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Maintaining Your Agilent GC System: Maximize Your Efficiency. Minimize Your Downtime
Maintaining Your Agilent GC System: Maximize Your Efficiency. Minimize Your Downtime
Introduction
With many labs today finding themselves
with reduced staff, our GC Maintenance
Guide was designed to put 35 years of
Agilents GC knowledge right in your lab.
We share everything from essential
maintenance schedules to keep you up
and running, to invaluable troubleshooting
tips and problem solving methods. Weve
even included an easy guide to help you
order the right Agilent PerfectFit parts
and supplies to keep your downtime to
a minimum.
At Agilent Technologies, we give you more
than the worlds best GC system. We give
you knowledge!
UT
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POST ER ENCL
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oting
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s
ble
Trou Guide
GC
3
4
5
5
13
14
15
16
Gas Management
Gas Types
Purities
Purifiers
Regulators
Tubing
Leak Detection
Flow Rates
19 Sample
Introduction
& Inlets
Sample Introduction
20 Vials & Syringes
Inlet Types
26 Packed Column
28 Split/Splitless
31 Cool on-Column
34 PTV
Inlet Accessories
36 Septa, Liners,
Ferrules
37
38
38
38
39
Columns
Column Maintenance
Column Selection
Installation/Setup
Column
Performance
43 Detectors
44 Thermal
Conductivity
Detector (TCD)
45 NitrogenPhosphorous
Detector (NPD)
48 Electron-Capture
Detector (ECD)
50 Flame Photometric
Detector (FPD)
52 Flame Ionization
Detector (FID)
55 Service & Support
56 Expert Training,
Service & Support
Dont Miss
GC Troubleshooting Guide (pullout poster)
GC Maintenance Schedule (inside back cover)
www.agilent.com/chem
GAS MANAGEMENT
Gas Management
The use of quality carrier gases is essential
for consistent and accurate GC analyses.
Proper gas management is key to achieving
this goal. Agilent provides a diverse line of
high quality gas management products
gas purifiers, regulators, leak detectors and
flowmeters all designed to prevent
column damage and improve the quality
and consistency of your GC separations.
This section explains how common
contaminants like oxygen, moisture and
hydrocarbons can damage your GC column,
and helps you understand how to prevent
it. Also, look for practical information
about regulators, the importance of clean
GC-tubing, and minimizing the likelihood
of GC system contamination.
www.agilent.com/chem
GAS MANAGEMENT
Gas Types
Carrier Gases
The most frequently used carrier gases are
helium and hydrogen, although nitrogen
and argon can be used. Purity is essential
for these gases since they sweep the
sample through the column where it is
separated into its component parts and
then through the detector for component
quantification. Carrier gas purity is also
critical to prevent degradation of
chromatographic hardware.
Contaminants in carrier gases can have
a significant effect on column life and
subsequent analyte detection. Harmful
effects include contaminant peaks
Support Gases
Purity Required*
Pneumatics
No
Low Grade
Pneumatics
No
Low Grade
Gas Type
Function
Air
Nitrogen
Hydrogen
1-1000 ppm
1000 ppm-1%
1%-100%
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
Hydrogen/Helium Mix
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
Methane/Argon
or Nitrogen
Carrier or make-up
for ECD
Yes
Research
Research
Research
N/A
Air
No
Ultra-Pure
Ultra-Pure
UHP/Zero
UHP/Zero
Nitrogen, Helium,
or Argon
Carrier or
make-up gas
Yes
Research
Ultra-Pure
Ultra-Pure
UHP/Zero
*Purities of gases depends upon the type of detector that is used. Use this table as a general guide only and refer to your detector manual for
specific gas purities that are needed.
Low Grade = Specialty or industrial gases (99.998%)
UHP/Zero Grade (99.999%)
Ultra-Pure Grade (99.9995%)
Research Grade (99.9999%)
www.agilent.com/chem
GAS MANAGEMENT
Moisture
Oxygen
Identifying Contaminants
To make a proper purity choice it is
helpful to understand the contaminants
most common in GC gases and how
they can affect your analysis. Common
contaminants are:
www.agilent.com/chem
Other Considerations
GAS MANAGEMENT
Gas supply
1 = Moisture Trap
2 = Hydrocarbon Trap
3 = Oxygen Trap
4 = Indicating Oxygen Trap
5 = Gas Purification System
6 = Combination Trap for
moisture, oxygen, and
hydrocarbon removal
Detector Gas Purification
FID make-up, air,
and H2
-ORCombination Trap
Gas supply
ECD make-up
Vent
MS carrier gas
Gas Traps
www.agilent.com/chem
GAS MANAGEMENT
Size
(cc)
H2O Removal
Capacity (g)
1/8 in.
Part No.
1/4 in.
Part No.
Molecular Sieve 13X and Indicating 4 Economy, with plastic Lexan body (other packings available, see Agilent catalog)
200
36
18
MT200-2
MT200-4
MSR-1
MSR-1
GMT-2-HP
GMT-4-HP
GMSR
GMSR
Glass Indicating Moisture Traps (larger size is available, see Agilent catalog)
100
250
16.3
5060-9084
750
www.agilent.com/chem
Moisture S-Trap
BMT-2
BMT-4
BMSR-1
BMSR-1
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
GAS MANAGEMENT
Oxygen Traps
Oxygen traps usually contain a metalcontaining inert support reagent. Most
oxygen traps reduce the oxygen
concentration to below 15-20 ppb. The
capacity of a standard oxygen trap is
approximately 30mg of oxygen per 100cc
of trap volume. Oxygen traps can remove
some small organics and sulfur compounds
from gas streams.
