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Operate your lab at peak performance

Troubleshoot difficult problems


Select the right Agilent supplies
Plan preventative maintenance

Maintaining your Agilent


GC and GC/MS Systems
Maximize your efficiency. Minimize your downtime.
Get the results you need.
Our GC and GC/MS Maintenance Guide puts
nearly 40 years of Agilent knowledge at your fingertips.

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

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

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

Maintaining Your Agilent GC and GC/MS Systems


Maximize your efficiency. Minimize your downtime.
Get the results you need.

2 Gas Management 56 Columns


3 Gas Types 57 Column Maintenance
4 Contaminants & Purities 57 Column Selection
4 Gas Purification Systems 58 Column Installation/Setup
12 Regulators & Conditioning
13 Tubing 59 Column Performance
14 Leak Detection 63 Columns Types and
Characteristics
15 Flow Rates
68 Detectors
18 Sample Introduction
Consumables & GC Inlets 69 Flame Ionization Detector (FID)
Sample Introduction Thermal Conductivity Detector
(TCD)
19 Vials
72 Electron-Capture Detector
21 Syringes
(ECD)
TIPS AND TOOLS Inlet Types 74 Thermal Conductivity Detector
26 Packed-Column (TCD)
28 Split/Splitless 76 Flame Photometric Detector
This icon denotes a helpful hint that provides useful information you 31 Cool On-Column (FPD)
can find throughout this guide and online at www.agilent.com/chem. 34 Programmed Temperature 78 Nitrogen-Phosphorus Detector
Vaporizer PTV (NPD)
Inlet Accessories 82 GC/MS Systems
36 Septa 83 Maintaining Mass Selective
42 Ferrules Detectors (MSDs)
47 Liners 87 Mass Spectrometer Symptoms
52 Flip Top Inlet Sealing System 88 Ion Source
VIDEO 54 Parts & Supplies 93 Vacuum Systems & Pumps
96 Electron Multipliers &
Replacement Horn
This icon denotes a video that is available to view on our website. 97 Maintaining the MS Engine
Just visit www.agilent.com/chem/techsupport to view how-to 99 Ion Source Parts & Supplies
videos and obtain more information. 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 www.agilent.com/chem
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 2
GAS MANAGEMENT

Gas Types
Carrier Gases
The most frequently used carrier gases are bleed, along with column and/or detector dioxide) and pneumatic gases (air or
helium and hydrogen, although nitrogen damage. The following sections describe nitrogen) generally do not come in contact
and argon can be used. Purity is essential the gases and purities that are necessary with the sample or detector. Therefore,
for these gases since they sweep the for gas chromatography carrier gases, as these non-contact gases do not have to
sample through the column where it is well as other support gases. be the highest purity available.
separated into its component parts and
Support Gases Fuels, oxidants and detector gases, in most
then through the detector for component
Support gases may be specific for cases, do come in contact with the sample
quantification. Carrier gas purity is also
detectors or for applications. These gases and detector, and require higher purity
critical to prevent degradation of
include fuels, oxidants, coolants, detector gases. Unfortunately, gas nomenclature as
chromatographic hardware.
gases, and pneumatic gases. The degree it relates to purity is not consistent across
Contaminants in carrier gases can have of purity required for support gases is specialty gas suppliers. It is important to
a significant effect on column life and dependent on how that gas is being used, recognize the impurities in your gas
subsequent analyte detection. Harmful and whether or not it will make contact supplier’s products, and to utilize the
effects of impure gases include with the sample. Coolant gases (carbon appropriate Agilent gas purification
contaminant peaks and elevated column products (see next section).

Carrier and Support Gases

Sample
Gas Type Function Contact Purity Required*

Air Pneumatics No Low Grade

Nitrogen Pneumatics No Low Grade

Limit of Detection required:

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

Hydrogen Carrier or fuel gas


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

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

Methane/Argon Carrier or make-up


or Nitrogen for ECD Yes Research Research Research N/A

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

Nitrogen, Helium, Carrier or


or Argon make-up gas Yes Research Ultra-Pure Ultra-Pure UHP/Zero
*Purities of gases 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 www.agilent.com/chem
GAS MANAGEMENT

Contaminants & Purities


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

Gas Purification Systems


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

www.agilent.com/chem 4
GAS MANAGEMENT

Carrier Gas Purification


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

Gas Purification System Detector Gas Purification


Gas supply

FID make-up, air,


and H2

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

ELCD reaction gas

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

Regulator = Brass dual stage regulator

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

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 www.agilent.com/chem
GAS MANAGEMENT

Moisture (Water) Traps


There are several different adsorbents and indicating materials Indicating moisture traps are available in plastic and glass bodies.
used in moisture traps. Moisture traps can be easily refilled. Glass body traps are used when potential contaminants from
Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap plastic trap bodies are a concern. Glass traps are normally
making refilling a more economical (and less wasteful) option. 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 H2O Removal Maximum Effluent H2O 1/8 in. 1/4 in.
Description (cc) Capacity (g) Concentration (ppb) Part No. Part No.

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

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

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

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

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

Molecular Sieve Refill for GMT Series 250 GMSR GMSR

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

Moisture S-Trap – preconditioned 5060-9084

Big Moisture Traps – for the Ultimate Moisture Capacity

Big Moisture Trap 750 BMT-2 BMT-4

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

Refillable Moisture Trap Moisture S-Trap Big Moisture Trap

www.agilent.com/chem 6
GAS MANAGEMENT

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

Big Oxygen Trap 750 BOT-2 BOT-4

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

Big Hydrocarbon Trap 750 BHT-2 BHT-4

Refill for Big Hydrocarbon Trap (2 refills) BACR BACR

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

Hydrocarbon S-Trap 5060-9096

Capillary Grade Hydrocarbon Traps – for crucial capillary applications

Capillary Grade Hydrocarbon Trap 100 HT3-2 HT3-4

Adsorbent Refill (1 pint, 3 refills) ACR ACR


Hydrocarbon Trap

7 www.agilent.com/chem
GAS MANAGEMENT

Hydrocarbon Traps continued


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

Hydrocarbon S-Trap

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

1/8 in. 1/4 in.


Description Size (cc) Part No. Part No.

Oxygen/Moisture Traps

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

Hydrocarbon/Moisture Traps

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

Refill for Hydrocarbon/


Moisture Trap (1 pint, 2 refills) HCRMS HCRMS

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

Big Universal Trap – Helium


purged (also recommended
for GC Mass Spec) 750 RMSH-2 RMSH-4

Big Universal Trap – Hydrogen purged 750 RMSHY-2 RMSHY-4

Big Universal Trap – Nitrogen purged 750 RMSN-2 RMSN-4


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

www.agilent.com/chem 8
GAS MANAGEMENT

High Capacity
Gas Purification System
Three Cartridge System Single-Cartridge System
• Agilent’s highest capacity and most • Contains a triple-combination cartridge
economical gas purification system. that offers the same highly efficient
Three Cartridge
High Capacity contaminant removal properties from
• Provides low-cost gas contaminant
Gas Purification eight cylinders of carrier gas but without
System
removal for up to 18 cylinders of
the visual indicator.
carrier gas.
• Other cartridges are also available for
• Includes a manifold with cartridge
detector gas supplies and as individual
mounts and three replaceable cartridges:
filters for specialized requirements.
one moisture/hydrocarbon cartridge; one
oxygen cartridge; and one oxygen
indicating cartridge.
• Consists of a permanent all-welded
stainless steel manifold to minimize
the potential for leaks.
• Suitable for bench or wall mounting.

High Capacity Gas Purification System

Description Part No.

Three Cartridge System–Includes manifold


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

With 1/8 in. fittings 5183-1907

With 1/4 in. fittings 5182-9776

Replacement Cartridge Kit–


Includes all three cartridges for 5182-9780
above system

Single Cartridge System–Includes single


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

With 1/8 in. fittings 5183-4598

With 1/4 in. fittings 5183-4599

Triple combination replacement cartridge


for single cartridge system 5183-4600

9 www.agilent.com/chem
GAS MANAGEMENT

Quick Change Plus (QC+) Point of


Operation Panel
The QC+ Point of Operation Panel contains Filter cartridges are of all metal or glass
purifier cartridges that can be quickly construction, eliminating infusion and
changed. The cartridges are removed from resultant signal noise associated with
the panel without interruption of gas flow filters constructed from plastics. Cartridges
to the system, drastically minimizing costly are quickly installed via a simple knurled
instrument downtime. retaining nut, with no wrenches needed.
As many as four cartridges can be replaced RQC-P
in a matter of seconds, and because there
is low dead volume, a minimal amount of
gas system purge is required after
installation.

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

Description Fitting (in.) Part No.

4-Head

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

Replacement Cartridges

Description Part No.

High capacity oxygen GC-1

High capacity moisture GC-2

Indicating moisture GC-2-I

Hydrocarbon GC-3

Indicating oxygen GC-4

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

www.agilent.com/chem 10
GAS MANAGEMENT

Super-Clean Gas Filter System Super-Clean Gas Purification Systems


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

Replacement Filter Cartridges

Triple Filter Cartridge: A single carrier gas


filter now with hydrocarbon, moisture,
and oxygen trapping capability. Includes
moisture and oxygen indicator so you know
exactly when to replace the cartridge. 5182-9705

Filter cartridge bundle of 4 (oxygen,


moisture, and 2 hydrocarbon) 5183-4770

Universal/External Split Vent Trap


Description Part No. Split vent traps stop environmental
pollution. The split vent trap was designed
Universal/external split vent trap to protect the lab environment from the
with 3 cartridges contaminants released by split injection
(1/8 in. Swagelok fitting) RDT-1020 systems, which can vent up to 500 times
the amount of sample reaching the
Replacement cartridges (3/pk) RDT-1023
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 www.agilent.com/chem
GAS MANAGEMENT

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

Description Part No.

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

CGA 346, 125 psig max (8.6 bar), Air 5183-4641

CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642

CGA 540, 125 psig max (8.6 bar), O2 5183-4643

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

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

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

Regulator Outlet Adapters – Female NPT to Swagelok-style TIPS AND TOOLS


1/4 in. to 1/8 in. brass
(included with brass regulators) 0100-0118
Always depressurize a regulator before closing by
1/4 in. to 1/4 in. brass** 0100-0119 adjusting knob and removing the regulator from the
cylinder.
** Required for plumbing 1/4 in. tubing to regulators above

www.agilent.com/chem 12
GAS MANAGEMENT

Tubing
When constructing or maintaining a gas as pressurizing pneumatic lines; however,
delivery system for GC, choosing the be aware of its pressure limitations.
proper tubing material is very important
In view of these problems, the list of
and will help to eliminate potential
appropriate tubing materials has been
problems and improve the overall quality of
narrowed down to two: copper and
the gas system. Although there are many
stainless steel. Agilent recommends using
common tubing materials available, some
copper tubing for most applications, since
pose safety or cleanliness problems.
it is easy to bend and plumb and is less
Non-metallic types of tubing such as expensive than stainless steel. Use
polyethylene and Teflon are not stainless steel tubing only for crucial
recommended for GC applications due applications that require very high purity,
Spectra-Link Tubing Connecting System to their gas permeability and difficulty or where building codes mandate its use.
on a two-stage regulator in cleaning. This type of tubing can be
used for non-critical applications, such Cleaning Tubing
Before any tubing is placed into service,
or if it becomes contaminated with use,
Determining Tubing Length it is essential that it be properly cleaned.
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig Unclean or improperly cleaned tubing can
lead to contamination of the system with
Tubing Type Diameter Recommended Pressure Drop disastrous results.
(inches) Max. Length (feet) (psig)
Cleaning tubing requires the use of
Copper 1/8* 50 2 suitable detergents and solvents along
with nitrogen and a purgeable oven for
Copper 1/4* 300 0.5 drying. This may be done easily for small
lengths of tubing, but in larger systems the
*Recommended when multiple instruments are connected to the same source
cleaning procedure sometimes becomes
unwieldy, leaving behind a large quantity
of solvent requiring proper disposal.
Fortunately, Agilent provides clean, high
Tubing–Precleaned quality GC grade tubing for large systems
as an economical alternative.
Description Part No.

Copper tubing, 1/8 in., 50 ft. 5180-4196

Copper tubing, 1/8 in., 12 ft. 5021-7107

MAINTENANCE MINDER

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

13 www.agilent.com/chem
GAS MANAGEMENT

Spectra-Link is No Ordinary Flexible Tubing!


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

Description Part No.

Spectra-Link with 1/8 in. fittings


and 36 in. SS tubing SL-8

Spectra-Link with 1/4 in. fittings


and 36 in. SS tubing SL-4

Cylinder Bracket

Description Part No.

Cylinder wall bracket with strap and chain 5183-1941


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

Leak Detection
Leaks allow oxygen and other gas leaks for 12 common gases. Based on a
contaminants to enter the gas stream. dual cell micro volume thermal conductivity
Therefore, GC instrument maintenance system, this unit provides very high
should include checking fittings and sensitivity and eliminates contamination
connections with a gas leak detector. caused by soap solution methods.
Agilent’s Gas Leak Detector enables quick
and easy detection and measurement of

Gas Leak Detector Kit

Description Part No.

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

Gas leak detector, 115 V 5182-9646

Gas leak detector, 220 V 5182-9648

Gas Leak Detector

www.agilent.com/chem 14
GAS MANAGEMENT

Flow Rates
Setting and maintaining GC flow rates Selecting a Flowmeter
greatly affect the instrument accuracy Agilent manufactures the largest selection
and sensitivity. During maintenance, of volumetric and mass flowmeters for
verify carrier and support gas flows chromatography. We have developed
with the proper flowmeter. Choosing a flowmeters for measuring capillary column
flowmeter for your application depends flows, calibrating air pumps and flow
upon measurement speed, ease of use, controllers, and verifying instrument gas
accuracy, and flow rate range. flows. All flowmeters are calibrated to
NIST-traceable standards.

FlowTracker Flowmeters – volumetric, multimode flowmeters

Description Part No.

FlowTracker 1000 Flowmeter 5183-4779

FlowTracker 2000 Flowmeter and


FlowTracker 2000 Leak Detector 5183-4780

FlowTracker Universal AC Adapter (optional,


not supplied with FlowTracker units) 5183-4781

ADM 1000 features include: ADM 2000


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

15 www.agilent.com/chem
GAS MANAGEMENT

Flowmeters

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


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

ADM Flowmeters – volumetric, measures all gases*


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

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

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

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

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


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

Optiflow Flowmeters Gas Flowmeters – versatile volumetric flowmeters**


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

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

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

*non-corrosive gases only


**non-corrosive and mildly corrosive gases only

Veri-Flow 500
Optiflow 420

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 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 • A newly designed online store – with fast access to
screen resolution and optimizes the page size for pricing, order status, quotes, and local sales information.
less scrolling. • Direct links – to the services, parts, and consumables that
• An expanded navigation – that includes links to keep your instruments running in top condition.
product literature, technical support, education,
events, and news.

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


Sample
Gas Introduction
Management
Consumables &
The use of quality carrier gases is essential
GC Inlets
for consistent and accurate GC analyses.
Proper
Agilentgas management
offers a wide rangeis key to achieving
of high-quality
this goal.vials,
sample Agilent provides
septa, a diverse
syringes, liners line
and of
high
inlets for a broad range of gas-phase – gas
quality gas management products
purifiers, regulators,
applications. Just asleak
youdetectors
depend on our
and flowmeters
meticulously – all designed
engineered GC andto prevent
GC/MS
column damage,
instruments, youimprove
can count detector life, and
on Agilent
improve the quality and consistency
consumables. This section reviews these of your
GC separations.
critical components.This section explains
Also, look how
for useful
common
infofrom contaminants
proper syringelikeuseoxygen, moisture
and cleaning
and hydrocarbons
techniques can damage
to a detailed your GC
discussion on
column, and helps you
optimized inlet settings. 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.

