Agilent GC, GC-MS User manual
Maintaining your Agilent
GC and GC/MS Systems
Our measure is your success.
Table of Contents
Gas Management........................................................................................1
Gas Types ....................................................................................................................................................................................2
Gas Purification Systems.............................................................................................................................................................4
Gas Traps.....................................................................................................................................................................................6
Renewable Gas Purification System .........................................................................................................................................12
Universal/External Split Vent Trap.............................................................................................................................................13
egulators .................................................................................................................................................................................14
R
ubing........................................................................................................................................................................................15
T
Flowmeters ...............................................................................................................................................................................16
Gas Leak Detector.....................................................................................................................................................................18
Sample Introduction ..................................................................................19
Vials...........................................................................................................................................................................................20
Electronic Crimpers and Decappers..........................................................................................................................................25
Gold Standard Autosampler Syringes.......................................................................................................................................26
Headspace Sampler..................................................................................................................................................................34
CTC Autosampler Supplies........................................................................................................................................................37
Purge and Trap Supplies ...........................................................................................................................................................41
Markes Thermal Desorption .....................................................................................................................................................43
Inlets ..........................................................................................................45
Premium Non-Stick Septa.........................................................................................................................................................46
Ferrules .....................................................................................................................................................................................50
Capillary Flow Technology Supplies..........................................................................................................................................54
Split/Splitless Liners ..................................................................................................................................................................55
Direct Connect Liners................................................................................................................................................................59
Helix Liners................................................................................................................................................................................59
Split/Splitless Inlets...................................................................................................................................................................60
Cool On-Column Inlets ..............................................................................................................................................................69
Purged Packed Inlets ................................................................................................................................................................75
Programmed Temperature Vaporizer (PTV) Inlets.....................................................................................................................78
Detectors ...................................................................................................83
Flame Ionization Detector (FID)................................................................................................................................................84
Electron Capture Detector (ECD)..............................................................................................................................................91
Thermal Conductivity Detector (TCD) .......................................................................................................................................
Flame Photometric Detector (FPD)...........................................................................................................................................99
Nitrogen Phosphorus Detector (NPD) ....................................................................................................................................106
Nitrogen and Sulfur Chemiluminescence Detectors...............................................................................................................
94
113
GC/MS Systems ......................................................................................115
Maintaining Mass Selective Detectors (MSD).......................................................................................................................116
MSD Contamination ...............................................................................................................................................................118
Cleaning and Maintenance Supplies
Ion Source
Installing a Capillary Column in the GC/MSD Interface.........................................................................................................134
QuickSwap MS Interface Restrictors......................................................................................................................................135
MSD Filaments ......................................................................................................................................................................136
Vacuum Systems and Pumps .................................................................................................................................................138
MSD Electron Multipliers and Replacement Horn
MS Test and Performance Samples........................................................................................................................................143
...............................................................................................................................................................................
......................................................................................................................................
................................................................................................................
126
128
142
Gas Management
Avoid column damage, improve detector life,
and achieve reliable, consistent results.
Gas management means more than just selecting the appropriate carrier gas for
your needs. It also means taking steps to prevent contaminants like oxygen, moisture,
and hydrocarbons from damaging your GC column.
As you read through the following pages, you will find…
• Practical advice about carrier gas types, impurities, leak detection, and flow rates.
• Valuable techniques that can minimize the likelihood of GC system contamination.
• Tips and tools that will help your lab implement gas management protocols.
The latest details about Agilent-engineered gas purifiers, tubing, regulators,
•
leak detectors, and flowmeters.
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1
Gas Types
Carrier Gases
The most frequently used carrier gases are helium and hydrogen, although nitrogen
and argon can be used. Purity is essential for these gases since they sweep the sample
through the column where it is separated into its component parts and then through
the detector for component quantification. Carrier gas purity is also critical to prevent
degradation of chromatographic columns and hardware.
The following tables list minimum and maximum pressures in psi for inlets and detectors
measured at the bulkhead fitting at the back of the gas chromatograph.
Inlet Pressure Settings (psi)
Carrier max
(psi)
Carrier min
(psi)
Split/Splitless
(0-150 psi)
170 120 120 120 120
Must supply 20 psi greater than pressure used in method
Split/Splitless
(0-100 psi)
Cool On-Column Packed PTV
Detector Pressure Settings (psi)
FID NPD TCD ECD FPD
Hydrogen 35-100 35-100 45-100
Air 55-100 55-100 100-120
Make up 55-100 55-100 55-100 55-100 55-100
Reference 55-100
Conversions: 1 psi = 6.8947, kPa = 0.068947, Bar = 0.068 A
TM
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Gas Purity and Selection
Agilent recommends that carrier
and detector gases be 99.9995% pure.