Oxygen Traps
Description
1/8 in.
Part No.
Size (cc)
1/4 in.
Part No.
30
IOT-2-HP
IOT-4-HP
Big Oxygen Traps non-indicating, for the Ultimate Oxygen Capacity (smaller size
available, see Agilent catalog)
750
BOT-2
Hydrocarbon Traps
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
200
HT200-2
HT200-4
ACR
ACR
BOT-4
Hydrocarbon Traps
Description
750
BHT-2
BHT-4
BACR
BACR
Hydrocarbon S-Trap
5060-9096
100
Hydrocarbon Trap
HT3-2
HT3-4
ACR
ACR
www.agilent.com/chem
GAS MANAGEMENT
Hydrocarbon S-Trap
Combination Traps
Agilent carries several Combination Traps
that provide multiple contaminant removal
in a single trap. These traps offer:
Description
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
100
OT3-2
OT3-4
Oxygen/Moisture Traps
Hydrocarbon/Moisture Traps
200
HMT200-2 HMT200-4
HCRMS
HCRMS
Big Universal Traps for the Ultimate in Gas Purification, removes oxygen, moisture,
hydrocarbons, CO, and CO2
750
RMSH-2
RMSH-4
750
RMSHY-2
RMSHY-4
750
RMSN-2
RMSN-4
UMC-5-2
UMC-5-2
www.agilent.com/chem
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
GAS MANAGEMENT
High Capacity
Gas Purification System
Single-Cartridge System
Three Cartridge
High Capacity
Gas Purification
System
Part No.
5183-1907
5182-9776
5182-9780
10
5183-4598
5183-4599
5183-4600
www.agilent.com/chem
GAS MANAGEMENT
RQC-P
Fitting (in.)
Part No.
1/8
RQC-P
4-Head
Replacement Cartridges
Description
GC-1
GC-2
Indicating moisture
GC-2-I
Hydrocarbon
GC-3
Indicating oxygen
GC-4
www.agilent.com/chem
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
11
GAS MANAGEMENT
Part No.
5182-9704
5182-0816
Description
5182-9705
5183-4770
Part No.
RDT-1020
RDT-1023
12
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
www.agilent.com/chem
GAS MANAGEMENT
Regulators
Pressure regulators are an integral
component in any gas handling system.
Their function is to reduce the pressure
from a high pressure source, such as a
cylinder, to a suitable use pressure.
Although regulators are very good at
controlling pressure, they do not control
flow. They have a maximum flow rate
which is dictated by the design. Basically,
the flow is determined by the pressure
drop across the regulator.
Types of Regulators
There are primarily two types of
regulators: single stage and dual (or two)
stage. The difference is that a dual stage
regulator is actually two regulators
connected in a series.
Dual stage regulators provide more precise
and consistent pressure control than single
stage regulators. The reason is that in a
single stage regulator, as the gas cylinder
Regulator Materials
Regulators are usually constructed of brass
or stainless steel. The choice of material
follows the same guidelines as the choice
of tubing. Generally, it is not recommended
that the materials be interchanged. If
stainless steel tubing were chosen due
Description
Part No.
5183-4641
5183-4642
5183-4643
5183-4644
5183-4645
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
Regulator Outlet Adapters Female NPT to Swagelok-style
0100-0118
0100-0119
www.agilent.com/chem
13
GAS MANAGEMENT
Tubing
When constructing or maintaining a gas
delivery system for GC, choosing the proper
tubing material is very important and will
help to eliminate potential problems and
improve the overall quality of the gas
system. Although there are many common
tubing materials available, some pose
safety or cleanliness problems.
Cleaning Tubing
Determining Tubing Length
Parameters: 2000sccm (4.2 scfh); Temperature: 70F; Pressure 30 psig
Tubing Type
Diameter
(inches)
Recommended
Max. Length (feet)
Pressure Drop
(psig)
Copper
1/8*
50
Copper
1/4*
300
0.5
TubingPrecleaned
Description
Part No.
5180-4196
5021-7107
14
www.agilent.com/chem
GAS MANAGEMENT
Description
Part No.
SL-8
SL-4
Cylinder Bracket
Description
Part No.
5183-1941
Cylinder Wall Bracket
Leak Detection
Leaks allow oxygen and other
contaminants to enter the gas stream.
Therefore, GC instrument maintenance
should include checking fittings and
connections with a gas leak detector.
Agilents Gas Leak Detector enables quick
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
5182-9648
15
GAS MANAGEMENT
Flow Rates
Setting and maintaining GC flow rates
greatly affect the instrument accuracy
and sensitivity. During maintenance,
verify carrier and support gas flows
with the proper flowmeter. Choosing a
flowmeter for your application depends
upon measurement speed, ease of use,
accuracy, and flow rate range.
Selecting a Flowmeter
Agilent manufactures the largest selection
of volumetric and mass flowmeters for
chromatography. We have developed
flowmeters for measuring capillary column
flows, calibrating air pumps and flow
controllers, and verifying instrument gas
flows. All flowmeters are calibrated to
NIST-traceable standards.