“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 18
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

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

Vial Options

Glass–for general purpose Silanized–for use with Polypropylene –for use Amber Vials–for use with Microvolume Inserts–for High Recovery Vials–
use and for use with acids samples that bind to glass, with alcohols and aqueous light-sensitive samples use with very small sample for use with limited sample
and for trace analyses solvents 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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Selecting Vial Septa Materials


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

Red Rubber/Teflon
• Routine analysis Determining Your Quantity Needs
• Moderate resealing
To determine potential septa ordering
• Excellent chemical inertness
quantities, consider:
• Not recommended for multiple
• the number of samples run during a
injections or storage of samples
day/week
• Least expensive Unattended autosampler
• if samples are run in small or large
runs require a precise fit for

TIPS AND TOOLS


Silicone/Teflon batches
uninterrupted operation.
• Excellent resealing • if samples are run manually or with an Typically, automated sample
• Resists coring autosampler runs use a higher quality and
• Good for multiple injections
• if samples are run overnight, unattended quantity of vials.
Teflon/Silicone/Teflon
• Used in trace analysis applications
• Above average resealing Vials
• Most resistant to coring
• Least evaporation Description Quantity Part No.
• Use with large diameter, blunt tip
syringe needles Vials

Teflon Disc 2 mL Crimp top vial convenience


• Good for MS and ECD analysis pack with silver AI caps with
Teflon/Red rubber septa 500/pk 5181-3400
• Good for large-volume injections
• Chemically inert 2 mL Screw top vial convenience
• No resealing pack with blue screw caps and
• Single injection Teflon/Red rubber septa 500/pk 5182-0732
• No long-term sampling storage 2 mL Snap top vial convenience pack
with clear polypropylene snap caps
Viton
and Teflon/Red rubber septa 500/pk 5182-0547
• Chlorinated solvents
• Organic acids 100 µL Insert for wide opening vials 100/pk 5181-1270
• Limited resealing
250 µL Polypropylene flat bottom inserts 500/pk 5183-2087
• Not suitable for 32 gauge syringe
100 µL Glass lined polypropylene vials 100/pk 9301-0977

Less than 5 µL dead volume,


Micro-V vial, clear crimp top 100/pk 5184-3551

30 µL reservoir volume, High recovery


vial, crimp top 100/pk 5182-3454

www.agilent.com/chem 20
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringes Selecting Syringes


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

Needle Gauge Selection

Inlet Needle Gauge Column Type

Packed, split or
splitless (including PTV) 23 gauge or 23/26 gauge tapered any

Cool on-column 23/26 gauge tapered or 26 gauge 530 µm

Cool on-column 26/32 gauge tapered 320 µm

Cool on-column 26/32 gauge tapered 250 µm

Needle Tip Needle Shape

Needle tips
Sharp tip Cone tip

Tapered needle

Use syringe needles with an Agilent dual-


taper needle or a conical tip. Sharp-tipped
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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Syringe Characteristics and Recommended Uses

Syringe Advantage Limitations Recommended Use

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


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

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


plunger • Most reliable fitted for 1 µL and larger syringe
plunger syringe injections • Clean samples
• Less bending • Plunger not • Routine analysis
• Better for high replaceable
viscosity samples

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


gas-tight for reduced than fitted plunger • Gases and volatile
repair cost • Not available in samples
• Less plunger binding 5 µL size • Reactive samples
than fitted plunger
• Tight seal between
plunger and barrel

Replacing On-column Syringe Needles


The stainless steel needles used for To insert a needle into a syringe barrel:
250-µm and 320-µm injections must
1. Unscrew the syringe barrel cap and
be inserted into a glass syringe barrel.
remove the spring.
Select the correct size needle for the
column you plan to use. 2. Make sure the needle has the Teflon
disk. If the syringe barrel does not
have the Teflon disk, use the instructions
in the syringe box to wrap the needle
yourself.
3. Slide the spring and the cap down over
the needle.
4. Insert the needle into the syringe barrel.
5. Screw the cap back on the syringe barrel.

TIPS AND TOOLS

Failure to use an on-column syringe when injecting into


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

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

Syringe Tips
• Make sure to input the proper syringe • Remove a gas-tight plunger from the • To maximize the lifetime of standard
size when setting up the injection section syringe for long-term storage to keep the plungers, rinse the syringe and wipe
of your data handling device. Teflon tip leak-free. If a gas-tight plunger the plunger with solvent (isopropanol
does not fit properly, place it in hot water or acetone) and a lint-free wipe, as
• Rinse syringes and clean their plungers
for about 10 minutes then press the tip specified in the syringe cleaning
before use to maximize syringe lifetime.
uniformly on a clean, hard surface and let procedure included with each syringe.
• Rinse the syringe 5-8 times between cool to room temperature. The plunger
injections to minimize sample carryover. should reseal correctly to provide 10-25%
more injections.
• Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
• A 26-gauge syringe can be used for
on-column injections into a 0.53mm id
column. Always check that on-column
syringe needles fit inside the capillary
column before installing the column
and syringe in the GC.
• For on-column injections, always use
the proper septum nut and stainless steel
insert for the column dimension you are
using. Use a septum with a molded
through-hole with injections onto 0.32mm
and 0.25mm columns.
• The more polar the solvent, the more
likely it is to contain water. Trace
amounts of water, especially when
combined with water-extractable
materials from samples, can accelerate
syringe wear dramatically. With these
types of samples, use a Teflon tipped
syringe plunger. Even better, proactively
replace syringes, since plunger bends
may be inevitable.

NEW! Agilent Gold Standard


GC Autosampler Syringes
see page 25

VIDEO

To view a video on syringe installation,


visit www.agilent.com/chem/techsupport.

23 www.agilent.com/chem
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, • If the plunger’s movement feels “gritty,”
metal, or glass can fill the narrow gap between remove the plunger from the barrel, flush the
the plunger shaft and the inside wall of the shaft with solvent, and wipe it dry with a lint-
barrel. free 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 • Improper needle alignment. • Use only Agilent autosamplers. They are
• Narrow-gauge needles (26 gauge) bend more precision-designed to ensure proper
easily than larger (23 gauge) needles. alignment with the syringe needle.

• Needles tend to bend when inserted into the • Use 23 to 26-gauge tapered needles to get
sample vial – not the inlet port. This can be the combined benefits of greater septa life
caused by septa that are too “tough.” and fewer bent needles.

• If the needle has been slightly bent when • Only use Agilent vials and septa.
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.

Blocked needles • Sample material or contaminants may be • Remove the plunger and use a second
trapped inside the needle. syringe to fill the blocked syringe with
• The needle may not have been properly cleaned. solvent. Then, insert the plunger and gently
push solvent through needle. Important: Try
to use a cleaning agent that is appropriate for
the contaminant. Common choices are
methanol, methylene chloride, acetonitrile,
and acetone.

Rust • During normal use, the shaft rubs against the • To slow this process, remove the water from
Note: even minor rust can cause the plunger glass walls of the barrel. This gradually wears the syringe at the end of each day.
to become stuck in the barrel. away the rust-resistant metal on the shaft’s 1. Rinse the syringe several times with a “dry”
surface. solvent, such as acetone.
• Rusting happens most rapidly when using water 2. Remove the syringe from the autosampler,
or solvents that may contain (or absorb) water. and wipe the plunger dry with a lint-free
cloth
3. Let syringe and plunger air dry.

“Ring around the neck” (A dark ring between • Skin oils and other organic material. • Never touch the plunger shaft with your
the top of the barrel and the end of the • Fine metal and glass particles from the syringe fingers.
volume scale.) plunger and barrel may be rubbing together. • If build-up appears when water is the
Once this happens, the plunger may bend if solvent: rinse syringe with acetone and wipe
used further. the plunger clean at the end of each day.

Loose plungers – accompanied by syringe • The syringe is nearing the end of its useful life. • Replace the syringe.
leaks and area count reproducibility problems. Note: Plungers normally feel “loose” when
non-polar solvents (like hexane and toluene)
are used.

www.agilent.com/chem 24
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Gold Standard GC Autosampler Syringes

Description Gauge/Length Quantity Part No.

Tapered Needle Syringes


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

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

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

Straight Needle Syringes


(use with Merlin Microseal)

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

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

GC Automatic Liquid Sampler Supplies

Description Unit Part No.

Miscellaneous Autosampler Supplies

4 mL Clear screw top wash vials Gold Standard GC


with screw caps (no Septa) 144/pk 9301 0723 ALS Syringe Features
Lot Numbers ensure certified
Septa for 4 mL vial 144/pk 9301-1031 performance to all specifications
Diffusion caps for 4 mL vials 12/pk 07673-40180
Gold protective cap prevents chipping
4 mL wash vial with fill marking, caps 25/pk 5182-0551 of the glass syringe barrel as it contacts
the septum retainer nut
Screw for mounting syringe 07673-20570
Black ink and gold illuminating backdrop
Quadrant kit (4 tray sections) 18596-40015 for easier viewing of the volume scale
7673/83 Basic Supply Kit contains: Individually sealed packaging for
10 mL syringes (6/ea), 23/26 gauge contaminant-free use
needles, 4 mL vials with diffusion caps
(144/pk), 2 mL automatic sampler
vials with screw caps (1,000/pk),
GC septa (25/pk), Vial racks (5/pk) 07673-60840

25 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

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

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

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

6890/6850 Series GC Packed Port Supplies*

Item Description Unit Part No.


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

3 Top insert weldment 19243-80570

4 Viton O-rings 12/pk 5080-8898

5 Glass liner, disposable 25/pk 5080-8732

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

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

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


Liner
Adapters with glass liners

8 0.53 mm column adapter 19244-80540

1/8 in. column adapter 19243-80530


5

1/4 in. column adapter 19243-80540


6
9 Upper insulation 19243-00067 7

10 Nut warmer cup with insulation 19234-60720 8


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

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


Inside
1/4
1/4 in. nut
in. nut
OvenOven
1/8 in.
1/8 in.oror1/4
1/4in.in.
For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals. 9 stainless steel
stainless linerliner
steel
* For Model 6890/6850 only
10

11

5890 Packed-Column Inlet Supplies

Description Unit Part No.

Nonpurging septum nut assembly


for manual flow control only, not EPC 19243-60570

Adapters without glass liners

1/8 in. column adapter 19243-80510


TIPS AND TOOLS

1/4 in. column adapter 19243-80520


Tap Agilent’s GC knowledge over the phone, Universal Packed-Column Inlet (non-purged)
online, in the classroom, even at your site.
See pages 104-115 for more information Septum retainer nut for
about our services and support. headspace sampling, nonpurging 19243-605050

Brass nut, 1/4 in. 10/pk 5180-4105

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

Split/Splitless Inlets
The combined “split/splitless” inlet is the Troubleshooting
most popular inlet for capillary column gas Split inlets are spared from most band- A majority of the problems encountered
chromatography. Because it can be used in broadening phenomena, since narrow with split inlets are related to discrimination
either split or splitless mode, it provides a peaks are generated as part of the splitting and decomposition. Both analytical
very effective combination that can cover process. Therefore, any peak broadening accuracy and reproducibility decrease
most analysis requirements. or tailing observed with split injection is with the increases in discrimination
usually due to improper column and decomposition. Split inlets suffer
Split Mode installation, low split flow, (<20 mL/min from both needle discrimination and
Split injection is an effective way to on 6890) or low inlet temperature. If you inlet discrimination.
introduce small amounts of sample without suspect that the inlet temperature may be
overloading the column. Split injection is too low, increase it by 50˚C and compare
required for samples that: the results to the lower temperature
• cannot be diluted for analysis (for analysis. Repeat if results are positive
example, solvents) until no further improvement is seen.
• 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 Mode Variables, Practices, and Rationales

Split injection is also good for screening Parameter Selection/Setting Rationale


samples of which little is known or for
those that have widely differing Inlet temperature Try 250˚C or BP of Ensures flash vaporization
concentrations, since the split ratio last eluting compound Minimizes inlet discrimination
can be adjusted easily. Split inlets are
Inlet liner Large volume, deactivated Minimizes flashback
also a good choice for dirty samples. Minimizes degradation
Inlet packing Silanized glass wool Retains non-volatiles
Minimizes inlet discrimination
Glass beads or frit Less active than wool
None Least active
Injection volume 0.5-3 µL liquid Split easily adjusted
0.10-10 mL gas Split adjusted accordingly
Injection technique Fast autoinjection Less needle discrimination
Hot-needle fast manual Reproducible discrimination
injection
Split ratio 50:1 to 500:1 Depends on sample and
injection volume, and column ID
Initial column Not critical Narrow initial peaks
temperatures
Septum purge 2-3 mL/min Minimizes ghosting

TIPS AND TOOLS

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

www.agilent.com/chem 28
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Split Mode Variables, Practices, and Rationales Splitless Mode


For splitless injection, a conventional split
Parameter Selection/Setting Rationale injector is operated in a nonsplitting mode
by closing the split valve during injection.
Inlet temperature Just above highest Ensures flash vaporization The sample is flash-vaporized in the liner,
boiling point of Reduce if degradation occurs and sample vapors are carried into the
solutes (+20˚C) Use higher for dirty samples column by the carrier gas where they are
and higher-boiling solutes recondensed at temperatures below the
Inlet liner Large volume >0.8mL Use with autoinjector boiling point of the solvent. After most of
Small volume <0.2mL Use only for slow manual the sample has been transferred into the
injections, and gas injections column, vapors remaining in the liner are
cleared by opening the split vent which
Inlet packing None Use only with slow injection remains open for the duration of the run.
Decreases degradation
The most important benefit of splitless
Silanized glass wool Use for fast autoinjection injection is that a majority of the injected
& dirty samples sample is introduced into the column. This
results in much higher sensitivity than that
Injection volume 0.5-2 µL liquid Depends on solvent, liner, achieved using split injection.
& conditions
Solvent Effect
Injection technique Fast autoinjection Most reproducible
One requirement of splitless injections is
Less needle discrimination
that the initial column temperature should
Hot-needle slow manual Inject 1-2µL.sec if narrow liner
be kept at least 10˚C below the boiling
is used and >1µL injection
point of the sample solvent. This allows
Hot-needle fast manual Use for <1µL injections
the sample solvent to condense at the
Purge flow 20-50 mL/min Higher if using constant flow front of the column trapping the solvent
molecules into a tight, narrow band.
Purge delay time 20-80 sec Adjust according to column Additionally, use a solvent that is similar in
flow rate/liner type polarity to the column stationary phase,
& sample conditions and avoid mixed solvents. Breaking these
rules may result in split peaks.
Oven temperature 10-25˚C below solvent BP Necessary for solvent focusing
Splitless injection is routinely used in
Column flow >2mL/min when possible Clears inlet fast areas such as:
Reduces backflash and
decomposition • environmental analysis

Septum purge 2-3mL/min Reduces ghosting • pesticide monitoring of foods

Quantification Internal standard Maximizes reproducibility • drug screening


Standard addition Use only with constant In these applications, sample preparation
injection volume requirements are significant, and it is not
always possible or economically justifiable
Retention gap 1-3m, deactivated Reduces peak distortion
to clean up a sample extensively. So
(1-2m per µL injected) Promotes solvent and
column protection becomes as important
stationary phase focusing
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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Troubleshooting
Most problems encountered with splitless Decomposition
injection are related to incorrect purge Loss of peak area or generation of new
time, degradation, improper focusing, and peaks, can sometimes be dramatically
flashback. reduced by changing liner type or by
deactivating the liner and inlet with
Appropriate initial column temperature is
silanizing reagents. Removing or reducing
critical. Sample vapors can be lost through
the amount of liner packing can also
the septum purge line if the insert is
decrease inlet activity.
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.

6890/6850 Split/Splitless Inlet Supplies*

Item Description Unit Part No.

1 Septum retainer nut 18740-60835


2 Septa See page 36
3 Insert Weldment G1544-60575
4 Liner O-ring See page 52
1
5 Liner See page 47
2

3 6 Split vent trap assembly (6890/6850 only) G1544-80550


4
7 Retaining nut (6890/6850 only) G1544-20590
6
5
Retaining nut (5890 only) 19251-20620
8 SS seal 18740-20880
Gold-plated seal 18740-20885
9 Washer, 0.375 in. od 12/pk 5061-5869
10 Reducing nut 18740-20800
11 Insulation (requires 3) 19243-00067
12 Lower insulation cover 19243-00070
13 Ferrule
14 Column nut (6890/5890 only) 2/pk 5181-8830
Column nut (6850 only) 2/pk 5183-4732
7 Angled wrench for split/splitless inlet 19251-00100
* 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.
13
14 (See page 61).

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

Cool On-Column Inlets


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

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 Projects droplets away from syringe tip
Fused silica needle Use for manual injection into small id columns
Oven temperature Inlet temperature or slightly lower Prevents backflash
Column flow 50-80cm/sec Use for H2 carrier gas
30-50cm/sec 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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Sample Considerations Troubleshooting


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

Column/Retention Gap Installation Consumables

Description Unit Part No.

Column nut 2/pk 5181-8830

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

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

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

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

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

Quartz deactivated column connector fits 0.18-0.53 mm 5/pk 5181-3396

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 32
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 Series Cool On-Column Inlet Supplies*

Item Description Unit Part No.


1a
Manual injection 1b 1c
1d
1c Cooling tower assembly 19320-80625
1d Duckbill septum 10/pk 19245-40050
Fused silica syringe needles 6/pk 19091-63000 2
3
4
Syringe barrel for use with
fused-silica needles,10 µL 9301-0658
Common Supplies
3 Spring 19245-60760
4 Inserts for capillary columns
For 200 µm columns (one ring) 19245-20510
For 250 µm columns (six rings) 19245-20515
For 320 µm columns (five rings) 19245-20525
For 530 µm columns (no rings) 19245-20580
For 530 µm Al clad columns (four rings) 19245-207804 5
6
5 Ferrule 5080-8853
6 Column nut 2/pk 5181-8830
6890 Series GC Cool On-Column Inlet Supplies
Automatic Injection
1a Septum nut base for 320 mm assembly 19245-80521
1b Septum nut base for 530 mm assembly G1545-80520
2 Advanced green 5 mm through hole septa 50/pk 5183-4760
BTO 5 mm through hole septa 50/pk 5183-4758
5890 Series Cool On-Column Inlet Supplies
Automatic Injection
1a Septum nut (5890 Series II GC) 19245-80520
1b Needle guide (for 7673A only) 19245-20670
* For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.

