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GC Agilent Troubleshooting 1
GC Agilent Troubleshooting 1
Gas Management
Gas Types
Contaminants & Purities
Gas Purification Systems
Regulators
Tubing
Leak Detection
Flow Rates
18 Sample Introduction
Consumables & GC Inlets
Sample Introduction
19 Vials
21 Syringes
VIDEO
This icon denotes a video that is available to view on our website.
Just visit www.agilent.com/chem/techsupport to view how-to
videos and obtain more information.
26
28
31
34
36
42
47
52
54
Inlet Types
Packed-Column
Split/Splitless
Cool On-Column
Programmed Temperature
Vaporizer PTV
Inlet Accessories
Septa
Ferrules
Liners
Flip Top Inlet Sealing System
Parts & Supplies
56
57
57
58
Columns
Column Maintenance
Column Selection
Column Installation/Setup
& Conditioning
59 Column Performance
63 Columns Types and
Characteristics
68 Detectors
69 Flame Ionization Detector (FID)
Thermal Conductivity Detector
(TCD)
72 Electron-Capture Detector
(ECD)
74 Thermal Conductivity Detector
(TCD)
76 Flame Photometric Detector
(FPD)
78 Nitrogen-Phosphorus Detector
(NPD)
82 GC/MS Systems
83 Maintaining Mass Selective
Detectors (MSDs)
87 Mass Spectrometer Symptoms
88 Ion Source
93 Vacuum Systems & Pumps
96 Electron Multipliers &
Replacement Horn
97 Maintaining the MS Engine
99 Ion Source Parts & Supplies
100 General GC/MS Supplies
101 Test & Performance Samples
104 Services & Support
105 Expert Service, Training
& Support
Dont Miss
GC Maintenance Schedule (inside back cover)
1
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.
CATALOG
For a complete selection of gas management supplies, see Agilents
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
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 of impure gases include
contaminant peaks and elevated column
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 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%)
www.agilent.com/chem
GAS MANAGEMENT
Identifying Contaminants
To make a proper purity choice it is
helpful to understand the contaminants
most common in GC gases and how
they can affect your analysis. Common
contaminants are:
Hydrocarbons and Halocarbons
decrease detector sensitivity by
increasing detector background noise
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
www.agilent.com/chem
Other Considerations
determine desired purity level
keep number of fittings in gas line
to a minimum
install purifiers in a convenient location
close to the GC
purifier log books are useful for
determining maintenance schedule
use indicating traps closest to the GC so
you can determine when to change the
traps that are upstream
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
The purpose of gas traps is to remove
detrimental impurities from the carrier
and detector gases. Moisture (water),
oxygen and hydrocarbon traps are the
most common traps used with GC
systems. A few combination traps are
available which remove moisture, oxygen
and/or organics with a single trap. The
effectiveness of the traps depends on the
initial quality of the gas. Little
enhancement by traps to the GC system is
obtained by traps when using very high
purity gases (e.g., ultra-high purity or
similar grades) while obvious improvement
is obtained with lower grades of gas.
www.agilent.com/chem
GAS MANAGEMENT
Description
1/8 in.
Part No.
1/4 in.
Part No.
Price
MT200-2
MT200-4
$104
MSR-1
MSR-1
$ 55
GMT-2-HP
GMT-4-HP
$119
GMSR
GMSR
$ 63
Molecular Sieve 13X and Indicating 4 Economy, with plastic Lexan body (other packings available, see Agilent catalog)
200
36
18
100
250
16.3
5060-9084
$226
750
www.agilent.com/chem
Moisture S-Trap
BMT-2
BMT-4
$235
BMSR-1
BMSR-1
$ 58
GAS MANAGEMENT
Oxygen Traps
Oxygen traps usually include a metalcontaining inert support reagent. Most
oxygen traps reduce the oxygen
concentration to below 15-20 ppb. The
capacity of a standard oxygen trap is
approximately 30mg of oxygen per 100cc
of trap volume. Oxygen traps can also
remove some small organic and sulfur
compounds from gas streams, but this is
not their primary application.
Oxygen Traps
Description
1/8 in.
Part No.
Size (cc)
1/4 in.
Part No.
Price
IOT-4-HP
$143
30
IOT-2-HP
Big Oxygen Traps non-indicating, for the Ultimate Oxygen Capacity (smaller size
available, see Agilent catalog)
750
BOT-2
BOT-4
Hydrocarbon Traps
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
Price
200
HT200-2
HT200-4
$106
ACR
ACR
$ 63
BHT-2
BHT-4
$235
BACR
BACR
$ 52
$235
Hydrocarbon Traps
Description
750
Hydrocarbon S-Trap
5060-9096
$232
100
HT3-2
HT3-4
$ 98
ACR
ACR
$ 63
Hydrocarbon Trap
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.
Price
100
OT3-2
OT3-4
$104
Oxygen/Moisture Traps
Hydrocarbon/Moisture Traps
200
HMT200-2 HMT200-4
HCRMS
HCRMS
$ 98
$ 63
Big Universal Traps for the Ultimate in Gas Purification, removes oxygen, moisture,
hydrocarbons, CO, and CO2
750
RMSH-2
RMSH-4
$261
RMSHY-2
RMSHY-4
$261
RMSN-2
RMSN-4
$261
UMC-5-2
UMC-5-2
$ 21
www.agilent.com/chem
750
GAS MANAGEMENT
High Capacity
Gas Purification System
Three Cartridge System
Single-Cartridge System
Three Cartridge
High Capacity
Gas Purification
System
Part No.
Price
5183-1907
$612
5182-9776
$567
5182-9780
$393
5183-4598
$239
5183-4599
$255
5183-4600
$136
www.agilent.com/chem
GAS MANAGEMENT
RQC-P
Fitting (in.)
Part No.
Price
1/8
RQC-P
$1604
Part No.
Price
GC-1
$ 64
GC-2
$ 64
Indicating moisture
GC-2-I
$106
Hydrocarbon
GC-3
$ 64
Indicating oxygen
GC-4
$155
4-Head
Replacement Cartridges
Description
www.agilent.com/chem
10
GAS MANAGEMENT
Part No.
Price
5182-9704
$ 398
5182-0816
$1291
5182-9705
$ 186
5183-4770
$ 530
Part No.
Price
RDT-1020
$ 94
RDT-1023
$ 45
11
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
empties and the inlet pressure to the
regulator decreases (inlet decay), the
pressure on the diaphragm is reduced.
Without proper adjustment, the outlet
pressure might slowly rise.
Regulator Materials
Regulators are usually constructed of brass
or stainless steel. The choice of material
follows the same guidelines as the choice
of tubing. Generally, it is not recommended
that the materials be interchanged. If
stainless steel tubing were chosen due
to purity considerations, then a stainless
steel regulator should be chosen for the
same reasons. Steel regulators are more
expensive, which is why Agilent offers
brass regulators for less demanding
applications.
Description
Part No.
Price
5183-4641
$275
5183-4642
$275
5183-4643
$275
5183-4644
$275
5183-4645
$275
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
0100-0118
$ 14
0100-0119
$ 15
www.agilent.com/chem
12
GAS MANAGEMENT
Tubing
When constructing or maintaining a gas
delivery system for GC, choosing the
proper tubing material is very important
and will help to eliminate potential
problems and improve the overall quality of
the gas system. Although there are many
common tubing materials available, some
pose safety or cleanliness problems.
Diameter
(inches)
Recommended
Max. Length (feet)
Pressure Drop
(psig)
Copper
1/8*
50
Copper
1/4*
300
0.5
Cleaning Tubing
Before any tubing is placed into service,
or if it becomes contaminated with use,
it is essential that it be properly cleaned.
Unclean or improperly cleaned tubing can
lead to contamination of the system with
disastrous results.
Cleaning tubing requires the use of
suitable detergents and solvents along
with nitrogen and a purgeable oven for
drying. This may be done easily for small
lengths of tubing, but in larger systems the
cleaning procedure sometimes becomes
unwieldy, leaving behind a large quantity
of solvent requiring proper disposal.
Fortunately, Agilent provides clean, high
quality GC grade tubing for large systems
as an economical alternative.
TubingPrecleaned
Description
Part No.
Price
5180-4196
$56
5021-7107
$28
MAINTENANCE MINDER
Always replace cylinders at around 500 psi, to reduce the risk of having
a drastic pressure drop right in the middle of an important analysis.
13
www.agilent.com/chem
GAS MANAGEMENT
Description
Part No.
Price
SL-8
$496
SL-4
$496
Part No.
Price
5183-1941
$ 60
Cylinder Bracket
Description
Cylinder wall bracket with strap and chain
(cylinder size up to 14 in., 35 cm)
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
and easy detection and measurement of
Part No.
Price
Leak detector includes probe, extended flexible probe, range extension nozzle,
probe clip and template, cable, AC power adapter/battery charger, battery, user
manual, cleaning wipe, and carrying case (available in 115 V or 220 V).
Gas leak detector, 115 V
5182-9646
$1915
5182-9648
$1915
www.agilent.com/chem
14
GAS MANAGEMENT
Flow Rates
Setting and maintaining GC flow rates
greatly affect the instrument accuracy
and sensitivity. During maintenance,
verify carrier and support gas flows
with the proper flowmeter. Choosing a
flowmeter for your application depends
upon measurement speed, ease of use,
accuracy, and flow rate range.