Air needs to be zero grade or better.
Agilent also recommends using traps to
remove hydrocarbons, water and oxygen.
When used with capillary columns, GC
detectors require a separate makeup gas
for optimum sensitivity. For each detector
and carrier gas, there is a preferred choice
for makeup gas. This table lists gas
recommendations for capillary columns.
Gas Management
Detector Carrier Gas Make up
1st choice
Electron capture Hydrogen Argon/methane Nitrogen Anode purge must
Helium Argon/methane Nitrogen
Nitrogen Nitrogen Argon/methane
Argon/methane Argon/methane Nitrogen
Flame ionization Hydrogen Nitrogen Helium Hydrogen and air
Helium Nitrogen Helium
Nitrogen Nitrogen Helium
Flame
photometric
Mass selective Hydrogen None None
Nitrogen
phosphorous
Thermal
conductivity
Hydrogen Nitrogen None Hydrogen and air
Helium Nitrogen
Nitrogen Nitrogen
Argon Nitrogen
Helium None None
Helium Nitrogen Helium Hydrogen and air
Nitrogen Nitrogen Helium
Hydrogen Must be same as
Helium
Nitrogen
carrier and
reference
Make up
2nd choice
Must be same as
carrier and
reference
Purge or
Reference
be same as
makeup
for detector
for detector
for detector
Reference must
be same as carrier
and makeup
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Contaminants & Purities
Contaminants in gases are major contributors to capillary column degradation
and detector noise, and can interfere with chromatographic results. Concentration
of these contaminants vary by the grade of gas.
Hydrocarbons and Halocarbons
• Decrease detector sensitivity by increasing detector background noise.
• Can also cause baseline drift or wander, contaminant peaks, and noisy
or high offsets of baselines.
Moisture
• Can be introduced by improper handling and/or installation of plumbing.
• A common cause of column stationary phase degradation.
• Can damage instrument.
Oxygen
• Most common contaminant.
• A common cause of column stationary phase and inlet liner degradation.
• Can cause decomposition of labile analytes.
• Opportunity for introduction at every fitting present in the gas line or during
use of gas permeable tubing.
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Tips & Tools
Gas purifiers should always be
oriented vertically
, not horizontally
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Gas Purification Systems
Purifiers are available in a variety of sizes and configurations to remove common
contaminants like oxygen, moisture, and hydrocarbons. In-line gas purifiers, including
refillable, indicating, S-shaped, and metal body types, are made to remove specific
.
contaminants. Agilent also offers gas purification systems with removable cartridges.
These systems provide the ability to design the right combination of filters needed
for your application to achieve the proper gas purity.
Carrier Gas Purification
Gas Management
The Carrier Gas Purification illustration
shows the most common gas purification
configurations used in gas chromatography.
Regardless of which purification
system is employed, proper installation
and maintenance is required to
achieve optimal performance from
the purification system(s). A purifier
that is not maintained will eventually
expire and become ineffective, or worse,
a source of contamination.
• Determine desired purity level.
• Keep number of fittings in gas line
to a minimum.
• Install purifiers in a convenient location
close to the GC.
• Purifier log books are useful for
determining maintenance schedule.
• Use indicating traps closest to the GC
so you can determine when to change
the traps that are upstream.
In-Line Gas Purifiers
-OR-
Gas supply
-OR-
Gas supply
Gas supply = cylinder, in-house line, or gas generator
Regulator = brass dual stage regulator
Gas Purification System
Combination Trap
Vent
FID make-up, air, and H
ECD make-up
ELCD reaction gas
MS carrier gas
KeyDetector Gas Purification
1 = Moisture Trap
2
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2 = Hydrocarbon Trap
3 = Oxygen Trap
4 = Indicating Oxygen T
5 = Gas Purification System
6 = Combination Trap for
moisture, oxygen, and
hydrocarbon removal
rap
5
Gas Traps
The purpose of gas traps is to remove detrimental impurities from the carrier and detector
gases. Combination traps are available which remove moisture, oxygen and/or organics
with a single trap. The effectiveness of the traps depends on the initial quality of the gas.