33 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Programmed Temperature Vaporizer (PTV) Inlets


PTV inlets combine the benefits of split, PTV Inlet Procedures/Practices (cold split/splitless modes)
splitless and on-column inlets. The sample is
usually injected into a cool liner, so syringe Parameter Selection/Setting Rationale
needle discrimination does not occur. Then
the inlet temperature is increased to vaporize Injection mode Cold split For general use
the sample. The user programs vent times and sample screening
and temperature to achieve the equivalent of Cold splitless For trace analysis
split or splitless transfer of sample vapors to Inlet temperature Adjustable (i.e., 2˚C/sec Use slower ramp rates for
the column. PTV injection is considered the ramp rate to 12˚C/sec) labile, complex, or large
most universal sample introduction system volume samples
because of its flexibility. Use faster ramp rates for
most samples
Advantages Use faster ramp rates to
• no syringe-needle discrimination shorten splitless purge delay time
• minimal inlet discrimination Ballistic Simpler, less expensive
instrumentation
• no special syringe needed
• use of large injection volumes Inlet liner Straight with silanized wool For general use
Baffled For labile samples
• removal of solvent and low boiling Packed with an adsorbent For focusing gaseous
components injections from auxiliary
• trapping of nonvolatile components sampling devices
in liner
Injection volume 0.1-1.5µL Use lower volumes for
• split or splitless operation volatile solvents and fast
• retention time and area reproducibility ramp rates
approaching cool on-column injection Use volumes larger than
1.5µL only in solvent-
PTV inlets are actively cooled before and elimination mode
during injection by Peltier devices or by
forced gases (air, liquid N2, or liquid CO2). Sample Injection Autosampler or manual, Not critical for cold split
Cryogenic cooling of the inlet can reduce technique fast or slow & splitless modes
inlet temperature enough to thermally Oven temperature 10-25˚C below solvent BP For proper solvent effect in
focus gas injections from other sampling splitless mode
devices in the liner. This is a distinct Sample dependent For split mode
advantage of using PTV inlets in
comparison to conventional inlets for Column flow 30-50 cm/sec Clears inlet faster
coupling auxiliary sampling devices to Less backflash
capillary columns.
Septum purge 1-5mL/min Minimizes ghosting
Post-injection, PTV inlets are heated
using electrical heaters or preheated Quantification Any method Inherently reproducible
compressed air. Depending on design, Low discrimination in cold
injection modes
inlet temperature ramps are either
ballistic (i.e., ramped to the maximum Retention gap 1-3m, deactivated Compensates for extended
temperature at an uncontrolled maximum flooded zone and solvent-
rate) or programmable. column 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 34
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

6890 PTV Inlet 1


3
2
Item Description Column ID Unit Part No.

1 Septumless head G2617-60507


2 Septum head G2618-80500
3 Septum nut 18740-60835
4 PTV inlet assy G2617-60506 4

5 PTV LCO2 cooling jacket G2617-60508


6 PTV LN2 cooling jacket G2619-60501
7 Silver seal 5/pk 5182-9763
8 Graphpak inlet adapter 0.20 mm 5182-9754
0.25-0.33 mm 5182-9761 5, 6

0.53 mm 5182-9762 7
8
9 Ferrules for 0.20 mm 10/pk 5182-9756 9
10
Graphpak inlet 0.25 mm 10/pk 5182-9768
0.32 mm 10/pk 5182-9769
0.53 mm 10/pk 5182-9770
10 Split nut for inlet adapters 5062-3525 11

11 PTV insulation block G2617-20510


PTV cryo insulator (not shown) G2617-60510
Teflon ferrule (needle seal) 5182-9748
Kalrez seal 5182-9759
Valve body 5182-9757
Pressure spring 5182-9758
Viton seal 5182-9775
There are few choices in

TIPS AND TOOLS


Sealing element 5182-9760
liner design for PTV inlets.
CO2 Cryo inline filter 3150-0602 However, liner volume and
Service kit for septumless head 5182-9747 activity are still key issues to
contains Kalrez seal, valve body, be considered when selecting
and pressure spring among the few available PTV
Graphpak 3D ferrules 5/pk 5182-9749 liners. PTV liners require
packing or a modified surface
Installation tool for 3D ferrules G2617-80540 to hold the liquid sample in
place before and during the
vaporizing process.

PTV Liners

Description Part No.

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


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

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

Septa
One of the key components of sample What is the Function
introduction is the inlet septum. All The septum isolates the sample flow path
columns must have carrier gas head from the outside world. It must provide a
pressure to establish flow through the barrier that is readily penetrated by the
column. Septa maintain the leak-free seal injector needle while maintaining internal
and exclude air from the inlet. They come pressure without contaminating the
in many different sizes and are made from analysis. They are generally made of
many different types of material specific special high-temperature, low-bleed
to inlet type and analysis needs. silicone rubber formulations.
Septa are usually available according to Why Replace
their recommended upper temperature Septa should be replaced regularly to avoid:
limits. Lower temperature septa are • leaks
usually softer, seal better, and can • decomposition Agilent Introduces Innovative
withstand more punctures (injections) • sample loss
than their high-temperature counterparts.
Packaging for Inlet Septa
• reduced column or split vent flow
If used above their recommended • ghost peaks Agilent has recently introduced a new
temperatures, however, they can leak or • column degradation and innovative packaging design for
decompose. This causes sample losses, inlet septa. This new packaging is a
lower column flow, decreased column life How to Minimize Problems tri-fold blister pack that provides
and ghosting. Avoid problems by: cleanliness, convenience, and
• using within the recommended consistency for our complete line
temperature range of 11 mm and 9.5 mm septa.
• changing regularly
• installing “hand tight” Your 50th Septum will be
• using septum purge when available as Clean as Your 1st!
• using autoinjectors
• using sharp syringe needles The primary benefit behind the new
packaging is that each septum is
individually packaged for the ultimate
cleanliness. Each septum is easily
dispensed one at a time by pushing it
through the back foil, as is commonly
done with pharmaceutical capsules and
tablets. No longer do you need to reach
into a jar and wonder how clean the
septa are or if you are contaminating
other septa.
In addition, the new packaging delivers
the following features and added value:
• No more clumping or sticking: Septa
don’t stick to each or the jar
• Easy to see exactly how many are
left: Know exactly when to reorder
• Compact storage size: Fits easily into
drawers
• Convenient quantities: All septa are
packaged in either 50 or 100 packs
• High quality PET packaging: Tested by
GC-FID, GC/MS, and GC-ECD to
ensure the absence of interfering
background peaks

www.agilent.com/chem 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.

Normal Problem

Baseline Change After Large Peak Large leak at septum during injection and Replace septum and use smaller diameter
for a short time thereafter (common with needles.
large diameter needles).

Normal Problem Problem


(flow increase) (flow decrease)

Retention Times Prolonged Carrier gas leaks at septum or column Check for leaks. Replace septum or tighten
connection. connections if necessary.

Normal Problem Problem

MAINTENANCE MINDER

After repeated injections, septa can become prone to leakage.


To maintain system integrity, change septa regularly.

37 www.agilent.com/chem
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

www.agilent.com/chem 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 Figure 1. Comparison of Coring, With and Without CenterGuide
(30x magnification)
stamped out in large sheets, creating variations in geometry. Rather,
each Agilent premium septum is molded to a perfectly uniform size High-Temperature Septa Without CenterGuide: Major Coring Before 1
and shape. 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 100 autoinjections 700 autoinjections
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 Agilent BTO Septa With CenterGuide: Very Little Coring Even After
700 Autoinjections
• Virtually no septa material falling into the inlet liner, improving
chromatographic quality
• Up to 1,000 autoinjections under optimal conditions before failure
with HP Point syringes. The HP Point syringe yields optimal
performance and reliability and reduces coring by parting, not
cutting, the septum.

Agilent septa are made of highly durable, high-temperature tested


silicone rubber.

Each lot is tested to ensure low bleed at high temperatures.

Summary of Inlet Septum Characteristics

TEMPERATURE
SEPTUM TYPE BLEED LIFETIME LIMIT

BTO ✔✔✔ ✔ to 400ºC


(Bleed and (optimized for
Temperature high temperature)
Optimized)

Long Life ✔ ✔✔✔ to 350ºC

Advanced Green ✔✔ ✔✔ to 350ºC

✔✔✔ = best ✔✔ = very good ✔ = good

39 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

p/n 5183-4757 p/n 5183-4761 p/n 5183-4759

Agilent Bleed and Temperature Agilent Long-Life Non-Stick Septa Agilent Advance Green
Optimized Non-Stick Septa (BTO) • Pre-pierced for extended life and Non-Stick Septa
• Extended temperature range, low-bleed reduced coring • True Long-Life, High Temperature
• Maximum Injection Port Temperature • The preferred Septum for Autosamplers Green Septum
400ºC • Ideal for Overnight Runs • More Injections per Septum
• Virtually eliminates injection-port • Up to 400 Injections Per Septum injection • Reduced Injection Port Sticking
sticking • Maximum Injection Port Temperature
• Maximum Injection Port Temperature
• Pre-conditioned; packaged in glass 350ºC 350ºC
to prevent contamination • Packaged in glass vials for high purity
• Soft, 45 Durometer, Easy On
• Ideal for use with low-bleed, Autosampler Needles • Economical alternative to competitor’s
“Mass Spec” capillary columns “Green” Septa

General Purpose Septa


Agilent’s General Purpose Septa are Agilent’s General Purpose red/gray
made from an enhanced injection-molded septa are cost-effective choices
silicone rubber material. The septa material, which provide:
dark red or gray in color, is specified to
withstand over 200 automatic injections • Low bleed for reduced instrument • While general purpose septa do not have
at an injection port temperature of maintenance downtime and increased the centerguide of premium septa,
350ºC. You can have confidence in your laboratory productivity they are made of durable material to
chromatographic results knowing that • Less frequent replacement for long minimize the risk of contamination and
each lot of septa is placed through a lifetime and the ability to withstand more the need for reconditioning
demanding QC test to ensure that only than 200 autosampler injections at • Convenient blister packs of 50 or 100
the highest quality product is delivered maximum injection port temperatures septa minimize risk of contamination
to your laboratory.
and need for reconditioning

www.agilent.com/chem 40
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Septa Ordering Information

Part No.
Premium Non-Stick Septa
Agilent Bleed and Temperature Optimized Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4757
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4757-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4758

Agilent Advanced Green Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4759
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4759-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4760

Agilent Long-Life Non-Stick Septa

11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4761
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4761-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4762

General Purpose Septa

Gray Septa

11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk) 5080-8896-50


11 mm for 5880, 5890, 6850 and 6890 GCs (100/pk) 5080-8894-100
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5080-8728-50
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5080-8728-100

Red Septa

11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk) 5181-1263-50
11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk) 5181-1263-100
11 mm with partial through-hole for 5880, 5890, (50/pk) 5181-3383-50
6850 and 6890 GCs
11 mm with partial through-hole for 5880, 5890, (100/pk) 5181-3383-100
6850 and 6890 GCs
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5181-1283-50
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5181-1283-100
5 mm through-hole for on-column inlets, (25/pk) 5181-1260
automatic or manual injections*
5 mm solid for high column backpressure, on-column inlets* (25/pk) 5181-1261
* 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 www.agilent.com/chem
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
Column Ferrule Types
high as 450ºC, and Vespel and Vespel- Advantages Limitations
graphite ferrules are rated to 280ºC and
350ºC, respectively. Graphite Easy-to-use, stable seal Soft, easily deformed or destroyed

What is the Function Higher temperature limit • possible system contamination


Ferrules seal the connection of the column • not for use with GC/MS
or liner to the system. The ideal ferrule transfer-lines
provides a leak-free seal, accommodates
various column outer diameters, seals with Vespel or Mechanically robust Flows at elevated temperature
minimum torque, will not stick to the Vespel-graphite Long lifetime • must retighten frequently
column or fittings, and will tolerate
temperature cycling. • prone to leakage

Why Replace Polymer bleed problematic with


Signals that a ferrule is damaged include: some detectors (NPD and ECD)

• background noise from oxygen diffusing


into the system How to Minimize Problems
• column bleed catalyzed by oxygen General technique for installing ferrules:
• sample degradation • don’t overtighten – finger-tighten column
• loss of sample nut, then use wrench to tighten
• increase in detector signal/noise • maintain cleanliness
• poor retention time reproducibility • bake out ferrules prior to use (Vespel and
Vespel/Graphite only)
• avoid contamination – such as
fingerprint oils
• inspect used ferrules with magnifier for
cracks, chips, or other damage before
reusing them
• change ferrules when new columns or
injector/detector parts are installed

www.agilent.com/chem 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 Column positioned incorrectly in the Column positioned incorrectly in the inlet
injection port and FID injection port, or possible ferrule or septum (either too far or not far enough; verify
particle in the carrier gas flow path 4-6mm installation distance)

100% Graphite Ferrules


Reusing a ferrule – or using off-brand Two different types of Agilent column nuts
ferrules – may be a costly mistake. That’s can be used with these ferrules:
because you’ll increase the likelihood of
• The universal column nut (p/n 5181-
dangerous leaks that can damage the GC
8830) has a hexagonal head requiring the
column and sensitive detector parts.
use of a wrench to tighten it completely.
For best results, always use new Agilent • The finger-tight column nut (p/n 5020-
ferrules, which feature the highest quality 8293 for 530um columns and p/n 5020-
design, and are supported by decades of 8292 for columns 320µm or less) does
technical expertise. 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 www.agilent.com/chem
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 Two different lengths of Vespel/graphite When using Vespel/graphite ferrules,
turn with a wrench. ferrules are available for capillary column Agilent recommends tightening the column
use. The standard sized ferrule is nut to a 1/4 turn after the first temperature
These ferrules are very hard and cannot compatible with the universal column nut. program runs. Even preconditioned ferrules
be deformed sufficiently to seal multiple The second ferrule size is slightly longer can exhibit some shrinkage after a
column diameters. The ferrule hole must and is specifically designed to fit with the temperature programmed run.
match the column OD exactly to ensure a MS interface nut used for the GC/MS
leak-free seal. For capillary column transfer line connection. The larger ferrule
applications, there is a specific ferrule for can also be used to make column
each column diameter. Choosing a ferrule connections to inlets and other detectors
with a larger hole than is specified for a but requires a specially designed column
given column dimension can result in a nut (p/n 05988-20066) to accommodate
large leak. If left unchecked, an improper the longer ferrule.
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 Vespel/Graphite Nut & Ferrule Combinations
source which can increase the frequency
of detector maintenance.
Standard ferrule and standard nut
Universal Column Nut + Vespel/Graphite Ferrules
5181-8830 5181-3323 (0.1, 0.2, 0.25 mm ID columns)
5062-3514 (0.32 mm)
5062-3512 (0.45 and 0.53 mm)

Longer ferrule with MS interface nut


MS Interface Column Nut + Vespel/Graphite Ferrules
05988-20066 5062-3508 (0.1, 0.2, and 0.25 mm ID columns)
5062-3506 (0.32 mm)
5062-3538 (0.45 and 0.53 mm)

www.agilent.com/chem 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 Upper Usages Limitations


Type Temperature
Limit
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Ferrule Ordering Information


Ferrule Id Column Id Quantity Part No.
(mm) (mm)

General Purpose Graphite Ferrules (Short Ferrules)


0.5 0.1, 0.2, 0.25, 0.32 10/pk 5080-8853
1.0 0.53 10/pk 5080-8773
0.4 0.05-0.25 10/pk 500-2114
0.8 0.45, 0.53 10/pk 500-2118

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


0.80.3 0.1, 0.2 10/pk 5062-3516
0.80.4 0.1, 0.2, 0.25 10/pk 5181-3323
0.80.5 0.32 10/pk 5062-3514
0.80.8 0.45, 0.53 10/pk 5062-3512

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


0.3 0.1 10/pk 5062-3507
0.4 0.1, 0.2, 0.25 10/pk 5062-3508
0.5 0.32 10/pk 5062-3506
0.8 0.53 10/pk 5062-3538
These ferrules are recommended for use with GC/MS.

100% Vespel High-Performance Ferrules (Short Ferrules)


0.4 0.1, 0.2, 0.25 10/pk 5181-3322
0.5 0.32 10/pk 5062-3513
0.8 0.45, 0.53 10/pk 5062-3511
These ferrules are recommended for use in isothermal analysis only.