Selecting a Flowmeter
Agilent manufactures the largest selection
of volumetric and mass flowmeters for
chromatography. We have developed
flowmeters for measuring capillary column
flows, calibrating air pumps and flow
controllers, and verifying instrument gas
flows. All flowmeters are calibrated to
NIST-traceable standards.
FlowTracker 2000
Part No.
Price
5183-4779
$ 816
5183-4780
$1143
$ 43
ADM 2000
Accuracy 3%
15
www.agilent.com/chem
GAS MANAGEMENT
Flowmeters
Flow Rate (mL/min)
Low
High
Description
Gases
Measured
Accuracy
(%)
Power
Supply
RS-232 Data
Output
Part No.
Price
220-1170
$620
0.5
1000
All
9V Battery
None
ADM2000
0.5
1000
All
Yes
220-1171-U
$725
ADM2000E
0.5
1000
All
Yes
220-1171-E
$725
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
$681
Veri-Flow 500
(220 V)
5.0
500
Rechargeable Battery
or 220 VAC
Yes
HVF-500-2
$681
0.1
50
All
+/- 3
9V Battery
None
HFM-420
$573
Optiflow 570
0.5
700
All
+/- 3
9V Battery
None
HFM-570
$573
Optiflow 650
5.0
5,000
All
+/- 2
9V Battery
None
HFM-650
$677
Veri-Flow 500
Optiflow 420
www.agilent.com/chem
16
Sample
Introduction
Gas
Management
Consumables &
GC Inlets
CATALOG
For a complete selection of vials, syringes, and inlets, see Agilents
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
18
Sample Introduction
Vials
Vial Filling
Vial Options
1 mL
50 L
3.6 mm*
100 L vial
*Needle position based on standard sampling depth.
19
www.agilent.com/chem
Red Rubber/Teflon
Determining Your Quantity Needs
To determine potential septa ordering
quantities, consider:
the number of samples run during a
day/week
Silicone/Teflon
Excellent resealing
Resists coring
Good for multiple injections
Unattended autosampler
runs require a precise fit for
uninterrupted operation.
Typically, automated sample
runs use a higher quality and
quantity of vials.
Teflon/Silicone/Teflon
Used in trace analysis applications
Above average resealing
Most resistant to coring
Least evaporation
Use with large diameter, blunt tip
syringe needles
Teflon Disc
Good for MS and ECD analysis
Good for large-volume injections
Chemically inert
No resealing
Single injection
No long-term sampling storage
Viton
Chlorinated solvents
Organic acids
Limited resealing
Not suitable for 32 gauge syringe
www.agilent.com/chem
Routine analysis
Moderate resealing
Excellent chemical inertness
Not recommended for multiple
injections or storage of samples
Least expensive
Vials
Description
Quantity
Part No.
Price
500/pk
5181-3400
$115
500/pk
5182-0732
$183
500/pk
5182-0547
$154
100/pk
5181-1270
$ 88
5183-2087
$ 57
100/pk
9301-0977
$158
100/pk
5184-3551
$ 69
100/pk
5182-3454
$109
Vials
20
Syringes
Selecting Syringes
Needle Gauge
Column Type
Packed, split or
splitless (including PTV)
any
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
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.
21
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
www.agilent.com/chem
22
Syringe Tips
Make sure to input the proper syringe
size when setting up the injection section
of your data handling device.
Rinse syringes and clean their plungers
before use to maximize syringe lifetime.
Rinse the syringe 5-8 times between
injections to minimize sample carryover.
Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
VIDEO
To view a video on syringe installation,
visit www.agilent.com/chem/techsupport.
23
www.agilent.com/chem
Problem
Possible Cause(s)
Suggested Action(s)
Bent needles
Blocked needles
Rust
Note: even minor rust can cause the plunger
to become stuck in the barrel.
www.agilent.com/chem
24
Gauge/Length
Quantity
Part No.
Price
Tapered
Fixed Needle
23-26s/42
6/pk
5181-3360
$198
5 L
Tapered
Fixed Needle
23-26s/42
6/pk
5181-8810
$303
10 L
Straight
Fixed Needle
23/42
6/pk
9301-0725
$191
5 L
Straight
Fixed Needle
23/42
6/pk
5182-0875
$292
Unit
Part No.
Price
144/pk
9301 0723
$ 64
Gold Standard GC
ALS Syringe Features
144/pk
9301-1031
$ 21
12/pk
07673-40180
$ 19
25/pk
5182-0551
$ 26
07673-20570
$ 13
18596-40015
$ 75
25
07673-60840
$755
www.agilent.com/chem
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.
www.agilent.com/chem
Flashback
The negative side of low inlet volume,
however, means that excessively large
sample injections will easily exceed the
capacity of the liner and will flash back into
gas supply lines and onto the septum. This
can cause several maladies, including
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.
Leaks
Since packed-column inlets are usually
flow-controlled, septum and column leaks
will have a direct impact on retention times
and peak areas. Sample can be lost
through the leak holes, and air can diffuse
back into the inlet to cause column
degradation. Change the septum on a
regular basis and check column
connections at the first stage of problems.
To prevent stationary phase decomposition,
make sure that the oven and inlet are at
room temperature when not in use and
when changing the septum.
26
Description
Septum nut
Unit
Part No.
Price
18740-60835
$ 37
1
2
3
4
50/pk
5183-4757
$ 67
19243-80570
$132
Viton O-rings
12/pk
5080-8898
$ 12
25/pk
5080-8732
$ 37
5/pk
5181-3382
$ 14
10/pk
5080-8774
$ 42
10/pk
5180-4105
$ 13
Liner
19244-80540
$119
19243-80530
$ 99
19243-80540
$141
Upper insulation
19243-00067
$ 5
10
19234-60720
$ 54
11
5181-8830
$ 25
2/pk
1/4
Vespel/
1/4 in.
in. Vespel/
graphite
ferrule
graphite ferrule
1/4
nut
1/4 in.
in. nut
Inside ofof
Inside
OvenOven
For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
* For Model 6890/6850 only
1/8 in.
1/8
in.oror1/4
1/4in.in.
stainless steel
linerliner
stainless
steel
9
10
11
Unit
Part No.
Price
19243-60570
$100
19243-80510
$ 88
19243-80520
$128
19243-60505
$ 70
5180-4105
$ 13
27
10/pk
www.agilent.com/chem
Split/Splitless Inlets
The combined split/splitless inlet is the
most popular inlet for capillary column gas
chromatography. Because it can be used in
either split or splitless mode, it provides a
very effective combination that can cover
most analysis requirements.
Split Mode
Split injection is an effective way to
introduce small amounts of sample without
overloading the column. Split injection is
required for samples that:
cannot be diluted for analysis (for
example, solvents)
Troubleshooting
Split inlets are spared from most bandbroadening phenomena, since narrow
peaks are generated as part of the splitting
process. Therefore, any peak broadening
or tailing observed with split injection is
usually due to improper column
installation, low split flow, (<20 mL/min
on 6890) or low inlet temperature. If you
suspect that the inlet temperature may be
too low, increase it by 50C and compare
the results to the lower temperature
analysis. Repeat if results are positive
until no further improvement is seen.
Selection/Setting
Rationale
Inlet temperature
Try 250C or BP of
last eluting compound
Inlet liner
Minimizes flashback
Minimizes degradation
Inlet packing
Retains non-volatiles
Minimizes inlet discrimination
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
www.agilent.com/chem
28
Selection/Setting
Rationale
Inlet temperature
Inlet liner
Inlet packing
None
0.5-2 L liquid
Injection volume
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
20-80 sec
Oven temperature
Column flow
Splitless Mode
For splitless injection, a conventional split
injector is operated in a nonsplitting mode
by closing the split valve during injection.
The sample is flash-vaporized in the liner,
and sample vapors are carried into the
column by the carrier gas where they are
recondensed at temperatures below the
boiling point of the solvent. After most of
the sample has been transferred into the
column, vapors remaining in the liner are
cleared by opening the split vent which
remains open for the duration of the run.
The most important benefit of splitless
injection is that a majority of the injected
sample is introduced into the column. This
results in much higher sensitivity than that
achieved using split injection.
Solvent Effect
One requirement of splitless injections is
that the initial column temperature should
be kept at least 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.
Additionally, use a solvent that is similar in
polarity to the column stationary phase,
and avoid mixed solvents. Breaking these
rules may result in split peaks.
Splitless injection is routinely used in
areas such as:
environmental analysis
Septum purge
2-3mL/min
Reduces ghosting
Quantification
Internal standard
Standard addition
Maximizes reproducibility
Use only with constant
injection volume
drug screening
1-3m, deactivated
(1-2m per L injected)
Retention gap
VIDEO
To view a video on liner and gold seal replacement, visit
www.agilent.com/chem/techsupport.
29
www.agilent.com/chem
Troubleshooting
Most problems encountered with splitless
injection are related to incorrect purge
time, degradation, improper focusing, and
flashback.
Appropriate initial column temperature is
critical. Sample vapors can be lost through
the septum purge line if the insert is
overfilled with sample vapor (either too
large injection volume or too small liner
volume), leading to irreproducibility and
nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
volume carefully to avoid backflash.