FlowTracker 2000
Part No.
5183-4779
5183-4780
Accuracy 3%
ADM 2000
In addition to the features of the ADM
1000, the ADM 2000 includes:
CE mark certified
ADM 1000
ADM 2000
16
www.agilent.com/chem
GAS MANAGEMENT
Flowmeters
Description
Gases
Measured
Accuracy
(%)
Power
Supply
RS-232 Data
Output
Part No.
0.5
1000
All
9V Battery
None
220-1170
ADM2000
0.5
1000
All
Yes
220-1171-U
ADM2000E
0.5
1000
All
Yes
220-1171-E
Electronic Mass Flowmeter dedicated mass flowmeter, very accurate for specific gases*
Veri-Flow 500
(110 V)
5.0
500
Rechargeable Battery
or 110 VAC
Yes
HVF-500
Veri-Flow 500
(220 V)
5.0
500
Rechargeable Battery
or 220 VAC
Yes
HVF-500-2
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
Veri-Flow 500
Optiflow 420
www.agilent.com/chem
Only a small sampling of flowmeters are shown here. For a complete selection of flowmeters, see the
Flowmeter Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
17
Theres More!
Agilent offers a series of free
Maintenance Guides for your GC System.
(publication # 5988-3466)
(publication # 5988-3960)
Sample Introduction
& Inlets
Agilent offers a wide range of GC sample
vials, septa, syringes, liners and inlets
for a broad range of gas-phase applications.
Our PerfectFit supplies have been designed
specifically for Agilent instruments so
they help to ensure GC results that are
reproducible and accurate. This section
reviews these critical components, and
helps you make the right choice. Also, look
for useful information from proper syringe
use and cleaning techniques to a detailed
discussion on optimized inlet settings. All
to make your GC analysis easier. All from
the GC experts.
www.agilent.com/chem
Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes, see the
Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
19
Sample Introduction
Vials
Vial Filling
Vial Options
Polypropylenefor use
with alcohols and aqueous
solvents
1 mL
50 L
3.6 mm*
*Needle position based on standard sampling depth.
20
100 L vial
www.agilent.com/chem
Red Rubber/Teflon
Routine analysis
Moderate resealing
Excellent chemical inertness
Not recommended for multiple
injections or storage of samples
Least expensive
Silicone/Teflon
Excellent resealing
Resists coring
Good for multiple injections
Teflon/Silicone/Teflon
Used in trace analysis applications
Above average resealing
Most resistant to coring
Least evaporation
Use with large diameter, blunt tip
syringe needles
Vials
Description
Quantity
Part No.
500/pk
5181-3400
500/pk
5182-0732
500/pk
5182-0547
100/pk
5181-1270
1000/pk
9301-0978
100/pk
9301-0977
100/pk
5184-3551
100/pk
5182-3454
Teflon Disc
Good for MS and ECD analysis
Chemically inert
No resealing
Single injection
No long-term sampling storage
Viton
Chlorinated solvents
Organic acids
Limited resealing
Not suitable for 32 gauge syringe
www.agilent.com/chem
Vials
21
Syringes
Selecting Syringes
Needle Gauge
Column Type
Packed, split or
splitless (including PTV)
any applicable
Cool on-column
530 m
Cool on-column
320 m
Cool on-column
250 m
Needle Tip
Needle Shape
Needle tips
Sharp tip
Cone tip
Tapered needle
22
Use syringe needles with an Agilent dualtaper needle or a conical tip. Sharp-tipped
needles tend to tear the inlet septum and
cause leaks. Also, a sharp-tipped needle
tends to leave residual amounts of sample
on the septum as it exits, resulting in a
large solvent tail on the chromatogram.
www.agilent.com/chem
Advantage
Limitations
Recommended Use
5 L, fitted
plunger
Most accurate
Thinnest plunger, 1 L injections
syringe for 1L
can bend
Clean samples
injection
more easily
Routine analysis
No hardware
Not ideal for higher
modification needed
viscosity samples
for 0.5 L injection
Plunger not
replaceable
10 L, fitted
plunger
Most economical
Most reliable fitted
plunger syringe
Less bending
Better for high
viscosity samples
10 L,
gas-tight
23
Syringe Tips
24
www.agilent.com/chem
Syringes
Description
Gauge
Quantity
Part No.
Tapered
Fixed Needle
23-26s/42
6/pk
5181-3360
5 L
Tapered
Fixed Needle
23-26s/42
6/pk
5181-8810
10 L
Straight
Fixed Needle
23/42
6/pk
9301-0725
5 L
Straight
Fixed Needle
23/42
6/pk
5182-0875
Unit
Part No.
144/pk
9301-0723
12/pk
07673-40180
144/pk
9301-1031
25/pk
5182-0551
07673-20570
18596-40015
07673-60840
www.agilent.com/chem
Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
25
Packed-Column Inlets
Packed-column direct inlets are very
popular. Packed-column analysis is
frequently done when high efficiency
separations are not needed or when gases
are analyzed by gas-solid chromatography.
Packed column inlets are simple in both
design and use. Few parameters need to be
set, and all carrier gas flow flushes through
the inlet into the column in the standard
configuration.