Specialty Ferrules, 85% Vespel, 15% Graphite


Two Hole 0.4 ID holes 0.1, 0.2, 0.25 10/pk 5062-3580
0.5 ID holes 0.32 10/pk 5062-3581
No Hole 10/pk 5181-3308

SilTite Metal Ferrules


For use with 0.20-0.25 mm ID 0.4 10/pk 5184-3569
capillary columns. Includes 2 column nuts
For use with 0.32 mm ID capillary 0.5 10/pk 5184-3570
columns. Includes 2 column nuts
For use with 1/16 in. od 10/pk 5184-3571
SS tubing. Includes 2 column nuts
For use with 0.53 mm ID capillary columns. 0.8 10/pk 5188-2789
Includes 2 nuts

Column Nuts
Short Nuts
Universal column nut, 1/16 in. hex 2/pk 5181-8830
Finger-tight column nut for 0.53 mm columns* 1 ea 5020-8293
Finger-tight column nut for 0.32 mm columns* and smaller 1 ea 5020-8292
Blanking plug, finger-tight style 1 ea 5020-8294
6850 Column Nut 2/pk 5183-4732

Long Nuts
MS interface column nut 1 ea 05988-20066
Column nut for GC/MS ferrules 1 ea 05921-21170
Column nut wrench, 1 /4 in. and 5 /16 in. 1 ea 8710-0510
* For use with graphite ferrules only.
Always match short nuts with short ferrules and long nuts with long ferrules.

www.agilent.com/chema 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 How to Minimize Problems
Change liners on a regular basis
• ghost peaks determined by:
• reduced column life • 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 www.agilent.com/chem
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 Liner Deactivation
reproducibility and sensitivity. Backflash Active sites on inlet liners can adsorb With use, even deactivated liners can
also frequently results in sample carryover. sample components and cause peak tailing, begin to exhibit activity. When this occurs,
and potential loss of sensitivity and the liner should be replaced. Liners can be
Larger volume liners (> 800 µL) are
reproducibility. Deactivation agents are cleaned to remove particulate material or
characterized by larger inside diameters
used to cover or react with active sites on solvent rinsed to remove less volatile
(ID) and are typically used with injection
the glass surface of the liner. Agilent liners components. However, choosing the
sizes of 1 µL or more. The small volume
are deactivated using deactivation proper liner cleaning procedure can be
liners have a smaller ID and are usually
procedures that produce reproducible and difficult. Some solvents may remove the
used with small injection sizes (< 1 µL),
inert liners, with long lifetimes. For splitless deactivation layer, and tools might scratch
fast 100 µm ID columns, gas samples, or
applications or when even slightly polar the glass surface of the liner, resulting in
when using external sampling devices
compounds must be analyzed, a the generation of unwanted active sites.
like headspace and purge and trap.
deactivated liner should be used. 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 48
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Design Features


Dimensions Packing
• The outside diameter (OD) of the liner
determines if the liner is more effectively Glass Wool Glass Cups
used in split or splitless mode Many liner designs use deactivated Another design feature used to help
• Larger OD liners are designed for splitless glass wool packing. The glass wool is volatilize the sample and provide good
operation, fit tightly and limit sample positioned or held in place near the mixing is the incorporation of a glass cup
contact with metal parts of the inlet center of the liner to: inside the liner. Glass cup liners are also
• Larger OD liners improve analyte recovery available with additional glass wool and
by retaining more sample inside the liner • Provide additional surface area for
inert packing to increase reproducibility
• Agilent splitless liners are all designed complete volatilization of the sample to
and limit sample discrimination. Not
with exacting dimensional tolerances to minimize thermal discrimination
recommended for use with Electronic
fit tightly in the inlet and minimize sample • Trap non-volatile components and septum
Pressure Control Inlets on 6890 or 6850 GCs.
contact with metal surfaces particles before they reach the column
• Smaller OD liners are designed for split • Wipe any sample from the syringe needle,
injection because they produce less thereby increasing reproducibility and
resistance to carrier and split flow preventing sample residue build-up at the
through the inlet septum
• Large volume liners are used for split Glass wool liners that have glass wool near
injections with enforced dimensional the center of the liner, such as Agilent Part
stability for a wide range of split ratios Figure 1.
Nos. 5183-4647 and 5183-4711, are
Tapers recommended for automatic injections.
Tapering or narrowing the liner internal If glass wool is positioned at the bottom of
diameter (ID) is done for a number of the liner, its main purpose is simply to trap
purposes: non-volatile components. Glass wool is
• Bottom taper focuses sample onto the generally not recommended for the
head of the column following analytes:
• Bottom taper minimizes contact with • phenols
metal parts of the inlet • organic acids
• Center taper positions glass wool • pesticides
correctly • amines
• Top taper minimizes sample backflash • drugs of abuse
To operate properly, the column must be • reactive polar compounds
installed correctly in the injection port with • thermally labile compounds
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 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Troubleshooting
Symptom Possible Cause Remedy

Tailing Peaks Sample components adsorbed by column, Use new, deactivated liner or clean old
inlet liner or contaminated gold inlet seal. liner and replace glass wool.

Needle hitting and breaking packing in Partially remove packing from liner or use
inlet liner. without packing.

Normal Problem Column end poorly cut Remove column. Make a clean, square
(sample absorption). cut using a reliable capillary fused silica
Broken or chipped inlet liner. 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.

Baseline Rise Before or After Peak 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.

Normal Problem Problem

Baseline Change After Large Peak Column and inlet liner misaligned. Check installation of column end and inlet
See also”Septum Troubleshooting,” liner; adjust if necessary.
page 37

Normal Problem Problem

Unresolved Peaks Column or inlet liner contaminated or Use a guard column to prolong column life.
column deteriorating. Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass
wool and packing. Trim the front end of the
column a minimum of 6 inches.

Normal Problem Problem

www.agilent.com/chem 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.
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
Split injection: optimized by Agilent R&D engineers to
Agilent low-pressure-drop split liner with allow them to work with EPC.
glass wool, bottom taper, glass bead for Focus Liner
easy positioning, and deactivated, Agilent Improve reproducibility, improve results.
Part No. 5183-4647 (with extraordinarily The Focus Liner traps a precisely controlled
tight dimensional control for optimum amount of glass wool in the ideal position
split performance). in the injection port liner. At the point of
Splitless injection: injection, the glass wool provides extra
Single tapered liner without glass wool, surface area for vaporization, traps
deactivated, Agilent Part No. 5181-3316EN. nonvolatile sample residue, and wipes
any residual sample from the sample
Note: For pesticide analysis – especially needle – reproducibility is the result.
DDT and Endrin, where breakdown is a
problem – we recommend Agilent Part In addition to these liners we offer a
Nos. 5181-3316EN and 5181-3315EN. broad selection of liners for your specific
application needs.
General purpose split/
splitless injection: Liner O-Rings
Similar design to Agilent Part No. 5183- Liners are sealed in the inlet with O-rings
4647, but with an outer diameter that or graphite seals. O-ring seals are easier to
compromises for both split and splitless remove and to replace than graphite that
injections, Agilent Part No. 5183-4711. deforms and flakes apart. The graphite
seals should be used when inlet
temperatures exceed 350ºC.

51 www.agilent.com/chem
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 leak-
free 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.
To view videos on the Flip Top Inlet Sealing System,
Flip Top Inlet Sealing System 5188-2717 visit www.agilent.com/chem/fliptop2
Liner O-rings (10/pk) 5188-2741

www.agilent.com/chem 52
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Liner Ordering Information


Application Liner Single 5/pk 25/pk
Volume(µl) Liner
Agilent Choice Liners
Liner, split, low press. drop, For split injection 870 5183-4647 5183-4701 5183-4702
glass wool, taper, deactivated

Liner, splitless, single-taper, For splitless injection 900 5181-3316 5183-4695 5183-4696
no glass wool, deactivated

NEW! Liner, Splitless, For trace pesticide 900 5181-3316EN


Single-taper, no glass wool, analysis
polymerically deactivated

Liner, direct, 2 mm ID, For direct injection 250 5181-8818 5183-4703 5183-4704
deactivated (use for gas samples,
headspace, or purge
and trap applications)

Liner, general purpose For split/splitless 870 5183-4711 5183-4712 5183-4713


split/splitless, glass wool, injection
taper, deactivated

Splitless Inlet Liners


Liner, splitless, single-taper, glass wool, deactivated 900 5062-3587 5183-4693 5183-4694

Liner, splitless, double-taper, no glass wool, deactivated 800 5181-3315 5183-4705 5183-4706

NEW! Liner, Splitless, For trace pesticide 800 5181-3315EN


double-taper, no glass wool, analysis
polymerically deactivated

Direct Inlet Liners


Liner, direct, 2 mm ID, non-deactivated, quartz 250 18740-80220 5183-4707 5183-4708

Liner, direct, 1.5 mm ID, non-deactivated 140 18740-80200 5183-4709 5183-4710


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

Liner, straight, splitless 4.0 mm ID 990 210-3003 210-3003-5

Split Inlet Liner 990 19251-60540 5183-4691 5183-4692


Liner, split, glass wool, non-deactivated

Split Inlet Liners For Manual Injection 800 18740-80190 5183-4699 5183-4700
Liner, split, with cup, no glass wool

Liner, split, with cup, glass wool, and packing 800 18740-60840 5183-4697 5183-4698
[not recommended for use with electronic pressure
control (EPC)], for manual injection

Direct Connect Liners


Part No.
Single taper direct connect liner, 4 mm ID, deactivated G1544-80730
Dual taper direct connect liner, 4 mm ID, deactivated G1544-80700

Focus Liners
ID Wool Dimensions Part No.
Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4004-5
Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4022-5

Liner O-Rings Part No.


Fluorocarbon O-ring (12/pk) 5180-4182
Graphite O-ring for splitless liner (10/pk) 5180-4173
Graphite O-ring for split liner (10/pk) 5180-4168
Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk) 5188-2741

53 www.agilent.com/chem
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 Septum See page 36


Part No. 18740-60835
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 Gold-Plated Seal (Splitless)
www.agilent.com/chem. See page 55

Ferrules (85% Vespel, 15% Graphite)


– Part No. 5062-3516, 0.37 mm I.D.,
Retaining Nut for 100-200 µm Columns, 10/pk
Part No. G1544-20590 – Part No. 5181-3323, 0.40 mm I.D.,
for 250 µm Columns, 10/pk
Washer
Part No. 5061-5869, 12/pk – Part No. 5062-3514, 0.50 mm I.D.,
for 320 µm Columns, 10/pk
Reducing Nut – Part No. 5062-3512, 0.74 mm I.D.,
Part No. 18740-20800, for 530 µm Columns, 10/pk
1 each

Column Nut for 6890 GC


Part No. 5181-8830, 2/pk

www.agilent.com/chem 54
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS

Part No.

6890/6850 Split/Splitless Insert Assemblies


Standard manual pneumatics 19251-60575
Original standard EPC using 1/4" split vent filter. G1544-60575
Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to G1544-80580
clean carrier gas for ECD operation.
S/SL insert weldment. Used with large charcoal canister type filter G1544-60585
for 6890/6850.
Similar to G1544-60575 except carrier lines separated for interface to valved G1580-60575
systems of a G1540A instrument.
S/SL insert assembly for G1540A with valved system option. This insert assembly G1580-60585
uses the large charcoal canister split vent filter for 6890/6850.

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 18740-20880
Gold-plated seal 18740-20885
Gold-plated seal with cross 5182-9652
Washers (12 pk) 5061-5869

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
Bottom

Gold-plated seal p/n 18740-20885 Gold-plated seal with cross p/n 5182-9652
Use when inlet flow exceeds 400 ml/min.

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

“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 HP-
capillary GC columns.”
Phil Stremple,
GC Columns Program Manager

CATALOG

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


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

www.agilent.com/chem 56
COLUMNS

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

Selection of Capillary Columns for GC and GC/MS


Phases
All phases can be used with conventional
GC systems, and most stationary phases Primary
“Quantion”
can be used with a GC/MS system. is hidden

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
Primary
appears as an elevated baseline as the “Quantion”
is enhanced
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.
There are a few simple rules for choosing Dimensions
columns with lower bleed levels: All dimensions can be used with
• Choose a low-bleed phase for your conventional GC systems. Many types of GC
application – Agilent has developed column phases can be used with the MSD,
several low-bleed versions of the most but there are some dimensional
popular phases. These are chemically considerations. The maximum allowable
designed to possess minimal levels of flow rate and optimal sensitivity flow rates
column bleed possible and often have will vary depending upon the type of pump.
the benefit of an increased upper- In general, the column flow should be
temperature limit. 1mL/min (2mL/min for Performance Turbo
• If a low-bleed column is not available, Pumps). Therefore, column length
choose a low-polarity column with a and internal diameter combinations are
moderate film thickness. The amount of restricted to provide the appropriate flow
bleed will rise with increases in polarity, to the GC/MS.
film thickness, and length. • Narrow-bore columns (0.25mm i.d. and
• Use more polar phases when difficult smaller) can be installed directly into the
isomer separations are required. (Choose GC interface.
a more polar phase when you must, but
try to make it the least polar column that
will do the job)

57 www.agilent.com/chem
COLUMNS

Popular Column Choices


• Wide-bore columns (0.32mm i.d.) that are
30m or longer can be installed directly Description Part No.
into the 5973 GC interface (other MSDs
may require 50m or longer). If using a DB-1ms, 0.25mm i.d., 30m, 0.25µm 122-0132
wide-bore column with a shorter length,
an effluent splitter or jet separator should HP-5ms, 0.25mm i.d., 30m, 0.25µm 19091S-433
be utilized.
• Columns with internal diameters greater DB-XLB, 0.25mm i.d., 30m, 0.25µm 122-1232
than 0.32mm should not be directly
DB-35ms, 0.25mm i.d., 30m, 0.25µm 122-3832
interfaced into the GC interface. For these
columns, an effluent splitter or jet HP-INNOWax, 0.25mm i.d.,
separator should be installed. 30m, 0.25µm 19091N-133

Column Installation, Setup, & Conditioning


The first step in obtaining optimal • Verify that all fittings are leak-free and
column performance and lifetime is the carrier gas is oxygen-free before
proper installation: heating the oven.
• Choose the appropriate size and • Briefly conditioning a column before
material ferrule for the column, installing it into the GC/MS interface is
injector and detector type. recommended. When the column and
• Avoid re-using ferrules. inlet are first heated, volatile materials
within the flow-path and a small portion
• Use an appropriate column cutting of the column stationary phase move into
tool such as a ceramic wafer or the gas phase. These materials are then
diamond tipped scribe. carried by the carrier gas into the MSD
• Make sure column ends are and can deposit in the MSD ion source.
cleanly cut and free of particulate This can decrease MSD performance.
matter before installing into the Conditioning the column briefly prior to
injector and detector. installation into the MSD will minimize
• Install the column the appropriate the contamination brought into the ion
distance into the injector and detector source.
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.

www.agilent.com/chem 58
COLUMNS

Column Installation & Setup continued


Description Part No.

Ceramic wafer (4/pk) 5181-8836


Bad 20x Magnifier 430-1020

General Purpose Graphite ferrule


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

General Purpose Graphite ferrule


Good (1.0mm ID, for 0.45-0.53mm
ID columns) 10/pk 5080-8773
Example of column cuts
Gas leak detector 115V 5182-9646
Gas leak detector 220V 5182-9648
• Check the installation and set the
linear velocity by injecting a non-retained
compound.
• Condition the column as specified in the
literature provided with each column.

Causes of Performance Degradation Description Part No.


Column Breakage Prevention
Fused Silica Union,
Fused silica columns can break wherever • Avoid scratches and abrasions by not Universal 2-way
there are small scratches or abrasions in exposing the column to sharp edges such (5/pk) 705-0905
the protective polyimide coating. as column hangers and tags, metal edges
Continuous heating and cooling of the in the GC oven, column cutters and other Quartz deactivated
oven, vibrations caused by the oven miscellaneous items on the lab bench. column connector
fan as well as being wound on a circular (5/pk) 5181-3396
• Avoid winding or bending the column
cage all place stress on the tubing.
too tightly. Polyimide Sealing
While under these stresses, flaws
Recovery resin (5 grams) 500-1200
will propagate until breakage occurs.
• If a broken column has been heated,
NOTE: Larger diameter columns damage to the stationary phase is very
(0.45- 0.53mm id) are more prone likely. Discard the back of the column
to breakage. (the column half without carrier gas).
Trim 6 inches off the end of the
column and reinstall.
• If the broken column has not been
heated, connect the two pieces with
a low volume union. No more than
2-3 unions should be installed for
one column.

59 www.agilent.com/chem
COLUMNS

Thermal Damage Recovery NOTE: Momentary exposure to oxygen


Exceeding a column’s upper temperature such as an injection of air or removing
• Disconnect column from detector
limit results in accelerated degradation of the septum nut for a short period of
the stationary phase and tubing surface. • Heat the column 8-16 hours at the time is not a problem.
This results in the premature onset of isothermal limit
excessive column bleed, peak tailing for Prevention
• Remove 10-15 cm from the column end Maintain an oxygen and leak-free
active compounds and/or loss of efficiency
(resolution). • Reinstall into the detector and condition system by:
as usual • performing periodic leak checks
Prevention
• Do not exceed the columns specified NOTE: Thermal damage cannot be reversed. • changing septa regularly
upper temperature limits: The column usually does not return to its
• using high quality carrier gases
original performance; however, it is often
– Isothermal limit: temperature that
still functional. The life of the column will • installing and maintaining oxygen traps
the column can be held at for an
be reduced after thermal damage.
indefinite time • changing gas cylinders before they are
Oxygen Damage completely empty
– Programmed limit: maximum column
temperature; column should only be Oxygen is an enemy to all capillary GC
Recovery
held there for about 5-10 minutes columns. Constant exposure to oxygen
Perform column “bakeout” as described
does not damage the column at or near
• Set the GC maximum oven temperature under thermal damage recovery.
ambient temperatures; however, severe
function at or a few degrees above the damage occurs as the column temperature NOTE: Oxygen damage occurs very rapidly.
temperature limit of the column. With increases. A leak in the carrier gas flow In less severe cases, the column may still
two columns in the oven be sure to set path (e.g., gas lines, fittings, injector, be functional but at a reduced performance
the maximum temperature to the septa) is the most common source of level. In more severe cases, the column is
temperature limit of the column with the oxygen exposure. As the column is heated, irreversibly damaged.
lowest value. 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.