Constant exposure of capillary columns to oxygen and moisture, especially at high
temperatures, results in rapid and severe column damage. The use of oxygen and
moisture traps for the carrier gas may extend column life and protect the instrument.
Any moisture or oxygen introduced into the gas stream due to a leak will be removed
by the trap until it expires.
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Moisture (Water) Traps
Indicating moisture traps are available in
plastic and glass bodies. Glass body traps
are used when potential contaminants
from plastic trap bodies are a concern.
Glass traps are normally encased in a
protective, plastic shrink wrap or a high
impact plastic shield (outer trap body).
Glass and plastic bodied traps are usually
pressure tested at 150 psi, thus they are
safe for use at the typical pressures
required by the GC.
Gas Management
oisture trap
M
Moisture Traps
Description Size
(cc)
Molecular Sieve 13X and Indicating 4A (MT Series)
Refillable
Moisture Trap
Refillable
Moisture Trap
Refillable
Moisture Trap
Adsorbent refill (1 pint) for MT series MSR-1 MSR-1
120 21.6 20 MT120-2 MT120-4
200 36.0 18 MT200-2 MT200-4
400 72.0 14 MT400-2 MT400-4
Removal
Capacity (g)
Max.
Effluent H
Concentration
(ppb)
O
2
1/8 in.
Part No.
1/4 in.
Part No.
Tips & Tools
Moisture traps are highly
recommended for carrier
and ECD gases.
Molecular Sieve 5A and Indicating Drierite (MT-D Series)
Refillable
Moisture Trap
Refillable
Moisture Trap
Refillable
Moisture Trap
Adsorbent Refill (1 pint) for MT-D Series MSR-2 MSR-2
120 21.6 22 MT120-2-D MT120-4-D
200 36.0 20 MT200-2-D MT200-4-D
400 72.0 16 MT400-2-D MT400-4-D
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Moisture Traps
Refillable glass moisture trap
Moisture S-trap
Description Size
(cc)
Removal
Capacity (g)
Max.
Effluent H
oncentration
C
1/8 in.
Part No.
O
2
1/4 in.
Part No.
(ppb)
ilica Gel, Grade 40, and Indicating Silica Gel, Grade 48 (MT-S Series)
S
Refillable
120 31.5 40 MT120-2-S MT120-4-S
Moisture Trap
Refillable
200 52.5 39 MT200-2-S MT200-4-S
Moisture Trap
Refillable
400 105.0 39 MT400-2-S MT400-4-S
Moisture Trap
Adsorbent Refill (1 pint) for MT-S series SGR SGR
Glass Indicating Moisture Traps (GMT and LGMT Series)
Glass Indicating
70 11.4 7 GMT-2GC-HP GMT-4GC-HP
Moisture Trap
Glass Indicating
100 16.3 6 GMT-2-HP GMT-4-HP
Moisture Trap
Glass Indicating
250 40.09 6 LGMT-2-HP LGMT-4-HP
Moisture Trap
Molecular Sieve Refill for GMT and LGMT series GMSR GMSR
Big moisture trap
Moisture Removal S-Traps
Moisture S-trap, preconditioned* 5060-9084
Moisture S-trap, unconditioned 5060-9077
Big Moisture T
Big Moisture
rap
T
raps (BMT Series)
750 BMT-2 BMT-4
Refill for Big Moisture Trap (enough for 2 refills) BMSR-1 BMSR-1
*Traps can be reconditioned by heating at a minimum of 350°C, with flow for 6 hours
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Hydrocarbon Traps
Hydrocarbon traps remove organics,
such as hydrocarbons and halocarbons,
from the gas stream. The adsorbent is
usually activated carbon or an impregnated
carbon filter media. Carbon removes
organic solvents from the gas stream,
including the typical solvents used
in nearly every lab. Hydrocarbon-moisture
combination traps are also available which
remove water in addition to organics.
Capillary grade hydrocarbon traps are
purged with ultra-high helium and packed
with a very efficient activated carbon
material. Metal trap bodies are used to
prevent any contaminants in plastic trap
bodies from contaminating the carbon
adsorbent. Most hydrocarbon traps
can be refilled by the end user.
Gas Management
ydrocarbon trap, HT200-2
H
Hydrocarbon Traps
Description Size
Hydrocarbon Traps (HT Series)
Hydrocarbon Trap 200 HT200-2 HT200-4
Adsorbent Refill (1 pint) ACR ACR
Big Hydrocarbon Traps (BHT Series)
Big Hydrocarbon Trap 750 BHT-2 BHT-4
Refill for Big Hydrocarbon Trap (enough for two refills) BACR BACR
(cc)
1/8 in.