Selection/Setting
Rationale
Inlet temperature
BP of solvent +50C
BP of major solute(s)
Insert type
Liner
Glass
Initial column
temperature
temperature programming
Column type
20-40 mL/min
30-60 mL/min
Troubleshooting
Most problems with packed-column inlets
involve sample decomposition, flashback,
or leaks.
Decomposition
Since packed-column inlets are active,
especially if glass liners are not used, polar
sample components will often tail or
degrade in the inlet. Sample decomposition
caused by the inlet is easily diagnosed; the
decomposition products will have peaks at
the same retention times as standards for
the decomposition product.
When inlet-caused decomposition is
suspected, try intracolumn direct injection,
deactivated glass liners, or lower inlet
temperatures, and remove any column
packing in the inlet zone.
26
Flashback
The negative side of low inlet volume,
however, means that excessively large
sample injections will easily exceed the
capacity of the liner and will flash back into
gas supply lines and onto the septum. This
can cause several maladies, including
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.
Leaks
Since packed-column inlets are usually
flow-controlled, septum and column leaks
will have a direct impact on retention times
and peak areas. Sample can be lost through
the leak holes, and air can diffuse back into
the inlet to cause column degradation.
Change the septum on a regular basis and
check column connections at the first stage
of problems. To prevent stationary phase
decomposition, make sure that the oven
and inlet are at room temperature when not
in use and when changing the septum.
www.agilent.com/chem
Description
Septum nut
Unit
Part No.
1
18740-60835
50/pk
2
3
4
5183-4757
19243-80570
Viton O-rings
12/pk
5080-8898
25/pk
5080-8732
5/pk
5181-3382
10/pk
5080-8774
10/pk
5180-4105
Liner
19244-80540
19243-80530
19243-80540
Upper insulation
19243-00067
10
19234-60720
11
2/pk
5181-8830
** For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
* For Model 6890/6850 only
** For a complete selection of inlet supplies, refer to Agilents GC Inlet Resource Guide.
Inside of
Oven
9
10
11
Unit
Part No.
19243-60570
19243-80510
19243-80520
www.agilent.com/chem
19243-60505
10/pk
5180-4105
27
Split/Splitless Inlets
The combined split/splitless inlet is the
most popular inlet for capillary column gas
chromatography. Because it can be used in
either split or splitless mode, it provides a
very effective combination that can cover
most analysis requirements.
Split Mode
Split injection is an effective way to
introduce small amounts of sample without
overloading the column. Split injection is
required for samples that:
Troubleshooting
Split inlets are spared from most bandbroadening phenomena, since narrow
peaks are generated as part of the
splitting process. Therefore, any peak
broadening or tailing observed with split
injection is usually due to improper
column installation, low split flow, or
low inlet temperature. If you suspect that
the inlet temperature may be too low,
increase it by 50C and compare the
Selection/Setting
Rationale
Inlet temperature
Inlet liner
Minimizes flashback
Minimizes degradation
Inlet packing
Retains non-volatiles
Stops flow of droplets
Less active than wool
Least active
0.5-3 L liquid
0.10-10 mL gas
Injection volume
Split ratio
50:1 to 500:1
Initial column
temperatures
Not critical
Septum purge
2-3 mL/min
Minimizes ghosting
28
www.agilent.com/chem
Splitless Mode
Parameter
Selection/Setting
Rationale
Inlet temperature
Inlet liner
Inlet packing
None
Injection volume
0.5-2 L liquid
Injection technique
Fast autoinjection
Most reproducible
Less needle discrimination
Hot-needle slow manual Inject 1-2L.sec if narrow liner
is used and >1L injection
Hot-needle fast manual Use for <1L injections
Purge flow
20-50 mL/min
Not critical
20-80 sec
Oven temperature
Column flow
Septum purge
2-3mL/min
Reduces ghosting
Quantification
Internal standard
Standard addition
Maximizes reproducibility
Use only with constant
injection volume
Retention gap
1-3m, deactivated
(1-2m per L injected)
www.agilent.com/chem
Solvent Effect
One requirement of splitless injections is
that the initial column temperature should
be kept at least 10C below the boiling
point of the sample solvent. This allows the
sample solvent to condense at the front of
the column trapping the solvent molecules
into a tight, narrow band.
29
environmental analysis
drug screening
Troubleshooting
Most problems encountered with splitless
injection are related to incorrect purge
time, degradation, improper focusing, and
flashback.
Appropriate initial column temperature is
critical. Sample vapors can be lost through
the septum purge line if the insert is
overfilled with sample vapor (either too
large injection volume or too small liner
Decomposition
Loss of peak area or generation of new
peaks, can sometimes be dramatically
reduced by changing liner type or by
deactivating the liner and inlet with
silanizing reagents. Removing or reducing
the amount of liner packing can also
decrease inlet activity.
Description
Unit
Part No.