FlowTracker 2000 Flowmeter and Leak Detector 5183-4780

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

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

Big Universal Trap (Combination Trap)


(750cc, 1/8" fitting, He) RMSH-2

Advanced Green Septa (11mm, 50/pk) 5183-4759

TIPS AND TOOLS

Install a moisture trap upstream of the oxygen trap to increase


the oxygen trap lifetime.

www.agilent.com/chem 60
COLUMNS

Chemical Damage GUARD COLUMN


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

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

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

61 www.agilent.com/chem
COLUMNS

Nonvolatile Contaminants
Nonvolatile contaminants or residues do Description Part No.
not elute and accumulate in the column
(most often confined to the first few Split/Splitless Inlet liner: glass wool,
meters). The column becomes coated with taper, deactivated (5/pk) 5183-4712
these residues which interfere with the
proper partitioning of solutes in and out Splitless Inlet liner: single-taper,
of the stationary phase. Also, the residues no glass wool, deactivated (5/pk) 5183-4695
may interact with active solutes resulting
in peak adsorption problems (evident as Quartz deactivated column
peak tailing or loss of peak size). Active connector (5/pk) 5181-3396
solutes are those containing a hydroxyl
Polyimide sealing resin (5 grams) 500-1200
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes. Deactivated Fused silica,
10m, 0.53mm i.d. 160-2535-10
Prevention
• Perform sample cleanup to remove Deactivated Fused silica,
nonvolatile materials from the sample 10m, 0.25mm i.d. 160-2255-10
• Use injection port liners packed with
glass wool (may not be feasible when Capillary column rinse kit 430-3000
analyzing active compounds)
• Install a guard column and trim regularly
Recovery
• Do not bakeout the column
• Front End Maintenance: Prevention Column Storage
• Perform sample cleanup to remove Capillary columns should be stored in their
– Clean or change the injection port liner
semi-volatile materials from the sample original box when removed from the GC.
– Clean out the injector • Increase the final temperature of the Place GC septa over the ends to prevent
GC run (not to exceed the temperature debris from entering the tubing. Upon
– Cut off typically 0.5 to 1 meter of the
limit of the column) reinstallation of the column, the column
front of the column
ends need to be trimmed by 2-4 cm to
• Change septa regularly ensure that a small piece of septa is not
• Turn the column around (install detector
end into injector). Not recommended for Recovery lodged in the column.
sensitive ECD, NPD, and MS detectors. • Bakeout the column: limit 1-2 hours If a column is left in a heated GC, there
• Solvent rinse the column (excess baking may polymerize some should always be carrier gas flow through
contamination and reduce column the column. The carrier gas flow can be
• Cut the column in half and use the back
lifetime) turned off only if the oven, injector,
half (detector side)
• Solvent rinse the column detector and transfer lines are turned off
Semivolatile Contaminants (i.e., not heated). Without carrier gas flow,
Semivolatile contaminants or residues Does Your Sample Have Residues? damage to the heated portion of the
accumulate in the column, but eventually Perform this simple test. column occurs.
elute. Hours to days may elapse before 1. Place 20-30 µL of the sample onto a
they completely leave the column. Like microscope slide.
nonvolatile residues, they may cause peak
shape and size problems and, in addition, 2. Put the slide over the heated GC inlet
are usually responsible for many baseline for 20 minutes.
problems (instability, wander, drift, ghost 3. Hold the slide up to the light.
peaks, etc.).
If you can see anything where the drop
was, your sample has residues.

www.agilent.com/chem 62
COLUMNS

Column Types and Characteristics

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


• 100% Dimethylpolysiloxane
• Identical selectivity to DB-1 I.D. Length Film Part No.
• Nonpolar
• Very low bleed characteristics 0.10 10 0.10 127-0112
• Improved acid performance compared to 0.10 10 0.40 127-0113
standard 100% Dimethylpolysiloxane 0.10 20 0.10 127-0122
columns 0.10 20 0.40 127-0123
• Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity 0.20 12 0.33 128-0112
• Excellent general purpose column 0.20 25 0.33 128-0122
• Bonded and cross-linked 0.25 30 0.10 122-0131
• Solvent rinsable 0.25 30 0.25 122-0132
0.25 60 0.25 122-0162
0.32 30 0.10 123-0131
0.32 30 0.25 123-0132
0.32 60 0.25 123-0162

Similar Phases Applications


HP-1ms, Rtx-1ms, CP-Sil 5CB General purpose: Amines, hydrocarbons,
pesticides, PCBs, phenols, sulfur
compounds, flavors and fragrances.

63 www.agilent.com/chem
COLUMNS

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


• Phenyl Arylene polymer equivalent to a
(5%-Phenyl)-methylpolysiloxane I.D. Length Film Part No.
• Nonpolar
• Very low bleed characteristics
0.18 20 0.18 121-5522
• Excellent inertness for active compounds
0.18 40 0.18 121-5542
• Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity 0.20 25 0.33 128-5522
• Bonded and cross-linked 0.20 50 0.33 128-5552
• Solvent rinsable
0.25 25 0.25 122-5522
• Certified for MS
0.25 25 0.40 122-552A
• Exact replacement of HP-5TA
0.25 30 0.10 122-5531
• Close equivalent to USP Phase G27
0.25 30 0.25 122-5532
0.25 30 0.50 122-5536
0.25 50 0.25 122-5552
0.25 60 0.10 122-5561
0.25 60 0.25 122-5562
0.32 30 0.10 123-5531
0.32 30 0.25 123-5532
0.32 30 0.50 123-5536
0.32 50 0.25 123-5552
0.32 60 0.10 123-5561
0.32 60 0.25 123-5562

Similar Phases Applications


Rtx-5ms, HP-5ms, PTE-5, CP-Sil 8CBms, Semivolatiles, alkaloids, drugs, FAMEs,
BPX-5 halogenated compounds, pesticides,
herbicides

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


• (5%-Phenyl)-methylpolysiloxane
• Nonpolar I.D. Length Film Part No.
• Very low bleed characteristics
• Excellent inertness for active compounds 0.20 12 0.33 19091S-101
• Improved signal-to-noise ratio for better 0.20 25 0.33 19091S-102
sensitivity and mass spectral integrity 0.20 50 0.33 19091S-105
• Bonded and cross-linked
• Solvent rinsable 0.25 15 0.10 19091S-331
• Certified for MS 0.25 15 0.25 19091S-431
• Equivalent to USP Phase G27 0.25 15 1.00 19091S-231
0.25 30 0.10 19091S-333
Similar Phases 0.25 30 0.25 19091S-433*
Rtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms, 0.25 30 0.50 19091S-133
BPX-5, Rtx-5 Amine 0.25 60 0.10 19091S-336
0.25 60 0.25 19091S-436
Applications 0.32 15 1.00 19091S-211
Semivolatiles, alkaloids, drugs, FAMEs, 0.32 25 0.52 19091S-112
halogenated compounds, pesticides, 0.32 30 0.10 19091S-313
herbicides 0.32 30 0.25 19091S-413
0.32 30 0.50 19091S-113
0.32 60 0.10 19091S-316
0.32 60 0.25 19091S-416
* This column is shipped with the 5973 MSD.

www.agilent.com/chem 64
COLUMNS

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


• Exceptionally low bleed
• Low polarity I.D. Length Film Part No.
• Extended temperature limit of 360°C
• Unique selectivity 0.18 20 0.18 121-1222
• Excellent inertness for active compounds 0.18 30 0.18 121-1232
• Ideal for confirmational analyses
• Excellent for pesticides, herbicides, PCBs 0.20 12 0.33 128-1212
and PAHs 0.20 25 0.33 128-1222
• Certified for MS 0.25 15 0.10 122-1211
• Bonded and cross-linked 0.25 15 0.25 122-1212
• Solvent rinsable 0.25 15 1.00 122-1213
0.25 30 0.10 122-1231
0.25 30 0.25 122-1232
0.25 30 0.50 122-1236
0.25 30 1.00 122-1233
0.25 60 0.25 122-1262
0.32 30 0.10 123-1231
0.32 30 0.25 123-1232
0.32 30 0.50 123-1236
0.32 60 0.25 123-1262

Similar Phase Applications


MDN-12 PCB congeners, pesticides, chlorinated
herbicides, phenoxy acid methyl esters,
haloacetic acids

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


• Equivalent to a (35%-Phenyl)-
methylpolysiloxane I.D. Length Film Part No.
• Midpolarity
• Very low bleed characteristics 0.20 15 0.33 128-3812
• Extended temperature limit of 360°C 0.20 25 0.33 128-3822
• Excellent inertness for active compounds
• Certified for MS 0.25 15 0.25 122-3812
• Ideal for confirmational analyses 0.25 30 0.15 122-3831
• Bonded and cross-linked 0.25 30 0.25 122-3832
• Solvent rinsable 0.25 60 0.25 122-3862
• Replaces HP-35ms 0.32 30 0.25 123-3832
• Close equivalent to USP Phase G42 0.32 60 0.25 123-3862

Similar Phases Applications


Rtx-35, SPB-35, AT-35, Sup-Herb Aroclors, PCBs, amines, pesticides,
chlorinated herbicides, haloacetic acids,
pharmaceuticals, drugs of abuse

65 www.agilent.com/chem
COLUMNS

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


• Equivalent to (50%-Phenyl)-
methylpolysiloxane I.D. Length Film Part No.
• 320/340°C Upper temperature limit
• Very low bleed midpolarity column 0.18 20 0.18 121-4722
• Excellent inertness for active compounds 0.25 15 0.15 122-4711
• Enhanced mass spectral integrity 0.25 15 0.25 122-4712
• Bonded and cross-linked 0.25 30 0.15 122-4731
• Solvent rinsable 0.25 30 0.25 122-4732
• Best column for CLP pesticides 0.25 60 0.25 122-4762
0.32 30 0.15 123-4731
0.32 30 0.25 123-4732

Similar Phases Applications


DB-17, HP-50+, Rtx-50, 007-17, SP-2250, Drugs, glycols, pesticides, steroids
SPB-50, BPX-50, SPB-17

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


• Equivalent to (50%-Cyanopropylphenyl)-
methylpolysiloxane I.D. Length Film Part No.
• Mid/high polarity
• Excellent for separations of cis- and 0.25 15 0.25 122-2912
trans-fatty acid methyl esters (FAMEs) 0.25 30 0.25 122-2932
• Low bleed 0.25 60 0.25 122-2962
• Bonded and cross-linked 0.32 30 0.25 123-2932
• Solvent rinsable
• Close equivalent to USP Phase G7
Similar Phases Applications
HP-225, SP-2330, CP-Sil 43CB, RSL-500, Alditol acetates, FAMEs, neutral sterols
Rtx-225, BP-225, CB-225, OV-225, 007-225

EASY ONLINE ORDERING

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


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

www.agilent.com/chem 66
COLUMNS

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


• Polyethylene glycol (PEG)
• High polarity I.D. Length Film Part No.
• Highest upper-temperature limits of the
bonded PEG phases 0.20 25 0.20 19091N-102
• Column-to-column repeatability 0.20 25 0.40 19091N-202
• Bonded and cross-linked 0.20 50 0.20 19091N-105
• Solvent rinsable 0.20 50 0.40 19091N-205
• Close equivalent to USP Phase G16 0.25 30 0.15 19091N-033
0.25 30 0.25 19091N-133
0.25 30 0.50 19091N-233
0.25 60 0.15 19091N-036
0.25 60 0.25 19091N-136
0.25 60 0.50 19091N-236
0.32 30 0.15 19091N-013
0.32 30 0.25 19091N-113
0.32 30 0.50 19091N-213
0.32 60 0.15 19091N-016
0.32 60 0.25 19091N-116
0.32 60 0.50 19091N-216

Similar Phases Applications


HP-20M, SUPELCOWAX 10, CP-WAX 52CB, Alcohols, aromatics, essential oils, solvents
SUPEROX II, CB-WAX, Stabilwax, BP-20,
007-CW, Carbowax, DB-WAXetr

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


• Unique bonded PLOT column technology
• Excellent choice for light hydrocarbons I.D. Length Part No.
and sulfur gases
• Retention stability not affected by water 0.32 30 113-4332
• Separates CO and CO2 on a single 0.32 60 113-4362
column
• Ideal PLOT column for GC/MS –
no particles 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.

67 www.agilent.com/chem
Detectors
Most detectors require simple but periodic
cleaning to maintain peak performance.
This is especially true for highly sensitive
GC detectors. Without routine detector
maintenance, GC system performance will
deteriorate and can cause detector failure.
Detailed procedures on how to clean,
maintain and replace common detectors,
including FID, TCD, NPD, ECD, and FPD are
summarized in this section. Also included
are special handling techniques and specific
recommendations to maximize specific
detector operations. For example, learn how
to resolve flame ignition problems associated
with your flame photometric detector and
test electron capture detectors for
radioactivity leaks.

“GC detectors are highly sensitive systems


that are often compromised by various
types of contamination. By implementing
some recommended detector
maintenance routines, you can minimize
instrument downtime and keep your GC
system working at peak efficiency.”
Bernhard Rothweiler
Applications Chemist

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 68
DETECTORS

Flame Ionization Detector (FID)


Flame Ionization Detectors require little
maintenance to keep them performing at
satisfactory levels. The primary task is to Igniter Glow Plug Assembly
occasionally measure hydrogen, air and
makeup gas flows. They can drift over time
or be changed unintentionally without Collector Assembly
knowledge of it occurring. Each gas flow
should be independently measured to
obtain the most accurate values.
Collector Body
Condensation
Since the FID combustion process
results in water formation, the detector
temperature must be kept above 100˚C to
prevent condensation. Such condensation,
FID Jets
especially when combined with chlorinated
solvents or samples, causes corrosion and
sensitivity loss.

Hardware Problems
If the flame goes out or will not light:
• Check the column flow rate. It may FID Ferrules
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
Cleaning & Replacement
Even with normal use, deposits develop in
completely plugged jet.
the jet and detector (usually white silica
• Check that the right type of jet is installed from column bleed or black carbonaceous
for the column you are using. soot). These deposits reduce sensitivity
• Injecting large volumes of aromatic and cause chromatographic noise and
solvent or water can cause the flame to spikes. Although you can clean the jet, it is
go out. Switch to a nonaromatic solvent usually more practical to replace dirty jets
or inject less solvent. with new ones. If you do clean the jet, be FID Cleaning Kit, P/N 9301-0985
• The lit offset value may be too low or too careful not to scratch the jet internally;
high. Adjust the value. scratches will ruin the jet

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
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 Item Description Unit Part No.
the jet. Run it back and forth a few times
until it moves smoothly. Be careful not to 1 PTFE chimney (optional)** 19231-21050
scratch the jet. (Do not force too large a 2 Collector nut 19231-20940
wire or probe into the jet opening or the
3 Spring washer 10/pk 5181-3311
opening will become distorted. A loss of
sensitivity, poor peak shape and/or 4 Ignitor castle 19231-20910
lighting difficulties may result if the Optional Hastelloy Ignitor Castle* 19231-21060
opening is deformed.)
5 Ignitor glow plug assembly 19231-60680
2. Fill an ultrasonic cleaning bath with
6 Collector insulator G1531-20700
aqueous detergent, and place the jet in
the bath. Sonicate for five minutes. 7 Collector body G1531-20690
Hastelloy Collector Body 61531-21090
3. Use a jet reamer to clean the inside of
the jet. 9 FID collector assembly 1 G1531-60690

4. Sonicate again for five minutes. Detector insulation assembly G1531-20700


FID collector cleaning brush 2/pk 8710-1346
NOTE: From this point on, handle the parts
only with forceps! Collector Housing G1531-20740

5. Remove the jet from the bath and rinse it FID retainer nut wrench 19301-00150
thoroughly, first with hot tap water and (5880, 5890, 6890)
then with a small amount of GC-grade 1/4 in. Nut Driver for FID jet-drilled shaft 8710-1561
methanol. FID supplies kit-Includes: 5182-3450
6. Blow the jet dry with a burst of Jet, packed standard 3 each 18710-20119
compressed air or nitrogen, and then FID performance evaluation sample kit 2 each 18710-60170
place the jet on a paper towel and allow Ignitor glow plug assembly 2 each 19231-60680
it to air dry. Jet, cap. series 530 µm 3 each 19244-80560
FID flow measuring insert 2 each 19301-60660
Cleaning wires for 0.03 in. ID jet 5180-4150
Cleaning wires: 0.018 in. ID/530 µm jet 1/pk 5180-4152
Wire, jet cleaning, 5 each 19301-20720
Capillary inlet cleaning wires 5180-4153
Detector cleaning kit 9301-0985
**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

www.agilent.com/chem 70
DETECTORS

FID Jets

Description Length(mm) Part No.


Jets for capillary dedicated FID
Capillary jet (0.011 in./0.29 mm ID tip) 48 G1531-80560
High-temperature jet (SimDIS 0.018 in. ID tip) 48 G1531-80620
Adaptable FID
Capillary 0.53 mm jet (0.011 in. ID tip) 61.5 19244-80560
Packed (0.018 in. ID tip) 63.5 18710-20119
Agilent FID Jets (from top to bottom): Dedicated
Packed (0.030 in. ID tip) 63.5 18789-80070 capillary, Adaptable capillary, Adaptable packed
0.53 mm high temp (0.018 in. ID tip) for SimDIS 61.5 19244-80620

3
FID Consumables
4
8 5
Description Unit Part No.
6
FID flow measuring insert 19301-60660
7
FID ignitor cable G1531-60680
FID Performance evaluation sample kit, 0.03% C14, 18710-60170 6
C15, and C16 normal alkanes in hexane
O-rings 12/pk 5080-4978
Cleaning wire 19301-20720
Jet cleaning wire for 0.03 in. ID jet 5/pk 5180-4150
Jet cleaning wire for Series 530 mm and 0.018 in. ID jet 5/pk 5180-4152

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 www.agilent.com/chem
DETECTORS

Electron-Capture Detector (ECD)

Agilent provides two types of electron Radioactivity Leak Test


capture detectors. The regular detector Electron capture detectors must be tested
(ECD) has a larger internal volume for radioactive leakage at least every six
(approximately 10 times) than the micro- months. Records of tests and results must
cell detector (µ-ECD). These two types can be maintained for possible inspection by
be distinguished by the top cover of the the Nuclear Regulatory Commission and/or
detector – the ECD has a solid cover and the responsible local agency. More frequent
the µ-ECD has a perforated cover. tests may be conducted when necessary.