Part No.
1/4 in.
Part No.
Hydrocarbon Removal S-Traps
Hydrocarbon S-Trap, used for trapping organics from gases 5060-9096
Capillary Grade Hydrocarbon Traps (HT3 Series)
Capillary Grade Hydrocarbon Trap 100 HT3-2 HT3-4
Adsorbent Refill (1 pint) ACR ACR
Tips & Tools
Hydrocarbon traps should be used with carrier, FID and ELCD gases.
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Indicating oxygen trap, IOT-2-HP
Oxygen Traps
Oxygen traps usually include a metal-containing inert support reagent. Most oxygen traps
reduce the oxygen concentration to below 15-20 ppb. The capacity of a standard oxygen
trap is approximately 30 mg of oxygen per 100 cc of trap volume. Oxygen traps can also
remove some small organic and sulfur compounds from gas streams, but this is not their
primary application.
Metal (usually aluminum) trap bodies are recommended for GC analyses. Some plastics
are permeable to air and contain contaminants that can degrade gas quality. In addition,
many of the metal bodied oxygen traps can withstand high pressures (up to 2000 psi).
Some oxygen traps also remove moisture from the gas stream without affecting the
oxygen removal capability.
Indicating oxygen traps change color when oxygen is present in the gas at harmful levels.
Indicating traps are not intended to be the primary oxygen removal trap, but should be
used in conjunction with a high capacity non-indicating oxygen trap. They are installed
after the high capacity oxygen trap in the gas line to indicate when the high capacity trap
has expired and needs to be changed. Expired oxygen traps need to be immediately
changed since they can contaminate the gas, in addition to failing to remove oxygen.
Oxygen Traps
Tips & Tools
Oxygen traps are critical on carrier
gas supplies to prevent column
bleed. They are also recommended
with ECD.
Description Size
Indicating Oxygen Traps (IOT and LIOT Series)
Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP
Large Indicating Oxygen Trap 150 LIOT-2 LIOT-4
Economy Non-Indicating Oxygen T
Oxygen Trap 70 OT1-2 OT1-4
Big Oxygen Traps (BOT Series)
Big Oxygen Trap 750 BOT-2 BOT-4
raps (OT1 Series)
(cc)
1/8 in.
Part No.
1/4 in.
Part No.
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Combination Traps
Agilent carries several Combination Traps
that provide multiple contaminant removal
in a single trap. These traps offer:
• Optimized adsorbents for maximum
surface area and capacity.
• Leak-free, one-piece design to eliminate
potential leaks from using multiple traps.
• Efficient design which prevents
channeling and promotes
efficient scrubbing.
The ultimate in purification with
•
the Big Universal Trap, which removes
oxygen, moisture, hydrocarbons,
carbon monoxide, and carbon dioxide.
Gas Management
Agilent OT3 trap
Combination T
Description Size
Oxygen/Moisture Traps (OT3 Series)
OT3 Trap 100 OT3-2 OT3-4
Hydrocarbon/Moisture Traps (HMT Series)
Hydrocarbon/Moisture Trap 200 HMT200-2 HMT200-4
Adsorbant Refill (1 pint) HCRMS HCRMS
raps
(cc)
1/8 in.
Part No.
1/4 in.
Part No.
Combination Traps for Chemical Ionization MS
Chemical Ionization for MS* G1999-80410
Big Universal Traps (RMS Series)
Hydrogen RMSHY-2
Helium (Ar/Me) RMSH-2 RMSH-4
Nitrogen RMSN-2 RMSN-4
*Isobutane or methane applications only
RMSHY-4
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NEW!
Renewable Gas Purification System
The Renewable Gas Purification System from Agilent not only traps large quantities of
contaminants and lasts a long time, but it is also recyclable. With average use, you'll only
have to purchase a replacement cartridge once per year or after approximately 20
cylinders worth of purification. And when you need a replacement, you have the option to
purchase a new or recycled cartridge. Recycled cartridges are refilled and certified to the
full specification of the new cartridges.
• All cartridges are environmentally friendly and reduce waste.
• High capacity – 850cc or more Oxygen filtration, 12g H
O, and approximately 8g
2
hydrocarbon filtration per cartridge – in a compact footprint.
• Improves 99.995% gas purity to 99.9995% purity.
• Dual indicators make it easy to see the purification results.