18740-60835
Septa**
Insert Weldment**
Liner O-ring**
Liner**
G1544-80550
G1544-20590
19251-20620
SS seal
Gold-plated seal
18740-20880
18740-20885
7
8
9
12/pk
5061-5869
10
Reducing nut
18740-20800
11
Insulation (requires 3)
19243-00067
12
19243-00070
13
Ferrule**
14
2/pk
5181-8830
2/pk
5183-4732
10
11
19251-00100
12
13
14
30
**For a complete parts breakdown, see the 6890/6850/5890 Series GC Instrument User and/or Service Manuals.
**For a complete selection of inlet supplies, refer to Agilents GC Inlet Resource Guide.
www.agilent.com/chem
Advantages:
Limitations:
Selection/Setting
Rationale
Initial inlet
temperature
= or 3C above column
oven temperature
Initial inlet
temperature ramp
Injection volume
0.1-2.0 L liquid
Injection technique
Fast autoinjection
Fused silica needle
Oven temperature
Inlet temperature or
slightly lower
Prevents backflash
Column flow
50-80cm/sec
30-50cm/sec
Septum purge
12-15mL/min
Quantification
All methods
Inherently reproducible
technique
Lack of discrimination
Retention gap
requirements
1-3m, deactivated
HELPFUL HINT: Since the sample is directly deposited into the column, nonvolatile sample
components can accumulate at the head of the column and will degrade efficiency and/or
interact with subsequent injections.
www.agilent.com/chem
Sample Considerations
Sample preparation is important for
on-column injection because of:
31
Troubleshooting
The major problems found with cool oncolumn injection are associated with
column overload, solvent/stationary phase
incompatibility, and column contamination.
If the flooded zone after injection is too
long (large injections, poor wettability),
peaks will be broad or split. A retention gap
usually will resolve this problem. Loss of
column efficiency with on-column injection
usually is caused by contamination or
degradation of the stationary phase at the
head of the column. Only columns with an
immobilized stationary phase should be
used with cool on-column injection to
Unit
Part No.
Column nut
2/pk
5181-8830
10/pk
5181-3323
10/pk
5062-3514
160-2255-5
160-2325-5
160-2535-5
5/pk
5181-3396
32
www.agilent.com/chem
Unit
Part No.
1a
1b
Manual injection
1c
1d
Duckbill septum
10/pk
19245-40050
6/pk
19091-63000
1c
1d
19320-80625
2
3
9301-0658
Common Supplies
3
Spring
19245-60760
19245-20510
19245-20515
19245-20525
19245-20580
19245-20780
Ferrule
5080-8853
Column nut
2/pk
5
6
5181-8830
19245-80521
1b
G1545-80520
50/pk
50/pk
5183-4760
5183-4758
19245-80520
1b
19245-20670
*For a complete parts breakdown, see the 6890/5890 Series GC Instrument User and/or Service Manuals.
www.agilent.com/chem
Only a small sampling of inlet supplies are shown here. For a complete selection of inlet supplies,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
33
Selection/Setting
Rationale
Injection mode
Cold split
Cold splitless
Inlet temperature
ramp rate
Advantages
no syringe-needle discrimination
minimal inlet discrimination
no special syringe needed
use of large injection volumes
removal of solvent and low boiling
components
trapping of nonvolatile components in liner
split or splitless operation
retention time and area reproducibility
approaching cool on-column injection
Ballistic
Inlet liner
Injection volume
0.1-1.5L
Sample Injection
technique
Autosampler or manual,
fast or slow
Oven temperature
Sample dependent
Column flow
30-50 cm/sec
Septum purge
1-5mL/min
Minimizes ghosting
Quantification
Any method
Inherently reproducible
Low discrimination in cold
injection modes
Retention gap
1-3m, deactivated
34
www.agilent.com/chem
Description
Column ID
Unit
Part No.
Septumless head
G2617-60507
Septum head
G2618-80500
Septum nut
18740-60835
G2617-60506
G2617-60508
G2619-60501
Silver seal
5/pk
3
2
5182-9763
0.20 mm
5182-9754
0.25-0.33 mm
5182-9761
0.53 mm
9
5182-9762
Ferrules for
0.20 mm
10/pk
5182-9756
5, 6
Graphpak inlet
0.25 mm
10/pk
5182-9768
0.32 mm
10/pk
5182-9769
7
8
0.53 mm
10/pk
5182-9770
10
5062-3525
11
G2617-20510
G2617-60510
5182-9748
Kalrez seal
5182-9759
Valve body
5182-9757
Pressure spring
5182-9758
Viton seal
5182-9775
Sealing element
5182-9760
3150-0602
5182-9747
5/pk
9
10
11
5182-9749
G2617-80540
PTV Liners
Description
Part No.
5183-2038
5183-2036
5183-2037
5183-2041
www.agilent.com/chem
35
Septa
The septum isolates the sample flow path
from the outside world. It must provide a
barrier that is readily penetrated by the
injector needle while maintaining internal
pressure without contaminating the
analysis. Septa are generally made of
special high temperature, low-bleed
silicone rubber formulations. Septa should
be replaced regularly to avoid leaks,
decomposition, sample loss, reduced
column or split vent flow, ghost peaks,
and column degradation.
To minimize problems:
use septa with the recommended
temperature range
change septa regularly
install the retainer nut hand tight
use septum purge when available
use autoinjectors
use Agilent dual-taper, conical point
syringe needles
Ferrules
Ferrules seal the connection of the column
or liner to the system. The ideal ferrule
provides a leak-free seal, accommodates
various column outer diameters, seals with
minimum torque, will not stick to the
column or fittings, and will tolerate
temperature cycling.
