm and 320-µm injections must
be inserted into a glass syringe barrel.
Select the correct size needle for the
column you plan to use.
To insert a needle into a syringe barrel:
1. Unscrew the syringe barrel cap and
remove the spring.
2. Make sure the needle has the Teflon
disk. If the syringe barrel does not
have the Teflon disk, use the instructions
in the syringe box to wrap the needle
yourself.
3. Slide the spring and the cap down over
the needle.
4. Insert the needle into the syringe barrel.
5. Screw the cap back on the syringe barrel.
TIPS AND TOOLS
Failure to use an on-column syringe when injecting into
an on-column inlet could damage the injector, syringe and column.
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800 227 9770
22
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Syringe Tips
• Make sure to input the proper syringe
size when setting up the injection section
of your data handling device.
• Rinse syringes and clean their plungers
before use to maximize syringe lifetime.
• Rinse the syringe 5-8 times between
injections to minimize sample carryover.
• Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
• Remove a gas-tight plunger from the
syringe for long-term storage to keep the
Teflon tip leak-free. If a gas-tight plunger
does not fit properly, place it in hot water
for about 10 minutes then press the tip
uniformly on a clean, hard surface and let
cool to room temperature. The plunger
should reseal correctly to provide 10-25%
more injections.
• To maximize the lifetime of standard
plungers, rinse the syringe and wipe
the plunger with solvent (isopropanol
or acetone) and a lint-free wipe, as
specified in the syringe cleaning
procedure included with each syringe.
• A 26-gauge syringe can be used for
on-column injections into a 0.53mm id
column. Always check that on-column
syringe needles fit inside the capillary
column before installing the column
and syringe in the GC.
• For on-column injections, always use
the proper septum nut and stainless steel
insert for the column dimension you are
using. Use a septum with a molded
through-hole with injections onto 0.32mm
and 0.25mm columns.
• The more polar the solvent, the more
likely it is to contain water. Trace
amounts of water, especially when
combined with water-extractable
materials from samples, can accelerate
syringe wear dramatically. With these
types of samples, use a Teflon tipped
syringe plunger. Even better, proactively
replace syringes, since plunger bends
may be inevitable.
NEW! Agilent Gold Standard
GC Autosampler Syringes
see page 25
VIDEO
To view a video on syringe installation,
visit www.agilent.com/chem/techsupport.
23
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Syringe Troubleshooting Guide
Proper care, cleaning, and handling of each syringe will help ensure correct performance and long life. When cleaning your syringe,
it is best to use solvents that effectively dissolve the sample you are working with. Try to avoid cleaning agents that are alkaline,
contain phosphates, or are strongly acidic.
Problem
Possible Cause(s)
Suggested Action(s)
Bent plungers or stuck syringes
• Particles such as dust, leftover samples, salts,
metal, or glass can fill the narrow gap between
the plunger shaft and the inside wall of the
barrel.
• If the plunger’s movement feels “gritty,”
remove the plunger from the barrel, flush the
shaft with solvent, and wipe it dry with a lintfree cloth. Then, carefully insert the plunger
back into the barrel. Finally, submerge the tip
of the needle into a container of solvent, and
cycle the plunger to pull the solvent into and
out of the barrel.
• Never cycle the plunger in a dry syringe.
• Do not “mix & match” plungers and barrels.
• Always clean syringes after use.
Bent needles
• Narrow-gauge needles (26 gauge) bend more
easily than larger (23 gauge) needles.
• Use only Agilent autosamplers. They are
precision-designed to ensure proper
alignment with the syringe needle.
• Needles tend to bend when inserted into the
sample vial – not the inlet port. This can be
caused by septa that are too “tough.”
• Use 23 to 26-gauge tapered needles to get
the combined benefits of greater septa life
and fewer bent needles.
• If the needle has been slightly bent when
mounted in the autosampler – or when the
syringe is installed into the autosampler – then
it is more likely to bend further when it pushes
through the septa on the sample vial caps.
• Only use Agilent vials and septa.
• Sample material or contaminants may be
trapped inside the needle.
• Remove the plunger and use a second
syringe to fill the blocked syringe with
solvent. Then, insert the plunger and gently
push solvent through needle. Important: Try
to use a cleaning agent that is appropriate for
the contaminant. Common choices are
methanol, methylene chloride, acetonitrile,
and acetone.
• Improper needle alignment.
Blocked needles
• The needle may not have been properly cleaned.
Rust
Note: even minor rust can cause the plunger
to become stuck in the barrel.
• During normal use, the shaft rubs against the
glass walls of the barrel. This gradually wears
away the rust-resistant metal on the shaft’s
surface.
• Rusting happens most rapidly when using water
or solvents that may contain (or absorb) water.
“Ring around the neck” (A dark ring between
the top of the barrel and the end of the
volume scale.)
• Skin oils and other organic material.
Loose plungers – accompanied by syringe
leaks and area count reproducibility problems.
• The syringe is nearing the end of its useful life.
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•
800 227 9770
• Fine metal and glass particles from the syringe
plunger and barrel may be rubbing together.
Once this happens, the plunger may bend if
used further.
• To slow this process, remove the water from
the syringe at the end of each day.
1. Rinse the syringe several times with a “dry”
solvent, such as acetone.
2. Remove the syringe from the autosampler,
and wipe the plunger dry with a lint-free
cloth
3. Let syringe and plunger air dry.
• Never touch the plunger shaft with your
fingers.
• If build-up appears when water is the
solvent: rinse syringe with acetone and wipe
the plunger clean at the end of each day.
• Replace the syringe.
Note: Plungers normally feel “loose” when
non-polar solvents (like hexane and toluene)
are used.
24
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Gold Standard GC Autosampler Syringes
Description
Gauge/Length
Quantity
Part No.
Price
Tapered Needle Syringes
(use for split/splitless or on-column injections with 0.53 mm id columns)
10 µL
Tapered
Fixed Needle
23-26s/42
6/pk
5181-3360
$198
5 µL
Tapered
Fixed Needle
23-26s/42
6/pk
5181-8810
$303
10 µL
Straight
Fixed Needle
23/42
6/pk
9301-0725
$191
5 µL
Straight
Fixed Needle
23/42
6/pk
5182-0875
$292
Straight Needle Syringes
(use with Merlin Microseal)
GC Automatic Liquid Sampler Supplies
Description
Unit
Part No.
Price
4 mL Clear screw top wash vials
with screw caps (no Septa)
144/pk
9301 0723
$ 64
Gold Standard GC
ALS Syringe Features
Septa for 4 mL vial
144/pk
9301-1031
$ 21
Lot Numbers ensure certified
performance to all specifications
Diffusion caps for 4 mL vials
12/pk
07673-40180
$ 19
4 mL wash vial with fill marking, caps
25/pk
5182-0551
$ 26
Screw for mounting syringe
07673-20570
$ 13
Quadrant kit (4 tray sections)
18596-40015
$ 75
Miscellaneous Autosampler Supplies
7673/83 Basic Supply Kit contains:
10 mL syringes (6/ea), 23/26 gauge
needles, 4 mL vials with diffusion caps
(144/pk), 2 mL automatic sampler
vials with screw caps (1,000/pk),
GC septa (25/pk), Vial racks (5/pk)
25
Gold protective cap prevents chipping
of the glass syringe barrel as it contacts
the septum retainer nut
Black ink and gold illuminating backdrop
for easier viewing of the volume scale
Individually sealed packaging for
contaminant-free use
07673-60840
$755
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Packed-Column Inlets
Packed-column direct inlets are very
popular. Packed-column analysis is
frequently done when high efficiency
separations are not needed or when gases
are analyzed by gas-solid chromatography.
Packed-column inlets are simple in both
design and use. Few parameters need to
be set, and all carrier gas flow flushes
through the inlet into the column in the
standard configuration.
Packed-Column Inlet Procedures/Practices
Parameter
Selection/Setting
Rationale
Inlet temperature
BP of solvent +50˚C
BP of major solute(s)
Ensures flash vaporization
Use for neat samples
Insert type
1/8-inch stainless steel
1/4-inch stainless steel
Use for ss column only
Inserts permit connection of
columns up to 1/4-inch od.
Liner
Glass
Use to lower activity
(replaceable)
Initial column
temperature
temperature programming
Sharpens peaks and
reduces run time
Column type
1/8-inch packed stainless
1/4-inch packed glass
Will not break
Better for polar or labile
compounds
Carrier gas flow
20-40 mL/min
30-60 mL/min
Use with N2 carrier gas
Use with He or
H2 carrier gas
Troubleshooting
Most problems with packed-column inlets
involve sample decomposition, flashback,
or leaks.
Decomposition
Since packed-column inlets are active,
especially if glass liners are not used, polar
sample components will often tail or
degrade in the inlet. Sample decomposition
caused by the inlet is easily diagnosed; the
decomposition products will have peaks at
the same retention times as standards for
the decomposition product.
When inlet-caused decomposition is
suspected, try intracolumn direct injection,
deactivated glass liners, or lower inlet
temperatures, and remove any column
packing in the inlet zone.
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•
800 227 9770
The inherent activity of packed-column
inlets is somewhat mediated by the fact
that they usually have low internal volume.
When this is coupled with the relatively
fast flow rates used with packed columns,
the residence time of sample in the inlet is
short and decomposition is reduced in
comparison to the decomposition that
occurs with some capillary inlets (for
example, splitless inlets).
Flashback
The negative side of low inlet volume,
however, means that excessively large
sample injections will easily exceed the
capacity of the liner and will flash back into
gas supply lines and onto the septum. This
can cause several maladies, including
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.
Leaks
Since packed-column inlets are usually
flow-controlled, septum and column leaks
will have a direct impact on retention times
and peak areas. Sample can be lost
through the leak holes, and air can diffuse
back into the inlet to cause column
degradation. Change the septum on a
regular basis and check column
connections at the first stage of problems.
To prevent stationary phase decomposition,
make sure that the oven and inlet are at
room temperature when not in use and
when changing the septum.
26
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
6890/6850 Series GC Packed Port Supplies*
Item
Description
1
Septum nut
2
Septa Bleed temperature,
optimized, 11 mm
Unit
Part No.
Price
18740-60835
$ 37
1
2
3
4
50/pk
5183-4757
$ 67
19243-80570
$132
3
Top insert weldment
4
Viton O-rings
12/pk
5080-8898
$ 12
5
Glass liner, disposable
25/pk
5080-8732
$ 37
Glass liner, disposable/deactivated
5/pk
5181-3382
$ 14
6
Vespel/graphite ferrules, 1/4 in. id
10/pk
5080-8774
$ 42
7
Tubing nut, 1/4 in. brass
10/pk
5180-4105
$ 13
Liner
Adapters with glass liners
8
0.53 mm column adapter
19244-80540
$119
1/8 in. column adapter
19243-80530
$ 99
1/4 in. column adapter
19243-80540
$141
Upper insulation
19243-00067
$ 5
7
10
Nut warmer cup with insulation
19234-60720
$ 54
8
11
Column nut for 0.53 mm column
5181-8830
$ 25
5
6
9
2/pk
1/4
Vespel/
1/4 in.
in. Vespel/
graphite
ferrule
graphite ferrule
1/4
nut
1/4 in.
in. nut
Inside ofof
Inside
OvenOven
For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
* For Model 6890/6850 only
1/8 in.
1/8
in.oror1/4
1/4in.in.
stainless steel
linerliner
stainless
steel
9
10
11
5890 Packed-Column Inlet Supplies
Description
Unit
Part No.
Price
19243-60570
$100
1/8 in. column adapter
19243-80510
$ 88
1/4 in. column adapter
19243-80520
$128
19243-60505
$ 70
5180-4105
$ 13
Nonpurging septum nut assembly
for manual flow control only, not EPC
TIPS AND TOOLS
Adapters without glass liners
27
Tap Agilent’s GC knowledge over the phone,
online, in the classroom, even at your site.
See pages 104-115 for more information
about our services and support.
Universal Packed-Column Inlet (non-purged)
Septum retainer nut for
headspace sampling, nonpurging
Brass nut, 1/4 in.
10/pk
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Split/Splitless Inlets
The combined “split/splitless” inlet is the
most popular inlet for capillary column gas
chromatography. Because it can be used in
either split or splitless mode, it provides a
very effective combination that can cover
most analysis requirements.
Split Mode
Split injection is an effective way to
introduce small amounts of sample without
overloading the column. Split injection is
required for samples that:
• cannot be diluted for analysis (for
example, solvents)
Troubleshooting
Split inlets are spared from most bandbroadening phenomena, since narrow
peaks are generated as part of the splitting
process. Therefore, any peak broadening
or tailing observed with split injection is
usually due to improper column
installation, low split flow, (<20 mL/min
on 6890) or low inlet temperature. If you
suspect that the inlet temperature may be
too low, increase it by 50˚C and compare
the results to the lower temperature
analysis. Repeat if results are positive
until no further improvement is seen.
A majority of the problems encountered
with split inlets are related to discrimination
and decomposition. Both analytical
accuracy and reproducibility decrease
with the increases in discrimination
and decomposition. Split inlets suffer
from both needle discrimination and
inlet discrimination.
• are gases that cannot be focused, or
that have long injection times (valve
injections)
• have important minor peaks eluting
directly before the solvent peak (as in
solvent analysis)
Split injection is also good for screening
samples of which little is known or for
those that have widely differing
concentrations, since the split ratio
can be adjusted easily. Split inlets are
also a good choice for dirty samples.
Split Mode Variables, Practices, and Rationales
Parameter
Selection/Setting
Rationale
Inlet temperature
Try 250˚C or BP of
last eluting compound
Ensures flash vaporization
Minimizes inlet discrimination
Inlet liner
Large volume, deactivated
Minimizes flashback
Minimizes degradation
Inlet packing
Silanized glass wool
Glass beads or frit
None
Retains non-volatiles
Minimizes inlet discrimination
Less active than wool
Least active
0.5-3 µL liquid
0.10-10 mL gas
Split easily adjusted
Split adjusted accordingly
Injection volume
Injection technique Fast autoinjection
Hot-needle fast manual
injection
Less needle discrimination
Reproducible discrimination
Split ratio
50:1 to 500:1
Depends on sample and
injection volume, and column ID
Initial column
temperatures
Not critical
Narrow initial peaks
Septum purge
2-3 mL/min
Minimizes ghosting
TIPS AND TOOLS
For fast and easy liner changes, check out Agilent’s new Flip Top Inlet Sealing System on page 52.
www.agilent.com/chem
•
800 227 9770
28
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Split Mode Variables, Practices, and Rationales
Parameter
Selection/Setting
Rationale
Inlet temperature
Just above highest
boiling point of
solutes (+20˚C)
Ensures flash vaporization
Reduce if degradation occurs
Use higher for dirty samples
and higher-boiling solutes
Inlet liner
Large volume >0.8mL
Small volume <0.2mL
Use with autoinjector
Use only for slow manual
injections, and gas injections
Inlet packing
None
Use only with slow injection
Decreases degradation
Silanized glass wool
Use for fast autoinjection
& dirty samples
0.5-2 µL liquid
Depends on solvent, liner,
& conditions
Injection volume
Injection technique Fast autoinjection
Most reproducible
Less needle discrimination
Hot-needle slow manual Inject 1-2µL.sec if narrow liner
is used and >1µL injection
Hot-needle fast manual Use for <1µL injections
Purge flow
20-50 mL/min
Higher if using constant flow
Purge delay time
20-80 sec
Adjust according to column
flow rate/liner type
& sample conditions
Oven temperature
10-25˚C below solvent BP Necessary for solvent focusing
Column flow
>2mL/min when possible Clears inlet fast
Reduces backflash and
decomposition
Splitless Mode
For splitless injection, a conventional split
injector is operated in a nonsplitting mode
by closing the split valve during injection.
The sample is flash-vaporized in the liner,
and sample vapors are carried into the
column by the carrier gas where they are
recondensed at temperatures below the
boiling point of the solvent. After most of
the sample has been transferred into the
column, vapors remaining in the liner are
cleared by opening the split vent which
remains open for the duration of the run.
The most important benefit of splitless
injection is that a majority of the injected
sample is introduced into the column. This
results in much higher sensitivity than that
achieved using split injection.
Solvent Effect
One requirement of splitless injections is
that the initial column temperature should
be kept at least 10˚C below the boiling
point of the sample solvent. This allows
the sample solvent to condense at the
front of the column trapping the solvent
molecules into a tight, narrow band.
Additionally, use a solvent that is similar in
polarity to the column stationary phase,
and avoid mixed solvents. Breaking these
rules may result in split peaks.
Splitless injection is routinely used in
areas such as:
• environmental analysis
Septum purge
2-3mL/min
Reduces ghosting
• pesticide monitoring of foods
Quantification
Internal standard
Standard addition
Maximizes reproducibility
Use only with constant
injection volume
• drug screening
1-3m, deactivated
(1-2m per µL injected)
Reduces peak distortion
Promotes solvent and
stationary phase focusing
Retention gap
In these applications, sample preparation
requirements are significant, and it is not
always possible or economically justifiable
to clean up a sample extensively. So
column protection becomes as important
as sensitivity. Also, samples with trace
quantities of important solutes that elute
on the solvent tail may be focused by the
solvent to yield more sensitive analyses.
VIDEO
To view a video on liner and gold seal replacement, visit
www.agilent.com/chem/techsupport.
29
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Troubleshooting
Most problems encountered with splitless
injection are related to incorrect purge
time, degradation, improper focusing, and
flashback.
Appropriate initial column temperature is
critical. Sample vapors can be lost through
the septum purge line if the insert is
overfilled with sample vapor (either too
large injection volume or too small liner
volume), leading to irreproducibility and
nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
volume carefully to avoid backflash.
Decomposition
Loss of peak area or generation of new
peaks, can sometimes be dramatically
reduced by changing liner type or by
deactivating the liner and inlet with
silanizing reagents. Removing or reducing
the amount of liner packing can also
decrease inlet activity.
6890/6850 Split/Splitless Inlet Supplies*
Item
1
2
3
4
6
Description
Unit
Price
$ 39
1
Septum retainer nut
18740-60835
2
Septa
See page 36
3
Insert Weldment
G1544-60575
4
Liner O-ring
See page 52
5
Liner
See page 47
6
Split vent trap assembly (6890/6850 only)
G1544-80550
$128
7
Retaining nut (6890/6850 only)
Retaining nut (5890 only)
G1544-20590
19251-20620
$ 26
$ 31
8
SS seal
Gold-plated seal
18740-20880
18740-20885
$ 26
$ 33
9
Washer, 0.375 in. od
5061-5869
$ 8
5
12/pk
$216
10
Reducing nut
18740-20800
$ 34
11
Insulation (requires 3)
19243-00067
$ 5
12
Lower insulation cover
19243-00070
$ 15
13
Ferrule
14
Column nut (6890/5890 only)
2/pk
5181-8830
$ 26
Column nut (6850 only)
2/pk
5183-4732
$ 47
19251-00100
$ 29
Angled wrench for split/splitless inlet
7
Part No.
* For a complete parts breakdown, see the 6890/6850 Series GC Instrument User and/or Service Manuals.
8
9
10
TIPS AND TOOLS
11
12
A guard column or retention gap is often beneficial for splitless injections,
improving peak shape and extending column life when analyzing dirty samples.
(See page 61).
13
14
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•
800 227 9770
30
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Cool On-Column Inlets
Cool on-column injection is superior in
many ways to other sample introduction
techniques.
Advantages:
• elimination of sample discrimination
• elimination of sample alteration
• solvent focusing of early eluting solutes
• high analytical precision
If done properly, cool on-column injection
provides the most accurate and precise
results of the available inlets. Syringe
discrimination is completely eliminated.
Moreover, inlet-related discrimination does
not occur, since the liquid is introduced
directly into the column. Automated oncolumn injection provides even higher
analytical precision. Add to this the
elimination of thermal decomposition and
rearrangement reactions, and it becomes
apparent that cool on-column injection
should be considered whenever high
precision and accurate results are required.
Limitations:
• maximum sample volumes are smaller compared
with other inlets (0.5 µL to 2.0 µL)
• solute peaks eluting just before the solvent
cannot be focused and are difficult to determine
• capillary columns (especially those with a large
phase ratio or small inner diameter) can be easily
overloaded with sample
• parameters such as initial column temperature,
solvent nature, and injection rate must often be
optimized
Cool On-Column Inlet Procedures/Practices
Parameter
Selection/Setting
Rationale
Initial inlet temperature
= or 3˚C above column oven temperature
Ensures sample focusing in solvent front
Initial inlet temperature ramp
Same as oven (oven track) Faster than oven
Simple and effective
Narrows initial peak width
Injection volume
0.1-2.0 µL liquid
Use smaller injections for small id columns;
Depends on column capacity
Injection technique
Fast autoinjection
Fused silica needle
Projects droplets away from syringe tip
Use for manual injection into small id columns
Oven temperature
Inlet temperature or slightly lower
Prevents backflash
Column flow
50-80cm/sec
30-50cm/sec
Use for H2 carrier gas
Use for He carrier gas
Septum purge
12-15mL/min
Use if installed to prevent ghosting
Quantification
All methods
Inherently reproducible technique
Lack of discrimination
Retention gap requirements
1-3m, deactivated
Corrects peak distortion
Protects column from non-volatile components
Permits autoinjection with narrow-bore columns
TIPS AND TOOLS
Since the sample is directly deposited into the column, nonvolatile sample components
can accumulate at the head of the column and will degrade efficiency and/or interact with
subsequent injections.
31
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Sample Considerations
Troubleshooting
Sample preparation is important for
on-column injection because of:
The major problems found with cool oncolumn injection are associated with
column overload, solvent/stationary phase
incompatibility, and column contamination.
• the potential for column overload,
column contamination,
• the incompatibility of some solvents
with the stationary phase,
• dependence of the initial column
temperature on the boiling point of
the solvent.
Many of the problems associated
with these variables can be resolved
by using a retention gap ahead of the
analytical column.
If the flooded zone after injection is too
long (large injections, poor wettability),
peaks will be broad or split. A retention gap
usually will resolve this problem. Loss of
column efficiency with on-column injection
usually is caused by contamination or
degradation of the stationary phase at the
head of the column. Only columns with an
immobilized stationary phase should be
used with cool on-column injection to
prevent displacement of the stationary
phase by solvents.
Immobilized stationary phases can be
washed to remove contaminants and
renew performance. If column performance
does not improve after washing, cut 0.5m
off the inlet side of the column. If that does
not return column performance, the
column must be replaced and a retention
gap should be used for all further injections
of dirty samples.
Column/Retention Gap Installation Consumables
Description
Unit
Part No.