Decomposition
Loss of peak area or generation of new
peaks, can sometimes be dramatically
reduced by changing liner type or by
deactivating the liner and inlet with
silanizing reagents. Removing or reducing
the amount of liner packing can also
decrease inlet activity.
1
2
3
4
6
Description
Unit
Price
$ 39
18740-60835
Septa
See page 36
Insert Weldment
G1544-60575
Liner O-ring
See page 52
Liner
See page 47
G1544-80550
$128
G1544-20590
19251-20620
$ 26
$ 31
SS seal
Gold-plated seal
18740-20880
18740-20885
$ 26
$ 33
5061-5869
$ 8
12/pk
$216
10
Reducing nut
18740-20800
$ 34
11
Insulation (requires 3)
19243-00067
$ 5
12
19243-00070
$ 15
13
Ferrule
14
2/pk
5181-8830
$ 26
2/pk
5183-4732
$ 47
19251-00100
$ 29
Part No.
* For a complete parts breakdown, see the 6890/6850 Series GC Instrument User and/or Service Manuals.
8
9
10
13
14
www.agilent.com/chem
30
Advantages:
elimination of sample discrimination
elimination of sample alteration
solvent focusing of early eluting solutes
high analytical precision
Limitations:
maximum sample volumes are smaller compared
with other inlets (0.5 L to 2.0 L)
solute peaks eluting just before the solvent
cannot be focused and are difficult to determine
capillary columns (especially those with a large
phase ratio or small inner diameter) can be easily
overloaded with sample
parameters such as initial column temperature,
solvent nature, and injection rate must often be
optimized
Selection/Setting
Rationale
Injection volume
0.1-2.0 L liquid
Injection technique
Fast autoinjection
Fused silica needle
Oven temperature
Prevents backflash
Column flow
50-80cm/sec
30-50cm/sec
Septum purge
12-15mL/min
Quantification
All methods
1-3m, deactivated
31
www.agilent.com/chem
Sample Considerations
Troubleshooting
The major problems found with cool oncolumn injection are associated with
column overload, solvent/stationary phase
incompatibility, and column contamination.
Unit
Part No.
Price
Column nut
2/pk
5181-8830
$ 26
10/pk
5181-3323
$ 55
10/pk
5062-3514
$ 51
160-2255-5
$ 39
160-2325-5
$ 42
160-2535-5
$ 59
5181-3396
$ 94
5/pk
VIDEO
To view a video on cool on-column installation and septum replacement,
visit www.agilent.com/chem/techsupport.
www.agilent.com/chem
32
Unit
Part No.
Price
1a
Manual injection
1c
1d
Duckbill septum
Fused silica syringe needles
19320-80625
$175
10/pk
19245-40050
$ 29
6/pk
19091-63000
$ 41
9301-0658
$ 90
19245-60760
$ 9
19245-20510
$ 89
19245-20515
$114
19245-20525
$ 78
19245-20580
$ 55
19245-20780
$ 54
Ferrule
5080-8853
$ 47
Column nut
5181-8830
$ 26
1b
2
3
1c
1d
Common Supplies
3
Spring
2/pk
5
6
19245-80521
$ 62
1b
G1545-80520
$ 63
5183-4760
5183-4758
$ 62
$ 72
50/pk
50/pk
19245-80520
$ 91
1b
19245-20670
$ 35
* For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
33
www.agilent.com/chem
Selection/Setting
Rationale
Injection mode
Cold split
Cold splitless
Inlet temperature
ramp rate
Advantages
no syringe-needle discrimination
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
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
1
3
Description
Column ID Unit
Part No.
Price
Septumless head
G2617-60507
$2661
Septum head
G2618-80500
$1078
Septum nut
18740-60835
$ 39
G2617-60506
$4850
G2617-60508
$ 544
G2619-60501
$ 473
Silver seal
5182-9763
$ 62
0.20 mm
5182-9754
$ 173
0.25-0.33 mm
5182-9761
$ 152
5, 6
0.53 mm
5182-9762
$ 146
7
8
5/pk
Ferrules for
0.20 mm
10/pk
5182-9756
$ 158
Graphpak inlet
0.25 mm
10/pk
5182-9768
$ 166
0.32 mm
10/pk
5182-9769
$ 166
0.53 mm
10/pk
5182-9770
$ 146
10
5062-3525
$ 159
11
G2617-20510
$ 61
G2617-60510
$ 53
5182-9748
$ 137
Kalrez seal
5182-9759
$ 110
Valve body
5182-9757
$ 91
Pressure spring
5182-9758
5182-9775
$ 24
Sealing element
5182-9760
$ 73
3150-0602
$ 137
5182-9747
$ 224
5182-9749
$ 143
G2617-80540
$ 208
9
10
11
Viton seal
5/pk
Item
PTV Liners
35
Description
Part No.
Price
5183-2038
$ 25
5183-2036
$ 20
5183-2037
$ 29
5183-2041
$ 55
www.agilent.com/chem
Septa
One of the key components of sample
introduction is the inlet septum. All
columns must have carrier gas head
pressure to establish flow through the
column. Septa maintain the leak-free seal
and exclude air from the inlet. They come
in many different sizes and are made from
many different types of material specific
to inlet type and analysis needs.
Why Replace
www.agilent.com/chem
36
Septa Troubleshooting
Symptom
Possible Cause
Remedy
Extra Peaks/Humps
Septum bleed.
Normal
Problem
Normal
Problem
Problem
(flow increase)
(flow decrease)
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
But Agilents 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.
www.agilent.com/chem
38
100 autoinjections
700 autoinjections
Agilent BTO Septa With CenterGuide: Very Little Coring Even After
700 Autoinjections
39
BLEED
LIFETIME
TEMPERATURE
LIMIT
(optimized for
high temperature)
to 400C
to 350C
to 350C
= very good
= good
www.agilent.com/chem
p/n 5183-4757
p/n 5183-4761
p/n 5183-4759
www.agilent.com/chem
40
Price
5183-4757
5183-4757-100
5183-4758
$72
$134
$72
5183-4759
5183-4759-100
5183-4760
$62
$107
$62
5183-4761
5183-4761-100
5183-4762
$84
$150
$84
5080-8896-50
5080-8894-100
5080-8728-50
5080-8728-100
$52
$93
$52
$93
5181-1263-50
5181-1263-100
5181-3383-50
$52
$93
$52
5181-3383-100
$93
5181-1283-50
5181-1283-100
5181-1260
$52
$93
$29
5181-1261
$29
41
www.agilent.com/chem
Ferrules
Using the wrong ferrule or a worn-out
ferrule to seal your column connection can
result in inconsistent and unreliable
chromatography. An improper ferrule can
cause leaks which allow air
and other contaminants to enter the
instrument through the column seal,
causing major interference with column
and detector performance. For optimum
performance, ferrules should be replaced
every time the column is replaced and
when performing column maintenance.
Agilent offers a comprehensive selection
of ferrules made of different materials and
configurations for a leak-free connection
between the column and injector.
Three main types of ferrules are used with
capillary GC columns: graphite, Vespel and
Vespel-graphite composites. Graphite
ferrules can withstand temperatures as
high as 450C, and Vespel and Vespelgraphite ferrules are rated to 280C and
350C, respectively.
Advantages
Limitations
Vespel or
Mechanically robust
Vespel-graphite
Long lifetime
Why Replace
Signals that a ferrule is damaged include:
background noise from oxygen diffusing
into the system
column bleed catalyzed by oxygen
sample degradation
loss of sample
increase in detector signal/noise
poor retention time reproducibility
www.agilent.com/chem
42
Ferrule Troubleshooting
Problems possible after changing ferrules
Normal Peaks
Normal Peaks
43
www.agilent.com/chem
Vespel/Graphite
(85%/15%) Ferrules
The combination of graphite and Vespel
results in a ferrule having low oxygen
diffusion rates which does not shrink to
the same extent as pure Vespel. These
ferrules are recommended for use with
GC/MS or other oxygen sensitive
detectors, like the ECD, but are also
compatible with other detectors like FID
and NPDs.
In addition, the Vespel/graphite ferrules
provide added confidence of leak-free
connections when installed correctly.
Proper installation requires a finger-tight
turn on the nut, then an additional 1/4 1/2
turn with a wrench.
These ferrules are very hard and cannot
be deformed sufficiently to seal multiple
column diameters. The ferrule hole must
match the column OD exactly to ensure a
leak-free seal. For capillary column
applications, there is a specific ferrule for
each column diameter. Choosing a ferrule
with a larger hole than is specified for a
given column dimension can result in a
large leak. If left unchecked, an improper
seal at the injector will result in high
column bleed and a shortened column
lifetime. An improper seal at the detector
can result in increased detector
signal/noise. In the case of the MSD it
can also contribute to oxidation of the ion
source which can increase the frequency
of detector maintenance.
5181-8830
Vespel/Graphite Ferrules
5181-3323 (0.1, 0.2, 0.25 mm ID columns)
5062-3514 (0.32 mm)
5062-3512 (0.45 and 0.53 mm)
Vespel/Graphite Ferrules
5062-3508 (0.1, 0.2, and 0.25 mm ID columns)
5062-3506 (0.32 mm)
5062-3538 (0.45 and 0.53 mm)
www.agilent.com/chem
44
VIDEO
Upper
Temperature
Limit
Usages
Limitations
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Graphite
450C
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
350C
General purpose for
Not reusable.