Installation
maintain cleanliness
sample degradation
loss of sample
Liners
Liners are the centerpiece of the inlet
system in which the sample is vaporized
and brought into the gas phase.
The liner should be changed on a regular
basis, and the correct liner must be used
to avoid peak shape degradation, solute
discrimination, poor reproducibility, sample
decomposition, and ghost peaks. Change
liners on a regular basis, as determined by:
sample cleanliness
36
www.agilent.com/chem
Columns
Choosing the right GC column and
following Agilents simple column care
recommendations will maximize GC
column performance and lifetime. In this
section our experts offer practical advice
on how to select, install and store your
GC column, plus give helpful hints about
avoiding thermal and oxygen degradation.
Because GC column contamination is
the primary cause of shortened column
lifetime, weve also included a detailed
discussion about the prevention of nonvolatile and semi-volatile contamination,
as well as appropriate recovery measures.
www.agilent.com/chem
37
COLUMNS
Column Maintenance
While GC column maintenance is
simple, the frequency and type of
column maintenance that is required
varies due to many system and sample
factors. Instead of simply following a
Column Selection
Choose the Column that offers the best
longevity:
Description
Part No.
122-0132
19091S-433
122-1232
122-3832
19091N-133
38
www.agilent.com/chem
COLUMNS
Bad
Good
Description
Part No.
5181-8836
20x Magnifier
430-1020
5080-8853
5080-8773
5182-9646
5182-9648
Prevention
www.agilent.com/chem
Recovery
Description
Part No.
This is a small sampling of the many GC columns and parts. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
39
COLUMNS
Thermal Damage
Oxygen Damage
Prevention
Prevention
Recovery
Perform column bakeout as described
under thermal damage recovery.
NOTE: Oxygen damage occurs very rapidly.
Recovery
40
Description
Part No.
5183-4780
BOT-2
BMT-2
RMSH-2
5183-4759
www.agilent.com/chem
COLUMNS
Chemical Damage
GUARD COLUMN
Length should be from 1-10 meters. Typical lengths of 5-10 meters allow
substantial trimming before the entire guard column has to replaced.
A low volume union should be used to attach the tubing to the column.
Glass pressfit unions are inexpensive and easy to install. DuraGuard
columns offer the guard column built into the analytical column as a
single piece of fused silica, eliminating the need for unions.
Prevention
Perform sample preparation to remove
inorganic acids and bases from the
sample
Install guard column and trim frequently
If acids or bases must be used choose an
organic alternative or HCl or NH4OH
Recovery
Guard Column
INJECTOR
DETECTOR
Column
Guard Column
Column Contamination
Column contamination is the most common
problem encountered in capillary GC.
Unfortunately, it mimics most other
chromatographic problems and is often
misdiagnosed. A contaminated column is
usually not damaged, but it may be
rendered unusable. There are two basic
types of contaminants: nonvolatile and
semivolatile.
www.agilent.com/chem
Union
This is a small sampling of the many GC columns and parts. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
41
COLUMNS
Nonvolatile Contaminants
Nonvolatile contaminants or residues do
not elute and accumulate in the column
(most often confined to the first few
meters). The column becomes coated with
these residues which interfere with the
proper partitioning of solutes in and out
of the stationary phase. Also, the residues
may interact with active solutes resulting
in peak adsorption problems (evident as
peak tailing or loss of peak size). Active
solutes are those containing a hydroxyl
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes.
Prevention
Description
Part No.
Pub#5988-2685EN
5183-4712
5183-4695
5181-3396
500-1200
160-2535-10
160-2255-10
430-3000
Recovery
Prevention
Recovery
Semivolatile Contaminants
Semivolatile contaminants or residues
accumulate in the column, but eventually
elute. Hours to days may elapse before they
completely leave the column. Like
nonvolatile residues, they may cause peak
shape and size problems and, in addition,
42
Column Storage
Capillary columns should be stored in their
original box when removed from the GC.
Place GC septa over the ends to prevent
debris from entering the tubing. Upon
reinstallation of the column, the column
ends need to be trimmed by 2-4 cm to
ensure that a small piece of septa is not
lodged in the column.
If a column is left in a heated GC, there
should always be carrier gas flow through
the column. The carrier gas flow can be
turned off only if the oven, injector, detector
and transfer lines are turned off (i.e., not
heated). Without carrier gas flow, damage
to the heated portion of the column occurs.
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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.
www.agilent.com/chem
Only a small sampling of FID supplies are shown here. For a complete selection of FID supplies,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
43
DETECTORS
Filament Maintenance
The primary maintenance for a TCD
involves the filament. Most procedures
involve improving filament life or keep the
filament from becoming damaged or
contaminated.
A constant presence of oxygen can
permanently damage filaments through
oxidative processes. The most common
source of oxygen is elevated levels in the
carrier or makeup gas or a leak near the
detector. Oxygen traps are recommended
for the carrier and makeup gases to reduce
oxygen levels. Proper column installation
techniques and regular leak checks
(especially after column installation) help
to keep leak problems to a minimum.
The damage caused by oxygen is more
severe at high filament currents.
Chemically active sample components
such as acids and halogenated compounds
may attack and damage the filaments.
Avoiding these compounds when possible
increases filament life. Turning off or
substantially reducing the filament current
when the TCD is not in use also prolongs
filament life.