Price
Column nut
2/pk
5181-8830
$ 26
250 µm graphite/Vespel ferrule
10/pk
5181-3323
$ 55
320 µm 0.5 mm graphite/Vespel ferrule
10/pk
5062-3514
$ 51
250 µm retention gap (one 5 m piece)
160-2255-5
$ 39
320 µm retention gap (one 5 m piece)
160-2325-5
$ 42
530 µm retention gap (one 5 m piece)
160-2535-5
$ 59
5181-3396
$ 94
Quartz deactivated column connector fits 0.18-0.53 mm
5/pk
TIPS AND TOOLS
Sample degradation can occur with cool on-column injection if column
or retention gap activity is high. Use only well-deactivated retention
gaps and high quality capillary columns from Agilent.
VIDEO
To view a video on cool on-column installation and septum replacement,
visit www.agilent.com/chem/techsupport.
www.agilent.com/chem
•
800 227 9770
32
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
6890 Series Cool On-Column Inlet Supplies*
Item Description
Unit
Part No.
Price
1a
Manual injection
1c
Cooling tower assembly
1d
Duckbill septum
Fused silica syringe needles
19320-80625
$175
10/pk
19245-40050
$ 29
6/pk
19091-63000
$ 41
Syringe barrel for use with
fused-silica needles,10 µL
9301-0658
$ 90
19245-60760
$ 9
For 200 µm columns (one ring)
19245-20510
$ 89
For 250 µm columns (six rings)
19245-20515
$114
For 320 µm columns (five rings)
19245-20525
$ 78
For 530 µm columns (no rings)
19245-20580
$ 55
For 530 µm Al clad columns (four rings)
19245-20780
$ 54
5
Ferrule
5080-8853
$ 47
6
Column nut
5181-8830
$ 26
1b
2
3
1c
1d
4
Common Supplies
3
Spring
4
Inserts for capillary columns
2/pk
5
6
6890 Series GC Cool On-Column Inlet Supplies
Automatic Injection
1a
Septum nut base for 320 mm assembly
19245-80521
$ 62
1b
Septum nut base for 530 mm assembly
G1545-80520
$ 63
2
Advanced green 5 mm through hole septa
BTO 5 mm through hole septa
5183-4760
5183-4758
$ 62
$ 72
50/pk
50/pk
5890 Series Cool On-Column Inlet Supplies
Automatic Injection
1a
Septum nut (5890 Series II GC)
19245-80520
$ 91
1b
Needle guide (for 7673A only)
19245-20670
$ 35
* For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
33
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Programmed Temperature Vaporizer (PTV) Inlets
PTV inlets combine the benefits of split,
splitless and on-column inlets. The sample is
usually injected into a cool liner, so syringe
needle discrimination does not occur. Then
the inlet temperature is increased to vaporize
the sample. The user programs vent times
and temperature to achieve the equivalent of
split or splitless transfer of sample vapors to
the column. PTV injection is considered the
most universal sample introduction system
because of its flexibility.
PTV Inlet Procedures/Practices (cold split/splitless modes)
Parameter
Selection/Setting
Rationale
Injection mode
Cold split
For general use
and sample screening
For trace analysis
Cold splitless
Inlet temperature
ramp rate
Adjustable (i.e., 2˚C/sec
to 12˚C/sec)
Advantages
• no syringe-needle discrimination
Ballistic
• minimal inlet discrimination
• no special syringe needed
• use of large injection volumes
Inlet liner
Straight with silanized wool
Baffled
Packed with an adsorbent
For general use
For labile samples
For focusing gaseous
injections from auxiliary
sampling devices
Injection volume
0.1-1.5µL
Use lower volumes for
volatile solvents and fast
ramp rates
Use volumes larger than
1.5µL only in solventelimination mode
Sample Injection
technique
Autosampler or manual,
fast or slow
Not critical for cold split
& splitless modes
Oven temperature
10-25˚C below solvent BP
For proper solvent effect in
splitless mode
For split mode
• removal of solvent and low boiling
components
• trapping of nonvolatile components
in liner
• split or splitless operation
• retention time and area reproducibility
approaching cool on-column injection
PTV inlets are actively cooled before and
during injection by Peltier devices or by
forced gases (air, liquid N2, or liquid CO2).
Cryogenic cooling of the inlet can reduce
inlet temperature enough to thermally
focus gas injections from other sampling
devices in the liner. This is a distinct
advantage of using PTV inlets in
comparison to conventional inlets for
coupling auxiliary sampling devices to
capillary columns.
Post-injection, PTV inlets are heated
using electrical heaters or preheated
compressed air. Depending on design,
inlet temperature ramps are either
ballistic (i.e., ramped to the maximum
temperature at an uncontrolled maximum
rate) or programmable.
Use slower ramp rates for
labile, complex, or large
volume samples
Use faster ramp rates for
most samples
Use faster ramp rates to
shorten splitless purge delay time
Simpler, less expensive
instrumentation
Sample dependent
Column flow
30-50 cm/sec
Clears inlet faster
Less backflash
Septum purge
1-5mL/min
Minimizes ghosting
Quantification
Any method
Inherently reproducible
Low discrimination in cold
injection modes
Retention gap
1-3m, deactivated
Compensates for extended
flooded zone and solventcolumn incompatibility
VIDEO
To view a video on PTV column installation, liner installation and silver
seal replacement, visit www.agilent.com/chem/techsupport.
www.agilent.com/chem
•
800 227 9770
34
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
6890 PTV Inlet
1
3
Description
Column ID Unit
Part No.
Price
2
1
Septumless head
G2617-60507
$2661
2
Septum head
G2618-80500
$1078
3
Septum nut
18740-60835
$ 39
4
PTV inlet assy
G2617-60506
$4850
5
PTV LCO2 cooling jacket
G2617-60508
$ 544
6
PTV LN2 cooling jacket
G2619-60501
$ 473
7
Silver seal
5182-9763
$ 62
8
Graphpak inlet adapter
0.20 mm
5182-9754
$ 173
0.25-0.33 mm
5182-9761
$ 152
5, 6
0.53 mm
5182-9762
$ 146
7
8
9
5/pk
Ferrules for
0.20 mm
10/pk
5182-9756
$ 158
Graphpak inlet
0.25 mm
10/pk
5182-9768
$ 166
0.32 mm
10/pk
5182-9769
$ 166
0.53 mm
10/pk
5182-9770
$ 146
10
Split nut for inlet adapters
5062-3525
$ 159
11
PTV insulation block
G2617-20510
$ 61
PTV cryo insulator (not shown)
G2617-60510
$ 53
Teflon ferrule (needle seal)
5182-9748
$ 137
Kalrez seal
5182-9759
$ 110
Valve body
5182-9757
$ 91
Pressure spring
5182-9758
$
5182-9775
$ 24
Sealing element
5182-9760
$ 73
CO2 Cryo inline filter
3150-0602
$ 137
Service kit for septumless head
contains Kalrez seal, valve body,
and pressure spring
Graphpak 3D ferrules
5182-9747
$ 224
5182-9749
$ 143
G2617-80540
$ 208
Installation tool for 3D ferrules
9
10
11
6
Viton seal
5/pk
4
There are few choices in
liner design for PTV inlets.
However, liner volume and
activity are still key issues to
be considered when selecting
among the few available PTV
liners. PTV liners require
packing or a modified surface
to hold the liquid sample in
place before and during the
vaporizing process.
TIPS AND TOOLS
Item
PTV Liners
35
Description
Part No.
Price
PTV Liner Single Baffle, 2 mm id 180 µL volume, deactivated, glasswool
5183-2038
$ 25
PTV Liner Single Baffle, 2 mm id 200 µL volume, deactivated
5183-2036
$ 20
PTV Liner Multi Baffle, 1.5 mm id 150 µL volume, deactivated
5183-2037
$ 29
PTV Liner Fritted Glass, 1.5 mm id 150 µL volume, deactivated
5183-2041
$ 55
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Septa
One of the key components of sample
introduction is the inlet septum. All
columns must have carrier gas head
pressure to establish flow through the
column. Septa maintain the leak-free seal
and exclude air from the inlet. They come
in many different sizes and are made from
many different types of material specific
to inlet type and analysis needs.
What is the Function
Septa are usually available according to
their recommended upper temperature
limits. Lower temperature septa are
usually softer, seal better, and can
withstand more punctures (injections)
than their high-temperature counterparts.
If used above their recommended
temperatures, however, they can leak or
decompose. This causes sample losses,
lower column flow, decreased column life
and ghosting.
Why Replace
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•
800 227 9770
The septum isolates the sample flow path
from the outside world. It must provide a
barrier that is readily penetrated by the
injector needle while maintaining internal
pressure without contaminating the
analysis. They are generally made of
special high-temperature, low-bleed
silicone rubber formulations.
Septa should be replaced regularly to avoid:
• leaks
• decomposition
• sample loss
• reduced column or split vent flow
• ghost peaks
• column degradation
How to Minimize Problems
Avoid problems by:
• using within the recommended
temperature range
• changing regularly
• installing “hand tight”
• using septum purge when available
• using autoinjectors
• using sharp syringe needles
Agilent Introduces Innovative
Packaging for Inlet Septa
Agilent has recently introduced a new
and innovative packaging design for
inlet septa. This new packaging is a
tri-fold blister pack that provides
cleanliness, convenience, and
consistency for our complete line
of 11 mm and 9.5 mm septa.
Your 50th Septum will be
as Clean as Your 1st!
The primary benefit behind the new
packaging is that each septum is
individually packaged for the ultimate
cleanliness. Each septum is easily
dispensed one at a time by pushing it
through the back foil, as is commonly
done with pharmaceutical capsules and
tablets. No longer do you need to reach
into a jar and wonder how clean the
septa are or if you are contaminating
other septa.
In addition, the new packaging delivers
the following features and added value:
• No more clumping or sticking: Septa
don’t stick to each or the jar
• Easy to see exactly how many are
left: Know exactly when to reorder
• Compact storage size: Fits easily into
drawers
• Convenient quantities: All septa are
packaged in either 50 or 100 packs
• High quality PET packaging: Tested by
GC-FID, GC/MS, and GC-ECD to
ensure the absence of interfering
background peaks
36
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Septa Troubleshooting
Symptom
Possible Cause
Remedy
Extra Peaks/Humps
Septum bleed.
Turn off injector heater. If extra peaks
disappear, clean the inlet and change the
liner. If cored septa particles are present,
use a centerguide septa and a 23-26 gauge
tapered syringe. Important: always use the
septum specified for higher temperature or
analyze at lower inlet temperature.
Large leak at septum during injection and
for a short time thereafter (common with
large diameter needles).
Replace septum and use smaller diameter
needles.
Carrier gas leaks at septum or column
connection.
Check for leaks. Replace septum or tighten
connections if necessary.
Normal
Problem
Baseline Change After Large Peak
Normal
Problem
Problem
(flow increase)
(flow decrease)
Retention Times Prolonged
Normal
Problem
Problem
MAINTENANCE MINDER
After repeated injections, septa can become prone to leakage.
To maintain system integrity, change septa regularly.
37
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Premium Non-Stick Septa
Our premium non-stick septa have a recess on the injection side, to guide the syringe
needle to the same point with every injection.
• Proprietary plasma treatment ensures non-stick septa without the use of potentially
damaging talcum powder
• Center point guides the needle for easy penetration and less coring
• Reduce needle bending
• Precision molding assures accurate fit in the inlet
• Each batch tested on an Agilent 6890 GC-FID for bleed
Introducing Agilent Premium Non-Stick Septa –
featuring a proprietary plasma coating that won’t
stick or clump.
Other suppliers coat their septa with powder to prevent sticking. However, this
coating can accumulate inside split vent lines and interfere with the analysis of
active analytes.
Agilent’s plasma-treated non-stick septa
But Agilent’s new non-stick septa are plasma coated, which eliminates chemical
bleed and contamination from foreign substances. So your GC system will maintain
its integrity, stay cleaner and require less maintenance.
Available in Bleed Optimized, Long-Life, and Advance Green.
Competitor “non-stick” septa
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•
800 227 9770
38
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Because bleed from septa can be a major contributor to the overall
signal, a high-quality septum is an absolute necessity for analyses
demanding increased sensitivity.
Agilent’s premium GC inlet septa are not garden-variety septa
stamped out in large sheets, creating variations in geometry. Rather,
each Agilent premium septum is molded to a perfectly uniform size
and shape.
Figure 1. Comparison of Coring, With and Without CenterGuide
(30x magnification)
High-Temperature Septa Without CenterGuide: Major Coring Before 1
00 Autoinjections
Individual molding lets us put a dimple in the center of each septum
to guide the syringe needle into the inlet.
With the dimpled CenterGuide, the syringe needle enters the
septum at precisely the same spot each time.
1 autoinjection
The result: minimal coring (see Figure 1).
• Less chance that a cone of material will be punched out of the
bottom during the first few injections
• Virtually no septa material falling into the inlet liner, improving
chromatographic quality
100 autoinjections
700 autoinjections
Agilent BTO Septa With CenterGuide: Very Little Coring Even After
700 Autoinjections
• Up to 1,000 autoinjections under optimal conditions before failure
with HP Point syringes. The HP Point syringe yields optimal
performance and reliability and reduces coring by parting, not
cutting, the septum.
Agilent septa are made of highly durable, high-temperature tested
silicone rubber.
Each lot is tested to ensure low bleed at high temperatures.
Summary of Inlet Septum Characteristics
SEPTUM TYPE
BTO
(Bleed and
Temperature
Optimized)
Long Life
Advanced Green
✔✔✔ = best
39
BLEED
LIFETIME
TEMPERATURE
LIMIT
✔✔✔
(optimized for
high temperature)
✔
to 400ºC
✔
✔✔✔
to 350ºC
✔✔
✔✔
to 350ºC
✔✔ = very good
✔ = good
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
p/n 5183-4757
p/n 5183-4761
p/n 5183-4759
Agilent Bleed and Temperature
Optimized Non-Stick Septa (BTO)
Agilent Long-Life Non-Stick Septa
Agilent Advance Green
Non-Stick Septa
• Extended temperature range, low-bleed
• Pre-pierced for extended life and
reduced coring
• Maximum Injection Port Temperature
400ºC
• The preferred Septum for Autosamplers
• True Long-Life, High Temperature
Green Septum
• Ideal for Overnight Runs
• More Injections per Septum
• Virtually eliminates injection-port
sticking
• Up to 400 Injections Per Septum injection
• Reduced Injection Port Sticking
• Maximum Injection Port Temperature
350ºC
• Maximum Injection Port Temperature
350ºC
• Soft, 45 Durometer, Easy On
Autosampler Needles
• Packaged in glass vials for high purity
• Pre-conditioned; packaged in glass
to prevent contamination
• Ideal for use with low-bleed,
“Mass Spec” capillary columns
• Economical alternative to competitor’s
“Green” Septa
General Purpose Septa
Agilent’s General Purpose Septa are
made from an enhanced injection-molded
silicone rubber material. The septa material,
dark red or gray in color, is specified to
withstand over 200 automatic injections
at an injection port temperature of
350ºC. You can have confidence in your
chromatographic results knowing that
each lot of septa is placed through a
demanding QC test to ensure that only
the highest quality product is delivered
to your laboratory.
www.agilent.com/chem
•
800 227 9770
Agilent’s General Purpose red/gray
septa are cost-effective choices
which provide:
• Low bleed for reduced instrument
maintenance downtime and increased
laboratory productivity
• Less frequent replacement for long
lifetime and the ability to withstand more
than 200 autosampler injections at
maximum injection port temperatures
• While general purpose septa do not have
the centerguide of premium septa,
they are made of durable material to
minimize the risk of contamination and
the need for reconditioning
• Convenient blister packs of 50 or 100
septa minimize risk of contamination
and need for reconditioning
40
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Septa Ordering Information
Part No.
Price
5183-4757
5183-4757-100
5183-4758
$72
$134
$72
5183-4759
5183-4759-100
5183-4760
$62
$107
$62
5183-4761
5183-4761-100
5183-4762
$84
$150
$84
5080-8896-50
5080-8894-100
5080-8728-50
5080-8728-100
$52
$93
$52
$93
5181-1263-50
5181-1263-100
5181-3383-50
$52
$93
$52
5181-3383-100
$93
5181-1283-50
5181-1283-100
5181-1260
$52
$93
$29
5181-1261
$29
Premium Non-Stick Septa
Agilent Bleed and Temperature Optimized Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
Agilent Advanced Green Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
Agilent Long-Life Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
General Purpose Septa
Gray Septa
11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk)
11 mm for 5880, 5890, 6850 and 6890 GCs (100/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)
Red Septa
11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk)
11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk)
11 mm with partial through-hole for 5880, 5890, (50/pk)
6850 and 6890 GCs
11 mm with partial through-hole for 5880, 5890, (100/pk)
6850 and 6890 GCs
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)
5 mm through-hole for on-column inlets, (25/pk)
automatic or manual injections*
5 mm solid for high column backpressure, on-column inlets* (25/pk)
* 5 mm septa are packaged in glass jars
EASY ONLINE ORDERING
Our online store offers every GC inlet and consumable that your system
might need – including pieces that are hard to find.
Just visit www.agilent.com/chem/4ecatalog
41
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Ferrules
Using the wrong ferrule or a worn-out
ferrule to seal your column connection can
result in inconsistent and unreliable
chromatography. An improper ferrule can
cause leaks which allow air
and other contaminants to enter the
instrument through the column seal,
causing major interference with column
and detector performance. For optimum
performance, ferrules should be replaced
every time the column is replaced and
when performing column maintenance.
Agilent offers a comprehensive selection
of ferrules made of different materials and
configurations for a leak-free connection
between the column and injector.
Three main types of ferrules are used with
capillary GC columns: graphite, Vespel and
Vespel-graphite composites. Graphite
ferrules can withstand temperatures as
high as 450ºC, and Vespel and Vespelgraphite ferrules are rated to 280ºC and
350ºC, respectively.
Column Ferrule Types
Graphite
What is the Function
Ferrules seal the connection of the column
or liner to the system. The ideal ferrule
provides a leak-free seal, accommodates
various column outer diameters, seals with
minimum torque, will not stick to the
column or fittings, and will tolerate
temperature cycling.
Advantages
Limitations
Easy-to-use, stable seal
Soft, easily deformed or destroyed
Higher temperature limit
• possible system contamination
• not for use with GC/MS
transfer-lines
Vespel or
Mechanically robust
Flows at elevated temperature
Vespel-graphite
Long lifetime
• must retighten frequently
• prone to leakage
Polymer bleed problematic with
some detectors (NPD and ECD)
Why Replace
Signals that a ferrule is damaged include:
• background noise from oxygen diffusing
into the system
• column bleed catalyzed by oxygen
• sample degradation
• loss of sample
• increase in detector signal/noise
• poor retention time reproducibility
www.agilent.com/chem
•
800 227 9770
How to Minimize Problems
General technique for installing ferrules:
• don’t overtighten – finger-tighten column
nut, then use wrench to tighten
• maintain cleanliness
• bake out ferrules prior to use (Vespel and
Vespel/Graphite only)
• avoid contamination – such as
fingerprint oils
• inspect used ferrules with magnifier for
cracks, chips, or other damage before
reusing them
• change ferrules when new columns or
injector/detector parts are installed
42
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Ferrule Troubleshooting
Problems possible after changing ferrules
Normal Peaks
Tailing Solvent Peaks
Wrong Peak Ratios
Normal Peaks
Tailing Solvent Peaks
Wrong Peak Ratios
Correct column positioning in both
injection port and FID
Column positioned incorrectly in the
injection port, or possible ferrule or septum
particle in the carrier gas flow path
Column positioned incorrectly in the inlet
(either too far or not far enough; verify
4-6mm installation distance)
100% Graphite Ferrules
Reusing a ferrule – or using off-brand
ferrules – may be a costly mistake. That’s
because you’ll increase the likelihood of
dangerous leaks that can damage the GC
column and sensitive detector parts.
For best results, always use new Agilent
ferrules, which feature the highest quality
design, and are supported by decades of
technical expertise.
Two different types of Agilent column nuts
can be used with these ferrules:
• The universal column nut (p/n 51818830) has a hexagonal head requiring the
use of a wrench to tighten it completely.
• The finger-tight column nut (p/n 50208293 for 530um columns and p/n 50208292 for columns 320µm or less) does
not require a wrench to tighten.
It can only be used with the 100%
graphite ferrules.
TIPS AND TOOLS
Do not use 100% graphite ferrules in GC/MS transfer lines. They will
deform and leak over time, due to the softness of the graphite.
43
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Vespel/Graphite
(85%/15%) Ferrules
The combination of graphite and Vespel
results in a ferrule having low oxygen
diffusion rates which does not shrink to
the same extent as pure Vespel. These
ferrules are recommended for use with
GC/MS or other oxygen sensitive
detectors, like the ECD, but are also
compatible with other detectors like FID
and NPDs.
In addition, the Vespel/graphite ferrules
provide added confidence of leak-free
connections when installed correctly.
Proper installation requires a finger-tight
turn on the nut, then an additional 1/4 – 1/2
turn with a wrench.
These ferrules are very hard and cannot
be deformed sufficiently to seal multiple
column diameters. The ferrule hole must
match the column OD exactly to ensure a
leak-free seal. For capillary column
applications, there is a specific ferrule for
each column diameter. Choosing a ferrule
with a larger hole than is specified for a
given column dimension can result in a
large leak. If left unchecked, an improper
seal at the injector will result in high
column bleed and a shortened column
lifetime. An improper seal at the detector
can result in increased detector
signal/noise. In the case of the MSD it
can also contribute to oxidation of the ion
source which can increase the frequency
of detector maintenance.
Two different lengths of Vespel/graphite
ferrules are available for capillary column
use. The standard sized ferrule is
compatible with the universal column nut.
The second ferrule size is slightly longer
and is specifically designed to fit with the
MS interface nut used for the GC/MS
transfer line connection. The larger ferrule
can also be used to make column
connections to inlets and other detectors
but requires a specially designed column
nut (p/n 05988-20066) to accommodate
the longer ferrule.
When using Vespel/graphite ferrules,
Agilent recommends tightening the column
nut to a 1/4 turn after the first temperature
program runs. Even preconditioned ferrules
can exhibit some shrinkage after a
temperature programmed run.
Vespel/Graphite Nut & Ferrule Combinations
Standard ferrule and standard nut
Universal Column Nut
+
5181-8830
Vespel/Graphite Ferrules
5181-3323 (0.1, 0.2, 0.25 mm ID columns)
5062-3514 (0.32 mm)
5062-3512 (0.45 and 0.53 mm)
Longer ferrule with MS interface nut
MS Interface Column Nut
05988-20066
+
Vespel/Graphite Ferrules
5062-3508 (0.1, 0.2, and 0.25 mm ID columns)
5062-3506 (0.32 mm)
5062-3538 (0.45 and 0.53 mm)
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800 227 9770
44
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
100% Vespel Ferrules
Vespel is a high-temperature polyimide based
material which is very hard. This material has
the lowest permeability to oxygen, making it an
excellent sealing material when making metal
or glass connections. These ferrules do not
deform easily. So, it is important to match the
ferrule hole size to the proper column diameter.