(85%/15%)
capillary columns.
Recommended for
MS or oxygen sensitive
detectors. Most reliable
leak-free connection.
-----------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------Vespel
280C
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
Column Id
(mm)
Quantity
Part No.
Price
10/pk
10/pk
10/pk
10/pk
5080-8853
5080-8773
500-2114
500-2118
$
$
$
$
47
38
26
26
0.1, 0.2
0.1, 0.2, 0.25
0.32
0.45, 0.53
10/pk
10/pk
10/pk
10/pk
5062-3516
5181-3323
5062-3514
5062-3512
$
$
$
$
51
55
51
53
0.1
0.1, 0.2, 0.25
0.32
0.53
10/pk
10/pk
10/pk
10/pk
5062-3507
5062-3508
5062-3506
5062-3538
$
$
$
$
62
62
56
48
10/pk
10/pk
10/pk
5181-3322
5062-3513
5062-3511
$ 55
$ 51
$ 51
10/pk
10/pk
10/pk
5062-3580
5062-3581
5181-3308
$ 79
$ 79
$ 47
0.4
10/pk
5184-3569
$ 87
0.5
10/pk
5184-3570
$ 87
10/pk
5184-3571
$ 85
10/pk
5188-2789
$135
2/pk
1 ea
1 ea
1 ea
2/pk
5181-8830
5020-8293
5020-8292
5020-8294
5183-4732
$
$
$
$
$
1 ea
1 ea
1 ea
05988-20066
05921-21170
8710-0510
$ 13
$ 16
$ 24
0.5
1.0
0.4
0.8
85% Vespel, 15% Graphite Ferrules (Short Ferrules)
0.80.3
0.80.4
0.80.5
0.80.8
Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)
0.3
0.4
0.5
0.8
These ferrules are recommended for use with GC/MS.
0.4
0.5
0.8
These ferrules are recommended for use in isothermal analysis only.
Two Hole
0.4 ID holes
0.5 ID holes
No Hole
SilTite Metal Ferrules
0.8
Column Nuts
Short Nuts
26
18
18
12
47
Long Nuts
www.agilent.com/chem
46
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 manufacturers liners,
Agilent liners are built to Agilents 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
Why Replace
These problems will occur if the liner is not
changed on a regular basis or if the correct
liner is not used:
peak shape degradation
solute discrimination
poor reproducibility
sample decomposition
ghost peaks
reduced column life
VIDEO
47
www.agilent.com/chem
Discussion
of Liner
Characteristics
Liner Volume
The purpose of the injection port is to allow
the introduction of a sample into the gas
chromatograph in an accurate, reproducible
manner. The vaporized sample should be
a true representation of the liquid sample
and, unless specifically desired, should
be injected without chemical change. The
elevated temperatures used in the inlet
vaporize the liquid sample to a gas for
transfer to the head of the column. This
phase transition is accompanied by a very
significant volume change. The volume of
the resulting vapor must be small enough
to fit within the volume of the liner. If the
volume is too great for the liner, it could
result in backflash, or sample loss caused
by expansion into the septum purge or split
vent lines. Both can compromise
reproducibility and sensitivity. Backflash
also frequently results in sample carryover.
Larger volume liners (> 800 L) are
characterized by larger inside diameters
(ID) and are typically used with injection
sizes of 1 L or more. The small volume
liners have a smaller ID and are usually
used with small injection sizes (< 1 L),
fast 100 m ID columns, gas samples, or
when using external sampling devices
like headspace and purge and trap.
Liner Deactivation
Active sites on inlet liners can adsorb
sample components and cause peak tailing,
and potential loss of sensitivity and
reproducibility. Deactivation agents are
used to cover or react with active sites on
the glass surface of the liner. Agilent liners
are deactivated using deactivation
procedures that produce reproducible and
inert liners, with long lifetimes. For splitless
applications or when even slightly polar
compounds must be analyzed, a
deactivated liner should be used.
www.agilent.com/chem
48
Tapers
Tapering or narrowing the liner internal
diameter (ID) is done for a number of
purposes:
Bottom taper focuses sample onto the
head of the column
Bottom taper minimizes contact with
metal parts of the inlet
Center taper positions glass wool
correctly
Top taper minimizes sample backflash
To operate properly, the column must be
installed correctly in the injection port with
the tip of the column ideally located about
halfway into the taper, or about 4-6 mm
from the column tip to the top of the ferrule
(See Figure 1). Some applications will work
better with different column installation
depths. Therefore, you should check the
instrument manual for proper installation
distances and determine which distance is
appropriate for your application.
Reproducible positioning is important
for repeatable quantitative results.
49
Packing
Glass Wool
Glass Cups
Figure 1.
www.agilent.com/chem
Liner Troubleshooting
Symptom
Possible Cause
Remedy
Tailing Peaks
Sample decomposing.
Normal
Problem
Normal
Problem
Problem
Normal
Problem
Problem
Unresolved Peaks
Normal
www.agilent.com/chem
Problem
Problem
50
Agilent Liners
Our engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Intensive liner
development and testing have resulted in a set of liners that we recommend whenever new methods are being developed, when
methods are being optimized, or when problems with existing methods are encountered. These liners are:
Direct injection:
Straight liner without glass wool,
deactivated, Agilent Part No. 5181-8818
(use only for gas samples, headspace, or
purge and trap applications).
Direct Connect
Direct Connect liners are ideal for
customers running highly sensitive
compounds, or for users who require
maximum inertness performance and
minimal inlet discrimination for trace GC
and GC/MS applications. Direct Connect
liners also eliminate sample exposure to
metal parts, minimizing inlet-related
degradation. These liners are included in
our new 8270 EPA Applications kit
designed specifically for optimizing a
6890/5973 GC/MSD to this method.
Split injection:
Agilent low-pressure-drop split liner with
glass wool, bottom taper, glass bead for
easy positioning, and deactivated, Agilent
Part No. 5183-4647 (with extraordinarily
tight dimensional control for optimum
split performance).
Splitless injection:
Single tapered liner without glass wool,
deactivated, Agilent Part No. 5181-3316EN.
Note: For pesticide analysis especially
DDT and Endrin, where breakdown is a
problem we recommend Agilent Part
Nos. 5181-3316EN and 5181-3315EN.
51
Focus Liner
Improve reproducibility, improve results.
The Focus Liner traps a precisely controlled
amount of glass wool in the ideal position
in the injection port liner. At the point of
injection, the glass wool provides extra
surface area for vaporization, traps
nonvolatile sample residue, and wipes
any residual sample from the sample
needle reproducibility is the result.
In addition to these liners we offer a
broad selection of liners for your specific
application needs.
Liner O-Rings
Liners are sealed in the inlet with O-rings
or graphite seals. O-ring seals are easier to
remove and to replace than graphite that
deforms and flakes apart. The graphite
seals should be used when inlet
temperatures exceed 350C.
www.agilent.com/chem
VIDEO
Description
Part No.
Price
5188-2717
$514
5188-2741
$19
www.agilent.com/chem
52
Liner
Volume(l)
Single
Liner
870
5183-4647
$35
5183-4701
$157
5183-4702
$700
900
5181-3316
$29
5183-4695
$124
5183-4696
$533
900
5181-3316EN
$32
250
5181-8818
$24
5183-4703
$95
5183-4704
$414
For split/splitless
injection
870
5183-4711
$27
5183-4712
$112
5183-4713
$476
900
5062-3587
$30
5183-4693
$129
5183-4694
$560
800
5181-3315
$36
5183-4705
$163
5183-4706
$751
800
5181-3315EN
$43
250
18740-80220
$28
5183-4707
$124
5183-4708
$533
140
18740-80200
$17
5183-4709
$73
5183-4710
$308
990
$19
210-3003
$84
210-3003-5
5/pk
25/pk
990
19251-60540
$19
5183-4691
$78
5183-4692
$336
800
18740-80190
$40
5183-4699
$179
5183-4700
$784
800
18740-60840
$43
5183-4697
$191
5183-4698
$840
Price
$62
$62
Dimensions
6.3 mm X 78.5 mm
6.3 mm X 78.5 mm
Part No.
210-4004-5
210-4022-5
Price
$98
$108
Liner O-Rings
Fluorocarbon O-ring (12/pk)
Graphite O-ring for splitless liner (10/pk)
Graphite O-ring for split liner (10/pk)
Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk)
Part No.
5180-4182
5180-4173
5180-4168
Price
$13
$52
$52
5188-2741 $19
53
ID
4.0 mm
4.0 mm
Wool
Yes
Yes
www.agilent.com/chem
Septum Nut
Part No. 18740-60835
Heater-Sensor Assembly
Part No. G1544-61140
Retaining Nut
Part No. G1544-20590
Washer
Part No. 5061-5869, 12/pk
Reducing Nut
Part No. 18740-20800,
1 each
www.agilent.com/chem
54
Part No.