Cell Contamination
Cell contamination is a problem when a
lower detector temperature is used to
improve sensitivity. Also, low filament
currents promote contamination since
the filament is maintained at a lower
temperature at lower currents. If the cell
becomes contaminated, a solvent flush
of the detector may help to remove the
condensed material.
Unit
Part No.
G1532-60675
10/pk
18740-20950
18740-20960
10/pk
5080-8773
10/pk
5080-8853
2/pk
5181-8830
2/pk
5183-4732
G1532-20710
44
19232-80550
19302-80020
19232-60676
www.agilent.com/chem
DETECTORS
Thermal Cleaning
The TCD can become contaminated with
deposits from such things as column bleed
or dirty samples. A wandering baseline,
increased noise level, or changes in
response on a checkout chromatogram all
indicate contamination. Thermal cleaning,
or bakeout (heating the detector block to
evaporate the contaminant), should be
performed only after you have confirmed
www.agilent.com/chem
Bead Life
To extend the life of the bead:
45
DETECTORS
Gas Flow
Gas Purity
Because of its high sensitivity, the NPD
requires very pure gases (99.999% or
better). We strongly recommend that
moisture and hydrocarbon traps be used
on the carrier gas and all detector gases,
including the detector hydrogen, air, and
makeup gases. Dirty gases will not only
give poor chromatographic performance,
but will shorten the bead life as well.
Contaminants
Some chemical problems can also arise
when using the NPD. Because it is a trace
detector, be careful not to contaminate the
analytical system.
Glassware
Glassware must be very clean. Phosphate
detergents should be avoided, so acid
washing of glassware followed by distilled
water and solvent rinsing is recommended.
Solvents
Solvents should be checked for purity.
Chlorinated solvents and silanizing
reagents can decrease the useful lifetime
of the alkali source; excess reagent should
be removed prior to injection, if possible.
NPD Jets
Description
Length (mm)
Part No.
48
G1531-80560
61.5
19244-80560
63.5
18710-20119
6890/5890 Adaptable
46
www.agilent.com/chem
DETECTORS
Description
Part No.
0515-0655
G1534-60570
5183-2007
Lid weldment
G1534-80510
0905-2580
G1534-40020
Collector funnel
G1534-20530
G1534-40030
0905-1284
Screw, M4 x 10 mm
0515-2495
10
J-Clamp
1400-0015
11
Screw, M4 x 10 mm
0515-2495
12
G1534-60610
13
Mounting pallet
G1531-40020
14
15
G1534-80500
G1534-80540
Lid stop
G1534-20590
5182-9722
16
17
18
9
10
11
12
4
5
6
13
14
15
16
17
18
19234-60720
19234-60540
5080-8872
19231-60790
*This bead is more sensitive but exhibits some tailing for phosphorous compounds.
Quantity discounts available.
**The black bead is potentially a little less sensitive but does not exhibit peak tailing and
typically has longer lifetime.
www.agilent.com/chem
47
DETECTORS
Thermal Cleaning
If your baseline is noisy or the output
value is abnormally high and you have
determined that these problems are not
being caused by leaks in the GC system,
you may have contamination in the
detector from column bleed. To remove
contamination, you should perform a
thermal cleaning (bakeout) of the detector.
Warning: Detector disassembly and/or
cleaning procedures other than thermal
should be performed only by personnel
trained and licensed appropriately to
handle radioactive materials. Trace
amounts of radioactive 63Ni may be
removed during other procedures,
causing possible hazardous exposure
to and x-radiation.
Gas Purity
For successful EC detection, its important
that the carrier and purge gases are very
clean and dry (99.9995%). Moisture, oxygen,
or other contaminants can be responsible
for improved sensitivity, but at a cost of
linear range. Always precondition the
column before connection to the detector.
ECD Warnings
Although beta particles at this energy level have little penetrating power the
surface layer of the skin or a few sheets of paper will stop most of them they
may be hazardous if the isotope is ingested or inhaled. For this reason the cell
must be handled with care. Radioactive leak tests must be performed at the
required intervals, the inlet and outlet fittings must be capped when the detector
is not in use, corrosive chemicals must not be introduced into the detector, and
the effluent from the detector must be vented outside the laboratory environment.
48
www.agilent.com/chem
DETECTORS
Unit
Part No.
G1533-80565
19234-60720
10/pk
5080-8774
Vespel/graphite 85%/15%
ferrule, 1/4 in. id
10/pk
0100-1331
10/pk
5180-4105
19301-80530
G2397-80520
19233-80565
7
6
5, 4
19233-20625
G2397-20540
19233-20755
18713-60050
www.agilent.com/chem
49
DETECTORS
50
www.agilent.com/chem
DETECTORS
Unit
Part No.