The main disadvantage of 100% Vespel ferrules
is the shrinkage of the material when exposed
to temperature cycling conditions. 100% Vespel
ferrules should only be used for isothermal
applications.
VIDEO
To view a video on ferrules, visit www.agilent.com/chem/techsupport.
Agilent Ferrule Selection Recommendations
Ferrule/Seal
Type
Upper
Temperature
Limit
Usages
Limitations
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Graphite
450ºC
General purpose
Not for MS or
(100%)
for capillary columns.
oxygen sensitive
Suitable for FID and NPD.
detectors.
Recommended for high
temperature and cool
on-column applications.
Can be removed easily.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel/Graphite
350ºC
General purpose for
Not reusable.
(85%/15%)
capillary columns.
Recommended for
MS or oxygen sensitive
detectors. Most reliable
leak-free connection.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel
280ºC
Isothermal operation.
Leaks after
(100%)
temperature cycle.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------SilTite
N/A
Use only with SilTite Nut Kits
Not Reusable
(100% metal)
45
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Ferrule Ordering Information
Ferrule Id
(mm)
Column Id
(mm)
Quantity
Part No.
Price
0.1, 0.2, 0.25, 0.32
0.53
0.05-0.25
0.45, 0.53
10/pk
10/pk
10/pk
10/pk
5080-8853
5080-8773
500-2114
500-2118
$
$
$
$
47
38
26
26
0.1, 0.2
0.1, 0.2, 0.25
0.32
0.45, 0.53
10/pk
10/pk
10/pk
10/pk
5062-3516
5181-3323
5062-3514
5062-3512
$
$
$
$
51
55
51
53
0.1
0.1, 0.2, 0.25
0.32
0.53
10/pk
10/pk
10/pk
10/pk
5062-3507
5062-3508
5062-3506
5062-3538
$
$
$
$
62
62
56
48
0.1, 0.2, 0.25
0.32
0.45, 0.53
10/pk
10/pk
10/pk
5181-3322
5062-3513
5062-3511
$ 55
$ 51
$ 51
0.1, 0.2, 0.25
0.32
10/pk
10/pk
10/pk
5062-3580
5062-3581
5181-3308
$ 79
$ 79
$ 47
0.4
10/pk
5184-3569
$ 87
0.5
10/pk
5184-3570
$ 87
10/pk
5184-3571
$ 85
10/pk
5188-2789
$135
2/pk
1 ea
1 ea
1 ea
2/pk
5181-8830
5020-8293
5020-8292
5020-8294
5183-4732
$
$
$
$
$
1 ea
1 ea
1 ea
05988-20066
05921-21170
8710-0510
$ 13
$ 16
$ 24
General Purpose Graphite Ferrules (Short Ferrules)
0.5
1.0
0.4
0.8
85% Vespel, 15% Graphite Ferrules (Short Ferrules)
0.80.3
0.80.4
0.80.5
0.80.8
Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)
0.3
0.4
0.5
0.8
These ferrules are recommended for use with GC/MS.
100% Vespel High-Performance Ferrules (Short Ferrules)
0.4
0.5
0.8
These ferrules are recommended for use in isothermal analysis only.
Specialty Ferrules, 85% Vespel, 15% Graphite
Two Hole
0.4 ID holes
0.5 ID holes
No Hole
SilTite Metal Ferrules
For use with 0.20-0.25 mm ID
capillary columns. Includes 2 column nuts
For use with 0.32 mm ID capillary
columns. Includes 2 column nuts
For use with 1/16 in. od
SS tubing. Includes 2 column nuts
For use with 0.53 mm ID capillary columns.
Includes 2 nuts
0.8
Column Nuts
Short Nuts
Universal column nut, 1/16 in. hex
Finger-tight column nut for 0.53 mm columns*
Finger-tight column nut for 0.32 mm columns* and smaller
Blanking plug, finger-tight style
6850 Column Nut
26
18
18
12
47
Long Nuts
MS interface column nut
Column nut for GC/MS ferrules
Column nut wrench, 1 /4 in. and 5 /16 in.
* For use with graphite ferrules only.
Always match short nuts with short ferrules and long nuts with long ferrules.
www.agilent.com/chem
•
800 227 9770a
46
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liners
Agilent offers a complete selection of
GC split and splitless inlet liners that
deliver consistent quality. So you can get
consistent results.
And unlike other manufacturer’s liners,
Agilent liners are built to Agilent’s precise
inlet tolerances which helps ensure
optimal dimensional accuracy and
inertness toward demanding compounds.
Choosing the proper liner for a specific
application can be a difficult and
challenging task. The three liner
characteristics that must be considered
for each application are:
• Liner volume
• Liner treatments or deactivation
• Any liner design features that might
affect carrier gas flow through the inlet
or sample vaporization
What is the Function
Liners are the centerpiece of the inlet
system in which the sample is evaporated
and brought into the gas phase.
Why Replace
These problems will occur if the liner is not
changed on a regular basis or if the correct
liner is not used:
• peak shape degradation
• solute discrimination
• poor reproducibility
• sample decomposition
• ghost peaks
• reduced column life
How to Minimize Problems
Change liners on a regular basis
determined by:
• previous use pattern
• sample cleanliness
• chromatographic abnormalities such as:
– peak shape changes
– peak discrimination
– poor reproducibility
– sample pyrolysis
– active analyte response loss
or decomposition
VIDEO
To view a video on Liners, visit www.agilent.com/chem/techsupport.
47
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•
800 227 9770
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Discussion
of Liner
Characteristics
Liner Volume
The purpose of the injection port is to allow
the introduction of a sample into the gas
chromatograph in an accurate, reproducible
manner. The vaporized sample should be
a true representation of the liquid sample
and, unless specifically desired, should
be injected without chemical change. The
elevated temperatures used in the inlet
vaporize the liquid sample to a gas for
transfer to the head of the column. This
phase transition is accompanied by a very
significant volume change. The volume of
the resulting vapor must be small enough
to fit within the volume of the liner. If the
volume is too great for the liner, it could
result in backflash, or sample loss caused
by expansion into the septum purge or split
vent lines. Both can compromise
reproducibility and sensitivity. Backflash
also frequently results in sample carryover.
Larger volume liners (> 800 µL) are
characterized by larger inside diameters
(ID) and are typically used with injection
sizes of 1 µL or more. The small volume
liners have a smaller ID and are usually
used with small injection sizes (< 1 µL),
fast 100 µm ID columns, gas samples, or
when using external sampling devices
like headspace and purge and trap.
Liner Deactivation
Active sites on inlet liners can adsorb
sample components and cause peak tailing,
and potential loss of sensitivity and
reproducibility. Deactivation agents are
used to cover or react with active sites on
the glass surface of the liner. Agilent liners
are deactivated using deactivation
procedures that produce reproducible and
inert liners, with long lifetimes. For splitless
applications or when even slightly polar
compounds must be analyzed, a
deactivated liner should be used.
With use, even deactivated liners can
begin to exhibit activity. When this occurs,
the liner should be replaced. Liners can be
cleaned to remove particulate material or
solvent rinsed to remove less volatile
components. However, choosing the
proper liner cleaning procedure can be
difficult. Some solvents may remove the
deactivation layer, and tools might scratch
the glass surface of the liner, resulting in
the generation of unwanted active sites.
A new liner almost always outperforms
a cleaned and re-deactivated one –
especially for trace analysis.
TIPS AND TOOLS
Agilent offers a free software tool that calculates the vapor volume of an extended list of
common solvents, based on your choice of inlet temperatures and pressures for a given
Agilent inlet liner. To download, go to www.agilent.com/chem/techsupport. Click “User
Contributed Software;” then, click “GC Pressure/Flow Calculator.”
www.agilent.com/chem
•
800 227 9770
48
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liner Design Features
Dimensions
• The outside diameter (OD) of the liner
determines if the liner is more effectively
used in split or splitless mode
• Larger OD liners are designed for splitless
operation, fit tightly and limit sample
contact with metal parts of the inlet
• Larger OD liners improve analyte recovery
by retaining more sample inside the liner
• Agilent splitless liners are all designed
with exacting dimensional tolerances to
fit tightly in the inlet and minimize sample
contact with metal surfaces
• Smaller OD liners are designed for split
injection because they produce less
resistance to carrier and split flow
through the inlet
• Large volume liners are used for split
injections with enforced dimensional
stability for a wide range of split ratios
Tapers
Tapering or narrowing the liner internal
diameter (ID) is done for a number of
purposes:
• Bottom taper focuses sample onto the
head of the column
• Bottom taper minimizes contact with
metal parts of the inlet
• Center taper positions glass wool
correctly
• Top taper minimizes sample backflash
To operate properly, the column must be
installed correctly in the injection port with
the tip of the column ideally located about
halfway into the taper, or about 4-6 mm
from the column tip to the top of the ferrule
(See Figure 1). Some applications will work
better with different column installation
depths. Therefore, you should check the
instrument manual for proper installation
distances and determine which distance is
appropriate for your application.
Reproducible positioning is important
for repeatable quantitative results.
49
Packing
Glass Wool
Glass Cups
Many liner designs use deactivated
glass wool packing. The glass wool is
positioned or held in place near the
center of the liner to:
Another design feature used to help
volatilize the sample and provide good
mixing is the incorporation of a glass cup
inside the liner. Glass cup liners are also
available with additional glass wool and
inert packing to increase reproducibility
and limit sample discrimination. Not
recommended for use with Electronic
Pressure Control Inlets on 6890 or 6850 GCs.
• Provide additional surface area for
complete volatilization of the sample to
minimize thermal discrimination
• Trap non-volatile components and septum
particles before they reach the column
• Wipe any sample from the syringe needle,
thereby increasing reproducibility and
preventing sample residue build-up at the
septum
Glass wool liners that have glass wool near
the center of the liner, such as Agilent Part
Nos. 5183-4647 and 5183-4711, are
recommended for automatic injections.
Figure 1.
If glass wool is positioned at the bottom of
the liner, its main purpose is simply to trap
non-volatile components. Glass wool is
generally not recommended for the
following analytes:
• phenols
• organic acids
• pesticides
• amines
• drugs of abuse
• reactive polar compounds
• thermally labile compounds
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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liner Troubleshooting
Symptom
Possible Cause
Remedy
Tailing Peaks
Sample components adsorbed by column,
inlet liner or contaminated gold inlet seal.
Use new, deactivated liner or clean old
liner and replace glass wool.
Needle hitting and breaking packing in
inlet liner.
Partially remove packing from liner or use
without packing.
Column end poorly cut
(sample absorption).
Broken or chipped inlet liner.
Remove column. Make a clean, square
cut using a reliable capillary fused silica
cutting tool (such as a ceramic wafer or
the Agilent Column Cutter), then reinstall
column.
Inlet flow too low.
Make sure total flow in inlet is above
40 mL/min.
Sample decomposing.
Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass
wool and packing. Column/sample
residues could also be the problem.
Column and inlet liner misaligned.
See also”Septum Troubleshooting,”
page 37
Check installation of column end and inlet
liner; adjust if necessary.
Column or inlet liner contaminated or
column deteriorating.
Use a guard column to prolong column life.
Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass
wool and packing. Trim the front end of the
column a minimum of 6 inches.
Normal
Problem
Baseline Rise Before or After Peak
Normal
Problem
Problem
Baseline Change After Large Peak
Normal
Problem
Problem
Unresolved Peaks
Normal
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Problem
•
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Problem
50
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Agilent Liners
Our engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Intensive liner
development and testing have resulted in a set of liners that we recommend whenever new methods are being developed, when
methods are being optimized, or when problems with existing methods are encountered. These liners are:
Direct injection:
Straight liner without glass wool,
deactivated, Agilent Part No. 5181-8818
(use only for gas samples, headspace, or
purge and trap applications).
Direct Connect
Direct Connect liners are ideal for
customers running highly sensitive
compounds, or for users who require
maximum inertness performance and
minimal inlet discrimination for trace GC
and GC/MS applications. Direct Connect
liners also eliminate sample exposure to
metal parts, minimizing inlet-related
degradation. These liners are included in
our new 8270 EPA Applications kit
designed specifically for optimizing a
6890/5973 GC/MSD to this method.
Split injection:
Agilent low-pressure-drop split liner with
glass wool, bottom taper, glass bead for
easy positioning, and deactivated, Agilent
Part No. 5183-4647 (with extraordinarily
tight dimensional control for optimum
split performance).
Splitless injection:
Single tapered liner without glass wool,
deactivated, Agilent Part No. 5181-3316EN.
Note: For pesticide analysis – especially
DDT and Endrin, where breakdown is a
problem – we recommend Agilent Part
Nos. 5181-3316EN and 5181-3315EN.
General purpose split/
splitless injection:
Similar design to Agilent Part No. 51834647, but with an outer diameter that
compromises for both split and splitless
injections, Agilent Part No. 5183-4711.
51
The liners are deactivated, come in either
a single or double taper, and utilize a press
fit connection to the column. In addition,
there is a small, drilled hole in the side of
the liner whose size and placement was
optimized by Agilent R&D engineers to
allow them to work with EPC.
Focus Liner
Improve reproducibility, improve results.
The Focus Liner traps a precisely controlled
amount of glass wool in the ideal position
in the injection port liner. At the point of
injection, the glass wool provides extra
surface area for vaporization, traps
nonvolatile sample residue, and wipes
any residual sample from the sample
needle – reproducibility is the result.
In addition to these liners we offer a
broad selection of liners for your specific
application needs.
Liner O-Rings
Liners are sealed in the inlet with O-rings
or graphite seals. O-ring seals are easier to
remove and to replace than graphite that
deforms and flakes apart. The graphite
seals should be used when inlet
temperatures exceed 350ºC.
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•
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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Flip Top Inlet Sealing System
Agilent’s NEW Flip Top Inlet Sealing System is the faster, smarter way to change
inlet liners on Agilent GC’s
• Cuts liner replacement time to as little as 30 seconds
• No more frustrating searches for special wrenches or tools
• Improved inlet ergonomics – no more handling of heated parts, no more burns or scrape
• Decreased downtime = increased productivity
• Minimizes exposure to ambient air extending column life
• Installs easily in 15 minutes (customer installable)
Questions to ask yourself:
1. Do you change liners more than 2-3 times per week?
2. How long does it take you to change a liner (total downtime)?
3. Do you want to increase your productivity and column life?
4. Have you ever burned your fingers or scraped your knuckles trying to open a hot inlet?
One of the most frequent maintenance tasks customers face when running a GC or GC/MS
system is changing the inlet liners. A hot inlet may have to be opened on each system every
24 to 48 hours to change a dirty inlet liner. The special wrench used for this operation is often
misplaced, bent at an odd angle, too thin, or simply awkward to use. In addition, the inlet nut
is usually too hot to handle so it must be turned several times with the wrench before it will
release the top assembly of the injection port.
Once the dirty liner is replaced, the inlet nut must be replaced on the injection port and
occasionally the wrench slips off the nut leading to scrapes, burns, and cuts. It can take at
least 5 minutes of wrestling with this hot injection port nut and wrench combination just to
take out the old liner and put in a new one. By the time the operator finishes the procedure
and re-equilibrates, it can result in 15 minutes of downtime!
Of course, doing this with a GC/MS causes even more problems as ambient air is drawn into the
capillary column, through the hot MS interface, and into the heated source resulting in multiple
problems for the operator including shortened column life and air background in the MS.
The Easiet Way to Change Inlet Liners!
Agilent’s new Flip Top Inlet Sealing System is a device designed to allow the user to safely
and reliably change an inlet liner in as little as 30 seconds without tools in a consistent leakfree manner. No longer will you have to contend with frustrating searches for wrenches or
burning your fingers on hot inlets.
Available exclusively from Agilent, the Flip Top has a levered arm that attaches to any
6890/6850/5890 insert weldment and locks to the injection port using an adapter ring
screwed onto the inlet. Once installed, the user simply lifts the arm of the Flip Top which
releases the insert weldment from the injection port, and allows instant access to the liner.
The process is simply reversed to re-seal the weldment to the port.
VIDEO
Description
Part No.
Price
Flip Top Inlet Sealing System
5188-2717
$514
Liner O-rings (10/pk)
5188-2741
$19
www.agilent.com/chem
•
800 227 9770
To view videos on the Flip Top Inlet Sealing System,
visit www.agilent.com/chem/fliptop2
52
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liner Ordering Information
Application
Liner
Volume(µl)
Single
Liner
For split injection
870
5183-4647
$35
5183-4701
$157
5183-4702
$700
Liner, splitless, single-taper,
no glass wool, deactivated
For splitless injection
900
5181-3316
$29
5183-4695
$124
5183-4696
$533
NEW! Liner, Splitless,
Single-taper, no glass wool,
polymerically deactivated
For trace pesticide
analysis
900
5181-3316EN
$32
Liner, direct, 2 mm ID,
deactivated
For direct injection
(use for gas samples,
headspace, or purge
and trap applications)
250
5181-8818
$24
5183-4703
$95
5183-4704
$414
Liner, general purpose
split/splitless, glass wool,
taper, deactivated
For split/splitless
injection
870
5183-4711
$27
5183-4712
$112
5183-4713
$476
Splitless Inlet Liners
Liner, splitless, single-taper, glass wool, deactivated
900
5062-3587
$30
5183-4693
$129
5183-4694
$560
Liner, splitless, double-taper, no glass wool, deactivated
800
5181-3315
$36
5183-4705
$163
5183-4706
$751
NEW! Liner, Splitless,
double-taper, no glass wool,
polymerically deactivated
800
5181-3315EN
$43
250
18740-80220
$28
5183-4707
$124
5183-4708
$533
140
18740-80200
$17
5183-4709
$73
5183-4710
$308
990
$19
210-3003
$84
210-3003-5
Agilent Choice Liners
Liner, split, low press. drop,
glass wool, taper, deactivated
For trace pesticide
analysis
Direct Inlet Liners
Liner, direct, 2 mm ID, non-deactivated, quartz
Liner, direct, 1.5 mm ID, non-deactivated
[use for gas samples, headspace, or purge
and trap applications]
Liner, straight, splitless 4.0 mm ID
5/pk
25/pk
Split Inlet Liner
Liner, split, glass wool, non-deactivated
990
19251-60540
$19
5183-4691
$78
5183-4692
$336
Split Inlet Liners For Manual Injection
Liner, split, with cup, no glass wool
800
18740-80190
$40
5183-4699
$179
5183-4700
$784
Liner, split, with cup, glass wool, and packing
[not recommended for use with electronic pressure
control (EPC)], for manual injection
800
18740-60840
$43
5183-4697
$191
5183-4698
$840
Direct Connect Liners
Part No.
G1544-80730
G1544-80700
Price
$62
$62
Dimensions
6.3 mm X 78.5 mm
6.3 mm X 78.5 mm
Part No.
210-4004-5
210-4022-5
Price
$98
$108
Liner O-Rings
Fluorocarbon O-ring (12/pk)
Graphite O-ring for splitless liner (10/pk)
Graphite O-ring for split liner (10/pk)
Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk)
Part No.
5180-4182
5180-4173
5180-4168
Price
$13
$52
$52
5188-2741 $19
Single taper direct connect liner, 4 mm ID, deactivated
Dual taper direct connect liner, 4 mm ID, deactivated
Focus Liners
Focus liner
Focus liner
53
ID
4.0 mm
4.0 mm
Wool
Yes
Yes
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SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Instrument Inlet Parts and Supplies
When it comes to inlet replacement parts for your Agilent GCs, don’t
settle for imitations; choose only genuine Agilent parts.
Our inlets are backed by the same 40 years of design experience that
you’ve come to expect from our instruments. So you get optimal
performance, plus the reproducible results that your lab demands.
What’s more, Agilent supplies every replacement part that your
system might need – not just a few select pieces. So you can get all
your consumables, all in one place.
Septum Nut
Part No. 18740-60835
Septum See page 36
Split/Splitless Inlet Weldment
Part No. G1544-60575, for 6890 GC
with EPC
Viton O-Ring
Part No. 5180-4182, 12/pk
Liners See page 47
Heater-Sensor Assembly
Part No. G1544-61140
TIPS AND TOOLS
For a complete parts breakdown, see the
5890, 6890, and 6850 series GC Instrument
User and/or Service Manuals, or visit
www.agilent.com/chem.
Gold-Plated Seal (Splitless)
See page 55
Retaining Nut
Part No. G1544-20590
Washer
Part No. 5061-5869, 12/pk
Reducing Nut
Part No. 18740-20800,
1 each
Ferrules (85% Vespel, 15% Graphite)
– Part No. 5062-3516, 0.37 mm I.D.,
for 100-200 µm Columns, 10/pk
– Part No. 5181-3323, 0.40 mm I.D.,
for 250 µm Columns, 10/pk
– Part No. 5062-3514, 0.50 mm I.D.,
for 320 µm Columns, 10/pk
– Part No. 5062-3512, 0.74 mm I.D.,
for 530 µm Columns, 10/pk
Column Nut for 6890 GC
Part No. 5181-8830, 2/pk
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54
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
6890/6850 Split/Splitless Insert Assemblies
Standard manual pneumatics
Original standard EPC using 1/4" split vent filter.
Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to
clean carrier gas for ECD operation.
S/SL insert weldment. Used with large charcoal canister type filter
for 6890/6850.
Similar to G1544-60575 except carrier lines separated for interface to valved
systems of a G1540A instrument.
S/SL insert assembly for G1540A with valved system option. This insert assembly
uses the large charcoal canister split vent filter for 6890/6850.
Part No.
Price
19251-60575
G1544-60575
G1544-80580
$230
$216
$73
G1544-60585
$330
G1580-60575
$261
G1580-60585
$236
5890 Split/Splitless Multimode Inlet Supplies
Septum retainer nut
18740-60835
Retainer nut for headspace sampling
18740-60830
Retaining nut
19251-20620
Reducing nut
18740-20800
For a complete parts breakdown, see the 5890, 6890 and 6850 series GC Instrument User and/or Service Manuals.
Liner Seals and Washers
Stainless steel
Gold-plated seal
Gold-plated seal with cross
Washers (12 pk)
18740-20880
18740-20885
5182-9652
5061-5869
$39
$106
$31
$35
$26
$33
$40
$8
Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity. Other manufacturers’ seals are not
machined, and may compromise your results.