Price
19251-60575
G1544-60575
G1544-80580
$230
$216
$73
G1544-60585
$330
G1580-60575
$261
G1580-60585
$236
18740-20880
18740-20885
5182-9652
5061-5869
$39
$106
$31
$35
$26
$33
$40
$8
Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity. Other manufacturers seals are not
machined, and may compromise your results.
Top
55
Bottom
Gold-plated seal with cross p/n 5182-9652
Use when inlet flow exceeds 400 ml/min.
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 non-volatile and semi-volatile
contamination, as well as appropriate
recovery measures.
CATALOG
For a complete selection of GC columns and parts, see Agilents 20052006 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
simple, the frequency and type of
column maintenance that is required
varies due to many system and sample
factors. Instead of simply following a
Primary
Quantion
is hidden
Primary
Quantion
is enhanced
57
Dimensions
All dimensions can be used with
conventional GC systems. Many types of GC
column phases can be used with the MSD,
but there are some dimensional
considerations. The maximum allowable
flow rate and optimal sensitivity flow rates
will vary depending upon the type of pump.
In general, the column flow should be
1mL/min (2mL/min for Performance Turbo
Pumps). Therefore, column length
and internal diameter combinations are
restricted to provide the appropriate flow
to the GC/MS.
Narrow-bore columns (0.25mm i.d. and
smaller) can be installed directly into the
GC interface.
www.agilent.com/chem
COLUMNS
Description
Part No.
Price
122-0132
$483
19091S-433
$483
122-1232
$483
122-3832
$483
19091N-133
$413
www.agilent.com/chem
58
COLUMNS
Bad
Good
Description
Part No.
Price
5181-8836
$ 15
20x Magnifier
430-1020
$ 42
5080-8853
$ 47
5080-8773
$ 38
5182-9646
5182-9648
$1859
$1859
Prevention
Recovery
Description
Part No.
Price
$ 50
Quartz deactivated
column connector
(5/pk)
5181-3396 $ 94
Polyimide Sealing
resin (5 grams) 500-1200
$ 24
59
www.agilent.com/chem
COLUMNS
Thermal Damage
Exceeding a columns upper temperature
limit results in accelerated degradation of
the stationary phase and tubing surface.
This results in the premature onset of
excessive column bleed, peak tailing for
active compounds and/or loss of efficiency
(resolution).
Prevention
Do not exceed the columns specified
upper temperature limits:
Isothermal limit: temperature that
the column can be held at for an
indefinite time
Programmed limit: maximum column
temperature; column should only be
held there for about 5-10 minutes
Set the GC maximum oven temperature
function at or a few degrees above the
temperature limit of the column. With
two columns in the oven be sure to set
the maximum temperature to the
temperature limit of the column with the
lowest value.
Recovery
Disconnect column from detector
Heat the column 8-16 hours at the
isothermal limit
Remove 10-15 cm from the column end
Reinstall into the detector and condition
as usual
NOTE: Thermal damage cannot be reversed.
The column usually does not return to its
original performance; however, it is often
still functional. The life of the column will
be reduced after thermal damage.
Oxygen Damage
Oxygen is an enemy to all capillary GC
columns. Constant exposure to oxygen
does not damage the column at or near
ambient temperatures; however, severe
damage occurs as the column temperature
increases. A leak in the carrier gas flow
path (e.g., gas lines, fittings, injector,
septa) is the most common source of
oxygen exposure. As the column is heated,
very rapid degradation of the stationary
phase occurs. This results in the premature
onset of excessive column bleed, peak
tailing for active compounds and/or loss of
efficiency (resolution).
Description
Part No.
Price
5183-4780
$1143
BOT-2
$ 235
BMT-2
$ 235
RMSH-2
$ 261
5183-4759
$ 62
Prevention
Maintain an oxygen and leak-free
system by:
performing periodic leak checks
changing septa regularly
using high quality carrier gases
installing and maintaining oxygen traps
changing gas cylinders before they are
completely empty
Recovery
Perform column bakeout as described
under thermal damage recovery.
NOTE: Oxygen damage occurs very rapidly.
In less severe cases, the column may still
be functional but at a reduced performance
level. In more severe cases, the column is
irreversibly damaged.
www.agilent.com/chem
60
COLUMNS
Chemical Damage
GUARD COLUMN
Prevention
Perform sample preparation to remove
inorganic acids and bases from the
sample
Install guard column and trim frequently
If acids or bases must be used choose an
organic alternative or HCl or NH4OH
Guard Column
INJECTOR
DETECTOR
Recovery
Remove 0.5 to 1 meter from the front
of the column
Severe cases may require the removal
of 5 or more meters
Column
Guard Column
Column Contamination
Column contamination is the most
common problem encountered in capillary
GC. Unfortunately, it mimics most other
chromatographic problems and is often
misdiagnosed. A contaminated column
is usually not damaged, but it may be
rendered unusable. There are two basic
types of contaminants: nonvolatile and
semivolatile.
61
Union
www.agilent.com/chem
COLUMNS
Nonvolatile Contaminants
Description
Part No.
Price
5183-4712
$112
5183-4695
$124
5181-3396
$ 94
500-1200
$ 24
160-2535-10
$110
160-2255-10
$ 73
430-3000
$ 78
Prevention
Recovery
Do not bakeout the column
Front End Maintenance:
Clean or change the injection port liner
Clean out the injector
Cut off typically 0.5 to 1 meter of the
front of the column
Turn the column around (install detector
end into injector). Not recommended for
sensitive ECD, NPD, and MS detectors.
Solvent rinse the column
Cut the column in half and use the back
half (detector side)
Semivolatile Contaminants
Semivolatile contaminants or residues
accumulate in the column, but eventually
elute. Hours to days may elapse before
they completely leave the column. Like
nonvolatile residues, they may cause peak
shape and size problems and, in addition,
are usually responsible for many baseline
problems (instability, wander, drift, ghost
peaks, etc.).
Prevention
Column Storage
Recovery
Bakeout the column: limit 1-2 hours
(excess baking may polymerize some
contamination and reduce column
lifetime)
Solvent rinse the column
www.agilent.com/chem
62
COLUMNS
DB-1ms
100% Dimethylpolysiloxane
Identical selectivity to DB-1
Nonpolar
Very low bleed characteristics
Improved acid performance compared to
standard 100% Dimethylpolysiloxane
columns
Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
Excellent general purpose column
Bonded and cross-linked
Solvent rinsable
63
Length
Film
Part No.
Price
0.10
0.10
0.10
0.10
10
10
20
20
0.10
0.40
0.10
0.40
127-0112
127-0113
127-0122
127-0123
$343
$343
$495
$495
0.20
0.20
12
25
0.33
0.33
128-0112
128-0122
$261
$400
0.25
0.25
0.25
30
30
60
0.10
0.25
0.25
122-0131
122-0132
122-0162
$483
$483
$823
0.32
0.32
0.32
30
30
60
0.10
0.25
0.25
123-0131
123-0132
123-0162
$521
$521
$896
Similar Phases
Applications
www.agilent.com/chem
COLUMNS
DB-5ms
HP-5ms
I.D.
Length
Film
Part No.
Price
0.18
0.18
20
40
0.18
0.18
121-5522
121-5542
$412
$740
0.20
0.20
25
50
0.33
0.33
128-5522
128-5552
$400
$674
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
25
25
30
30
30
50
60
60
0.25
0.40
0.10
0.25
0.50
0.25
0.10
0.25
122-5522
122-552A
122-5531
122-5532
122-5536
122-5552
122-5561
122-5562
$421
$421
$483
$483
$483
$753
$823
$823
0.32
0.32
0.32
0.32
0.32
0.32
30
30
30
50
60
60
0.10
0.25
0.50
0.25
0.10
0.25
123-5531
123-5532
123-5536
123-5552
123-5561
123-5562
$521
$521
$521
$804
$896
$896
Similar Phases
Applications
(5%-Phenyl)-methylpolysiloxane
Nonpolar
Very low bleed characteristics
Excellent inertness for active compounds
Improved signal-to-noise ratio for better
sensitivity and mass spectral integrity
Bonded and cross-linked
Solvent rinsable
Certified for MS
Equivalent to USP Phase G27
Similar Phases
Rtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms,
BPX-5, Rtx-5 Amine
Applications
Semivolatiles, alkaloids, drugs, FAMEs,
halogenated compounds, pesticides,
herbicides
I.D.
Length
Film
Part No.
Price
0.20
0.20
0.20
12
25
50
0.33
0.33
0.33
19091S-101
19091S-102
19091S-105
$261
$400
$674
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
15
15
15
30
30
30
60
60
0.10
0.25
1.00
0.10
0.25
0.50
0.10
0.25
19091S-331
19091S-431
19091S-231
19091S-333
19091S-433*
19091S-133
19091S-336
19091S-436
$295
$295
$295
$483
$483
$483
$823
$823
0.32
0.32
0.32
0.32
0.32
0.32
0.32
15
25
30
30
30
60
60
1.00
0.52
0.10
0.25
0.50
0.10
0.25
19091S-211
19091S-112
19091S-313
19091S-413
19091S-113
19091S-316
19091S-416
$319
$448
$521
$521
$521
$896
$896
www.agilent.com/chem
64
COLUMNS
DB-XLB
Exceptionally low bleed
Low polarity
Extended temperature limit of 360C
Unique selectivity
Excellent inertness for active compounds
Ideal for confirmational analyses
Excellent for pesticides, herbicides, PCBs
and PAHs
Certified for MS
Bonded and cross-linked
Solvent rinsable
DB-35ms
Equivalent to a (35%-Phenyl)methylpolysiloxane
Midpolarity
Very low bleed characteristics
Extended temperature limit of 360C
Excellent inertness for active compounds
Certified for MS
Ideal for confirmational analyses
Bonded and cross-linked
Solvent rinsable
Replaces HP-35ms
Close equivalent to USP Phase G42
65
Length
Film
Part No.