• Labeling displays indicator color and shape for accurate reading.
• Simple twist on/off knob and guide rod make cartridge changes quick and easy.
• One Renewable Purifier system can support up to four GC systems.
• Designed with efficiency, safety, and environmental responsibility in mind.
Renewable gas purification system
Renewable Gas Purification System
Description Part No.
Renewable gas purifier system startup kit
Includes one G3440-80007 base, one G3440-60003 renewable gas purifier
cartridge, and wall or bench mount hardware.
Renewable gas purifier system, base only G3440-80007
Renewable gas purifier cartridge, new G3440-60003
Renewable gas purifier recycled cartridge G3440-69003
G3440-60004
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Gas Management
Universal/External Split Vent Trap
Split vent traps stop environmental pollution. The split vent trap was designed to protect
the lab environment from the contaminants released by split injection systems, which can
vent up to 500 times the amount of sample reaching the detector into the laboratory's air.
A replaceable, impregnated carbon filter media traps and eliminates a broad range of
contaminants. The traps are also easy to change and come with three packs of
replacement cartridges each. Replace approximately every six months.
Split vent trap and cartridges, RDT-1020
Universal/External Split Vent Trap
Description Part No.
Universal/external split vent trap with 3 cartridges, 1/8 in. Swagelock fitting RDT-1020
Replacement cartridges, 3/pk RDT-1023
Split vent trap kit G1544-60610
ools
ips & T
T
Replace split vent traps every six months.
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Regulators
Agilent recommends using our economical brass body, dual stainless steel diaphragm
regulators for most GC applications. These regulators, combined with the proper
gas purification system, provide proper gas pressure control and purity for
gas chromatography.
Brass Body, Dual Stainless Steel Diaphragms, 1/8 in., U.S. Only*
Description Part No.
CGA 346, 125 psig max (8.6 bar), Air 5183-4641
CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642
Brass body regulator
Tips & T
ools
When ordering a regulator, be sure
to specify the proper connections.
In the US, most gas manufacturers
follow CGA connection guidelines.
In Europe, there are a number of
organizations designating cylinder
connections that are specific to
individual countries. It is best
to contact your local supplier for
the proper connection designation.
CGA 540, 125 psig max (8.6 bar), O
CGA 580, 125 psig max (8.6 bar), He, Ar, N
CGA 590, 125 psig max (8.6 bar), Air 5183-4645
*For 1/4 in. tubing, purchase a 1/4 in. adapter, U.S. only
2
2
5183-4643
5183-4644
Connectors (Swagelok to Female NPT)
Description Unit Part No.
1/8 in. (A) x 1/4 in. (B) connector, brass (included with brass regulators)
1/4 in. (A) x 1/4 in. (B) connector, brass* 1/ea 0100-0119
*Required for plumbing 1/4 in. tubing to regulators
1/ea 0100-0118
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Tubing
Gas Management
Cleaning Tubing
Before any tubing is placed into service,
or if it becomes contaminated with use,
it is essential that it be properly cleaned.
Unclean or improperly cleaned tubing can
lead to contamination of the system with
disastrous results. Never use chlorinated
solvents to clean tubing or fittings.
Agilent provides clean, high quality
GC grade tubing for large systems as
an economical alternative.
Agilent recommends using copper tubing for most applications, since it is easy to bend
and plumb and is less expensive than stainless steel. Use stainless steel tubing only for
crucial applications that require very high purity, or where building codes mandate its use.
Determining Tubing Length
Parameters: 2000 sccm (4.2 scfh); Temperature: 70°F; Pressure 30 psig
Tubing Type Diameter
(inches)
Copper 1/8 50 2
Copper 1/4* 300 0.5
*Recommended when multiple instruments are connected to the same source
Recommended
Max. Length (feet)
Pressure Drop
(psig)
Tubing - Precleaned
Description Part No.
Copper tubing, 1/8 in., 50 ft 5180-4196
Copper tubing, 1/8 in., 12 ft 5021-7107
Fittings
Cylinder wall bracket, 5183-1941
Description Part No.
Fittings Kit
Includes brass nuts, ferrules, caps, plugs, unions and reducers
1/8 in. brass nut and ferrule set 5080-8750
5180-4161
Cylinder wall bracket
Description Part No.
Cylinder wall bracket with strap & chain
(cylinder size up to 14 in., 35 cm)
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5183-1941
15
Flowmeters
Setting and maintaining GC flow rates greatly affects the instrument accuracy
and sensitivity. During maintenance, verify carrier and support gas flows with
the proper flowmeter.