Top
Gold-plated seal p/n 18740-20885
55
Bottom
Gold-plated seal with cross p/n 5182-9652
Use when inlet flow exceeds 400 ml/min.
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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.
“Agilent lets you choose from over 1,000
different columns. It’s no wonder that,
for nearly 40 years, customers have built
products – and entire businesses – around
the results they get from our DB- and HPcapillary GC columns.”
Phil Stremple,
GC Columns Program Manager
CATALOG
For a complete selection of GC columns and parts, see Agilent’s 20052006 Essential Chromatography Catalog. Or, visit our online catalog at
www.agilent.com/chem/4ecatalog.
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•
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56
COLUMNS
Column Maintenance
While GC column maintenance is
simple, the frequency and type of
column maintenance that is required
varies due to many system and sample
factors. Instead of simply following a
predefined timetable of maintenance items,
the main focus should be how to obtain
the highest performance and lifetime
from a capillary column. This depends on
choosing the right column, correct
installation/system setup, and avoiding
the primary factors that cause column
performance degradation (breakage,
thermal damage, oxygen damage, chemical
damage and contamination).
Selection of Capillary Columns for GC and GC/MS
Phases
All phases can be used with conventional
GC systems, and most stationary phases
can be used with a GC/MS system.
However, it is a good idea to choose a
phase for your application that has the
lowest amount of column bleed as
possible. Column bleed is the natural
degradation of the stationary phase that
occurs at higher temperatures, which
appears as an elevated baseline as the
temperature rises to the column’s upper
thermal limit. Column bleed will deposit in
the MSD ion source, which can decrease
MSD performance. By minimizing the
amount of column bleed, you will help
reduce the frequency of required ion
source maintenance.
Primary
“Quantion”
is hidden
Primary
“Quantion”
is enhanced
There are a few simple rules for choosing
columns with lower bleed levels:
• Choose a low-bleed phase for your
application – Agilent has developed
several low-bleed versions of the most
popular phases. These are chemically
designed to possess minimal levels of
column bleed possible and often have
the benefit of an increased uppertemperature limit.
• If a low-bleed column is not available,
choose a low-polarity column with a
moderate film thickness. The amount of
bleed will rise with increases in polarity,
film thickness, and length.
• Use more polar phases when difficult
isomer separations are required. (Choose
a more polar phase when you must, but
try to make it the least polar column that
will do the job)
57
Dimensions
All dimensions can be used with
conventional GC systems. Many types of GC
column phases can be used with the MSD,
but there are some dimensional
considerations. The maximum allowable
flow rate and optimal sensitivity flow rates
will vary depending upon the type of pump.
In general, the column flow should be
1mL/min (2mL/min for Performance Turbo
Pumps). Therefore, column length
and internal diameter combinations are
restricted to provide the appropriate flow
to the GC/MS.
• Narrow-bore columns (0.25mm i.d. and
smaller) can be installed directly into the
GC interface.
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•
800 227 9770
COLUMNS
Popular Column Choices
• Wide-bore columns (0.32mm i.d.) that are
30m or longer can be installed directly
into the 5973 GC interface (other MSDs
may require 50m or longer). If using a
wide-bore column with a shorter length,
an effluent splitter or jet separator should
be utilized.
• Columns with internal diameters greater
than 0.32mm should not be directly
interfaced into the GC interface. For these
columns, an effluent splitter or jet
separator should be installed.
Description
Part No.
Price
DB-1ms, 0.25mm i.d., 30m, 0.25µm
122-0132
$483
HP-5ms, 0.25mm i.d., 30m, 0.25µm
19091S-433
$483
DB-XLB, 0.25mm i.d., 30m, 0.25µm
122-1232
$483
DB-35ms, 0.25mm i.d., 30m, 0.25µm
122-3832
$483
HP-INNOWax, 0.25mm i.d.,
30m, 0.25µm
19091N-133
$413
Column Installation, Setup, & Conditioning
The first step in obtaining optimal
column performance and lifetime is
proper installation:
• Verify that all fittings are leak-free and
the carrier gas is oxygen-free before
heating the oven.
• Choose the appropriate size and
material ferrule for the column,
injector and detector type.
• Briefly conditioning a column before
installing it into the GC/MS interface is
recommended. When the column and
inlet are first heated, volatile materials
within the flow-path and a small portion
of the column stationary phase move into
the gas phase. These materials are then
carried by the carrier gas into the MSD
and can deposit in the MSD ion source.
This can decrease MSD performance.
Conditioning the column briefly prior to
installation into the MSD will minimize
the contamination brought into the ion
source.
• Avoid re-using ferrules.
• Use an appropriate column cutting
tool such as a ceramic wafer or
diamond tipped scribe.
• Make sure column ends are
cleanly cut and free of particulate
matter before installing into the
injector and detector.
• Install the column the appropriate
distance into the injector and detector
as specified by the GC manufacturer.
• The column should be placed on
a column hanger and no portion of
the capillary tubing should touch the
oven walls.
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom,
even at your site. See pages 104-115 for more information about our
services and support.
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•
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58
COLUMNS
Column Installation & Setup continued
Bad
Good
Example of column cuts
• Check the installation and set the
linear velocity by injecting a non-retained
compound.
Description
Part No.
Price
Ceramic wafer (4/pk)
5181-8836
$ 15
20x Magnifier
430-1020
$ 42
General Purpose Graphite ferrule
(0.5mm ID, for column IDs ≤ 0.32mm)
10/pk
5080-8853
$ 47
General Purpose Graphite ferrule
(1.0mm ID, for 0.45-0.53mm
ID columns) 10/pk
5080-8773
$ 38
Gas leak detector 115V
Gas leak detector 220V
5182-9646
5182-9648
$1859
$1859
• Condition the column as specified in the
literature provided with each column.
Causes of Performance Degradation
Column Breakage
Prevention
Fused silica columns can break wherever
there are small scratches or abrasions in
the protective polyimide coating.
Continuous heating and cooling of the
oven, vibrations caused by the oven
fan as well as being wound on a circular
cage all place stress on the tubing.
While under these stresses, flaws
will propagate until breakage occurs.
• Avoid scratches and abrasions by not
exposing the column to sharp edges such
as column hangers and tags, metal edges
in the GC oven, column cutters and other
miscellaneous items on the lab bench.
NOTE: Larger diameter columns
(0.45- 0.53mm id) are more prone
to breakage.
• Avoid winding or bending the column
too tightly.
Recovery
Description
Part No.
Price
Fused Silica Union,
Universal 2-way
(5/pk)
705-0905
$ 50
Quartz deactivated
column connector
(5/pk)
5181-3396 $ 94
Polyimide Sealing
resin (5 grams) 500-1200
$ 24
• If a broken column has been heated,
damage to the stationary phase is very
likely. Discard the back of the column
(the column half without carrier gas).
Trim 6 inches off the end of the
column and reinstall.
• If the broken column has not been
heated, connect the two pieces with
a low volume union. No more than
2-3 unions should be installed for
one column.
59
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•
800 227 9770
COLUMNS
Thermal Damage
Exceeding a column’s upper temperature
limit results in accelerated degradation of
the stationary phase and tubing surface.
This results in the premature onset of
excessive column bleed, peak tailing for
active compounds and/or loss of efficiency
(resolution).
Prevention
• Do not exceed the columns specified
upper temperature limits:
– Isothermal limit: temperature that
the column can be held at for an
indefinite time
– Programmed limit: maximum column
temperature; column should only be
held there for about 5-10 minutes
• Set the GC maximum oven temperature
function at or a few degrees above the
temperature limit of the column. With
two columns in the oven be sure to set
the maximum temperature to the
temperature limit of the column with the
lowest value.
Recovery
• Disconnect column from detector
• Heat the column 8-16 hours at the
isothermal limit
• Remove 10-15 cm from the column end
• Reinstall into the detector and condition
as usual
NOTE: Thermal damage cannot be reversed.
The column usually does not return to its
original performance; however, it is often
still functional. The life of the column will
be reduced after thermal damage.
Oxygen Damage
Oxygen is an enemy to all capillary GC
columns. Constant exposure to oxygen
does not damage the column at or near
ambient temperatures; however, severe
damage occurs as the column temperature
increases. A leak in the carrier gas flow
path (e.g., gas lines, fittings, injector,
septa) is the most common source of
oxygen exposure. As the column is heated,
very rapid degradation of the stationary
phase occurs. This results in the premature
onset of excessive column bleed, peak
tailing for active compounds and/or loss of
efficiency (resolution).
Description
Part No.
Price
FlowTracker 2000 Flowmeter and Leak Detector
5183-4780
$1143
Big Oxygen Trap (750 cc, 1/8" fitting)
BOT-2
$ 235
Big Moisture Trap (750 cc, 1/8" fitting)
BMT-2
$ 235
Big Universal Trap (Combination Trap)
(750cc, 1/8" fitting, He)
RMSH-2
$ 261
Advanced Green Septa (11mm, 50/pk)
5183-4759
$ 62
NOTE: Momentary exposure to oxygen
such as an injection of air or removing
the septum nut for a short period of
time is not a problem.
Prevention
Maintain an oxygen and leak-free
system by:
• performing periodic leak checks
• changing septa regularly
• using high quality carrier gases
• installing and maintaining oxygen traps
• changing gas cylinders before they are
completely empty
Recovery
Perform column “bakeout” as described
under thermal damage recovery.
NOTE: Oxygen damage occurs very rapidly.
In less severe cases, the column may still
be functional but at a reduced performance
level. In more severe cases, the column is
irreversibly damaged.
TIPS AND TOOLS
Install a moisture trap upstream of the oxygen trap to increase
the oxygen trap lifetime.
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60
COLUMNS
Chemical Damage
GUARD COLUMN
Inorganic or mineral acids and bases are
the primary sources of chemical damage
to stationary phases. Most of these acids
and bases have low volatility and
accumulate at the front of the column.
If allowed to remain, the acids or bases
damage the stationary phase. The only
organic compounds that have been
reported to chemically damage stationary
phases are perfluoroacids and these need
to be present at high levels (e.g., 1% or
higher). This results in the premature
onset of excessive column bleed, peak
tailing for active compounds and/or loss
of efficiency (resolution).
A guard column is a piece of fused silica tubing attached with a union to
the front of the analytical column with the following characteristics:
NOTE: Hydrochloric acid and ammonium
hydroxide are the least harmful of the
group as both tend to follow any water
that is present in the sample. Thus, if HCl
or NH4OH are present in a sample,
minimizing water retention will render
these compounds relatively harmless
to the column.
• Material should be deactivated fused silica tubing to minimize solute
interactions.
• Length should be from 1-10 meters. Typical lengths of 5-10 meters allow
substantial trimming before the entire guard column has to replaced.
• Internal diameter are generally the same as the column. Guard columns
with larger ids can be used for additional residue capacity.
• A low volume union should be used to attach the tubing to the column.
Glass pressfit unions are inexpensive and easy to install. DuraGuard
columns offer the guard column built into the analytical column as a
single piece of fused silica, eliminating the need for unions.
Guard columns are used to minimize the effect of non-volatile residues
on the analysis. The non-volatile residues deposit in the guard column and
not in the analytical column. This greatly reduces the interaction between
the residues and the sample. Periodic cutting or trimming of the guard
column is usually required upon a build-up of residues. The onset of peak
shape problems is the usual indicator that the guard column needs
trimming or changing.
Prevention
• Perform sample preparation to remove
inorganic acids and bases from the
sample
• Install guard column and trim frequently
• If acids or bases must be used choose an
organic alternative or HCl or NH4OH
Guard Column
INJECTOR
DETECTOR
Recovery
• Remove 0.5 to 1 meter from the front
of the column
• Severe cases may require the removal
of 5 or more meters
Column
Guard Column
Column Contamination
Column contamination is the most
common problem encountered in capillary
GC. Unfortunately, it mimics most other
chromatographic problems and is often
misdiagnosed. A contaminated column
is usually not damaged, but it may be
rendered unusable. There are two basic
types of contaminants: nonvolatile and
semivolatile.
61
Union
Guard column installation instructions are available at www.agilent.com/chem.
Click on “Technical Support,” then “GC Reference Library.” The procedure can be
found under “General Information.”
www.agilent.com/chem
•
800 227 9770
COLUMNS
Nonvolatile Contaminants
Description
Part No.
Price
Split/Splitless Inlet liner: glass wool,
taper, deactivated (5/pk)
5183-4712
$112
Splitless Inlet liner: single-taper,
no glass wool, deactivated (5/pk)
5183-4695
$124
Quartz deactivated column
connector (5/pk)
5181-3396
$ 94
Polyimide sealing resin (5 grams)
500-1200
$ 24
Deactivated Fused silica,
10m, 0.53mm i.d.
160-2535-10
$110
• Perform sample cleanup to remove
nonvolatile materials from the sample
Deactivated Fused silica,
10m, 0.25mm i.d.
160-2255-10
$ 73
• Use injection port liners packed with
glass wool (may not be feasible when
analyzing active compounds)
Capillary column rinse kit
430-3000
$ 78
Nonvolatile contaminants or residues do
not elute and accumulate in the column
(most often confined to the first few
meters). The column becomes coated with
these residues which interfere with the
proper partitioning of solutes in and out
of the stationary phase. Also, the residues
may interact with active solutes resulting
in peak adsorption problems (evident as
peak tailing or loss of peak size). Active
solutes are those containing a hydroxyl
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes.
Prevention
• Install a guard column and trim regularly
Recovery
• Do not bakeout the column
• Front End Maintenance:
– Clean or change the injection port liner
– Clean out the injector
– Cut off typically 0.5 to 1 meter of the
front of the column
• Turn the column around (install detector
end into injector). Not recommended for
sensitive ECD, NPD, and MS detectors.
• Solvent rinse the column
• Cut the column in half and use the back
half (detector side)
Semivolatile Contaminants
Semivolatile contaminants or residues
accumulate in the column, but eventually
elute. Hours to days may elapse before
they completely leave the column. Like
nonvolatile residues, they may cause peak
shape and size problems and, in addition,
are usually responsible for many baseline
problems (instability, wander, drift, ghost
peaks, etc.).
Prevention
Column Storage
• Perform sample cleanup to remove
semi-volatile materials from the sample
Capillary columns should be stored in their
original box when removed from the GC.
Place GC septa over the ends to prevent
debris from entering the tubing. Upon
reinstallation of the column, the column
ends need to be trimmed by 2-4 cm to
ensure that a small piece of septa is not
lodged in the column.
• Increase the final temperature of the
GC run (not to exceed the temperature
limit of the column)
• Change septa regularly
Recovery
• Bakeout the column: limit 1-2 hours
(excess baking may polymerize some
contamination and reduce column
lifetime)
• Solvent rinse the column
Does Your Sample Have Residues?
Perform this simple test.
If a column is left in a heated GC, there
should always be carrier gas flow through
the column. The carrier gas flow can be
turned off only if the oven, injector,
detector and transfer lines are turned off
(i.e., not heated). Without carrier gas flow,
damage to the heated portion of the
column occurs.
1. Place 20-30 µL of the sample onto a
microscope slide.
2. Put the slide over the heated GC inlet
for 20 minutes.
3. Hold the slide up to the light.
If you can see anything where the drop
was, your sample has residues.
www.agilent.com/chem
•
800 227 9770
62
COLUMNS
Column Types and Characteristics
DB-1ms
• 100% Dimethylpolysiloxane
• Identical selectivity to DB-1
• Nonpolar
• Very low bleed characteristics
• Improved acid performance compared to
standard 100% Dimethylpolysiloxane
columns
• Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
• Excellent general purpose column
• Bonded and cross-linked
• Solvent rinsable
63
DB-1ms Order Guide Temperature Limits (-60 to 340/360°C)
I.D.
Length
Film
Part No.
Price
0.10
0.10
0.10
0.10
10
10
20
20
0.10
0.40
0.10
0.40
127-0112
127-0113
127-0122
127-0123
$343
$343
$495
$495
0.20
0.20
12
25
0.33
0.33
128-0112
128-0122
$261
$400
0.25
0.25
0.25
30
30
60
0.10
0.25
0.25
122-0131
122-0132
122-0162
$483
$483
$823
0.32
0.32
0.32
30
30
60
0.10
0.25
0.25
123-0131
123-0132
123-0162
$521
$521
$896
Similar Phases
Applications
HP-1ms, Rtx-1ms, CP-Sil 5CB
General purpose: Amines, hydrocarbons,
pesticides, PCBs, phenols, sulfur
compounds, flavors and fragrances.
www.agilent.com/chem
•
800 227 9770
COLUMNS
DB-5ms
DB-5ms Order Guide Temperature Limits (-60 to 325/360°C)
• Phenyl Arylene polymer equivalent to a
(5%-Phenyl)-methylpolysiloxane
• Nonpolar
• Very low bleed characteristics
• Excellent inertness for active compounds
• Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Certified for MS
• Exact replacement of HP-5TA
• Close equivalent to USP Phase G27
HP-5ms
I.D.
Length
Film
Part No.
Price
0.18
0.18
20
40
0.18
0.18
121-5522
121-5542
$412
$740
0.20
0.20
25
50
0.33
0.33
128-5522
128-5552
$400
$674
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
25
25
30
30
30
50
60
60
0.25
0.40
0.10
0.25
0.50
0.25
0.10
0.25
122-5522
122-552A
122-5531
122-5532
122-5536
122-5552
122-5561
122-5562
$421
$421
$483
$483
$483
$753
$823
$823
0.32
0.32
0.32
0.32
0.32
0.32
30
30
30
50
60
60
0.10
0.25
0.50
0.25
0.10
0.25
123-5531
123-5532
123-5536
123-5552
123-5561
123-5562
$521
$521
$521
$804
$896
$896
Similar Phases
Applications
Rtx-5ms, HP-5ms, PTE-5, CP-Sil 8CBms,
BPX-5
Semivolatiles, alkaloids, drugs, FAMEs,
halogenated compounds, pesticides,
herbicides
HP-5ms Order Guide Temperature Limits (-60 to 325/350°C)
• (5%-Phenyl)-methylpolysiloxane
• Nonpolar
• Very low bleed characteristics
• Excellent inertness for active compounds
• Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Certified for MS
• Equivalent to USP Phase G27
Similar Phases
Rtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms,
BPX-5, Rtx-5 Amine
Applications
Semivolatiles, alkaloids, drugs, FAMEs,
halogenated compounds, pesticides,
herbicides
I.D.
Length
Film
Part No.
Price
0.20
0.20
0.20
12
25
50
0.33
0.33
0.33
19091S-101
19091S-102
19091S-105
$261
$400
$674
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
15
15
15
30
30
30
60
60
0.10
0.25
1.00
0.10
0.25
0.50
0.10
0.25
19091S-331
19091S-431
19091S-231
19091S-333
19091S-433*
19091S-133
19091S-336
19091S-436
$295
$295
$295
$483
$483
$483
$823
$823
0.32
0.32
0.32
0.32
0.32
0.32
0.32
15
25
30
30
30
60
60
1.00
0.52
0.10
0.25
0.50
0.10
0.25
19091S-211
19091S-112
19091S-313
19091S-413
19091S-113
19091S-316
19091S-416
$319
$448
$521
$521
$521
$896
$896
* This column is shipped with the 5973 MSD.
www.agilent.com/chem
•
800 227 9770
64
COLUMNS
DB-XLB
• Exceptionally low bleed
• Low polarity
• Extended temperature limit of 360°C
• Unique selectivity
• Excellent inertness for active compounds
• Ideal for confirmational analyses
• Excellent for pesticides, herbicides, PCBs
and PAHs
• Certified for MS
• Bonded and cross-linked
• Solvent rinsable
DB-35ms
• Equivalent to a (35%-Phenyl)methylpolysiloxane
• Midpolarity
• Very low bleed characteristics
• Extended temperature limit of 360°C
• Excellent inertness for active compounds
• Certified for MS
• Ideal for confirmational analyses
• Bonded and cross-linked
• Solvent rinsable
• Replaces HP-35ms
• Close equivalent to USP Phase G42
65
DB-XLB Order Guide Temperature Limits (30 to 340/360°C)
I.D.
Length
Film
Part No.
Price
0.18
0.18
20
30
0.18
0.18
121-1222
121-1232
$412
$579
0.20
0.20
12
25
0.33
0.33
128-1212
128-1222
$261
$400
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
15
15
15
30
30
30
30
60
0.10
0.25
1.00
0.10
0.25
0.50
1.00
0.25
122-1211
122-1212
122-1213
122-1231
122-1232
122-1236
122-1233
122-1262
$295
$295
$295
$483
$483
$483
$483
$823
0.32
0.32
0.32
0.32
30
30
30
60
0.10
0.25
0.50
0.25
123-1231
123-1232
123-1236
123-1262
$521
$521
$521
$896
Similar Phase
Applications
MDN-12
PCB congeners, pesticides, chlorinated
herbicides, phenoxy acid methyl esters,
haloacetic acids
DB-35ms Order Guide Temperature Limits (50 to 340/360°C)
I.D.
Length
Film
Part No.
Price
0.20
0.20
15
25
0.33
0.33
128-3812
128-3822
$261
$400
0.25
0.25
0.25
0.25
15
30
30
60
0.25
0.15
0.25
0.25
122-3812
122-3831
122-3832
122-3862
$295
$483
$483
$823
0.32
0.32
30
60
0.25
0.25
123-3832
123-3862
$521
$896
Similar Phases
Applications
Rtx-35, SPB-35, AT-35, Sup-Herb
Aroclors, PCBs, amines, pesticides,
chlorinated herbicides, haloacetic acids,
pharmaceuticals, drugs of abuse
www.agilent.com/chem
•
800 227 9770
COLUMNS
DB-17ms
DB-17ms Order Guide Temperature Limits (40 to 320/340°C)
• Equivalent to (50%-Phenyl)methylpolysiloxane
• 320/340°C Upper temperature limit
• Very low bleed midpolarity column
• Excellent inertness for active compounds
• Enhanced mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Best column for CLP pesticides
DB-225ms
I.D.
Length
Film
Part No.
Price
0.18
20
0.18
121-4722
$412
0.25
0.25
0.25
0.25
0.25
15
15
30
30
60
0.15
0.25
0.15
0.25
0.25
122-4711
122-4712
122-4731
122-4732
122-4762
$295
$295
$483
$483
$823
0.32
0.32
30
30
0.15
0.25
123-4731
123-4732
$521
$521
Similar Phases
Applications
DB-17, HP-50+, Rtx-50, 007-17, SP-2250,
SPB-50, BPX-50, SPB-17
Drugs, glycols, pesticides, steroids
DB-225ms Order Guide Temperature Limits (40 to 240°C)
• Equivalent to (50%-Cyanopropylphenyl)methylpolysiloxane
• Mid/high polarity
• Excellent for separations of cis- and
trans-fatty acid methyl esters (FAMEs)
• Low bleed
• Bonded and cross-linked
• Solvent rinsable
• Close equivalent to USP Phase G7
I.D.