Price
0.18
0.18
20
30
0.18
0.18
121-1222
121-1232
$412
$579
0.20
0.20
12
25
0.33
0.33
128-1212
128-1222
$261
$400
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
15
15
15
30
30
30
30
60
0.10
0.25
1.00
0.10
0.25
0.50
1.00
0.25
122-1211
122-1212
122-1213
122-1231
122-1232
122-1236
122-1233
122-1262
$295
$295
$295
$483
$483
$483
$483
$823
0.32
0.32
0.32
0.32
30
30
30
60
0.10
0.25
0.50
0.25
123-1231
123-1232
123-1236
123-1262
$521
$521
$521
$896
Similar Phase
Applications
MDN-12
Length
Film
Part No.
Price
0.20
0.20
15
25
0.33
0.33
128-3812
128-3822
$261
$400
0.25
0.25
0.25
0.25
15
30
30
60
0.25
0.15
0.25
0.25
122-3812
122-3831
122-3832
122-3862
$295
$483
$483
$823
0.32
0.32
30
60
0.25
0.25
123-3832
123-3862
$521
$896
Similar Phases
Applications
www.agilent.com/chem
COLUMNS
DB-17ms
Equivalent to (50%-Phenyl)methylpolysiloxane
320/340C Upper temperature limit
Very low bleed midpolarity column
Excellent inertness for active compounds
Enhanced mass spectral integrity
Bonded and cross-linked
Solvent rinsable
Best column for CLP pesticides
DB-225ms
I.D.
Length
Film
Part No.
Price
0.18
20
0.18
121-4722
$412
0.25
0.25
0.25
0.25
0.25
15
15
30
30
60
0.15
0.25
0.15
0.25
0.25
122-4711
122-4712
122-4731
122-4732
122-4762
$295
$295
$483
$483
$823
0.32
0.32
30
30
0.15
0.25
123-4731
123-4732
$521
$521
Similar Phases
Applications
Equivalent to (50%-Cyanopropylphenyl)methylpolysiloxane
Mid/high polarity
Excellent for separations of cis- and
trans-fatty acid methyl esters (FAMEs)
Low bleed
Bonded and cross-linked
Solvent rinsable
Close equivalent to USP Phase G7
I.D.
Length
Film
Part No.
Price
0.25
0.25
0.25
15
30
60
0.25
0.25
0.25
122-2912
122-2932
122-2962
$295
$483
$823
0.32
30
0.25
123-2932
$521
Similar Phases
Applications
www.agilent.com/chem
66
COLUMNS
HP-INNOWax
Polyethylene glycol (PEG)
High polarity
Highest upper-temperature limits of the
bonded PEG phases
Column-to-column repeatability
Bonded and cross-linked
Solvent rinsable
Close equivalent to USP Phase G16
GS-GasPro
Unique bonded PLOT column technology
Excellent choice for light hydrocarbons
and sulfur gases
Retention stability not affected by water
Separates CO and CO2 on a single
column
Ideal PLOT column for GC/MS
no particles
67
Length
Film
Part No.
Price
0.20
0.20
0.20
0.20
25
25
50
50
0.20
0.40
0.20
0.40
19091N-102
19091N-202
19091N-105
19091N-205
$379
$379
$636
$636
0.25
0.25
0.25
0.25
0.25
0.25
30
30
30
60
60
60
0.15
0.25
0.50
0.15
0.25
0.50
19091N-033
19091N-133
19091N-233
19091N-036
19091N-136
19091N-236
$413
$413
$413
$737
$737
$737
0.32
0.32
0.32
0.32
0.32
0.32
30
30
30
60
60
60
0.15
0.25
0.50
0.15
0.25
0.50
19091N-013
19091N-113
19091N-213
19091N-016
19091N-116
19091N-216
$447
$447
$447
$816
$816
$816
Similar Phases
Applications
Length
Part No.
Price
0.32
0.32
30
60
113-4332
113-4362
$627
$942
Similar Phase
Applications
CP-Silica PLOT
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.
CATALOG
For a complete selection of Detector supplies, see Agilents 2005-2006
Essential Chromatography Catalog. Or, visit our online catalog at
www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
68
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
If the flame goes out or will not light:
Check the column flow rate. It may
be too high. Decrease the flow rate or
pressure. Switch to a more restrictive
column (longer or with a smaller id).
If you must use a large id column, first
cool the GC oven to below 50C, then turn
off the carrier flow long enough to allow
the FID to light. Check for partially or
completely plugged jet.
Check that the right type of jet is installed
for the column you are using.
Injecting large volumes of aromatic
solvent or water can cause the flame to
go out. Switch to a nonaromatic solvent
or inject less solvent.
The lit offset value may be too low or too
high. Adjust the value.
FID Ferrules
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
Item Description
Unit
Part No.
Price
19231-21050
$ 14
Collector nut
19231-20940
$ 35
Spring washer
5181-3311
$ 9
Ignitor castle
19231-20910
$ 57
19231-21060
$184
19231-60680
$ 42
Collector insulator
G1531-20700
$ 17
Collector body
Hastelloy Collector Body
G1531-20690
61531-21090
$ 60
$260
G1531-60690
$194
G1531-20700
$ 17
8710-1346
$ 8
10/pk
2/pk
Collector Housing
G1531-20740
$175
19301-00150
$ 8
8710-1561
$ 13
5182-3450
18710-20119
18710-60170
19231-60680
19244-80560
19301-60660
5180-4150
5180-4152
19301-20720
5180-4153
9301-0985
$556
$ 49
$ 44
$ 42
$ 56
$ 53
$ 23
$ 23
$ 12
$ 8
$ 41
3 each
2 each
2 each
3 each
2 each
1/pk
5 each
70
DETECTORS
FID Jets
Description
Length(mm)
Part No.
Price
48
G1531-80560
$43
48
G1531-80620
$54
61.5
19244-80560
$56
63.5
18710-20119
$49
63.5
18789-80070
$55
61.5
19244-80620
$37
Adaptable FID
2
3
FID Consumables
4
Description
Unit
Part No.
Price
19301-60660
$53
G1531-60680
$41
18710-60170
$44
5080-4978
$ 7
19301-20720
$12
O-rings
12/pk
Cleaning wire
Jet cleaning wire for 0.03 in. ID jet
5/pk
5180-4150
$23
Jet cleaning wire for Series 530 mm and 0.018 in. ID jet
5/pk
5180-4152
$23
8
6
7
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
Thermal Cleaning
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 improve
sensitivity, but at a cost of linear range.
Always precondition the column before
connection to the detector.
ECD Warnings
Although beta particles at this energy level have little penetrating power the
surface layer of the skin or a few sheets of paper will stop most of them they
may be hazardous if the isotope is ingested or inhaled. For this reason the cell
must be handled with care. Radioactive leak tests must be performed at the
required intervals, the inlet and outlet fittings must be capped when the detector
is not in use, corrosive chemicals must not be introduced into the detector, and
the effluent from the detector must be vented outside the laboratory environment.
www.agilent.com/chem
72
DETECTORS
Part No.
Price
G1533-80565
$198
19234-60720
$ 58
19233-20625
$ 15
19233-20755
$ 32
18713-60040
$ 46
18713-60050
$ 31
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.
73
www.agilent.com/chem
DETECTORS
Filament Maintenance
The primary maintenance for a TCD
involves the filament. Most procedures
involve improving filament life or keeping
the filament from becoming damaged or
contaminated.
A constant presence of oxygen can
permanently damage filaments through
oxidative processes. The most common
source of oxygen is a leak(s) near the
detector or in the carrier or makeup
gas line fittings. Oxygen traps are
recommended for the carrier and makeup
gases to reduce oxygen levels. Proper
column installation techniques and regular
leak checks (especially after column
installation) help to keep leak problems to
a minimum.
The damage caused by oxygen is more
severe at high filament currents.
Chemically active sample components
such as acids and halogenated compounds
may attack and damage the filaments.
Avoiding these compounds when possible
increases filament life. Turning off or
substantially reducing the filament current
when the TCD is not in use also prolongs
filament life.
Cell Contamination
Unit
Part No.
Price
G1532-60675
$1030
18740-20950
$ 18
18740-20960
$ 33
10/pk
10/pk
5080-8773
$ 38
10/pk
5080-8853
$ 47
2/pk
5181-8830
$ 26
2/pk
5183-4732
$ 47
G1532-20710
$ 44
$ 45
www.agilent.com/chem
19232-80550
$ 126
19302-80020
$ 138
19232-60676
$1625
74
DETECTORS
75
Thermal Cleaning
The TCD can become contaminated with
deposits from such things as column bleed
or dirty samples. A wandering baseline,
increased noise level, or changes in
response on a checkout chromatogram all
indicate contamination. Thermal cleaning,
or bakeout (heating the detector block to
evaporate the contaminant), should be
performed only after you have confirmed
that the carrier gas and the flow system
components are leak-free and
contaminant-free.
www.agilent.com/chem
DETECTORS
www.agilent.com/chem
76
DETECTORS
Unit
Part No.