Thermal Cleaning The procedure used is a “wipe test.” A


If your baseline is noisy or the output wipe test kit is supplied with each new
value is abnormally high and you have detector. Refer to the information card
determined that these problems are not supplied in the Wipe Test Kit for
being caused by leaks in the GC system, instructions on performing the test.
you may have contamination in the
detector from column bleed and sample
Gas Purity
For successful EC detection, it’s important
residues. To remove contamination, you
that the carrier and purge gases are very
should perform a thermal cleaning
clean and dry (99.9995%). Moisture,
(bakeout) of the detector.
oxygen, or other contaminants can improve
Warning: Detector disassembly and/or sensitivity, but at a cost of linear range.
cleaning procedures other than thermal Always precondition the column before
should be performed only by personnel connection to the detector.
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.

ECD Warnings

Although beta particles at this energy level have little penetrating power – the
surface layer of the skin or a few sheets of paper will stop most of them – they
may be hazardous if the isotope is ingested or inhaled. For this reason the cell
must be handled with care. Radioactive leak tests must be performed at the
required intervals, the inlet and outlet fittings must be capped when the detector
is not in use, corrosive chemicals must not be introduced into the detector, and
the effluent from the detector must be vented outside the laboratory environment.

www.agilent.com/chem 72
DETECTORS

Electron-Capture Detector (ECD) Supplies

Item Description Part No.

1 ECD makeup gas adapter* G1533-80565

2, 3 Nut warmer cup with insulation 19234-60720

ECD adapter replacement liner, fused silica 19233-20625

ECD end cap 19233-20755

ECD chemical sample kit, 3 ampoules 18713-60040


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

ECD wipe test kit 18713-60050


*Includes one each of P/N 19233-20625 and P/N 19233-20755
1

6890 Series GC ECD Detector

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

TIPS AND TOOLS

Tap 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 www.agilent.com/chem
DETECTORS

Thermal Conductivity Detector (TCD)


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

Graphite ferrules, 0.5 mm id 10/pk 5080-8853

Capillary column nut, for 6890 2/pk 5181-8830

Capillary column nut, for 6850 2/pk 5183-4732

TCD packed column adapter (6890/6850 only) G1532-20710

TCD chemical sample kit, 3 ampoules,


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

5890 TCD Supplies

Makeup gas adapter, TCD 19232-80550

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

TCD replacement cartridge 19232-60676

www.agilent.com/chem 74
DETECTORS

Solvent Flush Procedure


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

75 www.agilent.com/chem
DETECTORS

Flame Photometric Detector (FPD)


Maintenance
Flame Photometric Detectors require High detector temperatures reduce the • If the flame doesn’t light at all, check the
minimal maintenance to keep them PMT life. When not in use, turn off the glow plug circuit. Observe the visual
performing at satisfactory levels. The PMT to maximize its usable lifetime. Some display, which will momentarily go to
hydrogen, air and makeup gas flows should PMTs may have a shelf life and should not greater than 65500 counts when the
be measured occasionally. They can drift be stored for prolonged periods before use. flame lights. If the display doesn’t
over time or be changed unintentionally change, check the pin connections at the
Column bleed and/or effluent can
without knowledge of it occurring. Each gas printed circuit board, the lead connection
contaminate the first quartz window (heat
flow should be measured independently to on the glow plug and the appropriate 5A
shield) nearest the detector module. Dust,
obtain the most accurate values. fuse on the GC main circuit board.
fingerprints, and atmospheric
Cleaning & Parts Replacement contaminants can dirty both quartz • The flame is easier to light at higher
The FPD requires periodic cleaning. In windows, the filter, and/or the detector temperatures.
most cases, this only involves the jet, and photomultiplier tube window.
• Under some operating conditions, the
less frequently, the filter. Agilent provides Contamination anywhere along the light
flame may be more easily lit with the
brushes and wires that simplify the path between flame and PMT can reduce
rubber drip tube removed. After lighting
cleaning of all detector parts (see FPD detector sensitivity.
the flame, reinstall the drip tube.
Supplies on page 77). The brushes are If a response problem is encountered
used to dislodge particulates clinging to • If the flame still won’t light, there could
(sensitivity, noise, selectivity) the FPD jet
the metal surfaces. A fine wire is used to be a large leak in the system. This results
should be inspected for deposits and, if
clean the jet opening of particulates. Do in measured flow rates being different
necessary, cleaned or replaced. To properly
not force too large a wire or probe into the from actual flow rates, causing non-ideal
service the jet, the detector module should
jet opening or the opening may become ignition conditions. Thoroughly leak
be removed from the instrument, and
distorted. A loss of sensitivity, poor peak check the whole system.
followed by appropriate service (see jet
shape, and/or lighting difficulties may cleaning procedure on page 70).
result if the opening is deformed. The filter
Flame Conditions & Gas Flows
Occasionally, the transfer line fused silica The flame conditions are critical to
or any of the window parts should be
liner between the column and FPD module successful operation. Since the detection
handled gently. Scratches or other surface
must be inspected, cleaned and/or replaced. zone is above the flame, the gas flows and
deformities reduce the amount of light
jet diameter must be optimized so that
passing through the filter, thus reducing
Flame Ignition Problems components burned (activated) in the
response. The filter and related parts
If the FPD flame won’t light or stay lit: flame will emit in the detection zone.
should be clean and free from fingerprints.
• Be sure there is a problem. Ignition is best Gas flows are also critical for optimized
The Photo Multiplier Tube (PMT) needs
confirmed by holding a mirror or shiny selectivity and sensitivity. The most critical
periodic replacement. The PMT is defective
surface near the aluminum exhaust tube, parameters are the hydrogen/air or
and needs to be rebuilt or replaced if:
with the rubber drip tube removed, and hydrogen/oxygen ratio, and the total gas
• high voltage is on and the flame is lit observe condensation if the flame is lit. flow, which effects flame temperature.
• low or no signal and/or noise not • Check Lit Offset. If it is zero, autoignition
attributed to any other source such as is turned off. If it is too large, the GC will
bad cables are observed not know that the flame is lit and will
shut down the detector.
• light leaks occur
• Increase the air supply pressure to the
• high temperatures are used
pneumatics module. This makes the
• defective signal boards are present flame easier to light but does not affect
the air flow rate setpoint.

www.agilent.com/chem 76
DETECTORS

6890/5890 FPD Supplies

Item Description Unit Part No.

1 Exit tube assembly 19256-60700


1
2 Nut, brass, 1/4 in. 10/pk 5180-4105 2
3
4 Weldment, block 19256-80560 4
9
5 O-ring, ignitor, Kalrez 0905-1610 5 10
6
7 11
6 Spacer, ignitor 19256-20590
12
7 FPD Ignitor Replacement Kit 19256-60800 8 13
14
8 Ignitor cable assembly (6890 only) G1535-60600 15

9 Gasket, heat shield 19256-80045


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

12 Coupling, SS 19256-20550 20

21
14 Screw, M3 x 12 (4 required) 0515-0911
15 Clamp 19256-00090
16 O-ring, inner window 12/pk 5061-5886
17 Window, second heat shield 19256-80060
18 O-ring, outer window 12/pk 5061-5891
19 Flange adapter 19256-20510
20 Flange ring 19256-00200
21 O-ring, Viton, 1.239 in. id 12/pk 5061-5890
Adapter weldment, 1/8 in. columns 19256-80590
Adapter weldment, capillary 19256-80570
Start-up kit (5890 only) 19256-60500
FPD O-ring (5890 only) 12/pk 5061-5867
Liner/ferrule kit 19256-60590
Sulfur filter 19256-80000
Phosphorus filter 19256-80010
Kalrez O-ring, size 2-002 0905-1609 Install the correct optical
MAINTENANCE MINDER

Kalrez O-ring, size 2-011 0905-1608 filter, depending on the


choice of Sulfur or
Fluorocarbon Elastomer O-ring,
brown, 0.926 in. id 12/pk 5061-5889 Phosphorus mode.
For Sulfur Mode, use
FPD Performance Evaluation Sample: Solution of the 393 nanometer filter.
20 ng/mL (20 ppm) dodecanethiol and
For Phosphorus Mode,
tributylphosphate in isooctane, 3 ampoules 19305-60580
use the 525 nanometer filter.

77 www.agilent.com/chem
DETECTORS

Nitrogen-Phosphorus Detector (NPD)


Bead Maintenance Bead Life Gas Flow
NPDs are temperamental and require To extend the life of the bead: The hydrogen, air and makeup gas flows
frequent maintenance. Small changes in any • Use the lowest practical adjust offset or should be measured frequently. They can
of a number of parameters can significantly bead voltage. drift over time or be changed unintentionally
change the performance characteristics of without knowledge of it occurring. Each gas
an NPD. The bead requires the most • Run clean samples and keep the inlet/liner flow should be measured independently to
maintenance. It needs to be changed clean to minimize contamination. obtain the most accurate values. NPDs are
frequently, thus a spare is a necessity. • Turn off the bead when not in use. very sensitive to changes in the gas flows
and consistent flows are necessary to
The beads have to be kept dry which limits • Keep the detector temperature high maintain performance levels.
their storage life to about six months. When (320 – 335˚C).
a new bead is installed, slowly raise the Gas Purity
detector temperature and bead current. • Turn off the hydrogen flow during solvent Because of its high sensitivity, the NPD
Rapid heating can crack or break the bead peaks and between runs. requires very pure gases (99.999% or better).
especially if it has been stored under humid • If the NPD is off for an extended period We strongly recommend that moisture and
conditions. It has been observed that higher of time in a high humidity environment, hydrocarbon traps be used on the carrier
hydrogen flows and bead currents decrease water may accumulate in the detector. gas and all detector gases, including the
bead life. If the NPD is not in use, the To evaporate this water, set the detector detector hydrogen, air, and makeup gases.
hydrogen flow and bead current should be temperature to 100˚C and maintain it Dirty gases will not only give poor
reduced or turned off to increase bead life. for 30 minutes. Then set the detector chromatographic performance, but will
Make sure there is some type of gas flow in temperature to 150˚C and maintain it shorten the bead life as well.
a heated detector or when there is current to for another 30 minutes.
the bead.

www.agilent.com/chem 78
DETECTORS

Cleaning & Replacement Contaminants


Some chemical problems can also arise
The NPD requires periodic cleaning. In most
when using the NPD. Because it is a trace
cases, this only involves the collector and
detector, be careful not to contaminate the
the jet. Agilent provides brushes and wires
analytical system.
that simplify the cleaning of all detector
parts (see NPD Supplies on page 79). The Glassware
brushes are used to dislodge particulates Glassware must be very clean. Phosphate
clinging to the metal surfaces. A fine wire is detergents should be avoided, so acid
used to clean the jet opening of particulates. washing of glassware followed by distilled
Do not force too large a wire or probe into water and solvent rinsing is recommended.
the jet opening or the opening will become
distorted. A loss of sensitivity or poor peak Solvents
shape may result if the opening is deformed. Solvents should be checked for purity.
The various parts can be ultrasonicated after Chlorinated solvents and silanizing reagents
cleaning with a brush. Eventually the jet can decrease the useful lifetime of the alkali
needs to be replaced, so it is strongly source; excess reagent should be removed
recommended to have spare jets on hand. prior to injection, if possible.
Over time, residue from the bead or sample Other Contamination Sources
can build up in the collector and cause Phosphate-containing leak detectors,
baseline problems. You should clean the phosphoric acid-treated columns or glass
collector after you have changed the bead wool, polyimide-coated columns, or
two or three times. nitrogen-containing liquid phases can add
The metal C-rings wear slightly with each noise to the system and should be avoided.
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 NPD Jets
jet, use the cleaning wire, taking care not to
damage the inside of the jet. You can also Description Length (mm) Part No.
use a sonicator bath to clean the jet.

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


(6890 only, dedicated) 48 G1531-80560

6890/5890 Adaptable

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

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

79 www.agilent.com/chem
DETECTORS

Nitrogen-Phosphorous Detector (NPD) Supplies

Item Description Part No.

6890 NPD Supplies

1 Screws, M3 x 0.5 x 8 mm (Pozidriv) 0515-0655

2 NPD white ceramic bead assembly* G1534-60570


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

3 Lid weldment G1534-80510 3

4 Metal C-ring, top 0905-2580


9
5 Alumina insulator, upper G1534-40020 11
10
4 12
6 Collector funnel G1534-20530
5
6
7 Alumina insulator, lower G1534-40030

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

9 Screw, M4 x 10 mm 0515-2495

10 J-Clamp 1400-0015

11 Screw, M4 x 10 mm 0515-2495

12 NPD interconnect assembly G1534-60610 13


14
13 Mounting pallet G1531-40020

14 Jets (see page 79)

15 Base weldment, Capillary NPD G1534-80500 15


16
Base Weldment, Packed NPD G1534-80540

16 Lid stop G1534-20590 17

NPD Ceramic Insulator Kit


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

18 Nut warmer cup with insulation 19234-60720

5890 NPD Supplies

NPD collector (NPD bead) 19234-60540

Recoating kit, sufficient for 10 collectors 5080-8872

Detector Trap Replacement Kit 19231-60790

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

www.agilent.com/chem 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.

www.agilent.com/chem 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 EVERY EVERY EVERY AS
WEEK 6 MONTHS YEAR NEEDED Every six months
Replace the foreline pump oil. Check,
and if necessary, refill the calibration vial.
Tune the MSD •
Change injection port liners •* Every year
Check the foreline pump oil level • Replace the diffusion pump fluid.
Gas ballast the foreline pump • Recondition or replace internal and external
Check the calibration vial • traps and chemical filters on the GC.
Replace the foreline pump oil • As needed
Check the diffusion pump fluid • Tune the MSD. Clean the ion source.
Replace the diffusion pump fluid • Replace the carrier gas trap. Replace
Replace the traps and filters • worn-out parts (filaments, EM, etc.).
Clean the ion source • Replace the column. Lubricate seals.
Change the carrier gas trap(s) and purifier • Monitor
Replace the worn out parts • Record all tune values such as electron
Lubricate seals (where appropriate) • multiplier and ion source parameters in
Replace column • 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 www.agilent.com/chem
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 The action required to remove the contamination depends on the type of
• foreline pump oil contamination and the level of contamination. Minor contamination by water
• fingerprints inside the manifold or solvents can usually be removed by allowing the system to pump (with a
flow of clean carrier gas) overnight. Serious contamination by rough pump
oil, diffusion pump fluid or fingerprints is much more difficult to remove; it
may require extensive cleaning. For further details contact your Agilent
Customer Engineer (CE).

Air Leaks Symptoms of leaks include:


Air leaks are a problem for any instrument • higher than normal vacuum manifold
that requires a vacuum to operate. Leaks pressure or foreline pressure
are generally caused by vacuum seals that • higher than normal background
are damaged or not fastened correctly. • peaks characteristic of air (m/z 18, 28,
32, and 44 or m/z 14 and 16)
• poor sensitivity
• low relative abundance of m/z 502
(this varies with the tune program and
MSD used)

www.agilent.com/chem 84
GC/MS SYSTEMS

Leaks can occur in many more places


in the MSD: Description Part No.
• GC/MSD interface column nut
MS interface column nut 05988-20066
• side/top plate O-ring (all the way around)
• vent valve O-ring Column nut for GC/MS and two-hole ferrules 05921-21170
• calibration valve Universal Column Nut (2/pk) 5181-8830
• 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 TIPS AND TOOLS
adapter O-ring
• turbomolecular pump O-ring
• new Vespel/graphite ferrules contract The most likely point for an air leak is a seal you recently opened.
when heated

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

Cleaning Solvents Corrective Action


It is common to see cleaning solvent peaks • Dry all cleaned metal parts in the GC • Use a temperature that’s just above
in the mass spectra shortly after the ion oven before reassembling and reinstalling the boiling point of the solvent.
source is cleaned. them. Refer to specific cleaning
procedures in your MSD Hardware
Manual.

Fingerprints
Fingerprints contain hydrocarbons that can Corrective Action
appear in mass spectra. Hydrocarbon • Reclean using clean, nylon gloves and
contamination is characterized by a series proper cleaning techniques.
of mass peaks 14 amu apart. The
abundances of these peaks decrease as
peak mass increases. Fingerprint
contamination is usually caused by the
Description Part No.
failure to wear lint-free, nylon gloves during
ion source cleaning, GC inlet maintenance, Nylon gloves, lint-free, Large 8650-0030
or from installing the column. Use special Nylon gloves, lint-free, Small 8650-0029
care to avoid recontamination of parts after
you clean them. This typically occurs after
some maintenance or part replacement.

Diffusion Pump Fluid


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

85 www.agilent.com/chem
GC/MS SYSTEMS

Foreline Pump Oil


Foreline pump oil contamination is Corrective Action
characterized by peaks spaced 14 amu • Call Agilent for assistance.
apart (hydrocarbons). Contamination with
foreline pump oil is less common than
contamination with diffusion pump fluid.