Length
Film
Part No.
Price
0.25
0.25
0.25
15
30
60
0.25
0.25
0.25
122-2912
122-2932
122-2962
$295
$483
$823
0.32
30
0.25
123-2932
$521
Similar Phases
Applications
HP-225, SP-2330, CP-Sil 43CB, RSL-500,
Rtx-225, BP-225, CB-225, OV-225, 007-225
Alditol acetates, FAMEs, neutral sterols
EASY ONLINE ORDERING
Need a column that’s custom-designed for your lab?
Just visit www.agilent.com/chem/4ecatalog
www.agilent.com/chem
•
800 227 9770
66
COLUMNS
HP-INNOWax
• Polyethylene glycol (PEG)
• High polarity
• Highest upper-temperature limits of the
bonded PEG phases
• Column-to-column repeatability
• Bonded and cross-linked
• Solvent rinsable
• Close equivalent to USP Phase G16
GS-GasPro
• Unique bonded PLOT column technology
• Excellent choice for light hydrocarbons
and sulfur gases
• Retention stability not affected by water
• Separates CO and CO2 on a single
column
• Ideal PLOT column for GC/MS –
no particles
67
HP-INNOWax Order Guide Temperature Limits (40 to 260/270°C)
I.D.
Length
Film
Part No.
Price
0.20
0.20
0.20
0.20
25
25
50
50
0.20
0.40
0.20
0.40
19091N-102
19091N-202
19091N-105
19091N-205
$379
$379
$636
$636
0.25
0.25
0.25
0.25
0.25
0.25
30
30
30
60
60
60
0.15
0.25
0.50
0.15
0.25
0.50
19091N-033
19091N-133
19091N-233
19091N-036
19091N-136
19091N-236
$413
$413
$413
$737
$737
$737
0.32
0.32
0.32
0.32
0.32
0.32
30
30
30
60
60
60
0.15
0.25
0.50
0.15
0.25
0.50
19091N-013
19091N-113
19091N-213
19091N-016
19091N-116
19091N-216
$447
$447
$447
$816
$816
$816
Similar Phases
Applications
HP-20M, SUPELCOWAX 10, CP-WAX 52CB,
SUPEROX II, CB-WAX, Stabilwax, BP-20,
007-CW, Carbowax, DB-WAXetr
Alcohols, aromatics, essential oils, solvents
GS-GasPro Order Guide Temperature Limits (-80 to 260/300°C)
I.D.
Length
Part No.
Price
0.32
0.32
30
60
113-4332
113-4362
$627
$942
Similar Phase
Applications
CP-Silica PLOT
C1 to C12 hydrocarbons, CO2, trace-level
sulfurs, hydride gases, inorganic gases,
halocarbons, SF6, oxygen/nitrogen
separation at -80°C.
www.agilent.com/chem
•
800 227 9770
Detectors
Most detectors require simple but periodic
cleaning to maintain peak performance.
This is especially true for highly sensitive
GC detectors. Without routine detector
maintenance, GC system performance will
deteriorate and can cause detector failure.
Detailed procedures on how to clean,
maintain and replace common detectors,
including FID, TCD, NPD, ECD, and FPD are
summarized in this section. Also included
are special handling techniques and specific
recommendations to maximize specific
detector operations. For example, learn how
to resolve flame ignition problems associated
with your flame photometric detector and
test electron capture detectors for
radioactivity leaks.
“GC detectors are highly sensitive systems
that are often compromised by various
types of contamination. By implementing
some recommended detector
maintenance routines, you can minimize
instrument downtime and keep your GC
system working at peak efficiency.”
Bernhard Rothweiler
Applications Chemist
CATALOG
For a complete selection of Detector supplies, see Agilent’s 2005-2006
Essential Chromatography Catalog. Or, visit our online catalog at
www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
•
800 227 9770
68
DETECTORS
Flame Ionization Detector (FID)
Flame Ionization Detectors require little
maintenance to keep them performing at
satisfactory levels. The primary task is to
occasionally measure hydrogen, air and
makeup gas flows. They can drift over time
or be changed unintentionally without
knowledge of it occurring. Each gas flow
should be independently measured to
obtain the most accurate values.
Igniter Glow Plug Assembly
Collector Assembly
Collector Body
Condensation
Since the FID combustion process
results in water formation, the detector
temperature must be kept above 100˚C to
prevent condensation. Such condensation,
especially when combined with chlorinated
solvents or samples, causes corrosion and
sensitivity loss.
FID Jets
Hardware Problems
If the flame goes out or will not light:
• Check the column flow rate. It may
be too high. Decrease the flow rate or
pressure. Switch to a more restrictive
column (longer or with a smaller id).
If you must use a large id column, first
cool the GC oven to below 50˚C, then turn
off the carrier flow long enough to allow
the FID to light. Check for partially or
completely plugged jet.
• Check that the right type of jet is installed
for the column you are using.
• Injecting large volumes of aromatic
solvent or water can cause the flame to
go out. Switch to a nonaromatic solvent
or inject less solvent.
• The lit offset value may be too low or too
high. Adjust the value.
FID Ferrules
Cleaning & Replacement
Even with normal use, deposits develop in
the jet and detector (usually white silica
from column bleed or black carbonaceous
soot). These deposits reduce sensitivity
and cause chromatographic noise and
spikes. Although you can clean the jet, it is
usually more practical to replace dirty jets
with new ones. If you do clean the jet, be
careful not to scratch the jet internally;
scratches will ruin the jet
FID Cleaning Kit, P/N 9301-0985, $41
VIDEO
To view a video on FID column installation, jet replacement,
collector maintenance, or ignitor replacement, visit
www.agilent.com/chem/techsupport.
69
www.agilent.com/chem
•
800 227 9770
DETECTORS
Jet Cleaning Procedure
6890/6850 Ionization Detector (FID) Supplies
(using Agilent’s FID Cleaning Kit #9301-0985)
1. Run a cleaning wire through the top of
the jet. Run it back and forth a few times
until it moves smoothly. Be careful not to
scratch the jet. (Do not force too large a
wire or probe into the jet opening or the
opening will become distorted. A loss of
sensitivity, poor peak shape and/or
lighting difficulties may result if the
opening is deformed.)
2. Fill an ultrasonic cleaning bath with
aqueous detergent, and place the jet in
the bath. Sonicate for five minutes.
3. Use a jet reamer to clean the inside of
the jet.
4. Sonicate again for five minutes.
NOTE: From this point on, handle the parts
Item Description
Unit
Part No.
Price
1
PTFE chimney (optional)**
19231-21050
$ 14
2
Collector nut
19231-20940
$ 35
3
Spring washer
5181-3311
$ 9
4
Ignitor castle
19231-20910
$ 57
Optional Hastelloy Ignitor Castle*
19231-21060
$184
5
Ignitor glow plug assembly
19231-60680
$ 42
6
Collector insulator
G1531-20700
$ 17
7
Collector body
Hastelloy Collector Body
G1531-20690
61531-21090
$ 60
$260
9
FID collector assembly 1
G1531-60690
$194
Detector insulation assembly
G1531-20700
$ 17
8710-1346
$ 8
10/pk
FID collector cleaning brush
2/pk
only with forceps!
Collector Housing
G1531-20740
$175
5. Remove the jet from the bath and rinse it
thoroughly, first with hot tap water and
then with a small amount of GC-grade
methanol.
FID retainer nut wrench
(5880, 5890, 6890)
19301-00150
$ 8
1/4 in. Nut Driver for FID jet-drilled shaft
8710-1561
$ 13
5182-3450
18710-20119
18710-60170
19231-60680
19244-80560
19301-60660
5180-4150
5180-4152
19301-20720
5180-4153
9301-0985
$556
$ 49
$ 44
$ 42
$ 56
$ 53
$ 23
$ 23
$ 12
$ 8
$ 41
6. Blow the jet dry with a burst of
compressed air or nitrogen, and then
place the jet on a paper towel and allow
it to air dry.
FID supplies kit-Includes:
Jet, packed standard
FID performance evaluation sample kit
Ignitor glow plug assembly
Jet, cap. series 530 µm
FID flow measuring insert
Cleaning wires for 0.03 in. ID jet
Cleaning wires: 0.018 in. ID/530 µm jet
Wire, jet cleaning,
Capillary inlet cleaning wires
Detector cleaning kit
3 each
2 each
2 each
3 each
2 each
1/pk
5 each
**Not included in assembly.
*Hastelloy components may be used when analyzing highly corrosive materials.
1 Does not include Hastelloy component.
Plugged FID jet
EASY ONLINE ORDERING
Here’s another time-saving reason to place your order through our
website: you can instantly view and edit the items in your shopping cart
– while keeping track of your total order price.
Just visit www.agilent.com/chem/4ecatalog
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•
800 227 9770
70
DETECTORS
FID Jets
Description
Length(mm)
Part No.
Price
Jets for capillary dedicated FID
Capillary jet (0.011 in./0.29 mm ID tip)
48
G1531-80560
$43
High-temperature jet (SimDIS 0.018 in. ID tip)
48
G1531-80620
$54
Capillary 0.53 mm jet (0.011 in. ID tip)
61.5
19244-80560
$56
Packed (0.018 in. ID tip)
63.5
18710-20119
$49
Packed (0.030 in. ID tip)
63.5
18789-80070
$55
0.53 mm high temp (0.018 in. ID tip) for SimDIS
61.5
19244-80620
$37
Adaptable FID
Agilent FID Jets (from top to bottom): Dedicated
capillary, Adaptable capillary, Adaptable packed
1
2
3
FID Consumables
4
Description
Unit
Part No.
Price
FID flow measuring insert
19301-60660
$53
FID ignitor cable
G1531-60680
$41
FID Performance evaluation sample kit, 0.03% C14,
C15, and C16 normal alkanes in hexane
18710-60170
$44
5080-4978
$ 7
19301-20720
$12
O-rings
12/pk
Cleaning wire
Jet cleaning wire for 0.03 in. ID jet
5/pk
5180-4150
$23
Jet cleaning wire for Series 530 mm and 0.018 in. ID jet
5/pk
5180-4152
$23
5
8
6
7
6
6890 Series GC FID Detector
TIPS AND TOOLS
Collector Body, P/N G1531-20690
Different size jets are available to optimize flame shape for capillary columns, or
reduce contamination build-up for high molecular weight eluents. Usually, small
bore jets produce the greatest signal, but can plug up or contaminate more easily
relative to large jets, so compromise may be necessary.
71
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•
800 227 9770
DETECTORS
Electron-Capture Detector (ECD)
Agilent provides two types of electron
capture detectors. The regular detector
(ECD) has a larger internal volume
(approximately 10 times) than the microcell detector (µ-ECD). These two types can
be distinguished by the top cover of the
detector – the ECD has a solid cover and
the µ-ECD has a perforated cover.
Radioactivity Leak Test
Thermal Cleaning
The procedure used is a “wipe test.” A
wipe test kit is supplied with each new
detector. Refer to the information card
supplied in the Wipe Test Kit for
instructions on performing the test.
If your baseline is noisy or the output
value is abnormally high and you have
determined that these problems are not
being caused by leaks in the GC system,
you may have contamination in the
detector from column bleed and sample
residues. To remove contamination, you
should perform a thermal cleaning
(bakeout) of the detector.
Warning: Detector disassembly and/or
cleaning procedures other than thermal
should be performed only by personnel
trained and licensed appropriately to
handle radioactive materials. Trace
amounts of radioactive 63Ni may be
removed during other procedures,
causing possible hazardous exposure
to ß and x-radiation.
Electron capture detectors must be tested
for radioactive leakage at least every six
months. Records of tests and results must
be maintained for possible inspection by
the Nuclear Regulatory Commission and/or
the responsible local agency. More frequent
tests may be conducted when necessary.
Gas Purity
For successful EC detection, it’s important
that the carrier and purge gases are very
clean and dry (99.9995%). Moisture,
oxygen, or other contaminants can improve
sensitivity, but at a cost of linear range.
Always precondition the column before
connection to the detector.
ECD Warnings
Although beta particles at this energy level have little penetrating power – the
surface layer of the skin or a few sheets of paper will stop most of them – they
may be hazardous if the isotope is ingested or inhaled. For this reason the cell
must be handled with care. Radioactive leak tests must be performed at the
required intervals, the inlet and outlet fittings must be capped when the detector
is not in use, corrosive chemicals must not be introduced into the detector, and
the effluent from the detector must be vented outside the laboratory environment.
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•
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72
DETECTORS
Electron-Capture Detector (ECD) Supplies
Item Description
Part No.
Price
1
ECD makeup gas adapter*
G1533-80565
$198
2, 3 Nut warmer cup with insulation
19234-60720
$ 58
ECD adapter replacement liner, fused silica
19233-20625
$ 15
ECD end cap
19233-20755
$ 32
ECD chemical sample kit, 3 ampoules
solution of 33 pg/mL (0.033 ppm)
each of lindane and aldrin in isooctane
18713-60040
$ 46
ECD wipe test kit
18713-60050
$ 31
*Includes one each of P/N 19233-20625 and P/N 19233-20755
1
2
3
6890 Series GC ECD Detector
ECD Wipe Test: A wipe test kit (P/N 18713-60050) is supplied with each new ECD. The kit
includes an information card with instructions for performing the test. Records of tests and
results must be maintained for possible inspection by the NRC (Nuclear Regulatory
Commission) and/or responsible state agency.
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom,
even at your site. See pages 104-115 for more information about our
services and support.
73
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•
800 227 9770
DETECTORS
Thermal Conductivity Detector (TCD)
The TCD compares the thermal
conductivities of two gas flows – pure
carrier gas (also called the reference gas)
and carrier gas plus sample components
(also called column effluent).
Filament Maintenance
The primary maintenance for a TCD
involves the filament. Most procedures
involve improving filament life or keeping
the filament from becoming damaged or
contaminated.
A constant presence of oxygen can
permanently damage filaments through
oxidative processes. The most common
source of oxygen is a leak(s) near the
detector – or in the carrier or makeup
gas line fittings. Oxygen traps are
recommended for the carrier and makeup
gases to reduce oxygen levels. Proper
column installation techniques and regular
leak checks (especially after column
installation) help to keep leak problems to
a minimum.
The damage caused by oxygen is more
severe at high filament currents.
Chemically active sample components
such as acids and halogenated compounds
may attack and damage the filaments.
Avoiding these compounds when possible
increases filament life. Turning off or
substantially reducing the filament current
when the TCD is not in use also prolongs
filament life.
Increasing Filament Lifetime
Cell Contamination
Increased filament lifetime will result if the
following startup process is used:
Cell contamination is a problem when a
lower detector temperature is used to
improve sensitivity. Also, low filament
currents promote contamination since
the filament is maintained at a lower
temperature at lower currents. If the cell
becomes contaminated, a solvent flush
of the detector may help to remove the
condensed material.
1. Purge the detector with carrier and
makeup gas for 10-15 minutes before
turning on the filaments. This prevents
oxidation of the filaments due to the
presence of oxygen that has diffused
into the cell under no flow conditions.
2. Turn on the filaments at the lowest
possible current setting, then increase
the filament current in several
increments to the desired value. This
reduces the power surge upon current
introduction and prolongs filament
lifetime.
Thermal Conductivity Detector (TCD) Supplies
Description
Unit
Part No.
Price
G1532-60675
$1030
18740-20950
$ 18
18740-20960
$ 33
6890/6850/5890 Common TCD Supplies
TCD replacement cell (6890/6850 only)
TCD cap column adapter seal
10/pk
TCD cap column adapter
Graphite ferrules, 1.0 mm id
10/pk
5080-8773
$ 38
Graphite ferrules, 0.5 mm id
10/pk
5080-8853
$ 47
Capillary column nut, for 6890
2/pk
5181-8830
$ 26
Capillary column nut, for 6850
2/pk
5183-4732
$ 47
G1532-20710
$ 44
TCD chemical sample kit, 3 ampoules,
0.5 mL, 5 solution of 0.3% C14, C15, and C16, normal
alkanes in hexane
18711-60060
$ 45
TCD packed column adapter (6890/6850 only)
5890 TCD Supplies
www.agilent.com/chem
•
800 227 9770
Makeup gas adapter, TCD
19232-80550
$ 126
TCD column adapter, 1/8 to 1/4 in. glass
19302-80020
$ 138
TCD replacement cartridge
19232-60676
$1625
74
DETECTORS
Solvent Flush Procedure
1. Cool the cell to room temperature and
remove the column.
2. Place a septum in a nut or fitting
assembly that fits onto the detector
entrance.
3. Place the nut or assembly on the
detector fitting and tighten. Verify
the presence of makeup gas flow.
4. Inject 20-100 µL volumes of toluene or
benzene into the detector through the
septum. Inject a total volume of at
least 1mL of solvent. Do not inject
halogenated solvents such as methylene
chloride and chloroform into the
detector.
75
5. After the final injection, allow makeup
gas to flow for 10 minutes or more.
Slowly raise the temperature of the cell
to 20-30˚C above the normal operating
temperature.
6. After 30 minutes, decrease the
temperature to the normal value and
install the column as usual.
Thermal Cleaning
The TCD can become contaminated with
deposits from such things as column bleed
or dirty samples. A wandering baseline,
increased noise level, or changes in
response on a checkout chromatogram all
indicate contamination. Thermal cleaning,
or bakeout (heating the detector block to
evaporate the contaminant), should be
performed only after you have confirmed
that the carrier gas and the flow system
components are leak-free and
contaminant-free.
Watch out for decreased sensitivity caused
by samples that react with the filament,
originating from oxygen-contaminated
carrier gas, leaks in plumbing, or column
bleeding. Samples with active components,
such as acids and halogenated compounds
can chemically attack the filament as
well. Also, sample condensation will
contaminate the detector cell if the
temperature is too low.
Some types of contaminants can be
removed by temperature bakeout. Also,
in non-modulated designs, wandering
baselines due to temperature variation can
be corrected by making sure the detector
temperature remains constant.
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•
800 227 9770
DETECTORS
Flame Photometric Detector (FPD)
Maintenance
Flame Photometric Detectors require
minimal maintenance to keep them
performing at satisfactory levels. The
hydrogen, air and makeup gas flows should
be measured occasionally. They can drift
over time or be changed unintentionally
without knowledge of it occurring. Each gas
flow should be measured independently to
obtain the most accurate values.
Cleaning & Parts Replacement
The FPD requires periodic cleaning. In
most cases, this only involves the jet, and
less frequently, the filter. Agilent provides
brushes and wires that simplify the
cleaning of all detector parts (see FPD
Supplies on page 77). The brushes are
used to dislodge particulates clinging to
the metal surfaces. A fine wire is used to
clean the jet opening of particulates. Do
not force too large a wire or probe into the
jet opening or the opening may become
distorted. A loss of sensitivity, poor peak
shape, and/or lighting difficulties may
result if the opening is deformed. The filter
or any of the window parts should be
handled gently. Scratches or other surface
deformities reduce the amount of light
passing through the filter, thus reducing
response. The filter and related parts
should be clean and free from fingerprints.
The Photo Multiplier Tube (PMT) needs
periodic replacement. The PMT is defective
and needs to be rebuilt or replaced if:
• high voltage is on and the flame is lit
• low or no signal and/or noise not
attributed to any other source such as
bad cables are observed
• light leaks occur
• high temperatures are used
• defective signal boards are present
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•
800 227 9770
High detector temperatures reduce the
PMT life. When not in use, turn off the
PMT to maximize its usable lifetime. Some
PMTs may have a shelf life and should not
be stored for prolonged periods before use.
Column bleed and/or effluent can
contaminate the first quartz window (heat
shield) nearest the detector module. Dust,
fingerprints, and atmospheric
contaminants can dirty both quartz
windows, the filter, and/or the
photomultiplier tube window.
Contamination anywhere along the light
path between flame and PMT can reduce
detector sensitivity.
If a response problem is encountered
(sensitivity, noise, selectivity) the FPD jet
should be inspected for deposits and, if
necessary, cleaned or replaced. To properly
service the jet, the detector module should
be removed from the instrument, and
followed by appropriate service (see jet
cleaning procedure on page 70).
• If the flame doesn’t light at all, check the
glow plug circuit. Observe the visual
display, which will momentarily go to
greater than 65500 counts when the
flame lights. If the display doesn’t
change, check the pin connections at the
printed circuit board, the lead connection
on the glow plug and the appropriate 5A
fuse on the GC main circuit board.
• The flame is easier to light at higher
detector temperatures.
• Under some operating conditions, the
flame may be more easily lit with the
rubber drip tube removed. After lighting
the flame, reinstall the drip tube.
• If the flame still won’t light, there could
be a large leak in the system. This results
in measured flow rates being different
from actual flow rates, causing non-ideal
ignition conditions. Thoroughly leak
check the whole system.
Flame Conditions & Gas Flows
If the FPD flame won’t light or stay lit:
The flame conditions are critical to
successful operation. Since the detection
zone is above the flame, the gas flows and
jet diameter must be optimized so that
components burned (activated) in the
flame will emit in the detection zone.
• Be sure there is a problem. Ignition is best
confirmed by holding a mirror or shiny
surface near the aluminum exhaust tube,
with the rubber drip tube removed, and
observe condensation if the flame is lit.
Gas flows are also critical for optimized
selectivity and sensitivity. The most critical
parameters are the hydrogen/air or
hydrogen/oxygen ratio, and the total gas
flow, which effects flame temperature.
Occasionally, the transfer line fused silica
liner between the column and FPD module
must be inspected, cleaned and/or replaced.
Flame Ignition Problems
• Check Lit Offset. If it is zero, autoignition
is turned off. If it is too large, the GC will
not know that the flame is lit and will
shut down the detector.
• Increase the air supply pressure to the
pneumatics module. This makes the
flame easier to light but does not affect
the air flow rate setpoint.
76
DETECTORS
6890/5890 FPD Supplies
Item Description
1
Exit tube assembly
2
Nut, brass, 1/4 in.
Unit
Part No.