Precision gas flow meter, 5067-0223
NEW!
Agilent's Precision Gas Flow Meter is the ultimate gas flowmeter for chromatography
applications. This hand-held flowmeter incorporates industry leading performance and
features in a highly accurate and reliable package. The inherent stability of the rugged,
solid state components allows us to provide the longest calibration interval on the market,
all traceable to NIST standards.
• Highly accurate and reliable measurement of common carrier and fuel gases used
in GC, including nitrogen, air, carbon dioxide, hydrogen, helium, and argon/methane.
• Two year guaranteed calibration period traceable to NIST standards.
• Measures flow (0-500 mL/min.) based on gas viscosity properties with an accuracy
of ± 0.8% of reading + 0.2% of full scale.
• Flow rate range from 0-500 mL/min (no conversion necessary from SCCM) eliminates
the need for two separate meters to measure capillary and standard flows.
• Displays mass flow, volumetric flow, temperature, and pressure
readings simultaneously.
• Can be plumbed inline.
Precision Gas Flow Meter
Precision Gas Flow Meter
Description Part No.
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Precision gas flow meter 5067-0223
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ADM flowmeters
Gas Management
ADM 1000
• Accuracy ± 3%.
• Operating temperature range – 0 to 45ºC for the instrument, -70 to 135ºC
for the tubing.
• Calibration – traceable to NIST primary standards.
• Real time, split ratio measurement.
• 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
In addition to the features of the ADM 1000, the ADM 2000 includes:
• Mass flow measurements – measure flow rate, independent of atmospheric pressure
and temperature (calculated).
• Data output through RS-232 port.
• 9V battery and AC power adapter (120 or 220 VAC).
ADM Flowmeters
Description Flow Rate
(mL/min)
Low High
ADM 1000** 0.5 1000 All ± 3 9V Battery None 220-1170
ADM 2000** 0.5 1000 All ± 3 Battery or 120V AC Yes 220-1171-U
ADM 2000E** 0.5 1000 All ± 3 AC Adapter, 220V Yes 220-1171-E
Carrying Case for ADM 907-0056
*± 3% or ± 0.2 mL/min, whichever is greater with a flow rate of 0.5 - 1,000 mL/min
**Non-corrosive gases only
Gases
Measured*
Accuracy (%) Power
Supply
RS-232
Data Output
Part No.
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NEW!
Gas leaks can cause detector noise and baseline instability, shorten column life and waste
expensive carrier gas. Liquid leak detectors, although inexpensive, can contaminate your
system. Agilent's G3388A electronic leak detector is an easy way to quickly identify leaks
in your system.
Gas Leak Detector
Gas Leak Detector
Description Part No.
Gas leak detector
Handheld electronic gas leak detector
Includes probe, unit, AC power adapter/battery charger, battery, and user manual.
Check valves, fittings, and traps for leaks after every maintenance and thermal
cycling, as these can loosen some types of fittings.
Check for leaks at these connections:
• Gas supply bulkhead fittings
• Gas cylinder fitting
• Regulator fittings
• Traps
• Shut-off valves
• T-fittings
G3388A
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Sample Introduction
Ensure optimal peak shape and reproducibility
through accurate sample delivery.
They may be small, but sample introduction supplies can have a profound impact on
your results. That is why Agilent vials, septa, and syringes are meticulously engineered
to work seamlessly with your GC and GC/MS instruments. They can help you achieve
reliable, repeatable results even for your most complex runs.
This section guides you through…
• The selection, use, and maintenance of your essential sample introduction supplies.
• Troubleshooting common and unusual syringe problems.
• Essential procedures, such as vial filling, syringe cleaning, and choosing the right
septa material for your application.
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Vials
Agilent's wide opening vials are designed specifically for analyzing samples with your GC.
They have specially designed vial neck angles, bottom design, and height to ensure
compatibility with Agilent autosamplers with rotating or robotic arm trays. Agilent offers
a large variety of autosampler vials in different closures, cap colors, septa choices,
and package options. Agilent also offers convenience packs with 500 vials and caps
in a reusable blue storage box.
For small samples sizes, Agilent offers a variety of options. You can use microvolume
inserts with the wide opening vials or, for added convenience, use vials with small
volume capacity.