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, PFTBA and related ions PFTBA (tuning compound)
181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614
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 Foreline pump oil vapor or calibration valve leak
PFTBA
73, 147, 207, 221, 281, Dimethylpolysiloxane Septum bleed or methyl silicone column coating
295, 355, 429
77, 94, 115, 141, 168, 170, Diffusion pump fluid Diffusion pump fluid and related ions
262, 354, 446
149 Plasticizer (phthalates) Vacuum seals (O-rings) damaged by high temperatures,
use of vinyl or plastic gloves
Peaks spaced 14 amu apart Hydrocarbons Fingerprints, foreline pump oil

www.agilent.com/chem 86
GC/MS SYSTEMS

Mass Spectrometer Symptoms


Sensitivity
This section describes some of the Symptoms Corrective Action
symptoms you might observe – either in
the spectra of samples or in a tune report. Wrong retention time Check GC, method, application and carrier gas velocity
Typically, these symptoms fall into two
Low signal Check GC, tune vacuum system
broad classes:
1. those that affect the system Leaking injection port Clean the injection port
sensitivity. Replace the injection port liner and septa
2. those that affect the repeatability Air leak Check and tighten interface nut, leak test GC injection port
of a measurement.
Some symptoms can be corrected by Peak widths Do Autotune, check flow rate and temperature stability
following the suggested corrective actions. Interfering peaks Check time parameters, coeluting peaks, column type
Others require the services of an Agilent Excessive background Do Autotune and compare to background specifications
Customer Engineer. Check time parameters
Incorrect mass assignment Retune
Abnormal spectra – Check for contamination
excessive background
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
Variations in pressure, Ensure the MSD is located in an environment where
column flow, the temperature is stable
and temperature – 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 Check internal and external analyzer wiring connections,
in the analyzer make sure all are secure
Ground loops Check main electrical lines

87 www.agilent.com/chem
GC/MS SYSTEMS

Ion Source

The ion source operates by electron cules, ionizing and fragmenting them. The
ionization (EI) or chemical ionization (CI). positive voltage on the repeller pushes the
The sample enters the ion source from the positive ions into the lens stack, where
GC/MSD interface. Electrons emitted by a they pass through several electrostatic
filament enter the ionization chamber, lenses. These lenses concentrate the ions
guided by a magnetic field. The high-energy into a tight beam, which is directed into the
electrons interact with the sample mole- mass filter.

5973 Ion Source Assembly (EI)

Maintaining the Ion Source


Cleaning procedures for MSDs vary. Refer Selecting a Cleaning Method Preparing to Clean
to your MSD Hardware Manual for specific The primary action of any cleaning Prior to cleaning, the mass spectrometer
ion source cleaning procedures. procedure is to remove contamination from must be vented and the ion source must be
surfaces. Removing this contamination removed. Before venting the system, the
Common measures of instrument restores the electrostatic properties of the following conditions must be met:
performance: ion source lensing system. Numerous
• abundance of certain ions (e.g. cleaning methods have been developed for • heated zones are less than 100°C
percentage of the 502 ion from the restoring ion source performance. The • the diffusion pump is off and cool
Autotune report) cleaning methods include abrasive, sonic, • the turbo pump is off and not spinning
• shape of lens ramps and the chosen and electropolish. • the rough pump is off
voltages, especially Repeller Ramp
• sensitivity obtainable for a given analysis Abrasive methods offer several advantages: Always allow the automatic venting routine
• ability to tune to a given reference • provide adequate energy to remove to run its full course. Improper venting may
compound (e.g. DFTPP) contamination from surfaces cause diffusion pump fluid to be deposited
• require minimal equipment into the analyzer (backstreaming). It can
When to Clean: • pose minimal risks to the user also reduce the life of the multiplier, or
The ion source should be cleaned: other sensitive MS parts.
• according to a customer’s predefined A popular material used to abrasively clean
schedule stainless steel ion source parts is
• based on instrument performance (e.g. aluminum oxide. It is available in either
deteriorated performance over time) powder form or an abrasive film. After the
critical surfaces have been abrasively
Frequency of Cleaning cleaned, the loose particles must be
The cleaning frequency is determined by: removed. One method of removing particles
• the number of samples run (throughput) is swabbing with a cotton swab or a clean
• the type of samples cloth dipped in acetone. A clean swab
• unique, established laboratory protocol 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.

www.agilent.com/chem 88
GC/MS SYSTEMS

Cleaning and Maintenance Supplies

Description Part No.

Cleaning and Maintenance


Nylon gloves, lint-free, Large 8650-0030
Nylon gloves, lint-free, Small 8650-0029
Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk) 9310-4828
Generic ion source cleaning kit for all GC/MS types 5181-8863
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) 05980-60051
Abrasive Sheets, aluminum oxide green lapping paper for ion source 5061-5896
cleaning, 600 mesh (5 sheets)
Alumina powder, abrasive 8660-0791
PFTBA sample, certified (10 g) 8500-0656
PFTBA sample kit, 1 mL 05971-60571
Activated alumina, absorbent pellets for Edwards 8500-1233
rough pump traps, non-LC/MS (1 lb can)
PFTBA glass vial 05980-20018
Cotton swabs (100/pk) 5080-5400
Tools
Screwdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws 8710-0899
Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws 8710-0900
Wrench, open-end, 1/4 x 5/16 in. 8710-0510
Screwdriver, TORX, T15 8710-1622
Screwdriver, TORX, T10 5182-3466
Ferrules and O-rings
Teflon 1/4 in. ferrule (back) 0100-0160
Teflon 1/4 in. ferrule (front) 0100-0787
Retainer rings (10/pk) 5181-1258
5973 One Year Maintenance Kit (for diffusion pump systems) 5183-2096
Includes: Big Universal Trap for He, Abrasive sheets (5/pk),
Cloths, lint-free (15/pk), Cotton swabs (100/pk), SantoVac Ultra,
18.5 mL (2 ea.), Rough pump oil, 1 liter, Filament assembly,
Octafluoronapthalene (OFN)
MSD Tool Kit 05971-60561
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)

89 www.agilent.com/chem
GC/MS SYSTEMS

5973 MSD Ion Source Parts (EI)

Description 5973 Part No. A

(A) Ion source body G1099-20130


(B) Repeller G1099-20132
(C) Interface socket G1099-20136 C
(D) Drawout plate 05971-20134
(E) Drawout cylinder G1072-20008 H
M L
(F) Ion focus lens 05971-20143
(G) Entrance lens 05971-20126
(H) Repeller insulator G1099-20133
F G
(I) Set screw 0515-1446
E
(J) Washer, M3 (1/pk) 3050-0891
D
(K) Nut, 5.5 mm 0535-0071
(L) Ion Source Sensor G1099-60104 M
(M) Lens insulator, (2/pk) 05971-20130
Ion source assembly G1099-60106
Source heater assembly G1099-60177 5973 Ion Source Parts (EI).
Repeller assembly G1099-60170
Screw (for filament on the source) 0515-1046

MS Inert Ion Source Parts

Description 5973A 5973N 5973 inert** B


I
Drawout plate – 3 mm Inert G2589-20100
H
Drawout plate – 6 mm Inert** G2589-20045 G2589-20045 G2589-20045 I
EI High Temp Filament G2590-60053
Repeller assembly, Inert source G1099-60170 G1099-60170 G2589-60102 H L
J
Screws for filament High Temp 0515-1046 0515-1046 G1999-20021 K
Source body, Inert G1099-20130 G1099-20130 G2589-20043
Source Washer, Inert G2589-20101 5973 Repeller Assembly (EI).

**used in G2860A and G2860B extended linearity kits

www.agilent.com/chem 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 5972/5971/GCD Part No.

(A) Entrance lens 05971-20126


(B) Lens insulator, (2/pk) 05971-20130
(C) Ion focus lens 05971-20143
(D) Drawout cylinder G1072-20008
(E) Drawout plate 05971-20134
(F) Ion source body 05971-20128
(G) Set screw 0515-1446
(H) Repeller assembly 05971-60170
(I) Screw (for filament on the source) 0515-1046

Ion source assembly 5972 Part No.

05972-60226

Transfer line tip, gold-plated 5972/5971 Part No. GCD Part No.

05971-20305 G1800-20305

MSD Flowrates (ml/min)

Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates
below for flow limitations.
Min Max Diff Pump Max Turbo Pump Tuning Max
5973 0.1 2.0 4.0 2.0
5972 0.1 2.0 NA 2.0
5971 0.1 1.5 NA 1.0
GCD 0.1 1.0 NA 1.0

91 www.agilent.com/chem
GC/MS SYSTEMS

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

Maintaining the Filaments Tips to increase filament life


Like the filament in an incandescent light • When setting up data acquisition • Higher emission current will reduce
bulb, the ion source filaments will parameters, set the solvent delay so that filament life.
eventually burn out. Certain practices will the analyzer will not turn on while the • If you are controlling your MSD from the
reduce the chance of early failure: solvent peak is eluting. Edit Parameters screen, always select
• When the software prompts Override MS Off before changing any of the
solvent delay at the beginning of a run, filament parameters.
always select “No.”

It is very useful to switch from


one filament to the other every
Filament Assembly
three months so that when one
TIPS AND TOOLS

filament fails, you know the


other will fail soon. This will Description Unit Part No.
allow you to change both
filaments at the same time, Filament, 5973 (EI) 05972-60053
which helps to maximize your Filament, 5973 (CI) 2/pk G1099-80053
instrument uptime.
Filament, EI High Temperature for the 5973 inert G2590-60053
Filament, 5972 (EI/CI) 05972-60053
Filament, 5971 (EI/CI) / GCD (EI) 05971-60140

Quadrupole Mass Filter


The mass filter does not require periodic • Never put the quadrupole in an • Cleaning techniques appropriate for other
maintenance. It should not be removed ultrasonic cleaner. manufacturers’ instruments are not
from the radiator or distributed in any way. • Never change the physical orientation of suitable for Agilent MSDs – and may
the quadrupole mass filter. actually harm the mass filter.
• The fused-quartz quadrupole is fragile
and will break if dropped or handled • To save time and effort, use only Agilent
roughly. MSD mass filters, which do not require
• The material in the cusps of the periodic cleaning or maintenance.
quadrupole is very hygroscopic. If
exposed to water, the quadrupole must • In case of extreme contamination,
be dried very slowly to prevent damage. contact a trained Agilent service
representative to perform the mass
filter cleaning.

www.agilent.com/chem 92
GC/MS SYSTEMS

Vacuum Systems and Pumps


Vacuum System Operation
The vacuum system creates the high The major components of the vacuum A properly maintained vacuum system will:
vacuum (low pressure) required for the system are: • Prevent premature filament failure
MSD to operate. Without this vacuum, • Vacuum manifold • Provide better sensitivity
the molecular mean free path is too short. • Foreline gauge • Require less frequent source cleaning
• Calibration valve • Extend quadrupole lifetime
Ions cannot travel from the ion source • Gauge controller (optional) • Prevent premature EM Horn failure
through the mass filter to the electron • Vacuum seals
multiplier (detector) without colliding with • Foreline pump and/or trap
other molecules. • 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 How to Refill


The calibration valve is an electromechanical The calibration vial can be refilled without This sometimes causes an “Excess source
valve with a vial that contains a tuning venting the system. Fill the vial to 0.5 cm pressure” error message during the first
compound. Perfluorotribuylamine (PFTBA) from the top. DO NOT overfill. Air is tune after refilling. This is more likely if the
is the most commonly used tuning trapped in the vial when it is refilled. vial is overfilled. Be sure to purge the air
compound. It is required for automatic upon refilling the vial.
tuning of the MSD in EI mode. The tuning
compound is usually a liquid but can be
volatile or semi-volatile solid.

Description Part No.

PFTBA sample, certified (10 g) (EI) 8500-0656


PFDTD sample (10 g) (CI) 8500-8130

MAINTENANCE MINDER

If using the 5973 with a CI source, use Perfluorodimethyltrioxadodecane


(PFDTD) sample.

93 www.agilent.com/chem
GC/MS SYSTEMS

Pressure Symptoms
This section describes unusual pressure These pressures can vary widely from The vacuum manifold pressures can only be
readings and their possible causes. The instrument to instrument so it is important measured if your system is equipped with
symptoms in this section are based on that you are familiar with the pressures the optional gauge controller.
typical pressures. At typical column flow that are typical for your instrument at a
rates (0.5 – 2.0 ml/minute), the foreline given carrier gas flow and oven
pressure will be approximately 20 to 100 temperature.
mTorr. The vacuum manifold pressure will
be approximately 1 x 10-6 to 1.4 x 10-4 Torr. 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. Symptom • Pressure is above 1.4 x 10-4 Torr.
• Pressure for a given column flow has • Pressure for a given column flow has
increased over time. increased over time.

Possible Cause • Column (carrier gas) flow is too high Possible Cause • Column (carrier gas) flow is too high
• Wrong carrier gas • Wrong carrier gas
• Air leak (normally at transferline interface) • Air leak
• Foreline pump oil level is low or oil is • Foreline pump is not working correctly
contaminated • Diffusion pump fluid level is low or fluid is
• Foreline hose is constricted contaminated
• Foreline gauge is not working correctly • Foreline pump is not working correctly
• 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 Possible Cause • Column (carrier gas) flow is too low
• Wrong carrier gas • Wrong carrier gas
• Column plugged or crushed by an • Column plugged or crushed by an
overtightened nut overtightened nut
• Empty or insufficient carrier gas supply* • Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing* • Bent or pinched carrier gas tubing*
• Foreline gauge is not working correctly • Defective gauge controller
• Faulty ion gauge tube
* These could create a fault condition in the
GC that would prevent the GC from operating. * These could create a fault condition in the
GC that would prevent the GC from operating.

www.agilent.com/chem 94
GC/MS SYSTEMS

Diffusion Pump
It is not necessary to change the diffusion How to Check the Fluid Level 6a. Use a metal ruler to determine the
pump fluid more than once a year, unless 1. If it is not vented already, shut down and depth of the fluid. A pump that has
you observe symptoms that suggest a vent the MSD according to instrument been in operation should have a pool
problem with the diffusion pump fluid. The manual. 9 mm plus or minus 1 mm deep. Fluid
MSD must be vented in order to check the in freshly charged pumps will be 12
2. Unplug the MSD power cord.
diffusion pump fluid (except for the 5973). mm deep. It is normal that up to 2 ml
Therefore, the best time to check the fluid 3. Remove the pump and cover the top of oil may be in the rear portion of the
is when the instrument is already vented with aluminum foil. vacuum manifold. The recommended
for other maintenance. 4. After heating the pump in a GC oven total fluid charge for the 5971/5972 is
at 60°C for 15 minutes to make the 18 ml (plus or minus 2 ml).
Importance of the Fluid Level fluid flow down into the reservoir at 6b. For the 5973 use the sight glass
The amount of fluid in the pump affects the bottom, remove the stack parts. to determine the depth of the fluid.
the amount of vapor and the temperature The recommended total fluid charge
of the base plate. Too little fluid will cause 5. Inspect the pump fluid, if the fluid
is discolored or contains particulate is approximately 37 ml.
the pump to run at a higher temperature
because there is less fluid to carry away the material, the fluid must be changed.
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.

Description Part No.

Diffusion pump fluid: SantoVac Ultra 5P,


18.5 ml (5973, 5972 or 5971/GCD) 6040-0809
Ion gauge controller (5973/5972A) 59864B
Ion gauge tube for measuring vacuum (5971/5972) 0960-0376
Triode gauge tube for measuring vacuum (5972/5973) 0960-0897

Foreline Pump
The oil in the foreline or rough pump Avoid contact with the pump oil. The
should be replaced on average once every residue from some samples may be toxic.
six months, but can vary depending upon Dispose of used oil properly.
applications. After oil replacement, if the
foreline trap is present, the molecular
sieves should be replaced.

Description Part No.

Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD) 6040-0798


Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD) 6040-0834
Molecular sieve (5973, 5972 or 5971/GCD) 9301-1104
Oil mist filter RV3/E1M18/E2M18/E2M2 3162-1056
Oil mist filter E2M1.5 G1099-80037
Oil mist filter E2M18 5063-5224

95 www.agilent.com/chem
GC/MS SYSTEMS

General Instructions on How to Replace the 8. Reconnect the MSD power cord.
Pump Oil 9. Start up and pump down the MSD
1. Shutdown and vent the MSD. according to the Instrument Manual
2. Place a container under the drain plug on the procedure.
foreline pump.
3. Remove the fill cap from the top of the pump to
expose the fill hole.
4. Remove the drain plug from the pump.
5. Reconnect the MSD to its power source. Switch TIPS AND TOOLS
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.

Symptom
Description Part No. • Voltage is over 2500 volts
• Poor vacuum
Electron multiplier replacement horn 05971-80103
(5973, 5972, 5971/GCD) Corrective Action
High energy dynode (5973 only) G1099-80001 • Replace electron multiplier
Electron multiplier kit (5972, 5971/GCD only) 05971-80102

TIPS AND TOOLS

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

www.agilent.com/chem 96
GC/MS SYSTEMS

Maintaining the MS Engine


Maintenance Schedule
• Always wear clean, lint-free, nylon gloves • If you must set parts down, place them on • Do not leave the interior of the vacuum
when handling parts which will come in clean, lint-free cloths or clean aluminum system open to the atmosphere. For
contact with the sample stream. Oil from foil, not directly onto a laboratory bench. example, if you are removing the ion source
your fingers is a particularly difficult for cleaning, put the vacuum manifold cover
contaminant to remove. • Keep parts covered so that dust does not back in its normal position after you have
accumulate on them. removed the source. Re-establish a low
vacuum in the vacuum manifold until you
need to reinstall the ion source.

Common maintenance tasks are listed on


page 83. Performing these tasks on a regular
basis can reduce overall operating costs.
Keep a record (logbook) of system
performance characteristics and
maintenance operations performed.
This makes it easier to detect variances
from normal operation and to take
corrective action.

Cleaning the Ion Source


There is not a regular interval for ion source
cleaning. The ion source should be cleaned
when symptoms indicate. Symptoms of a
dirty ion source include poor sensitivity and
inadequate abundances at high masses.
See the Troubleshooting chapter in your
hardware manual for more information about
these symptoms.

MS Engine Pump Lubricants and Oils

5989 or Thermo or 5985 or 5999x, 5993x


Lubricant Oil 5988 Electro Spray 5987 or 5995x Part No.