Price
19256-60700
$ 72
5180-4105
$ 13
10/pk
2
3
Weldment, block
19256-80560
$536
0905-1610
$ 42
Spacer, ignitor
19256-20590
$ 15
19256-60800
$ 68
G1535-60600
$ 22
19256-80045
$ 83
10
19256-80030
$ 38
11
19256-20580
$ 80
12
Coupling, SS
19256-20550
$165
14
Screw, M3 x 12 (4 required)
0515-0911
$ 1
15
Clamp
19256-00090
$ 59
16
5061-5886
$ 24
17
19256-80060
$ 40
18
5061-5891
$ 24
19
Flange adapter
19256-20510
$131
20
Flange ring
19256-00200
$ 22
21
5061-5890
$ 21
19256-80590
$141
19256-80570
$114
19256-60500
$434
5061-5867
$ 17
Liner/ferrule kit
19256-60590
$ 89
Sulfur filter
19256-80000
$378
Phosphorus filter
19256-80010
$378
0905-1609
$ 42
0905-1608
$ 42
5061-5889
$ 19
19305-60580
$ 40
10
11
12
8
13
14
15
16
17
18
12/pk
12/pk
12/pk
12/pk
77
20
21
www.agilent.com/chem
MAINTENANCE MINDER
12/pk
19
DETECTORS
Bead Life
Gas Flow
www.agilent.com/chem
Gas Purity
Because of its high sensitivity, the NPD
requires very pure gases (99.999% or better).
We strongly recommend that moisture and
hydrocarbon traps be used on the carrier
gas and all detector gases, including the
detector hydrogen, air, and makeup gases.
Dirty gases will not only give poor
chromatographic performance, but will
shorten the bead life as well.
78
DETECTORS
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
Part No.
Price
48
G1531-80560
$ 43
61.5
19244-80560
$ 56
63.5
18710-20119
$ 49
Length (mm)
6890/5890 Adaptable
79
www.agilent.com/chem
DETECTORS
Description
Part No.
Price
0515-0655
$ 1
G1534-60570
$368
5183-2007
$379
Lid weldment
G1534-80510
$160
0905-2580
$ 53
G1534-40020
$ 72
Collector funnel
G1534-20530
$ 64
G1534-40030
$ 42
0905-1284
$ 53
Screw, M4 x 10 mm
0515-2495
$ 1
10
J-Clamp
1400-0015
$ 1
11
Screw, M4 x 10 mm
0515-2495
$ 1
12
G1534-60610
$160
13
Mounting pallet
G1531-40020
$ 29
14
15
G1534-80500
$501
G1534-80540
$532
Lid stop
G1534-20590
$ 36
5182-9722
$175
19234-60720
$ 58
19234-60540
$289
5080-8872
$216
19231-60790
$284
16
17
18
9
10
11
12
4
5
6
13
14
15
16
17
18
*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
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.
CATALOG
For a complete selection of gas management supplies, see Agilents
2005-2006 Essential Chromatography Catalog. Or, visit our online
catalog at www.agilent.com/chem/4ecatalog.
www.agilent.com/chem
82
GC/MS SYSTEMS
Every day
Check, and if necessary, replace the
septum. Check the injection port liners.
Check the tightness of the column nuts.
Hint: With Agilents new Flip Top Inlet
Sealing System, you dont 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
WEEK
EVERY
6 MONTHS
EVERY
YEAR
AS
NEEDED
Every year
Replace the diffusion pump fluid.
Recondition or replace internal and external
traps and chemical filters on the GC.
As needed
Monitor
Record all tune values such as electron
multiplier and ion source parameters in
a log book to monitor instrument
performance. In addition note the high
vacuum and foreline vacuum pressures.
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
foreline pump oil
fingerprints inside the manifold
Air Leaks
www.agilent.com/chem
84
GC/MS SYSTEMS
Description
Part No.
Price
05988-20066
$13
05921-21170
$16
5181-8830
$26
The most likely point for an air leak is a seal you recently opened.
Corrective Action
Check interface nut for tightness.
Replace if necessary.
Check leak/test the GC injection port.
Cleaning Solvents
It is common to see cleaning solvent peaks
in the mass spectra shortly after the ion
source is cleaned.
Corrective Action
Dry all cleaned metal parts in the GC
oven before reassembling and reinstalling
them. Refer to specific cleaning
procedures in your MSD Hardware
Manual.
Fingerprints
Fingerprints contain hydrocarbons that can
appear in mass spectra. Hydrocarbon
contamination is characterized by a series
of mass peaks 14 amu apart. The
abundances of these peaks decrease as
peak mass increases. Fingerprint
contamination is usually caused by the
failure to wear lint-free, nylon gloves during
ion source cleaning, GC inlet maintenance,
or from installing the column. Use special
care to avoid recontamination of parts after
you clean them. This typically occurs after
some maintenance or part replacement.
Corrective Action
Reclean using clean, nylon gloves and
proper cleaning techniques.
Description
Part No.
Price
8650-0030
8650-0029
$16
$16
85
Corrective Action
If m/z 446 appears please call Agilent
for assistance.
www.agilent.com/chem
GC/MS SYSTEMS
Corrective Action
Call Agilent for assistance.
Contamination Identification
The following table lists some of the more common contaminants, the ion characteristic of those contaminants, and the likely sources
of those contaminants.
Common Contaminants
Ions (m/z)
Compound
Possible Source
13,14,15,16
Methane
CI gas
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
Dimethylpolysiloxane
149
Plasticizer (phthalates)
Hydrocarbons
www.agilent.com/chem
86
GC/MS SYSTEMS
Symptoms
Corrective Action
Low signal
Air leak
Peak widths
Interfering peaks
Excessive background
Retune
Abnormal spectra
excessive background
contamination
Incorrect tuning
Clean source
Repeatability
Symptoms
Corrective Action
Loose column connections Tighten column nuts on injection port or transfer line
Replace column nuts and ferrule
87
Variations in pressure,
column flow,
and temperature
Clean source
Loose connections
in the analyzer
Ground loops
www.agilent.com/chem
GC/MS SYSTEMS
Ion Source
The ion source operates by electron
ionization (EI) or chemical ionization (CI).
The sample enters the ion source from the
GC/MSD interface. Electrons emitted by a
filament enter the ionization chamber,
guided by a magnetic field. The high-energy
electrons interact with the sample mole-
Preparing to Clean
Prior to cleaning, the mass spectrometer
must be vented and the ion source must be
removed. Before venting the system, the
following conditions must be met:
www.agilent.com/chem
88
GC/MS SYSTEMS
Description
Part No.
Price
8650-0030
8650-0029
9310-4828
5181-8863
$ 16
$ 16
$185
$124
05980-60051
5061-5896
$ 64
$ 27
8660-0791
8500-0656
05971-60571
8500-1233
$ 29
$168
$ 85
$115
05980-20018
5080-5400
$ 14
$ 10
8710-0899
8710-0900
8710-0510
$ 16
$ 25
$ 24
8710-1622
5182-3466
$ 38
$ 24
0100-0160
0100-0787
5181-1258
$ 8
$ 8
$ 10
5183-2096
$657
05971-60561
$510
89
www.agilent.com/chem
GC/MS SYSTEMS
Description
Price
G1099-20130
$ 198
(B) Repeller
G1099-20132
$ 112
G1099-20136
$ 29
05971-20134
$ 69
(E)
Drawout cylinder
G1072-20008
$ 190
(F)
05971-20143
$ 263
05971-20126
$ 105
G1099-20133
$ 82
(I)
Set screw
0515-1446
(J)
Washer, M3 (1/pk)
3050-0891
0535-0071
(L)
G1099-60104
$ 200
05971-20130
$ 270
G1099-60106
$ 270
G1099-60177
$ 408
Repeller assembly
G1099-60170
$ 481
0515-1046
H
L
E
D
M
5973A
5973N
5973 inert**
Price
B
I
G2589-20045
G2589-20100
$ 99
G2589-20045
$ 225
G2590-60053
$ 97
G1099-60170
G2589-60102
$ 499
0515-1046
G1999-20021
G1099-20130
G2589-20043
$ 563
G2589-20101
$ 12
G1099-20130
H
I
www.agilent.com/chem
90
GC/MS SYSTEMS
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)
Price
05971-20126
$ 108
05971-20130
$ 278
05971-20143
$ 271
G1072-20008
$ 190
05971-20134
$ 71
05971-20128
$ 531
0515-1446
05971-60170
$ 593
0515-1046
Price
05972-60226
$3554
Price
Price
05971-20305
$ 242
G1800-20305
$259
91
Min
0.1
0.1
0.1
0.1
Tuning Max
2.0
2.0
1.0
1.0
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.
Filament Assembly
Description
Unit
Part No.