Price
19256-60700
$ 72
5180-4105
$ 13
1
10/pk
2
3
4
Weldment, block
19256-80560
$536
5
O-ring, ignitor, Kalrez
0905-1610
$ 42
6
Spacer, ignitor
19256-20590
$ 15
7
FPD Ignitor Replacement Kit
19256-60800
$ 68
8
Ignitor cable assembly (6890 only)
G1535-60600
$ 22
9
Gasket, heat shield
19256-80045
$ 83
10
Window, first heat shield
19256-80030
$ 38
11
Disk, heat shield
19256-20580
$ 80
12
Coupling, SS
19256-20550
$165
14
Screw, M3 x 12 (4 required)
0515-0911
$ 1
15
Clamp
19256-00090
$ 59
16
O-ring, inner window
5061-5886
$ 24
17
Window, second heat shield
19256-80060
$ 40
18
O-ring, outer window
5061-5891
$ 24
19
Flange adapter
19256-20510
$131
20
Flange ring
19256-00200
$ 22
21
O-ring, Viton, 1.239 in. id
5061-5890
$ 21
Adapter weldment, 1/8 in. columns
19256-80590
$141
Adapter weldment, capillary
19256-80570
$114
Start-up kit (5890 only)
19256-60500
$434
5061-5867
$ 17
Liner/ferrule kit
19256-60590
$ 89
Sulfur filter
19256-80000
$378
Phosphorus filter
19256-80010
$378
Kalrez O-ring, size 2-002
0905-1609
$ 42
Kalrez O-ring, size 2-011
0905-1608
$ 42
5061-5889
$ 19
19305-60580
$ 40
4
7
6
9
5
10
11
12
8
13
14
15
16
17
18
Fluorocarbon Elastomer O-ring,
brown, 0.926 in. id
12/pk
12/pk
12/pk
12/pk
FPD Performance Evaluation Sample: Solution of
20 ng/mL (20 ppm) dodecanethiol and
tributylphosphate in isooctane, 3 ampoules
77
20
21
Install the correct optical
filter, depending on the
choice of Sulfur or
Phosphorus mode.
For Sulfur Mode, use
the 393 nanometer filter.
For Phosphorus Mode,
use the 525 nanometer filter.
www.agilent.com/chem
•
MAINTENANCE MINDER
FPD O-ring (5890 only)
12/pk
19
800 227 9770
DETECTORS
Nitrogen-Phosphorus Detector (NPD)
Bead Maintenance
Bead Life
Gas Flow
NPDs are temperamental and require
frequent maintenance. Small changes in any
of a number of parameters can significantly
change the performance characteristics of
an NPD. The bead requires the most
maintenance. It needs to be changed
frequently, thus a spare is a necessity.
To extend the life of the bead:
• Use the lowest practical adjust offset or
bead voltage.
The beads have to be kept dry which limits
their storage life to about six months. When
a new bead is installed, slowly raise the
detector temperature and bead current.
Rapid heating can crack or break the bead
especially if it has been stored under humid
conditions. It has been observed that higher
hydrogen flows and bead currents decrease
bead life. If the NPD is not in use, the
hydrogen flow and bead current should be
reduced or turned off to increase bead life.
Make sure there is some type of gas flow in
a heated detector or when there is current to
the bead.
• Keep the detector temperature high
(320 – 335˚C).
The hydrogen, air and makeup gas flows
should be measured frequently. They can
drift over time or be changed unintentionally
without knowledge of it occurring. Each gas
flow should be measured independently to
obtain the most accurate values. NPDs are
very sensitive to changes in the gas flows
and consistent flows are necessary to
maintain performance levels.
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•
800 227 9770
• Run clean samples and keep the inlet/liner
clean to minimize contamination.
• Turn off the bead when not in use.
• Turn off the hydrogen flow during solvent
peaks and between runs.
• If the NPD is off for an extended period
of time in a high humidity environment,
water may accumulate in the detector.
To evaporate this water, set the detector
temperature to 100˚C and maintain it
for 30 minutes. Then set the detector
temperature to 150˚C and maintain it
for another 30 minutes.
Gas Purity
Because of its high sensitivity, the NPD
requires very pure gases (99.999% or better).
We strongly recommend that moisture and
hydrocarbon traps be used on the carrier
gas and all detector gases, including the
detector hydrogen, air, and makeup gases.
Dirty gases will not only give poor
chromatographic performance, but will
shorten the bead life as well.
78
DETECTORS
Cleaning & Replacement
The NPD requires periodic cleaning. In most
cases, this only involves the collector and
the jet. Agilent provides brushes and wires
that simplify the cleaning of all detector
parts (see NPD Supplies on page 79). The
brushes are used to dislodge particulates
clinging to the metal surfaces. A fine wire is
used to clean the jet opening of particulates.
Do not force too large a wire or probe into
the jet opening or the opening will become
distorted. A loss of sensitivity or poor peak
shape may result if the opening is deformed.
The various parts can be ultrasonicated after
cleaning with a brush. Eventually the jet
needs to be replaced, so it is strongly
recommended to have spare jets on hand.
Over time, residue from the bead or sample
can build up in the collector and cause
baseline problems. You should clean the
collector after you have changed the bead
two or three times.
The metal C-rings wear slightly with each
assembly and disassembly. After several
assemblies and disassemblies (five or more),
the rings may not seal effectively, causing an
erratic baseline. A ceramic insulator and seal
kit is available. Always cool the detector to
near-ambient when changing seals and
insulators.
Because there is no flame in the NPD, the
jet does not collect silica and soot as does
the FID jet. Although you can clean the jet, it
is usually more practical to simply replace
dirty jets with new ones. If you do clean the
jet, use the cleaning wire, taking care not to
damage the inside of the jet. You can also
use a sonicator bath to clean the jet.
Contaminants
Some chemical problems can also arise
when using the NPD. Because it is a trace
detector, be careful not to contaminate the
analytical system.
Glassware
Glassware must be very clean. Phosphate
detergents should be avoided, so acid
washing of glassware followed by distilled
water and solvent rinsing is recommended.
Solvents
Solvents should be checked for purity.
Chlorinated solvents and silanizing reagents
can decrease the useful lifetime of the alkali
source; excess reagent should be removed
prior to injection, if possible.
Other Contamination Sources
Phosphate-containing leak detectors,
phosphoric acid-treated columns or glass
wool, polyimide-coated columns, or
nitrogen-containing liquid phases can add
noise to the system and should be avoided.
NPD Jets
Description
Part No.
Price
48
G1531-80560
$ 43
Capillary 0.53 mm jet (0.011 in. id tip)
61.5
19244-80560
$ 56
Packed (0.018 in. id tip)
63.5
18710-20119
$ 49
Capillary jet (0.011 in./0.29 mm id tip)
(6890 only, dedicated)
Length (mm)
6890/5890 Adaptable
79
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•
800 227 9770
DETECTORS
Nitrogen-Phosphorous Detector (NPD) Supplies
Item
Description
Part No.
Price
6890 NPD Supplies
1
Screws, M3 x 0.5 x 8 mm (Pozidriv)
0515-0655
$ 1
2
NPD white ceramic bead assembly*
G1534-60570
$368
NPD black ceramic bead assembly**
5183-2007
$379
3
Lid weldment
G1534-80510
$160
4
Metal C-ring, top
0905-2580
$ 53
5
Alumina insulator, upper
G1534-40020
$ 72
6
Collector funnel
G1534-20530
$ 64
7
Alumina insulator, lower
G1534-40030
$ 42
8
Metal C-ring bottom and top
0905-1284
$ 53
9
Screw, M4 x 10 mm
0515-2495
$ 1
10
J-Clamp
1400-0015
$ 1
11
Screw, M4 x 10 mm
0515-2495
$ 1
12
NPD interconnect assembly
G1534-60610
$160
13
Mounting pallet
G1531-40020
$ 29
14
Jets (see page 79)
15
Base weldment, Capillary NPD
G1534-80500
$501
Base Weldment, Packed NPD
G1534-80540
$532
Lid stop
G1534-20590
$ 36
NPD Ceramic Insulator Kit
includes items 4, 5, 7, and 8
5182-9722
$175
19234-60720
$ 58
NPD collector (NPD bead)
19234-60540
$289
Recoating kit, sufficient for 10 collectors
5080-8872
$216
Detector Trap Replacement Kit
19231-60790
$284
16
17
Column adapters for packed NPD
18
Nut warmer cup with insulation
2
1
3
9
10
11
12
4
5
6
8
7
13
14
15
16
17
18
5890 NPD Supplies
*This bead is more sensitive, but exhibits some tailing for phosphorous compounds.
Quantity discounts available.
**The black bead is potentially a little less sensitive, but does not exhibit peak tailing and
typically has a longer lifetime.
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•
800 227 9770
80
You asked … we listened!
Our new e-Catalog makes online
ordering easier than ever.
We’ve streamlined our online store to complement
the design and content of our 2005-2006 Essential
Chromatography Catalog.
Visit www.agilent.com/chem/4ecatalog
for one-click access to:
• A time-saving “quick-buy” feature
• Product pricing links (when available)
• Local sales contact information
• Online quote requests
• Order status updates
• Real-time customer support … and more
GC/MS Systems
Your mass spectrometer is a sensitive,
highly specialized device that offers
more functionality – and requires more
maintenance – than other GC detectors.
Therefore, we have devoted an entire
section of this guide to MSDs.
“We offer intelligent, creative solutions
to help our customers maximize the
performance of their GC/MS systems.”
Jim McCurry
Senior Applications Chemist
CATALOG
For a complete selection of gas management supplies, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
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•
800 227 9770
82
GC/MS SYSTEMS
Maintaining Mass Selective Detectors (MSDs)
Some parts of the MSD require regularly scheduled maintenance.
Common maintenance tasks are listed in the table below. It is advisable to keep a log book
of system performance, Autotune, and maintenance operations performed. This makes it
easier to identify variations from normal performance and to take corrective action. Subtle
differences may exist between MSD models. Consult your hardware manual for specific
instruction.
Every day
Check, and if necessary, replace the
septum. Check the injection port liners.
Check the tightness of the column nuts.
Hint: With Agilent’s new Flip Top Inlet
Sealing System, you don’t have to check or
change liners. So you save time and effort.
See page 52 for ordering information.
Every week
Check the foreline pump oil level and
diffusion pump fluid. Change the injection
port liners and O-rings. Gas ballast the
foreline pump.
Every month
Clean the split/splitless inlet vent line
trap. Check for leaks (inlet and column
connections).
Every three months
Replace gas cylinders (when below
500 psig).
TASK
Tune the MSD
Change injection port liners
Check the foreline pump oil level
Gas ballast the foreline pump
Check the calibration vial
Replace the foreline pump oil
Check the diffusion pump fluid
Replace the diffusion pump fluid
Replace the traps and filters
Clean the ion source
Change the carrier gas trap(s) and purifier
Replace the worn out parts
Lubricate seals (where appropriate)
Replace column
EVERY
WEEK
EVERY
6 MONTHS
EVERY
YEAR
AS
NEEDED
•
•*
•
•
Every six months
Replace the foreline pump oil. Check,
and if necessary, refill the calibration vial.
Every year
Replace the diffusion pump fluid.
Recondition or replace internal and external
traps and chemical filters on the GC.
•
•
As needed
•
•
•
•
•
•
•
•
Tune the MSD. Clean the ion source.
Replace the carrier gas trap. Replace
worn-out parts (filaments, EM, etc.).
Replace the column. Lubricate seals.
Monitor
Record all tune values such as electron
multiplier and ion source parameters in
a log book to monitor instrument
performance. In addition note the high
vacuum and foreline vacuum pressures.
*For more information on inlet maintenance, see pages 26-34.
83
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•
800 227 9770
GC/MS SYSTEMS
Contamination
Contamination is usually identified by excessive background in the
mass spectra. It can come from the GC or from the MSD. The source
of the contamination can sometimes be determined by identifying the
contaminants. Some contaminants are much more likely to originate
in the GC, others are more likely to originate in the MSD.
Contamination sources in the GC:
• column or septum bleed
• dirty injection port
• injection port liner
• contaminated syringe
• poor quality carrier gas
• dirty carrier gas tubing
• fingerprints
• air leaks
• cleaning solvents and materials
Contamination sources in the MSD:
• air leak
• cleaning solvents and materials
• diffusion pump fluid
• foreline pump oil
• fingerprints inside the manifold
Air Leaks
Symptoms of leaks include:
Air leaks are a problem for any instrument
that requires a vacuum to operate. Leaks
are generally caused by vacuum seals that
are damaged or not fastened correctly.
www.agilent.com/chem
The action required to remove the contamination depends on the type of
contamination and the level of contamination. Minor contamination by water
or solvents can usually be removed by allowing the system to pump (with a
flow of clean carrier gas) overnight. Serious contamination by rough pump
oil, diffusion pump fluid or fingerprints is much more difficult to remove; it
may require extensive cleaning. For further details contact your Agilent
Customer Engineer (CE).
•
800 227 9770
• higher than normal vacuum manifold
pressure or foreline pressure
• higher than normal background
• peaks characteristic of air (m/z 18, 28,
32, and 44 or m/z 14 and 16)
• poor sensitivity
• low relative abundance of m/z 502
(this varies with the tune program and
MSD used)
84
GC/MS SYSTEMS
Leaks can occur in many more places
in the MSD:
• GC/MSD interface column nut
• side/top plate O-ring (all the way around)
• vent valve O-ring
• calibration valve
• high vacuum gauge tube fitting
• cracked ion gauge tube
• front and rear end plate O-rings
• GC/MSD interface O-ring (where the
interface attaches to the vacuum
manifold)
• diffusion pump co-seal and/or baffle
adapter O-ring
• turbomolecular pump O-ring
• new Vespel/graphite ferrules contract
when heated
Description
Part No.
Price
MS interface column nut
05988-20066
$13
Column nut for GC/MS and two-hole ferrules
05921-21170
$16
Universal Column Nut (2/pk)
5181-8830
$26
TIPS AND TOOLS
The most likely point for an air leak is a seal you recently opened.
Corrective Action
• Check interface nut for tightness.
Replace if necessary.
• Check leak/test the GC injection port.
Cleaning Solvents
It is common to see cleaning solvent peaks
in the mass spectra shortly after the ion
source is cleaned.
Corrective Action
• Dry all cleaned metal parts in the GC
oven before reassembling and reinstalling
them. Refer to specific cleaning
procedures in your MSD Hardware
Manual.
• Use a temperature that’s just above
the boiling point of the solvent.
Fingerprints
Fingerprints contain hydrocarbons that can
appear in mass spectra. Hydrocarbon
contamination is characterized by a series
of mass peaks 14 amu apart. The
abundances of these peaks decrease as
peak mass increases. Fingerprint
contamination is usually caused by the
failure to wear lint-free, nylon gloves during
ion source cleaning, GC inlet maintenance,
or from installing the column. Use special
care to avoid recontamination of parts after
you clean them. This typically occurs after
some maintenance or part replacement.
Corrective Action
• Reclean using clean, nylon gloves and
proper cleaning techniques.
Description
Part No.
Price
Nylon gloves, lint-free, Large
Nylon gloves, lint-free, Small
8650-0030
8650-0029
$16
$16
Diffusion Pump Fluid
If the diffusion pump is allowed to operate
with no column (carrier gas) flow into the
vacuum system, vapor from the diffusion
pump fluid can drift up into the vacuum
manifold. A more serious problem is when
fluid is back streamed into the vacuum
85
manifold by sudden or improper venting of
the vacuum system. If a diffusion pump
has back streamed, a prominent peak will
often be seen at m/z 446 and the spectral
baseline will exhibit increased background
noise.
Corrective Action
• If m/z 446 appears please call Agilent
for assistance.
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•
800 227 9770
GC/MS SYSTEMS
Foreline Pump Oil
Foreline pump oil contamination is
characterized by peaks spaced 14 amu
apart (hydrocarbons). Contamination with
foreline pump oil is less common than
contamination with diffusion pump fluid.
Corrective Action
• Call Agilent for assistance.
Contamination Identification
The following table lists some of the more common contaminants, the ion characteristic of those contaminants, and the likely sources
of those contaminants.
Common Contaminants
Ions (m/z)
Compound
Possible Source
13,14,15,16
Methane
CI gas
18, 28, 32, 44 or 14, 16
H2O, N2, O2, CO2 or N, O
Residual air and water, air leaks, outgassing from
Vespel™ ferrules
31, 51, 69, 100, 119, 131, 169,
181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614
PFTBA and related ions
PFTBA (tuning compound)
31
Methanol
Cleaning solvent
43, 58
Acetone
Cleaning solvent
78
Benzene
Cleaning solvent
91, 92
Toluene or xylene
Cleaning solvent
105, 106
Xylene
Cleaning solvent
151, 153
Trichloroethane
Cleaning solvent
69
Foreline pump fluid or
PFTBA
Foreline pump oil vapor or calibration valve leak
73, 147, 207, 221, 281,
295, 355, 429
Dimethylpolysiloxane
Septum bleed or methyl silicone column coating
77, 94, 115, 141, 168, 170,
262, 354, 446
Diffusion pump fluid
Diffusion pump fluid and related ions
149
Plasticizer (phthalates)
Vacuum seals (O-rings) damaged by high temperatures,
use of vinyl or plastic gloves
Peaks spaced 14 amu apart
Hydrocarbons
Fingerprints, foreline pump oil
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86
GC/MS SYSTEMS
Mass Spectrometer Symptoms
Sensitivity
This section describes some of the
symptoms you might observe – either in
the spectra of samples or in a tune report.
Typically, these symptoms fall into two
broad classes:
1. those that affect the system
sensitivity.
2. those that affect the repeatability
of a measurement.
Some symptoms can be corrected by
following the suggested corrective actions.
Others require the services of an Agilent
Customer Engineer.
Symptoms
Corrective Action
Wrong retention time
Check GC, method, application and carrier gas velocity
Low signal
Check GC, tune vacuum system
Leaking injection port
Clean the injection port
Replace the injection port liner and septa
Air leak
Check and tighten interface nut, leak test GC injection port
Peak widths
Do Autotune, check flow rate and temperature stability
Interfering peaks
Check time parameters, coeluting peaks, column type
Excessive background
Do Autotune and compare to background specifications
Check time parameters
Incorrect mass assignment
Retune
Abnormal spectra –
excessive background
contamination
Check for contamination
Incorrect tuning
Check tune file, retune, check sample
Repeller voltage is too low
Raise voltage to test for response
Dirty ion source
Clean source
Repeatability
Symptoms
Corrective Action
Dirty syringe needle
Clean or replace the syringe
Wrong syringe needle
Replace syringe and septa
Leaking injection port
Perform injection port maintenance
Replace the injection port liner, septa, and liner o-ring
Injection is too large
Check method and injection volume, split ratio
and/or splitless purge time
Loose column connections Tighten column nuts on injection port or transfer line
Replace column nuts and ferrule
87
Variations in pressure,
column flow,
and temperature
Ensure the MSD is located in an environment where
the temperature is stable
– Keep MSD out of drafts and direct sunlight
– Check that the carrier gas is steady and well regulated
– Service the foreline pump and/or diffusion pump
Dirty ion source
Clean source
Loose connections
in the analyzer
Check internal and external analyzer wiring connections,
make sure all are secure
Ground loops
Check main electrical lines
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GC/MS SYSTEMS
Ion Source
The ion source operates by electron
ionization (EI) or chemical ionization (CI).
The sample enters the ion source from the
GC/MSD interface. Electrons emitted by a
filament enter the ionization chamber,
guided by a magnetic field. The high-energy
electrons interact with the sample mole-
cules, ionizing and fragmenting them. The
positive voltage on the repeller pushes the
positive ions into the lens stack, where
they pass through several electrostatic
lenses. These lenses concentrate the ions
into a tight beam, which is directed into the
mass filter.
Selecting a Cleaning Method
The primary action of any cleaning
procedure is to remove contamination from
surfaces. Removing this contamination
restores the electrostatic properties of the
ion source lensing system. Numerous
cleaning methods have been developed for
restoring ion source performance. The
cleaning methods include abrasive, sonic,
and electropolish.
Preparing to Clean
Prior to cleaning, the mass spectrometer
must be vented and the ion source must be
removed. Before venting the system, the
following conditions must be met:
Abrasive methods offer several advantages:
• provide adequate energy to remove
contamination from surfaces
• require minimal equipment
• pose minimal risks to the user
Always allow the automatic venting routine
to run its full course. Improper venting may
cause diffusion pump fluid to be deposited
into the analyzer (backstreaming). It can
also reduce the life of the multiplier, or
other sensitive MS parts.
5973 Ion Source Assembly (EI)
Maintaining the Ion Source
Cleaning procedures for MSDs vary. Refer
to your MSD Hardware Manual for specific
ion source cleaning procedures.
Common measures of instrument
performance:
• abundance of certain ions (e.g.
percentage of the 502 ion from the
Autotune report)
• shape of lens ramps and the chosen
voltages, especially Repeller Ramp
• sensitivity obtainable for a given analysis
• ability to tune to a given reference
compound (e.g. DFTPP)
When to Clean:
The ion source should be cleaned:
• according to a customer’s predefined
schedule
• based on instrument performance (e.g.
deteriorated performance over time)
Frequency of Cleaning
The cleaning frequency is determined by:
• the number of samples run (throughput)
• the type of samples
• unique, established laboratory protocol
• heated zones are less than 100°C
• the diffusion pump is off and cool
• the turbo pump is off and not spinning
• the rough pump is off
A popular material used to abrasively clean
stainless steel ion source parts is
aluminum oxide. It is available in either
powder form or an abrasive film. After the
critical surfaces have been abrasively
cleaned, the loose particles must be
removed. One method of removing particles
is swabbing with a cotton swab or a clean
cloth dipped in acetone. A clean swab
should be used for each element followed
by a sonication. These cleaning supplies
are listed on page 89.
TIPS AND TOOLS
Agilent’s new MS Inert Ion Source improves inertness –
and maintains it over multiple cleanings. For more information
see page 90.
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•
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88
GC/MS SYSTEMS
Cleaning and Maintenance Supplies
Description
Part No.