Turbo pump lubricant:


Balzers turbo pump lubricant, 0.25 liter • • 6040-0468

Diffusion pump oil:


SantoVac 5, 1 liter • • • 6040-0370
SantoVac 5, 128 ml • • • 6040-0819

Rough pump oil:


Rough pump oil, 1 gal Inland 45 • • • • 6040-0798
Rough pump oil, 1 liter Inland 45 • • • • 6040-0834
Particle Beam pump oil, Fomblin • 6040-0730

97 www.agilent.com/chem
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 Every Every As


Week 3 Months 6 Months Needed

Autotune or manual tune (save results) •


Cabinet Maintenance
Clean the cabinet •
Inspect hoses and cords •
Vacuum the fan filter •
Vacuum System Maintenance
Check mech. pump oil •

TIPS AND TOOLS


Replace mech. pump oil We recommend
keeping a separate
Replace mech. pump traps • set of tools that have
Check diffusion pump fluid • been thoroughly
Degas ion gauge tube • cleaned for working
with the MS engine.
Replace ion gauge tube • These tools are
Replace seals & O-rings • needed to prevent
contamination when
Analyzer Maintenance reassembling or
installing clean
Clean ion source • assemblies such as
Replace filament • the ion source.
Replace ion source heater •
Replace mass filter heater •
Replace electron multiplier horn •
GC/MS Interface Maintenance
Refill EI calibration vial •
Refill CI calibration vial •
Replace interface heater •

www.agilent.com/chem 98
GC/MS SYSTEMS

Ion Source Parts and Supplies

Many of the tools and supplies needed to


service the 5989 MS Engine are included B
in the installation kit supplied with the
instrument. The following tables list
common consumable parts and supplies
used in the maintenance of the MS Engine.

C
A
D
5989 Lens Stack

Description Part No.

(A) Clamp insulator, ion source 05989-20110


(B) Entrance lens 05989-67002
(C) Lens insulator, ion source 05989-20111 E
(D) Plate insulator, ion source 05989-20109
(E) EI/CI repeller 05989-20145
(F) Repeller insulator 05989-20119 F
Filament block 05989-20165
Filament assembly 05985-60179
Heater cartridge 05989-60098
5989 Repeller Assembly

Replacement Parts and Supplies

The electron multiplier lifetime on the 5989


may be 6 to 9 months or shorter, especially Description Part No.
with the following applications:
5989
• Thermospray Electron multiplier kit 05989-80043
• Particle Beam Electron multiplier replacement horn 05971-80103
• Purge and trap, with no jet separator
• Extensive CI Parts and Supplies
• High sensitivity work with high EM voltage Ion gauge tube, K-25 flange 0960-0799

O-rings and Seals


Insulating ring 05989-20705
O-ring, detector flange (5/pk) 5181-3367
Diffusion pump fluid fitting
fill and drain cap O-ring (12/pk) 0905-1145
KF 25 centering ring and O-ring 3162-0110
O-ring, manifold window 0905-1189

99 www.agilent.com/chem
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 • Pre-tested column, 30m x 250um x 0.5um
• Application Note, “Improvements in the HP-5 MS, part no. 19091S – 139
Agilent 6890/5973 GC/MSD System for • Single-taper splitless liner, 4mm i.d.,
use with USEPA Method 8270”, pub. no. deactivated, part no. 5181-3316
5988-3072EN • Direct Connect Liner, single taper, 4mm
• Ultra Ion Source Chamber i.d., deactivated, part no. G1544-80730
• Ultra Repeller • Direct Connect Liner, dual taper, 4mm
• Ultra Large Aperture Drawout Plate i.d., deactivated, part no. G1544-80700
• Floppy Disk with tuning macros

Description Part No.

8270 Semi-Volatiles Applications Kit G2860A

LIBRARY

There are many ways to perform semi-volatile analysis. For another option that
also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem
and do a library search for 5989-1510EN.

www.agilent.com/chem0 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

EI CI Negative Positive
MSD Tune Tune EI Mode CI Mode CI Semi-Volatile Volatile

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

MS Engine

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

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 www.agilent.com/chem
GC/MS SYSTEMS

Description Quantity Part No.

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 05970-60045

GC/MS Tuning Standard contains:


DFTPP, Benzidine, Pentachlorophenol, and
p,p’-DDT 1 mg/mL in methylene chloride 8500-5995

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 8500-6406

Extended Mass Performance Sample 0.5 g, fomblin oil 8500-5500

PFTBA certified 1 bottle, 10 g 8500-0656

PFTBA Sample Kit 0.5 mL 05971-60571

PFDTD 10 g 8500-8130

Benzophenone 100 pg/µL,


5 ampoules 8500-5440

Hexachlorobenzene 10 pg/µL, 4 ampoules 8500-5808


1 ng/µL, 2 ampoules

Hexachlorobenzene 20 pg/µL 8500-6405

Methyl stearate (in methanol);

PFTBA not certified 1 ng/µL (2 ea) 05990-60075

Octafluoronapthalene (OFN) 1 pg/µL,


5 ampoules 8500-5441

Octafluoronapthalene (OFN) 500 fg/µL 8500-6572

p-Bromofluorobenzene (BFB) 25 µg/mL 8500-5851

www.agilent.com/chem 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 • A newly designed online store – with fast access to
screen resolution and optimizes the page size for pricing, order status, quotes, and local sales information.
less scrolling. • Direct links – to the services, parts, and consumables that
• An expanded navigation – that includes links to keep your instruments running in top condition.
product literature, technical support, education,
events, and news.

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

www.agilent.com/chem 104
SERVICES & SUPPORT

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

A Total Commitment The Unmatched Expertise The Flexibility to Select The


to Your Lab for One Fixed Cost. of Fully Trained Engineers. Solution That’s Right for You.
Agilent service agreements operate You can rest assured that the engineer Our team will work with you to help your
under a yearly fixed cost, which includes who arrives at your site will perform the laboratory achieve …
preventative maintenance, compliance, requested service with optimum skill.
• Maximum uptime
telephone support, repairs, parts, and That’s because Agilent engineers …
labor. No matter how many service visits • High productivity
• Are experts in instrument operation,
or replacement parts you need, this fixed
maintenance, compliance, and repair. • Total compliance
cost covers it all – at no additional charge.
• Continually update their training • Extended instrument life
If you choose, you can also consolidate
and qualifications.
instrument maintenance and repair • Fast problem resolution
services into multi-year agreements • Use only Agilent factory-approved
• Verified system performance
for administrative ease and greater replacement parts, columns, and
cost savings. supplies to ensure peak instrument • The skills and knowledge you need for
reliability. efficient operation and maintenance
• Carry calibrated, traceable tools and • Consistent, in-depth documentation
testing equipment, as well as Agilent
• Reduced administrative burdens
hardware and software qualification
protocols.
What’s more, most Agilent engineers are
part of the Agilent product development
team. So you can be certain that ease of
repair, maintenance, and compliance are
built into your GC and GC/MS systems
right from the start.

105 www.agilent.com/chem
SERVICES & SUPPORT

Agilent Services Features Advantages to You

Telephone Service • Telephone access to skilled Agilent service • Fast identification and resolution
professionals. of hardware problems.

• Available parts option. • Low cost.

Software Service • Telephone access to trained technical • Fast identification and resolution
professionals. of software problems.

• Enhancements to the original application • A fixed annual cost for software


software purchase. upgrades makes budget management
more predictable.
• 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 • A fixed annual cost for parts makes
to skilled, factory-trained Agilent service budget management more predictable.
professionals.
• You can choose the response
• Travel expenses and labor. method that fits your business
needs and budget.
• Optional coverage for consumables
used during repair.

Offsite Instrument Repair • Option 1: Replacement with an identical • Less expensive than onsite repair.
For selected Agilent analysis instruments instrument (your fastest choice).
• 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 • Expert cleaning, adjustment, lubrication, • Maximum uptime.


For selected Agilent analysis instruments and inspection of your instrument.
• Extended instrument life.
• Travel expenses and labor.
• Confidence in the integrity
• Coverage for consumables used. of your measurements.

www.agilent.com/chem 106
SERVICES & SUPPORT

Agilent Services Features Advantages to You

Installation Qualification (IQ) • Qualification and documentation of • Supplies the evidence you need to
shipment completeness. satisfy regulatory agencies.

• Comprehensive system and application • Helps fulfill the master validation plan –
software verification tests. and change-control SOP requirements –
for the IQ phase.
• Delivered by professionals with training
certification.

Operational Qualification/Performance • Verification and documentation of an • Supplies the evidence you need to
Verification (OQ/PV) instrument’s ability to meet specified satisfy regulatory agencies.
For selected Agilent analysis instruments criteria.
• No need to write your own SOPs to
Note: We recommend Preventative • Procedures and documentation that fit the qualify Agilent instruments – or to train
Maintenance before OQ/PV. requirements of GLP, ISO 9000, and other your staff.
regulatory agencies.
• Consistent, traceable results among all
• Full automation to increase the your laboratories – and improved
qualification scope without excess time method transfer.
requirements.
• Confidence in the integrity of your
• Measuring equipment that is traceable to measurements, with traceable,
national and international standards. 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 • Verification that a system is performing • Minimal system downtime after
For instruments that have their at operation specifications after repair. completion of instrument repair.
operational performance verified
by an annual OQ/PV. • Complete system operation testing. • Efficient system requalification by
performing the appropriate tests based
Note: only a subset of the Operational on the components repaired.
Qualification test is performed, based on
the type and extent of the repair. • Assurance that all instrument
subsystems are performing within
• A comprehensive test of the repaired specifications.
module using established conditions and
known sample characteristics to ensure • All procedures and documentation meet
the basic accuracy and precision of your regulatory agency requirements.
module.

• Measuring equipment is traceable to


national and international standards.

107 www.agilent.com/chem
SERVICES & SUPPORT

Agilent Services Features Advantages to You

Network Qualification • Network definition and performance • Significant time savings.


testing using established Agilent Design,
Installation Qualification, and Operational • Increased uptime – issues that might
Qualification protocols. impact application performance are
quickly identified and resolved.
• Documentation of the definition, integrity,
supportability, and health of high-risk • Improved consistency – network
network segments. qualification protocols are developed
according to a quality lifecycle, and are
• Completed protocols, created using maintained under version and revision
hardware and software network testing control.
tools. Protocols include:
- A physical and logical inventory. • Increased control – Agilent will verify
- A graphical network topology map. known elements and identify unknown
- A snapshot of network health, as network contingency states that may
installed. impact application performance.

• Network Operational Qualification testing, • Reduced regulatory exposure –


which monitors the network over time, and audit-ready documentation establishes
evaluates its operation over a controlled evidence of network system control.
range of traffic conditions. We’ll also
provide the following reports:
- Long Duration Network Characterization,
which analyzes each function in its
operating environment.

- Performance Predictability Analysis,


which documents reserve capacity and
stability over a range of operating
demands.

Mass Spectrometer Ion Source Cleaning • Your staff can devote more time to
For selected Agilent analysis instruments • Onsite disassembling chemistry, not instrument maintenance.

• Cleaning • Efficient cleaning with minimal


downtime.
• Reassembling

• Testing

www.agilent.com/chem 108
SERVICES & SUPPORT

Agilent Services Features Advantages to You

Software Backup • Telephone or onsite factory support to • Fast and easy – you simply insert a disk
facilitate restoration. … reboot … and you’ll be back in
operation in as little as two hours.
• Captures the unique system settings for all Normally, you would have to reload and
software components needed to reconfigure your software – a process
reconstruct your system including: that can take days.
- Network information
- Printers and peripherals • A complete solution – the initial
- Configurations configuration backup includes:
- User settings and operations - Simple backup software
- System registry - Ten CD-ROMs
- Application software - Ten 3.5-in. floppy disks
- Settings - A storage case
- Operating system - One full system backup
- Customizations - Installation of the backup software
- Analytical hardware and optional CD writer
- Directory structure
- Security information

TIPS AND TOOLS

To learn more about Agilent’s complete portfolio of services, please


visit www.agilent.com/chem/service.

109 www.agilent.com/chem
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; Reviews the basic theory and operation
Four hours access 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; Reviews the basic theory and operation of
Four hours access 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; Reviews the basic theory and operation
Four hours access of the 6890 GC purged packed inlet.

Clarifies flow paths, so you can gain


the maximum benefit from this inlet.

Discusses typical problems and routine


maintenance procedures.

www.agilent.com/chem 110
SERVICES & SUPPORT

Course Title Duration Description

6890 GC Keyboard Operation Self-paced; Reviews the basic operation of the 6890
Four hours access GC keyboard.

Thoroughly describes all keys, so you can


gain the maximum benefit from your GC.

6890 GC FID Theory and Operation Self-paced; Reviews the basic theory and operation
Four hours access 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; Reviews the basic theory and operation
Four hours access 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; Reviews the basic theory and operation
Four hours access 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; Reviews the basic operation of the 7683A
60-90 minutes automatic liquid sampler system (ALS).

Shows you how to gain maximum


productivity from the ALS.

Discusses routine maintenance


procedures, and how to return an ALS
to Agilent for repair or exchange.

111 www.agilent.com/chem
SERVICES & SUPPORT

Course Title Duration Description

Logical GC Troubleshooting Instructor-led; Teaches a methodical process for


60-90 minutes troubleshooting GC system problems.

Helps you identify the source of problems


quickly, making troubleshooting less
daunting.

Note: This course does not discuss hardware-


specific problems or solutions.

Using the GC/MSD Instructor-led; Describes in detail how to operate the


Security ChemStation to Achieve 60-90 minutes GC/MSD Security ChemStation software
FDA CFR Part 11 Compliance in accordance with FDA CFR Part 11
requirements.

Managing and Administering the Instructor-led; Shows you how to manage the GC/MSD
GC/MSD Security ChemStation 60-90 minutes Security ChemStation software in
to Meet FDA CFR Part 11 accordance with FDA CFR Part 11
Compliance Requirements requirements.

Designed for systems administrators

www.agilent.com/chem 112
SERVICES & SUPPORT

Classroom Training
Agilent’s training courses for gas also target those who want to broaden
chromatography and mass spectrometry or sharpen their troubleshooting,
help new and experienced lab maintenance, and system operation skills.
professionals learn proper and efficient
Contact Agilent today for more information
ways to use analytical instruments and
about our training and services. Or visit
software. These ISO-registered courses
www.agilent.com/chem and select
“Education.”

Course Title 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.

113 www.agilent.com/chem
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.

www.agilent.com/chem 114
SERVICES & SUPPORT

Support
Tap Agilent’s GC and GC/MS • Software Downloads and Utilities Feature
expertise anytime. patches and status bulletins, tools and
utilities, firmware, and revision tables.
Just give us a call to discuss hardware,
• How-to Videos Show you how to perform
software, application concerns, or basic
common installation and maintenance
operation techniques.
procedures for Agilent products.
Visit Agilent online • Chromatogram Library A searchable
For a wealth of knowledge, tips, and collection of GC, LC, and CE
insights, go to www.agilent.com/chem. chromatograms for nearly a thousand
You’ll find: chemical compounds.
• Frequently Asked Questions about Agilent • Instrument and Software Demos Such as
instruments and supplies. product videos, 3D animations and
• Interactive Troubleshooter A step-by-step interactive software demos.
approach to help you solve common problems.
• Find a Part Includes parts information,
pricing, and availability, plus an illustrated
parts breakdown.

aTechnical Support Consultation

Have a technical GC column, method, or troubleshooting question? Agilent’s technical GC and GC/MS
experts are available to answer your questions by phone, fax or e-mail for free. With years of experience in
running samples, developing methods and troubleshooting GC systems, our chemists are promptly able to
help you consistently achieve excellent performance and high productivity in your lab.
For GC Technical Support go to www.agilent.com/chem/techsupport
and click on “Interactive Troubleshooter.”

115 www.agilent.com/chem
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
Receive a year’s worth of current chromatography insights with a
FREE subscription to Separation Times.

For more than 18 years, Separation Times has


been one of the scientific community’s most
respected newsletters devoted to chemical
analysis. And now, it’s available online!

Each issue is packed with …


• Application details geared toward specific
industries – such as environmental,
chemical, petroleum, forensic, and
agricultural.
• Handy tools, tips, and tricks designed to
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• Exclusive promotional offers and regional
event announcements.

Best of all,
Separation Times is absolutely FREE …
and we’ll automatically e-mail it to you
seven times per year.
To reserve your subscription today, go to
www.agilent.com/chem/separationtimes
GC System Recommended Maintenance Schedule

Gas Management
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

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

Sample Introduction Consumables and GC Inlets


ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

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

Remember, the downtime for scheduled


maintenance is always less disruptive
than the downtime for unscheduled
maintenance and troubleshooting!
Columns
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

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

Detectors
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS

FID/NPD Jets As needed Clean when deposits are present. Replace when they become scratched,
& Collector bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead As needed Replace when signal drifts or there is a dramatic change in sensitivity.
FID Every 6 months Measure hydrogen, air, and makeup gas flows.
TCD As needed Thermally clean by “baking-out” when a wandering baseline, increased
noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.
ECD Every 6 months Wipe test.
As needed Thermally clean by “baking-out” when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD Every 6 months Measure hydrogen, air, and makeup gas flows.
As needed Clean/replace FPD windows, and seals when detector sensitivity
is reduced.
MSD
Components require regular maintenance. For complete MSD maintenance schedule, please see page 83.

*Schedule is an approximation of average usage requirements.


Frequency may vary widely based upon application and sample type.

www.agilent.com/chem
www.agilent.com/chem

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
5989-1925EN

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