19256-60700
10/pk
5180-4105
2
3
Weldment, block
19256-80560
0905-1102
Spacer, ignitor
19256-20590
Glow plug
0854-0141
G1535-60600
19256-80040
10
19256-80030
11
19256-20580
12
Coupling, SS
19256-20550
14
Screw, M3 x 12 (4 required)
0515-0911
15
Clamp
19256-00090
16
17
18
19
Flange adapter
19256-20510
20
Flange ring
19256-00200
21
10
11
12
8
13
14
15
16
17
18
12/pk
12/pk
12/pk
5061-5891
5061-5890
19256-80570
19256-60500
12/pk
5061-5867
Liner/ferrule kit
19256-60590
Sulfur filter
19256-80000
Phosphorus filter
19256-80010
0905-1101
0905-1103
12/pk
www.agilent.com/chem
21
19256-80060
19256-80590
20
5061-5886
19
5061-5889
19305-60580
51
DETECTORS
Collector Assembly
Collector Body
Condensation
Since the FID combustion process
results in water formation, the detector
temperature must be kept above 100C to
prevent condensation. Such condensation,
especially when combined with chlorinated
solvents or samples, causes corrosion and
sensitivity loss.
FID Jets
Hardware Problems
FID Ferrules
52
www.agilent.com/chem
DETECTORS
Description
Unit
Part No.
6890/6850 Supplies
Collector insulator
G1531-20700
Collector body
G1531-20690
G1531-60690
G1531-20700
G1531-60680
Collector Housing
G1531-20740
5890 Supplies
Collector assembly*
19231-60690
19231-20970
Collector body
19231-20960
Hastelloy collector
19231-21080
19231-20950
19231-21050
Collector nut
19231-20940
Ignitor castle
19231-20910
19231-21060
19231-60680
Spring washer
10/pk
2/pk
5181-3311
8710-1346
19301-00150
8710-1561
19301-60660
12/pk
5080-4978
18710-60170
5/pk
5180-4150
5/pk
5180-4152
9301-0985
*Assembly Contains: Gasket, Ignitor Castle, Ignitor Glow Plug Assembly, Spring Washer-Wavy
Collector, Housing, Mount, Nut, Body, Spanner Nut, Insulator (upper and lower)
www.agilent.com/chem
Only a small sampling of FID supplies are shown here. For a complete selection,
see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide.
53
DETECTORS
FID Jets
Description
Length (mm)
Part No.
48
G1531-80560
G1531-80620
61.5
19244-80560
63.5
18710-20119
63.5
18789-80070
19244-80620
HELPFUL HINT: Different size jets are available to optimize flame shape for capillary
columns, or reduce contamination build-up for high molecular weight eluates. Usually,
small bore jets produce the greatest signal, but can plug up or contaminate more easily
relative to large jets, so compromise may be necessary.
54
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www.agilent.com/chem
55
GC Training
Agilents training courses for gas
chromatography helps new and
experienced lab professionals learn
proper and efficient ways to use
analytical instruments and software.
These ISO-registered courses also target
those who want to broaden or sharpen
their troubleshooting and maintenance,
and system operation skills. Contact
Agilent today for more information about
our training and other Support Services.
Or visit www.agilent.com/chem and
select Education.
GC Troubleshooting/
Maintenance Training
Agilent offers a four-day hands-on course
providing practical information for
troubleshooting and maintenance for the
complete Agilent Gas Chromatography
System. Its designed for the professional
with a fundamental GC knowledge and
who is responsible for troubleshooting
and maintenance. Learn how preventive
maintenance can ensure the long-term
reliability and proper operation of your
Agilent GC system. For more information
on all Agilent Training offerings, visit
www.agilent.com/chem and select
Education.
56
www.agilent.com/chem
www.agilent.com/chem
Operational Re-Qualification
After Repair
For instruments that require qualification,
Agilents Re-qualification After Repair
service verifies that a system is still
performing to Agilents operational
specifications after a repair, including
documentation that meets audit
requirements. Contact Agilent today for
more information about this and other
service contracts.
57
Software Support
Only Agilent can provide expert assistance
to isolate and resolve software problems.
Well provide telephone assistance from
highly trained experts. Well provide all
enhancements to the original chemical
analysis software purchased. Well even
send you Software Bulletins to let you
know about ongoing issues and
recommended workarounds. Contact
Agilent today for more information about
these and other Support Services.
GC System
Recommended
Maintenance
Schedule
Hardware Support
Agilents highly trained technical staff is
just a phone call away to offer you basic
hardware troubleshooting, operation
assistance, instrument and system
configuration, and remote diagnostics. Call
us toll-free today, or submit your question
on-line at www.agilent.com/chem.
58
Open inside cover for:
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TYPICAL SCHEDULE
ACTIONS/COMMENTS
Gas purifiers
(carrier gas &
detector gas)
Every 6 months*
Replace.
Flowmeter
calibration
TYPICAL SCHEDULE
ACTIONS/COMMENTS
Syringes
and/or syringe
needles
Every 3 months*
Inlet liner
Weekly*
Liner O-rings
Monthly*
Inlet septum
Daily*
Inlet Hardware
Every 6 months
Every year
Check parts and replace when parts are worn, scratched, or broken.
Schedule
Columns
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
Front-end
Maintenance
Weekly monthly*
Solvent rinse
As needed
Replacement
As needed
Ferrules
Detectors
ITEM
TYPICAL SCHEDULE
ACTIONS/COMMENTS
FID/NPD Jets
& Collector
As needed
Clean when deposits are present. Replace when they become scratched,
bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead
As needed
FID
Every 6 months
TCD
As needed
ECD
Every 6 months
As needed
Wipe test.
Thermally clean by baking-out when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD
Every 6 months
As needed
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