Price
8650-0030
8650-0029
9310-4828
5181-8863
$ 16
$ 16
$185
$124
05980-60051
5061-5896
$ 64
$ 27
8660-0791
8500-0656
05971-60571
8500-1233
$ 29
$168
$ 85
$115
05980-20018
5080-5400
$ 14
$ 10
8710-0899
8710-0900
8710-0510
$ 16
$ 25
$ 24
Screwdriver, TORX, T15
Screwdriver, TORX, T10
8710-1622
5182-3466
$ 38
$ 24
Ferrules and O-rings
Teflon 1/4 in. ferrule (back)
Teflon 1/4 in. ferrule (front)
Retainer rings (10/pk)
0100-0160
0100-0787
5181-1258
$ 8
$ 8
$ 10
5973 One Year Maintenance Kit (for diffusion pump systems)
Includes: Big Universal Trap for He, Abrasive sheets (5/pk),
Cloths, lint-free (15/pk), Cotton swabs (100/pk), SantoVac Ultra,
18.5 mL (2 ea.), Rough pump oil, 1 liter, Filament assembly,
Octafluoronapthalene (OFN)
5183-2096
$657
MSD Tool Kit
Includes: Small cleaning rod, Large cleaning rod, Source hold tool,
Cotton swabs (100/pk), Nylon gloves, lint-free, Abrasive sheet,
30 mm (5/pk), Tool kit (wrenches, driving tools)
05971-60561
$510
Cleaning and Maintenance
Nylon gloves, lint-free, Large
Nylon gloves, lint-free, Small
Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk)
Generic ion source cleaning kit for all GC/MS types
Includes: Cloths, lint-free (15/pk), Abrasive sheets (5/pk), Cotton swabs
(100/pk), Nylon gloves, lint-free, Alumina powder, abrasive
Cloths, lint-free (15/pk)
Abrasive Sheets, aluminum oxide green lapping paper for ion source
cleaning, 600 mesh (5 sheets)
Alumina powder, abrasive
PFTBA sample, certified (10 g)
PFTBA sample kit, 1 mL
Activated alumina, absorbent pellets for Edwards
rough pump traps, non-LC/MS (1 lb can)
PFTBA glass vial
Cotton swabs (100/pk)
Tools
Screwdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws
Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws
Wrench, open-end, 1/4 x 5/16 in.
89
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GC/MS SYSTEMS
5973 MSD Ion Source Parts (EI)
Item
Description
5973 Part No.
Price
(A) Ion source body
G1099-20130
$ 198
(B) Repeller
G1099-20132
$ 112
(C) Interface socket
G1099-20136
$ 29
(D) Drawout plate
05971-20134
$ 69
(E)
Drawout cylinder
G1072-20008
$ 190
(F)
Ion focus lens
05971-20143
$ 263
(G) Entrance lens
05971-20126
$ 105
(H) Repeller insulator
G1099-20133
$ 82
(I)
Set screw
0515-1446
$
3
(J)
Washer, M3 (1/pk)
3050-0891
$
1
(K) Nut, 5.5 mm
0535-0071
$
1
(L)
G1099-60104
$ 200
05971-20130
$ 270
Ion source assembly
G1099-60106
$ 270
Source heater assembly
G1099-60177
$ 408
Ion Source Sensor
(M) Lens insulator, (2/pk)
Repeller assembly
G1099-60170
$ 481
Screw (for filament on the source)
0515-1046
$
A
C
H
L
M
F
G
E
D
M
5973 Ion Source Parts (EI).
2
MS Inert Ion Source Parts
Description
5973A
5973N
5973 inert**
Price
B
I
Drawout plate – 3 mm Inert
Drawout plate – 6 mm Inert** G2589-20045
G2589-20045
EI High Temp Filament
G2589-20100
$ 99
G2589-20045
$ 225
G2590-60053
$ 97
Repeller assembly, Inert source G1099-60170
G1099-60170
G2589-60102
$ 499
Screws for filament High Temp 0515-1046
0515-1046
G1999-20021
$
G1099-20130
G2589-20043
$ 563
G2589-20101
$ 12
Source body, Inert
Source Washer, Inert
G1099-20130
3
H
I
J
H
L
K
5973 Repeller Assembly (EI).
**used in G2860A and G2860B extended linearity kits
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•
800 227 9770
90
GC/MS SYSTEMS
B
A
H
D
F
TIPS AND TOOLS
C
E
B
I
It is good practice to replace scratched lenses and other ion source parts.
Scratched source parts lead to poor performance.
G
5972/5971/GCD Ion Source (EI)
5972/5971/GCD MSD Ion Source Parts (EI)
Description
(A) Entrance lens
5972/5971/GCD Part No.
Price
05971-20126
$ 108
(B) Lens insulator, (2/pk)
05971-20130
$ 278
(C) Ion focus lens
05971-20143
$ 271
(D) Drawout cylinder
G1072-20008
$ 190
(E) Drawout plate
05971-20134
$ 71
(F) Ion source body
05971-20128
$ 531
(G) Set screw
0515-1446
(H) Repeller assembly
$
05971-60170
(I) Screw (for filament on the source)
Ion source assembly
Transfer line tip, gold-plated
3
$ 593
0515-1046
$
2
5972 Part No.
Price
05972-60226
$3554
5972/5971 Part No.
Price
GCD Part No.
Price
05971-20305
$ 242
G1800-20305
$259
MSD Flowrates (ml/min)
Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates
below for flow limitations.
5973
5972
5971
GCD
91
Min
0.1
0.1
0.1
0.1
Max Diff Pump
2.0
2.0
1.5
1.0
Max Turbo Pump
4.0
NA
NA
NA
Tuning Max
2.0
2.0
1.0
1.0
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GC/MS SYSTEMS
Filaments
Two filaments are located on opposite
sides outside of the ion source. The active
filament carries an adjustable ac emission
current. The emission current heats the
filament, causing it to emit electrons; these
electrons ionize the sample molecules. In
addition, for the 5973 and 5972, both
filaments have an adjustable dc bias
voltage. The bias voltage determines the
energy on the electrons, usually -70 eV.
TIPS AND TOOLS
Maintaining the Filaments
Like the filament in an incandescent light
bulb, the ion source filaments will
eventually burn out. Certain practices will
reduce the chance of early failure:
It is very useful to switch from
one filament to the other every
three months so that when one
filament fails, you know the
other will fail soon. This will
allow you to change both
filaments at the same time,
which helps to maximize your
instrument uptime.
Tips to increase filament life
• When setting up data acquisition
parameters, set the solvent delay so that
the analyzer will not turn on while the
solvent peak is eluting.
• When the software prompts Override
solvent delay at the beginning of a run,
always select “No.”
• Higher emission current will reduce
filament life.
• If you are controlling your MSD from the
Edit Parameters screen, always select
MS Off before changing any of the
filament parameters.
Filament Assembly
Description
Unit
Part No.
Price
05972-60053
$ 90
G1099-80053
$282
Filament, EI High Temperature for the 5973 inert
G2590-60053
$ 97
Filament, 5972 (EI/CI)
05972-60053
$ 90
Filament, 5971 (EI/CI) / GCD (EI)
05971-60140
$159
Filament, 5973 (EI)
Filament, 5973 (CI)
2/pk
Quadrupole Mass Filter
The mass filter does not require periodic
maintenance. It should not be removed
from the radiator or distributed in any way.
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•
800 227 9770
• Never put the quadrupole in an
ultrasonic cleaner.
• Never change the physical orientation of
the quadrupole mass filter.
• The fused-quartz quadrupole is fragile
and will break if dropped or handled
roughly.
• The material in the cusps of the
quadrupole is very hygroscopic. If
exposed to water, the quadrupole must
be dried very slowly to prevent damage.
• Cleaning techniques appropriate for other
manufacturers’ instruments are not
suitable for Agilent MSDs – and may
actually harm the mass filter.
• To save time and effort, use only Agilent
MSD mass filters, which do not require
periodic cleaning or maintenance.
• In case of extreme contamination,
contact a trained Agilent service
representative to perform the mass
filter cleaning.
92
GC/MS SYSTEMS
Vacuum Systems and Pumps
Vacuum System Operation
The vacuum system creates the high
vacuum (low pressure) required for the
MSD to operate. Without this vacuum,
the molecular mean free path is too short.
Ions cannot travel from the ion source
through the mass filter to the electron
multiplier (detector) without colliding with
other molecules.
A properly maintained vacuum system will:
• Prevent premature filament failure
• Provide better sensitivity
• Require less frequent source cleaning
• Extend quadrupole lifetime
• Prevent premature EM Horn failure
The major components of the vacuum
system are:
• Vacuum manifold
• Foreline gauge
• Calibration valve
• Gauge controller (optional)
• Vacuum seals
• Foreline pump and/or trap
• Diffusion/turbo pump and fan
• High vacuum gauge tube
MAINTENANCE MINDER
Keeping a pan under the vacuum pump helps to
detect and identify the origin of oil leaks.
Calibration
The calibration valve is an electromechanical
valve with a vial that contains a tuning
compound. Perfluorotribuylamine (PFTBA)
is the most commonly used tuning
compound. It is required for automatic
tuning of the MSD in EI mode. The tuning
compound is usually a liquid but can be
volatile or semi-volatile solid.
How to Refill
The calibration vial can be refilled without
venting the system. Fill the vial to 0.5 cm
from the top. DO NOT overfill. Air is
trapped in the vial when it is refilled.
Description
Part No.
Price
PFTBA sample, certified (10 g) (EI)
PFDTD sample (10 g) (CI)
8500-0656
8500-8130
$168
$ 43
This sometimes causes an “Excess source
pressure” error message during the first
tune after refilling. This is more likely if the
vial is overfilled. Be sure to purge the air
upon refilling the vial.
MAINTENANCE MINDER
If using the 5973 with a CI source, use Perfluorodimethyltrioxadodecane
(PFDTD) sample.
93
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GC/MS SYSTEMS
Pressure Symptoms
This section describes unusual pressure
readings and their possible causes. The
symptoms in this section are based on
typical pressures. At typical column flow
rates (0.5 – 2.0 ml/minute), the foreline
pressure will be approximately 20 to 100
mTorr. The vacuum manifold pressure will
be approximately 1 x 10-6 to 1.4 x 10-4 Torr.
These pressures can vary widely from
instrument to instrument so it is important
that you are familiar with the pressures
that are typical for your instrument at a
given carrier gas flow and oven
temperature.
The vacuum manifold pressures can only be
measured if your system is equipped with
the optional gauge controller.
The foreline pressures listed can only be
measured on diffusion pump-equipped
systems. Turbomolecular pumps are
controlled according to their speed and
do not have foreline pressure gauges.
Foreline pressure is too high
Vacuum manifold pressure is too high
Symptom
• Pressure is above 100 mTorr.
• Pressure for a given column flow has
increased over time.
Symptom
• Pressure is above 1.4 x 10-4 Torr.
• Pressure for a given column flow has
increased over time.
Possible Cause
• Column (carrier gas) flow is too high
• Wrong carrier gas
• Air leak (normally at transferline interface)
• Foreline pump oil level is low or oil is
contaminated
• Foreline hose is constricted
• Foreline gauge is not working correctly
• Foreline pump is not working correctly
Possible Cause
• Column (carrier gas) flow is too high
• Wrong carrier gas
• Air leak
• Foreline pump is not working correctly
• Diffusion pump fluid level is low or fluid is
contaminated
• Foreline pump is not working correctly
• Defective gauge controller
• Faulty ion gauge tube
Foreline pressure is too low
Vacuum manifold pressure is too low
Symptom
• Pressure is below 20 mTorr.
Symptom
• Pressure is below 1.4 x 10-6 Torr.
Possible Cause
• Column (carrier gas) flow is too low
• Wrong carrier gas
• Column plugged or crushed by an
overtightened nut
• Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing*
• Foreline gauge is not working correctly
Possible Cause
• Column (carrier gas) flow is too low
• Wrong carrier gas
• Column plugged or crushed by an
overtightened nut
• Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing*
• Defective gauge controller
• Faulty ion gauge tube
* These could create a fault condition in the
GC that would prevent the GC from operating.
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•
800 227 9770
* These could create a fault condition in the
GC that would prevent the GC from operating.
94
GC/MS SYSTEMS
Diffusion Pump
It is not necessary to change the diffusion
pump fluid more than once a year, unless
you observe symptoms that suggest a
problem with the diffusion pump fluid. The
MSD must be vented in order to check the
diffusion pump fluid (except for the 5973).
Therefore, the best time to check the fluid
is when the instrument is already vented
for other maintenance.
Importance of the Fluid Level
The amount of fluid in the pump affects
the amount of vapor and the temperature
of the base plate. Too little fluid will cause
the pump to run at a higher temperature
because there is less fluid to carry away the
heat resulting in fluid cracking or degradation
and loss of high vacuum. It will also lower
the pumping speed because there is less
fluid vapor available to pump away gases
which can especially affect operation in
CI Mode due to higher flow rates.
How to Check the Fluid Level
1. If it is not vented already, shut down and
vent the MSD according to instrument
manual.
2. Unplug the MSD power cord.
3. Remove the pump and cover the top
with aluminum foil.
4. After heating the pump in a GC oven
at 60°C for 15 minutes to make the
fluid flow down into the reservoir at
the bottom, remove the stack parts.
5. Inspect the pump fluid, if the fluid
is discolored or contains particulate
material, the fluid must be changed.
Description
Part No.
Price
Diffusion pump fluid: SantoVac Ultra 5P,
18.5 ml (5973, 5972 or 5971/GCD)
Ion gauge controller (5973/5972A)
Ion gauge tube for measuring vacuum (5971/5972)
Triode gauge tube for measuring vacuum (5972/5973)
6040-0809
59864B
0960-0376
0960-0897
$ 82
$1399
$ 195
$ 358
6a. Use a metal ruler to determine the
depth of the fluid. A pump that has
been in operation should have a pool
9 mm plus or minus 1 mm deep. Fluid
in freshly charged pumps will be 12
mm deep. It is normal that up to 2 ml
of oil may be in the rear portion of the
vacuum manifold. The recommended
total fluid charge for the 5971/5972 is
18 ml (plus or minus 2 ml).
6b. For the 5973 use the sight glass
to determine the depth of the fluid.
The recommended total fluid charge
is approximately 37 ml.
Foreline Pump
The oil in the foreline or rough pump
should be replaced on average once every
six months, but can vary depending upon
applications. After oil replacement, if the
foreline trap is present, the molecular
sieves should be replaced.
95
Avoid contact with the pump oil. The
residue from some samples may be toxic.
Dispose of used oil properly.
Description
Part No.
Price
Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD)
6040-0798
$122
Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD)
6040-0834
$ 39
Molecular sieve (5973, 5972 or 5971/GCD)
9301-1104
$ 57
Oil mist filter RV3/E1M18/E2M18/E2M2
3162-1056
$430
Oil mist filter E2M1.5
G1099-80037
$173
Oil mist filter E2M18
5063-5224
$417
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800 227 9770
GC/MS SYSTEMS
General Instructions on How to Replace the
Pump Oil
1. Shutdown and vent the MSD.
2. Place a container under the drain plug on the
foreline pump.
8. Reconnect the MSD power cord.
9. Start up and pump down the MSD
according to the Instrument Manual
procedure.
3. Remove the fill cap from the top of the pump to
expose the fill hole.
4. Remove the drain plug from the pump.
TIPS AND TOOLS
5. Reconnect the MSD to its power source. Switch
on for 2 or 3 seconds, and then switch it off
again. This displaces old oil from the internal
pump cavities. Disconnect the power cord again.
Use chemical-resistant gloves and safety glasses when replacing pump
fluid. Avoid contact with the fluid. Always dispose of used oil properly.
6. Reinstall the drain plug and pour pump oil into
the fill hole.
7. Reinstall the fill cap.
Electron Multipliers and Replacement Horn
Maximize Lifetime
The lifetime of an EM is directly related to the current that
flows through it and the extent of contamination or
condensation that it experiences. To maximize electron
multiplier life:
• Maintain the best possible vacuum, especially in the
analyzer manifold.
• Use extreme caution and be conservative with venting,
pumpdown, and all vacuum system procedures to keep
pump fluid background to a minimum.
• After venting, allow four hours for pumpdown and
thermal equilibration before scanning.
• Actively look for background contamination and leaks
and repair them immediately.
• Don’t tune excessively. PFTBA can result in higher
background over an extended period of time.
Description
Part No.
Price
Electron multiplier replacement horn
(5973, 5972, 5971/GCD)
High energy dynode (5973 only)
Electron multiplier kit (5972, 5971/GCD only)
05971-80103
$1004
G1099-80001
05971-80102
$2131
$1136
Symptom
• Voltage is over 2500 volts
• Poor vacuum
Corrective Action
• Replace electron multiplier
TIPS AND TOOLS
Use only Agilent replacement multipliers and horns for Agilent MSDs.
Other manufacturers’ products can increase noise, while reducing
sensitivity and linearity.
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96
GC/MS SYSTEMS
Maintaining the MS Engine
Maintenance Schedule
• Always wear clean, lint-free, nylon gloves
when handling parts which will come in
contact with the sample stream. Oil from
your fingers is a particularly difficult
contaminant to remove.
• If you must set parts down, place them on
clean, lint-free cloths or clean aluminum
foil, not directly onto a laboratory bench.
• Keep parts covered so that dust does not
accumulate on them.
• Do not leave the interior of the vacuum
system open to the atmosphere. For
example, if you are removing the ion source
for cleaning, put the vacuum manifold cover
back in its normal position after you have
removed the source. Re-establish a low
vacuum in the vacuum manifold until you
need to reinstall the ion source.
Common maintenance tasks are listed on
page 83. Performing these tasks on a regular
basis can reduce overall operating costs.
Keep a record (logbook) of system
performance characteristics and
maintenance operations performed.
This makes it easier to detect variances
from normal operation and to take
corrective action.
Cleaning the Ion Source
There is not a regular interval for ion source
cleaning. The ion source should be cleaned
when symptoms indicate. Symptoms of a
dirty ion source include poor sensitivity and
inadequate abundances at high masses.
See the Troubleshooting chapter in your
hardware manual for more information about
these symptoms.
MS Engine Pump Lubricants and Oils
Lubricant Oil
Turbo pump lubricant:
Balzers turbo pump lubricant, 0.25 liter
Diffusion pump oil:
SantoVac 5, 1 liter
SantoVac 5, 128 ml
Rough pump oil:
Rough pump oil, 1 gal Inland 45
Rough pump oil, 1 liter Inland 45
Particle Beam pump oil, Fomblin
97
5989 or
5988
Thermo or
Electro Spray
5985 or
5987
5999x, 5993x
or 5995x
Part No.
Price
6040-0468
$ 134
•
•
•
•
•
•
•
•
6040-0370
6040-0819
$2553
$ 283
•
•
•
•
6040-0798
6040-0834
6040-0730
$ 133
$ 40
$ 760
•
•
•
•
•
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•
800 227 9770
GC/MS SYSTEMS
We strongly recommend keeping a log of all system performance and routine maintenance
operations. That way, problems that might impact performance can be identified and
resolved quickly.
The most common maintenance tasks are listed in the table below.
Task
Every
Week
Every
3 Months
Every
6 Months
As
Needed
•
Autotune or manual tune (save results)
Cabinet Maintenance
•
Clean the cabinet
•
Inspect hoses and cords
•
Vacuum the fan filter
Vacuum System Maintenance
Replace mech. pump oil
Replace mech. pump traps
Check diffusion pump fluid
Degas ion gauge tube
Replace ion gauge tube
Replace seals & O-rings
•
•
•
•
•
•
•
Analyzer Maintenance
Clean ion source
Replace filament
Replace ion source heater
Replace mass filter heater
Replace electron multiplier horn
•
•
•
•
•
We recommend
keeping a separate
set of tools that have
been thoroughly
cleaned for working
with the MS engine.
These tools are
needed to prevent
contamination when
reassembling or
installing clean
assemblies such as
the ion source.
TIPS AND TOOLS
Check mech. pump oil
GC/MS Interface Maintenance
Refill EI calibration vial
Refill CI calibration vial
Replace interface heater
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•
•
•
98
GC/MS SYSTEMS
Ion Source Parts and Supplies
Many of the tools and supplies needed to
service the 5989 MS Engine are included
in the installation kit supplied with the
instrument. The following tables list
common consumable parts and supplies
used in the maintenance of the MS Engine.
B
A
C
D
5989 Lens Stack
Description
Part No.
Price
(A) Clamp insulator, ion source
(B) Entrance lens
(C) Lens insulator, ion source
(D) Plate insulator, ion source
(E) EI/CI repeller
(F) Repeller insulator
Filament block
Filament assembly
Heater cartridge
05989-20110
05989-67002
05989-20111
05989-20109
05989-20145
05989-20119
05989-20165
05985-60179
05989-60098
$108
$990
$ 62
$ 88
$318
$580
$448
$ 58
$926
E
F
5989 Repeller Assembly
Replacement Parts and Supplies
The electron multiplier lifetime on the 5989
may be 6 to 9 months or shorter, especially
with the following applications:
• Thermospray
• Particle Beam
• Purge and trap, with no jet separator
• Extensive CI
• High sensitivity work with high EM voltage
Description
Part No.
Price
05989-80043
05971-80103
$2012
$1004
0960-0799
$ 448
05989-20705
5181-3367
$ 18
$ 47
0905-1145
3162-0110
0905-1189
$ 19
$ 39
$ 38
5989
Electron multiplier kit
Electron multiplier replacement horn
Parts and Supplies
Ion gauge tube, K-25 flange
O-rings and Seals
Insulating ring
O-ring, detector flange (5/pk)
Diffusion pump fluid fitting
fill and drain cap O-ring (12/pk)
KF 25 centering ring and O-ring
O-ring, manifold window
99
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GC/MS SYSTEMS
General GC/MS Supplies
G2860A 8270 Semi-Volatiles
Applications Kit
The G2860A 8270 Semi-Volatiles
Applications Kit is designed for use in
Agilent 6890/5973A and 6890/5973N
GC/MSD Systems. The kit provides
modified and/or pretested components to
improve system performance for USEPA
Method 8270. With the kit, system linearity
is maximized and activity is minimized.
Contents:
• Start-Up Guide, pub. No. 5988-3073EN
• Application Note, “Improvements in the
Agilent 6890/5973 GC/MSD System for
use with USEPA Method 8270”, pub. no.
5988-3072EN
• Ultra Ion Source Chamber
• Ultra Repeller
• Ultra Large Aperture Drawout Plate
• Pre-tested column, 30m x 250um x 0.5um
HP-5 MS, part no. 19091S – 139
• Single-taper splitless liner, 4mm i.d.,
deactivated, part no. 5181-3316
• Direct Connect Liner, single taper, 4mm
i.d., deactivated, part no. G1544-80730
• Direct Connect Liner, dual taper, 4mm
i.d., deactivated, part no. G1544-80700
• Floppy Disk with tuning macros
Description
Part No.
Price
8270 Semi-Volatiles Applications Kit
G2860A
$2333
LIBRARY
There are many ways to perform semi-volatile analysis. For another option that
also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem
and do a library search for 5989-1510EN.
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•
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100
GC/MS SYSTEMS
Test and Performance Samples
Each GC/MS has a specific test and performance sample. Refer to the chart below for the exact sample.