Vial Options
Agilent Certified Vials
Agilent certified vials undergo
stringent testing of critical
dimensions to ensure that each
vial works flawlessly with your GC
and GC/MS systems. Additionally,
each certified vial is made from
first hydrolytical class, borosilicate
glass type 1 then packed in a
clean, sealed environment to
prevent contamination.
Glass - for general purpose
use and for use with acids
Polypropylene - for use with
alcohols and aqueous solvents
Amber Vials - for use with
light-sensitive samples
Silanized - for use with
samples that bind to glass,
and for trace analysis
High Recovery Vials for use with limited sample vials
Microvolume Inserts for use with very small
sample volumes
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Sample Introduction
Vial Filling
When filling sample vials, keep in mind:
• If you need to test a large amount of sample over repeated injections, divide the sample
among several vials to obtain reliable results.
• When sample volume in the vial is low, contaminants from the previous sample
injection or solvent washes may have a greater impact on the sample.
The airspace in the vial is necessary to avoid forming a vacuum when sample
is withdrawn. This could affect reproducibility.
Preparing Sample V
ials
The Agilent 7683 Automatic Liquid Sampler Injector and the tray use clear or amber
glass sample vials with crimp, snap, or screw top vials. The following diagram shows
the critical dimensions for sample vials and microvial inserts to be used with the 7683
Automatic Liquid Sampler. These dimensions do not make up a complete set of
specifications. Incompatible sample vials cause tray and turret errors.
5 minimum 6.25
3.7
8.2
32
11.7
Microvial insert Crimp cap sample vial Maximum height of a capped vial
All dimensions in millimeters
34.5 maximum
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21
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.
Type Uses
Tips & Tools
To determine potential septa
quantities, consider:
• The number of samples
run during a day/week.
If samples are run in small
•
or large batches.
• If samples are run manually
or with an autosampler
• If samples are run overnight,
unattended.
.
Red Rubber/PTFE
Silicone/PTFE
PTFE/Silicone/PTFE
PTFE Disc
Viton
• Routine analysis
• Moderate resealing
• Excellent chemical inertness
• Not recommended for multiple injections or storage of samples
• Least expensive
• Excellent resealing
• Resists coring
• Good for multiple injections
• Used in trace analysis applications
• Above average resealing
• Most resistant to coring
• Least evaporation
• Use with large diameter, blunt tip syringe needles
• Good for MS and ECD analysis
• Good for large-volume injections
• Chemically inert
• No resealing
• Single injection
• No long-term sampling storage
• Chlorinated solvents
• Organic acids
• Limited resealing
• Not suitable for 32 guage syringe
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onvenience vial and cap pack
C
Sample Introduction
Convenience Vial and Cap Packs
Vials Caps Unit Part No.
Certified Screw Top Vial Convenience Packs
Clear Blue screw caps, PTFE/red
ubber septa
r
Clear with write-on spot Blue screw caps, PTFE/red
rubber septa
Amber with write-on spot Green screw caps, PTFE/red
rubber septa
Clear Blue screw caps,
PTFE/silicone/PTFE septa
Clear with write-on spot Blue screw caps,
PTFE/silicone/PTFE septa
Amber with write-on spot Green screw caps,
PTFE/silicone/PTFE septa
Clear Blue screw caps, PTFE/silicone
septa
Clear with write-on spot Blue screw caps, PTFE/silicone
septa
Amber with write-on spot Green screw caps, PTFE/silicone
septa
Clear Blue screw caps, pre-slit
PTFE/silicone septa
Clear with write-on spot Blue screw caps, pre-slit
PTFE/silicone septa
Amber with write-on spot Green screw caps, pre-slit
PTFE/silicone septa
Clear Blue screw caps, pre-slit
PTFE/silicone septa
500/pk 5182-0732
500/pk 5182-0867
500/pk 5182-0733
500/pk 5182-0736
500/pk 5182-0869
500/pk 5182-0737
500/pk 5182-0734
500/pk 5182-0868
500/pk 5182-0735
500/pk 5183-2079
500/pk 5183-2080
500/pk 5183-2081
500/pk 5067-0205
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23
Certified crimp top vial convenience pack
Convenience Vial and Cap Packs
Certified Crimp Top Vial Convenience Packs
Clear Silver aluminum crimp caps,
PTFE/red rubber septa
Amber with write-on spot Silver aluminum crimp caps,
PTFE/red rubber septa
Snap Top Vial Convenience Packs
Clear Clear polypropylene snap caps,
PTFE/red rubber septa
Amber, with write-on spot Clear polypropylene snap caps,
PTFE/red rubber septa
500/pk 5181-3400
500/pk 5181-8801
500/pk 5182-0547
500/pk 5182-0548
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24
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lectronic crimper, 5062-0207
E
Sample Introduction
Electronic Crimpers and Decappers
Whenever large amounts of crimp vials need to be crimped or decapped,
the electronic crimper or decapper is the right tool. It reduces stress and repetitive
motion injury associated with manual plier-style crimpers and decappers. Agilent's
newly-designed crimper offers easy, hand-held pushbutton operation and provides the
following advantages:
• Stronger and sturdier crimping and decapping.