Price
05972-60053
$ 90
G1099-80053
$282
G2590-60053
$ 97
05972-60053
$ 90
05971-60140
$159
2/pk
www.agilent.com/chem
92
GC/MS SYSTEMS
MAINTENANCE MINDER
Calibration
The calibration valve is an electromechanical
valve with a vial that contains a tuning
compound. Perfluorotribuylamine (PFTBA)
is the most commonly used tuning
compound. It is required for automatic
tuning of the MSD in EI mode. The tuning
compound is usually a liquid but can be
volatile or semi-volatile solid.
How to Refill
The calibration vial can be refilled without
venting the system. Fill the vial to 0.5 cm
from the top. DO NOT overfill. Air is
trapped in the vial when it is refilled.
Description
Part No.
Price
8500-0656
8500-8130
$168
$ 43
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
readings and their possible causes. The
symptoms in this section are based on
typical pressures. At typical column flow
rates (0.5 2.0 ml/minute), the foreline
pressure will be approximately 20 to 100
mTorr. The vacuum manifold pressure will
be approximately 1 x 10-6 to 1.4 x 10-4 Torr.
Symptom
Symptom
Possible Cause
Possible Cause
Symptom
Symptom
Possible Cause
Possible Cause
www.agilent.com/chem
94
GC/MS SYSTEMS
Diffusion Pump
It is not necessary to change the diffusion
pump fluid more than once a year, unless
you observe symptoms that suggest a
problem with the diffusion pump fluid. The
MSD must be vented in order to check the
diffusion pump fluid (except for the 5973).
Therefore, the best time to check the fluid
is when the instrument is already vented
for other maintenance.
Importance of the Fluid Level
The amount of fluid in the pump affects
the amount of vapor and the temperature
of the base plate. Too little fluid will cause
the pump to run at a higher temperature
because there is less fluid to carry away the
heat resulting in fluid cracking or degradation
and loss of high vacuum. It will also lower
the pumping speed because there is less
fluid vapor available to pump away gases
which can especially affect operation in
CI Mode due to higher flow rates.
Description
Part No.
Price
6040-0809
59864B
0960-0376
0960-0897
$ 82
$1399
$ 195
$ 358
Foreline Pump
The oil in the foreline or rough pump
should be replaced on average once every
six months, but can vary depending upon
applications. After oil replacement, if the
foreline trap is present, the molecular
sieves should be replaced.
95
Description
Part No.
Price
6040-0798
$122
6040-0834
$ 39
9301-1104
$ 57
3162-1056
$430
G1099-80037
$173
5063-5224
$417
www.agilent.com/chem
GC/MS SYSTEMS
Description
Part No.
Price
05971-80103
$1004
G1099-80001
05971-80102
$2131
$1136
Symptom
Voltage is over 2500 volts
Poor vacuum
Corrective Action
Replace electron multiplier
www.agilent.com/chem
96
GC/MS SYSTEMS
Lubricant Oil
Turbo pump lubricant:
Balzers turbo pump lubricant, 0.25 liter
97
5989 or
5988
Thermo or
Electro Spray
5985 or
5987
5999x, 5993x
or 5995x
Part No.
Price
6040-0468
$ 134
6040-0370
6040-0819
$2553
$ 283
6040-0798
6040-0834
6040-0730
$ 133
$ 40
$ 760
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
Week
Every
3 Months
Every
6 Months
As
Needed
Cabinet Maintenance
Analyzer Maintenance
Clean ion source
Replace filament
Replace ion source heater
Replace mass filter heater
Replace electron multiplier horn
We recommend
keeping a separate
set of tools that have
been thoroughly
cleaned for working
with the MS engine.
These tools are
needed to prevent
contamination when
reassembling or
installing clean
assemblies such as
the ion source.
www.agilent.com/chem
98
GC/MS SYSTEMS
C
D
Description
Part No.
Price
05989-20110
05989-67002
05989-20111
05989-20109
05989-20145
05989-20119
05989-20165
05985-60179
05989-60098
$108
$990
$ 62
$ 88
$318
$580
$448
$ 58
$926
E
F
Description
Part No.
Price
05989-80043
05971-80103
$2012
$1004
0960-0799
$ 448
05989-20705
5181-3367
$ 18
$ 47
0905-1145
3162-0110
0905-1189
$ 19
$ 39
$ 38
5989
Electron multiplier kit
Electron multiplier replacement horn
99
www.agilent.com/chem
GC/MS SYSTEMS
Contents:
Start-Up Guide, pub. No. 5988-3073EN
Application Note, Improvements in the
Agilent 6890/5973 GC/MSD System for
use with USEPA Method 8270, pub. no.
5988-3072EN
Ultra Ion Source Chamber
Ultra Repeller
Ultra Large Aperture Drawout Plate
Description
Part No.
Price
G2860A
$2333
LIBRARY
There are many ways to perform semi-volatile analysis. For another option that
also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem
and do a library search for 5989-1510EN.
www.agilent.com/chem
100
GC/MS SYSTEMS
Tuning Samples
Checkout Samples
Semi-Volatile Volatile
MSD
EI
Tune
CI
Tune
EI
Negative
Mode CI
Positive
Mode CI
5973
PFTBA
PFDTD
OFN 1 pg/L
OFN 1 pg/L
DFTPP
BFB
5972
PFTBA
PFTBA
HCB 10 pg/L
NA
DFTPP
BFB
5971
PFTBA
PFTBA
HCB 10 pg/L
NA
DFTPP
BFB
GCD
PFTBA
NA
NA
NA
DFTPP
BFB
5989A
PFTBA
PFTBA
HCB 50 pg/L
OFN 1 pg/L
DFTPP
BFB
5989B
PFTBA
PFTBA
HCB 20 pg/L
DFTPP
BFB
MS Engine
101
www.agilent.com/chem
GC/MS SYSTEMS
Description
Quantity
Part No.
Price
05970-60045
$ 46
8500-5995
$ 62
8500-6406
$ 38
8500-5500
$141
PFTBA certified
1 bottle, 10 g
8500-0656
$168
0.5 mL
05971-60571
$ 85
PFDTD
10 g
8500-8130
$ 44
Benzophenone
100 pg/L,
5 ampoules
8500-5440
$ 74
Hexachlorobenzene
10 pg/L, 4 ampoules
1 ng/L, 2 ampoules
8500-5808
$ 39
Hexachlorobenzene
20 pg/L
8500-6405
$ 32
1 ng/L (2 ea)
05990-60075
$ 67
Octafluoronapthalene (OFN)
1 pg/L,
5 ampoules
8500-5441
$ 67
Octafluoronapthalene (OFN)
500 fg/L
8500-6572
$ 30
p-Bromofluorobenzene (BFB)
25 g/mL
8500-5851
$ 39
www.agilent.com/chem
102
www.agilent.com/chem
104
A Total Commitment
to Your Lab for One Fixed Cost.
Maximum uptime
High productivity
Total compliance
Extended instrument life
Fast problem resolution
Verified system performance
The skills and knowledge you need for
efficient operation and maintenance
Consistent, in-depth documentation
Reduced administrative burdens
105
www.agilent.com/chem
Agilent Services
Features
Advantages to You
Telephone Service
Low cost.
Software Service
Maximum uptime.
Extended instrument life.
www.agilent.com/chem
106
Agilent Services
Features
Advantages to You
107
www.agilent.com/chem
Agilent Services
Features
Advantages to You
Network Qualification
Onsite disassembling
Cleaning
Reassembling
Testing
www.agilent.com/chem
108
Agilent Services
Features
Advantages to You
Software Backup
109
www.agilent.com/chem
Course Title
Duration
Description
Self-paced;
Four hours access
Self-paced;
Four hours access
Self-paced;
Four hours access
www.agilent.com/chem
110
Course Title
Duration
Description
Self-paced;
Four hours access
Self-paced;
Four hours access
Self-paced;
Four hours access
Self-paced;
Four hours access
Instructor-led;
60-90 minutes
111
www.agilent.com/chem
Course Title
Duration
Description
Logical GC Troubleshooting
Instructor-led;
60-90 minutes
Instructor-led;
60-90 minutes
Instructor-led;
60-90 minutes
www.agilent.com/chem
112
Classroom Training
Agilents training courses for gas
chromatography and mass spectrometry
help new and experienced lab
professionals learn proper and efficient
ways to use analytical instruments and
software. These ISO-registered courses
Course Title
113
Course No.
No. of Days
Description
Technique
Introduction to Capillary GC
H2615A
Techniques of GC
H4002A
Introduction to GC-MS
H2609A
Techniques of GC-MS
H4040A
Hardware/Software Operation
ChemStation Operation for the 6890 GC/ALS
H5926A
H4043A
H4050A
H5308A
5890 GC Maintenance
H4001A
H5309A
www.agilent.com/chem
Course Title
Course No.
No. of Days
Description
H5947A
H2294A
H2606A
H4076A
H4053A
www.agilent.com/chem
114
Support
Tap Agilents GC and GC/MS
expertise anytime.
Just give us a call to discuss hardware,
software, application concerns, or basic
operation techniques.
115
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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
Gas Management
ITEM
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.
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
MSD
Components require regular maintenance. For complete MSD maintenance schedule, please see page 83.
www.agilent.com/chem
800 227 9770
www.agilent.com/chem
800 227 9770