Tuning Samples
Verification Samples Performance
Checkout Samples
Semi-Volatile Volatile
MSD
EI
Tune
CI
Tune
EI
Negative
Mode CI
Positive
Mode CI
5973
PFTBA
PFDTD
OFN 1 pg/µL
OFN 1 pg/µL
Benzophenone 100 pg/µL
DFTPP
BFB
5972
PFTBA
PFTBA
HCB 10 pg/µL
NA
Benzophenone 100 pg/µL
DFTPP
BFB
5971
PFTBA
PFTBA
HCB 10 pg/µL
NA
Benzophenone 100 pg/µL
DFTPP
BFB
GCD
PFTBA
NA
Sample A (10 ng/µL)
NA
NA
DFTPP
BFB
5989A
PFTBA
PFTBA
HCB 50 pg/µL
OFN 1 pg/µL
Benzophenone 100 pg/µL
DFTPP
BFB
5989B
PFTBA
PFTBA
HCB 20 pg/µL
OFN 500 fg/µL
Benzophenone 100 pg/µL
DFTPP
BFB
MS Engine
EASY ONLINE ORDERING
Visit the Agilent website at www.agilent.com/chem/4ecatalog for
one-click access to:
• Product pricing links (when available)
• Local sales contact information
• Online quote requests
• Order status updates … and more
101
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•
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GC/MS SYSTEMS
Description
Quantity
Part No.
Price
05970-60045
$ 46
8500-5995
$ 62
8500-6406
$ 38
Evaluation Sample for GC/MS Systems
Contains 6 vials: 4 vials (Sample A, 10 ng/µL), 1 vial (Sample B, 100 pg/µL),
and 1 vial (Sample C, 100 ng/µL) each of dodecane biphenyl,
p-chlorodiphenyl, and methyl palmitate in isooctane, 1 mL ampoule
GC/MS Tuning Standard contains:
DFTPP, Benzidine, Pentachlorophenol, and
p,p’-DDT 1 mg/mL in methylene chloride
5989 Installation Sample Kit contains:
HCB 50 pg/µL, HCB 20 pg/mL, Benzophenone 100 pg/µL,
OFN 1 pg/µL, mix of HCB, OFN and Benzophenone 5 ng/µL
Extended Mass Performance Sample
0.5 g, fomblin oil
8500-5500
$141
PFTBA certified
1 bottle, 10 g
8500-0656
$168
PFTBA Sample Kit
0.5 mL
05971-60571
$ 85
PFDTD
10 g
8500-8130
$ 44
Benzophenone
100 pg/µL,
5 ampoules
8500-5440
$ 74
Hexachlorobenzene
10 pg/µL, 4 ampoules
1 ng/µL, 2 ampoules
8500-5808
$ 39
Hexachlorobenzene
20 pg/µL
8500-6405
$ 32
PFTBA not certified
1 ng/µL (2 ea)
05990-60075
$ 67
Octafluoronapthalene (OFN)
1 pg/µL,
5 ampoules
8500-5441
$ 67
Octafluoronapthalene (OFN)
500 fg/µL
8500-6572
$ 30
p-Bromofluorobenzene (BFB)
25 µg/mL
8500-5851
$ 39
Methyl stearate (in methanol);
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102
You asked … we listened!
Announcing the launch of
our new Life Sciences and
Chemical Analysis website.
Based on customer feedback, we’ve rebuilt our site navigation
and layout to help you more quickly find the information you
need about Agilent products and services.
The new site features:
• A coherent page design – that Automatically detects
screen resolution and optimizes the page size for
less scrolling.
• An expanded navigation – that includes links to
product literature, technical support, education,
events, and news.
• A newly designed online store – with fast access to
pricing, order status, quotes, and local sales information.
• Direct links – to the services, parts, and consumables that
keep your instruments running in top condition.
To experience these exciting new changes for yourself, go to www.agilent.com/chem.
Services & Support
Every Agilent GC and GC/MS system is backed
by our nearly 40 years of experience with
instrument design, lab operations, business
processes, and regulatory requirements.
We stand behind our products with …
• Immediate technical assistance by phone or
online.
• Prompt onsite service from Agilent-certified
Engineers.
• A variety of service options, including
maintenance, repair, compliance, and
consultation.
• Industry-leading training courses to help
increase your lab’s overall knowledge base.
Our professionals are standing by to help you
solve problems and optimize your resources.
So you can spend more time running samples,
developing methods and meeting production
deadlines – and less time arranging for
instrument services.
“Our customers know they can rely
on Agilent's expertise and resources
to keep their instruments running at
top performance."
Yukiko Sameshima
Customer Engineer
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•
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104
SERVICES & SUPPORT
Our focus is on keeping your lab running at peak performance.
A Total Commitment
to Your Lab for One Fixed Cost.
The Unmatched Expertise
of Fully Trained Engineers.
The Flexibility to Select The
Solution That’s Right for You.
Agilent service agreements operate
under a yearly fixed cost, which includes
preventative maintenance, compliance,
telephone support, repairs, parts, and
labor. No matter how many service visits
or replacement parts you need, this fixed
cost covers it all – at no additional charge.
You can rest assured that the engineer
who arrives at your site will perform the
requested service with optimum skill.
That’s because Agilent engineers …
Our team will work with you to help your
laboratory achieve …
If you choose, you can also consolidate
instrument maintenance and repair
services into multi-year agreements
for administrative ease and greater
cost savings.
• Are experts in instrument operation,
maintenance, compliance, and repair.
• Continually update their training
and qualifications.
• Use only Agilent factory-approved
replacement parts, columns, and
supplies to ensure peak instrument
reliability.
• Carry calibrated, traceable tools and
testing equipment, as well as Agilent
hardware and software qualification
protocols.
• Maximum uptime
• High productivity
• Total compliance
• Extended instrument life
• Fast problem resolution
• Verified system performance
• The skills and knowledge you need for
efficient operation and maintenance
• Consistent, in-depth documentation
• Reduced administrative burdens
What’s more, most Agilent engineers are
part of the Agilent product development
team. So you can be certain that ease of
repair, maintenance, and compliance are
built into your GC and GC/MS systems
right from the start.
105
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SERVICES & SUPPORT
Agilent Services
Features
Advantages to You
Telephone Service
• Telephone access to skilled Agilent service
professionals.
• Fast identification and resolution
of hardware problems.
• Available parts option.
• Low cost.
• Telephone access to trained technical
professionals.
• Fast identification and resolution
of software problems.
• Enhancements to the original application
software purchase.
• A fixed annual cost for software
upgrades makes budget management
more predictable.
Software Service
• Software bulletins that identify discovered
defects and recommend workarounds.
• A single cost-effective source
for telephone support and
software updates.
• A convenient way to keep up with
the latest software enhancements.
Onsite Instrument Repair
• Hardware telephone support with access
to skilled, factory-trained Agilent service
professionals.
• Travel expenses and labor.
• A fixed annual cost for parts makes
budget management more predictable.
• You can choose the response
method that fits your business
needs and budget.
• Optional coverage for consumables
used during repair.
Offsite Instrument Repair
For selected Agilent analysis instruments
• Option 1: Replacement with an identical
instrument (your fastest choice).
• Less expensive than onsite repair.
• Fast and easy.
• Option 2: Return to Agilent for repair.
• Includes extensive diagnostics and
testing that are not feasible with onsite
maintenance or repair.
Preventative Maintenance
For selected Agilent analysis instruments
• Expert cleaning, adjustment, lubrication,
and inspection of your instrument.
• Maximum uptime.
• Extended instrument life.
• Travel expenses and labor.
• Coverage for consumables used.
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800 227 9770
• Confidence in the integrity
of your measurements.
106
SERVICES & SUPPORT
Agilent Services
Features
Advantages to You
Installation Qualification (IQ)
• Qualification and documentation of
shipment completeness.
• Supplies the evidence you need to
satisfy regulatory agencies.
• Comprehensive system and application
software verification tests.
• Helps fulfill the master validation plan –
and change-control SOP requirements –
for the IQ phase.
• Delivered by professionals with training
certification.
Operational Qualification/Performance
Verification (OQ/PV)
For selected Agilent analysis instruments
• Verification and documentation of an
instrument’s ability to meet specified
criteria.
Note: We recommend Preventative
Maintenance before OQ/PV.
• Procedures and documentation that fit the
requirements of GLP, ISO 9000, and other
regulatory agencies.
• Full automation to increase the
qualification scope without excess time
requirements.
• Measuring equipment that is traceable to
national and international standards.
• Supplies the evidence you need to
satisfy regulatory agencies.
• No need to write your own SOPs to
qualify Agilent instruments – or to train
your staff.
• Consistent, traceable results among all
your laboratories – and improved
method transfer.
• Confidence in the integrity of your
measurements, with traceable,
documented chains from sample
introduction to reporting.
• Less risk of financial loss due to
noncompliance.
• Meaningful, relevant, and
understandable system tests.
Requalification (RQ) After Repair
For instruments that have their
operational performance verified
by an annual OQ/PV.
• Verification that a system is performing
at operation specifications after repair.
• Minimal system downtime after
completion of instrument repair.
• Complete system operation testing.
• Efficient system requalification by
performing the appropriate tests based
on the components repaired.
Note: only a subset of the Operational
Qualification test is performed, based on
the type and extent of the repair.
• A comprehensive test of the repaired
module using established conditions and
known sample characteristics to ensure
the basic accuracy and precision of your
module.
• Assurance that all instrument
subsystems are performing within
specifications.
• All procedures and documentation meet
regulatory agency requirements.
• Measuring equipment is traceable to
national and international standards.
107
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SERVICES & SUPPORT
Agilent Services
Features
Advantages to You
Network Qualification
• Network definition and performance
testing using established Agilent Design,
Installation Qualification, and Operational
Qualification protocols.
• Significant time savings.
• Documentation of the definition, integrity,
supportability, and health of high-risk
network segments.
• Completed protocols, created using
hardware and software network testing
tools. Protocols include:
- A physical and logical inventory.
- A graphical network topology map.
- A snapshot of network health, as
installed.
• Network Operational Qualification testing,
which monitors the network over time, and
evaluates its operation over a controlled
range of traffic conditions. We’ll also
provide the following reports:
- Long Duration Network Characterization,
which analyzes each function in its
operating environment.
• Increased uptime – issues that might
impact application performance are
quickly identified and resolved.
• Improved consistency – network
qualification protocols are developed
according to a quality lifecycle, and are
maintained under version and revision
control.
• Increased control – Agilent will verify
known elements and identify unknown
network contingency states that may
impact application performance.
• Reduced regulatory exposure –
audit-ready documentation establishes
evidence of network system control.
- Performance Predictability Analysis,
which documents reserve capacity and
stability over a range of operating
demands.
Mass Spectrometer Ion Source Cleaning
For selected Agilent analysis instruments
• Onsite disassembling
• Cleaning
• Your staff can devote more time to
chemistry, not instrument maintenance.
• Efficient cleaning with minimal
downtime.
• Reassembling
• Testing
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108
SERVICES & SUPPORT
Agilent Services
Features
Advantages to You
Software Backup
• Telephone or onsite factory support to
facilitate restoration.
• Fast and easy – you simply insert a disk
… reboot … and you’ll be back in
operation in as little as two hours.
Normally, you would have to reload and
reconfigure your software – a process
that can take days.
• Captures the unique system settings for all
software components needed to
reconstruct your system including:
- Network information
- Printers and peripherals
- Configurations
- User settings and operations
- System registry
- Application software
- Settings
- Operating system
- Customizations
- Analytical hardware
- Directory structure
- Security information
• A complete solution – the initial
configuration backup includes:
- Simple backup software
- Ten CD-ROMs
- Ten 3.5-in. floppy disks
- A storage case
- One full system backup
- Installation of the backup software
and optional CD writer
TIPS AND TOOLS
To learn more about Agilent’s complete portfolio of services, please
visit www.agilent.com/chem/service.
109
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SERVICES & SUPPORT
Education & Training Services
Highly trained lab professionals can boost your productivity, minimize errors and
reruns, and expand your chromatography capabilities. And that’s why Agilent offers
several training options that cover everything from troubleshooting and maintenance
to the most advanced operational techniques.
eLearning
Agilent’s e-Learning program features a series of focused, economical and
individualized instrument training modules designed to enhance and simplify your
learning experience. From theory and operations... to common problems with your
instruments... eLearning is available when you want it, where you want it, and how
often you want it. All you need is Internet access!
You can review and register for our e-Learning offerings by visiting
www.agilent.com/chem/elearning
Course Title
Duration
Description
6890 GC Split Inlet Mode Operation
Self-paced;
Four hours access
Reviews the basic theory and operation
of the 6890 GC split/splitless capillary
inlet when running in split mode.
Clarifies flow paths, so you can gain
the maximum benefit from this inlet
operational mode.
Discusses typical problems and routine
maintenance procedures.
6890 GC Splitless Inlet Mode Operation
Self-paced;
Four hours access
Reviews the basic theory and operation of
the 6890 GC split/splitless capillary inlet
when running in splitless mode.
Clarifies flow paths, so you can gain
the maximum benefit from this inlet
operational mode.
Discusses typical problems and routine
maintenance procedures.
6890 GC Purged Packed Inlet Operation
Self-paced;
Four hours access
Reviews the basic theory and operation
of the 6890 GC purged packed inlet.
Clarifies flow paths, so you can gain
the maximum benefit from this inlet.
Discusses typical problems and routine
maintenance procedures.
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110
SERVICES & SUPPORT
Course Title
Duration
Description
6890 GC Keyboard Operation
Self-paced;
Four hours access
Reviews the basic operation of the 6890
GC keyboard.
Thoroughly describes all keys, so you can
gain the maximum benefit from your GC.
6890 GC FID Theory and Operation
Self-paced;
Four hours access
Reviews the basic theory and operation
of the FID.
Covers proper column installation,
keyboard setup, and flow optimization.
Discusses typical problems and routine
maintenance procedures.
6890 GC ECD Theory and Operation
Self-paced;
Four hours access
Reviews the basic theory and operation
of the ECD.
Covers proper column installation,
keyboard setup, and flow optimization.
Discusses typical problems and routine
maintenance procedures.
6890 GC TCD Theory and Operation
Self-paced;
Four hours access
Reviews the basic theory and operation
of the TCD.
Covers proper column installation,
keyboard setup, and flow optimization.
Discusses typical problems and routine
maintenance procedures.
GC Automatic Liquid Sampler Operation
Instructor-led;
60-90 minutes
Reviews the basic operation of the 7683A
automatic liquid sampler system (ALS).
Shows you how to gain maximum
productivity from the ALS.
Discusses routine maintenance
procedures, and how to return an ALS
to Agilent for repair or exchange.
111
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SERVICES & SUPPORT
Course Title
Duration
Description
Logical GC Troubleshooting
Instructor-led;
60-90 minutes
Teaches a methodical process for
troubleshooting GC system problems.
Helps you identify the source of problems
quickly, making troubleshooting less
daunting.
Note: This course does not discuss hardwarespecific problems or solutions.
Using the GC/MSD
Security ChemStation to Achieve
FDA CFR Part 11 Compliance
Instructor-led;
60-90 minutes
Describes in detail how to operate the
GC/MSD Security ChemStation software
in accordance with FDA CFR Part 11
requirements.
Managing and Administering the
GC/MSD Security ChemStation
to Meet FDA CFR Part 11
Compliance Requirements
Instructor-led;
60-90 minutes
Shows you how to manage the GC/MSD
Security ChemStation software in
accordance with FDA CFR Part 11
requirements.
Designed for systems administrators
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112
SERVICES & SUPPORT
Classroom Training
Agilent’s training courses for gas
chromatography and mass spectrometry
help new and experienced lab
professionals learn proper and efficient
ways to use analytical instruments and
software. These ISO-registered courses
also target those who want to broaden
or sharpen their troubleshooting,
maintenance, and system operation skills.
Contact Agilent today for more information
about our training and services. Or visit
www.agilent.com/chem and select
“Education.”
Course Title
113
Course No.
No. of Days
Description
Technique
Introduction to Capillary GC
H2615A
1
Provides an overview of capillary gas chromatography in a
lecture format.
Techniques of GC
H4002A
5
Presents the fundamental concepts of gas
chromatography.
Introduction to GC-MS
H2609A
1
Introduces the technique of GC-MS in a lecture format that
includes worksheet exercises.
Techniques of GC-MS
H4040A
3
Reviews the key concepts of the GC-MS analysis process,
as well as qualitative and quantitative GC-MS techniques.
Hardware/Software Operation
ChemStation Operation for the 6890 GC/ALS
H5926A
5
Explains how to operate the Agilent 6890 GC using GC
ChemStation software.
Operation of the GC-MSD System
Using the ChemStation for GC-MSD
H4043A
5
Enhances an operator’s efficiency and productivity when
using the Agilent GC-MSD system.
Provides experience in data acquisition and analysis, library
searching, reporting, and customizing the system to meet
specific laboratory or customer needs.
GC-MSD System for Environmental Applications
H4050A
5
Increases an operator’s skill in using a mass selective
detector with mass spectrometer EnviroQuant software.
Troubleshooting and Maintenance
6890 GC Maintenance
H5308A
4
Addresses preventative maintenance and first-level repair
for the Agilent 6890 GC.
5890 GC Maintenance
H4001A
4
Addresses preventative maintenance and first-level repair
for the Agilent 5890 GC.
6890 GC Troubleshooting and
Preventative Maintenance
H5309A
1
Introduces troubleshooting of the Agilent 6890 GC in a
lecture format.
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SERVICES & SUPPORT
Course Title
Course No.
No. of Days
Description
Introduction to 5973 GC-MSD Troubleshooting
and Preventative Maintenance
H5947A
1
Demonstrates how to perform preventative
maintenance and troubleshooting to keep the
Agilent 5973 GC-MSD system working properly.
Includes a discussion of typical vs. problem
Auto-Tunes.
Offers class exercises that enhance understanding
of troubleshooting and maintenance principles.
5973 GC-MSD Troubleshooting
and Preventative Maintenance
H2294A
3
Covers tuning and diagnostics, the vacuum
system, the 5973 MSD ion source, the quadrupole
mass filter, and the 5973 MSD.
Includes hands-on laboratory exercises to
demonstrate and practice the principles conveyed.
Data Analysis and Reporting
ChemStation for GC Data Analysis and Reporting
H2606A
3
Teaches the operation of the Agilent GC
ChemStation software through instructor
explanations, combined with extensive hands-on
and laboratory exercises.
Specifically focuses on data analysis
and reporting.
Data Analysis and Reporting Using the
ChemStation for GC-MSD
H4076A
3
Enhances skills in using the Agilent ChemStation
for GC-MSD.
Makes users more efficient and productive, while
expanding their ability to use ChemStation
features.
Describes how to customize the software for
laboratory and customer needs.
Data Analysis and Reporting Using
the EnviroQuant ChemStation for GC-MSD
H4053A
3
Improves proficiency in using the Agilent
EnviroQuant software.
Covers data analysis and reporting, including
completion of EPA-like forms.
Describes how to customize the software for
laboratory and customer needs.
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insights, go to www.agilent.com/chem.
You’ll find:
• Frequently Asked Questions about Agilent
instruments and supplies.
• Interactive Troubleshooter A step-by-step
approach to help you solve common problems.
• Find a Part Includes parts information,
pricing, and availability, plus an illustrated
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patches and status bulletins, tools and
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chromatograms for nearly a thousand
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Have a technical GC column, method, or troubleshooting question? Agilent’s technical GC and GC/MS
experts are available to answer your questions by phone, fax or e-mail for free. With years of experience in
running samples, developing methods and troubleshooting GC systems, our chemists are promptly able to
help you consistently achieve excellent performance and high productivity in your lab.
GC Technical Support in the United States:
Phone: 1-800-227-9770, press #4, then #1
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Online: go to www.agilent.com/chem/techsupport
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115
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GC System Recommended Maintenance Schedule
Gas Management
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
Gas purifiers
(carrier gas &
detector gas)
Every 6-12 months
Replacement schedule is based on capacity and grade of gases.
In general, replace non-indicating traps every 6-12 months or when
indicating traps start to change color. Replace indicating traps when
indicating material is spent.
Split vent trap
Every 6 months*
Replace.
Flowmeter
calibration
Every 1-2 years
Re-calibrate electronic flowmeters – follow recommended schedule for
the unit (shown on calibration certificate).
Sample Introduction Consumables and GC Inlets
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
Syringes
and/or syringe
needles
Every 3 months*
Replace syringe if dirt is noticeable in the syringe, if it cannot be
cleaned, if the plunger doesn’t slide easily, or if clogged. Replace
needle if septa wear is abnormal or the needle becomes clogged.
Inlet liner
Weekly*
Check often. Replace when dirt is visible in the liner or if
chromatography is degraded.
Liner O-rings
Monthly*
Replace with liner or with signs of wear.
Inlet septum
Daily*
Check often. Replace when signs of deterioration are visible
(gaping holes, fragments in inlet liner, poor chromatography,
low column pressure, etc.).
Inlet Hardware
Every 6 months
Check for leaks and clean.
Every year
Check parts and replace when parts are worn, scratched, or broken.
Remember, the downtime for scheduled
maintenance is always less disruptive
than the downtime for unscheduled
maintenance and troubleshooting!
Columns
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
Front-end
Maintenance
Weekly – monthly*
Remove 1⁄2 -1 meter from the front of the column when experiencing
chromatographic problems (peak tailing, decreased sensitivity, retention
time changes, etc.). Replace inlet liner, septum and clean inlet as
necessary. Guard column may be useful for increasing column lifetime.
Solvent rinse
As needed
When chromatography degradation is due to column contamination.
Only for bonded and cross-linked phases.
Replacement
As needed
When trimming and/or solvent rinsing no longer return chromatographic
performance.
Ferrules
Replace ferrules when changing columns and inlet/detector parts.
Detectors
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
FID/NPD Jets
& Collector
As needed
Clean when deposits are present. Replace when they become scratched,
bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead
As needed
Replace when signal drifts or there is a dramatic change in sensitivity.
FID
Every 6 months
Measure hydrogen, air, and makeup gas flows.
TCD
As needed
Thermally clean by “baking-out” when a wandering baseline, increased
noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.
ECD
Every 6 months
As needed
Wipe test.
Thermally clean by “baking-out” when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD
Every 6 months
As needed
Measure hydrogen, air, and makeup gas flows.
Clean/replace FPD windows, and seals when detector sensitivity
is reduced.
MSD
Components require regular maintenance. For complete MSD maintenance schedule, please see page 83.
*Schedule is an approximation of average usage requirements.
Frequency may vary widely based upon application and sample type.
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For detailed information about
supplies from Agilent, please
contact your local Agilent sales
representative, or your authorized
distributor, or visit us online.
Ask about Agilent’s other valuable
resources:
• Maintaining Your Agilent 1100 Series
HPLC System
• Essential Chromatography Catalog
• Online Library and Tech Support
The information and pricing in this guide
are subject to change without notice.
© Agilent Technologies, Inc. 2005
Printed in USA February 15, 2005
5989-1925ENUS