• Consistent seals.
Shorter recharging time and a larger number of battery charges.
•
• Better clearance and more flexibility thanks to improved crimp jaws.
• Individual test certificates.
Electronic Crimpers and Decappers
Description Part No.
11 mm Electronic Crimper with 4.8v rechargeable battery pack and charger 5062-0207
20 mm Electronic Crimper with 4.8v rechargeable battery pack and charger 5062-0208
11 mm Electronic Decapper with 4.8v rechargeable battery pack and charger 5062-0209
20 mm Electronic Decapper with 4.8v rechargeable battery pack and charger 5062-0210
4.8v nickel metal hydride replacement battery 5188-6565
Tips & Tools
For a consistent seal, make sure there are no folds or wrinkles
on the part of the cap that wraps under the neck of the vial.
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25
Gold standard autosampler syringes
Gold Standard Autosampler Syringes
With a broad selection of syringes for auto injection, Agilent has what you need for
accurate and effective sampling. Agilent delivers even more value in every autosampler
syringe with the introduction of many new features in our line of Gold Standard GC
Autosampler Syringes.
Agilent Gold Standard Autosampler syringes are designed:
• For reproducible sample volume delivery.
• Specifically for the Agilent inlet or autosampler.
• To maximize inlet septum lifetime.
Agilent Gold Standard Autosampler syringes feature:
• Lot numbers printed directly on the barrel with a corresponding Certificate of
Conformance ensuring certified performance to all specifications.
• Gold protective cap on the fused needle, preventing the glass syringe barrel from
chipping as it is pressed against the inlet.
• Black ink and gold illuminating backing strip, for effortless viewing of the volume scale,
which is easily discernible from imitators.
• Environmentally friendly packaging, an improved design that reduces waste.
• Individually sealed packaging, for contaminant-free use right out of the box.
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26
Tips & Tools
Use syringe needles with an Agilent dual-taper needle or a conical tip. Sharptipped needles tend to tear the inlet septum and cause leaks. Also, a sharptipped needle tends to leave residual amounts of sample on the septum as it
exits, resulting in a large solvent tail on the chromatogram.
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Sample Introduction
Needle Gauge Selection
• Syringe needles compatible with Agilent Automatic Liquid Samplers are 42 mm long
and have an HP style or cone shaped tip.
• The Merlin Microseal requires 23 gauge needles.
• The smaller the gauge, the larger the needle diameter.
Needle Gauge Selection
Inlet Needle Gauge Column Type
Tips & Tools
For highest productivity and
to minimize coring, use Agilent
Premium Non-Stick Inlet Septa
with Center Point Guide.
See page 46.
Packed, split or splitless (including
PTV)
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
Cone tip
Needle Shape
23 gauge or 23/26 gauge tapered Any
Needle tips
Tapered needle
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27
Syringe Characteristics and Recommended Uses
Syringe Advantage Limitations Recommended Use
10 µL, PTFE-tipped
10 µL, fitted plunger
5 µL, fitted plunger
• Less plunger binding than fitted
plunger
• Replaceable plunger for reduced
repair cost
• Tight seal between plunger and barrel
• Most economical
• Most reliable fitted plunger syringe
• Less bending
• Better for high viscosity samples
• Most accurate for 1 µL injection
• No hardware modification needed for
0.5 µL
• More expensive than fitted plunger
• PTFE-tipped syringes not available
in 5 µL size
• Most accurate only for 1 µL and
larger injections
• Plunger not replaceable
• Thinnest plunger, can bend more
easily
• Not ideal for higher viscosity
samples
• Plunger not replaceable
• High sample throughput
• Samples in polar solvents
• Dirty samples
• Gases and volatile samples
• Reactive samples
• General purpose syringe
• Clean samples
• Routine analysis
• 1 µL injections
• Clean samples
• Routine analysis
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