Professional Documents
Culture Documents
13 Regulators 39 Column
L
PU
14 Tubing Performance
oting
15 Leak Detection 43 Detectors
This icon denotes a video that is available to view on our Don’t Miss…
web site. Just visit www.agilent.com/chem/supplies to GC Troubleshooting Guide (pullout poster)
view videos and obtain more information. GC Maintenance Schedule (inside back cover)
2 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 3
GAS MANAGEMENT
Gas Types
Carrier Gases
The most frequently used carrier gases are and elevated column bleed, along with not it will make contact with the sample.
helium and hydrogen, although nitrogen column and/or detector damage. The Coolant gases (carbon dioxide) and
and argon can be used. Purity is essential following sections describe the gases pneumatic gases (air or nitrogen) generally
for these gases since they sweep the and purities that are necessary for gas do not come in contact with the sample or
sample through the column where it is chromatography carrier gases, as well detector. Therefore, these non-contact
separated into its component parts and as other support gases. gases do not have to be the highest purity
then through the detector for component available.
quantification. Carrier gas purity is also Support Gases For most applications, gases which are low
critical to prevent degradation of
Support gases may be specific for detectors in oils and particulates are desirable; thus,
chromatographic hardware.
or for applications. These gases include low-purity “specialty gas” grade products
Contaminants in carrier gases can have fuels, oxidants, coolants, detector gases, can be used. Fuels, oxidants and detector
a significant effect on column life and and pneumatic gases. The degree of purity gases, in most cases, do come in contact
subsequent analyte detection. Harmful required for support gases is dependent on with the sample and detector, and require
effects include contaminant peaks how that gas is being used, and whether or higher purity gases.
Sample
Gas Type Function Contact Purity Required*
Hydrogen/Helium Mix Fuel gas for detector 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%)
4 www.agilent.com/chem
GAS MANAGEMENT
Contaminants in gases are major ● can also cause baseline drift or wander, In some cases it may be difficult to
contributors to capillary column contaminant peaks, and noisy or high determine which contaminant presents
degradation and detector noise, and offsets of baselines the biggest problem in a given analysis. If
can interfere with chromatographic unsure, a call to your gas supplier may be
results. Concentration of these Moisture helpful. Once the problem contaminants
contaminants vary by the grade of gas. ● can be introduced by improper handling have been identified and a general
and/or installation of plumbing contaminant level is determined, the next
Analytical gases are available in many
step is to choose a gas purity level that
grades of quality, from high purity ● a common cause of column stationary comes closest to these requirements.
(99.995%) to chromatography grade purity phase degradation
(99.9995+%). The higher the purity, the Keep in mind that higher grades of gas
higher the cost.
● can damage instrument generally cost more. The greatest cost
savings can be achieved by using the
Oxygen
Identifying Contaminants lowest purity gas which will neither
● most common contaminant interfere with the analysis nor damage
To make a proper purity choice it is your equipment. Using the proper gas
● a common cause of column stationary
helpful to understand the contaminants purification equipment to remove common
phase and inlet liner degradation
most common in GC gases and how contaminants and achieve the desired
they can affect your analysis. Common ● can cause decomposition of labile purity level is essential.
contaminants are: analytes
Agilent brings the highest performance The illustration on the next page shows Other Considerations
and largest variety of gas purifiers (traps) the most common gas purification ● determine desired purity level
to gas chromatographers. Purifiers are configurations used in gas chromatography.
available in a variety of sizes and ● keep number of “breaks” in gas line
Regardless of which purification system to a minimum
configurations, to remove common
is employed, proper installation and
contaminants like oxygen, moisture, ● install purifiers in a convenient location
maintenance is required to achieve
and hydrocarbons. In-line gas purifiers, close to the GC
optimal performance from the purification
including refillable, indicating, S-shaped,
system(s). A purifier that is not maintained ● purifier log books are useful for
and metal body types, are made to remove
will eventually saturate and become determining maintenance schedule
specific contaminants. Agilent also offers
ineffective, or worse, a source of
gas purification systems with removable ● use indicating traps closest to the GC so
contamination.
cartridges. These systems provide the you can determine when to change the
ability to design the right combination traps that are upstream
of filters needed for your application to
achieve the proper gas purity.
www.agilent.com/chem 5
GAS MANAGEMENT
-OR-
Combination Trap ECD make-up
Gas supply Vent
MS carrier gas
Gas supply = cylinder, in-house line, or gas generator
Gas Traps
The purpose of gas traps is to remove Constant exposure of capillary columns to
detrimental impurities from the carrier oxygen and moisture, especially at high
and detector gases. Moisture (water), temperatures, results in rapid and severe
oxygen and hydrocarbon traps are the column damage. The use of oxygen and
most common traps used with GC moisture traps for the carrier gas may
systems. A few combination traps are extend column life and protect the
available which remove moisture, oxygen instrument. Traps may provide some
and/or organics with a single trap. The protection if there is a leak at or around
effectiveness of the traps depends on the the gas cylinder. Any moisture or oxygen
initial quality of the gas. Little enhancement introduced into the gas stream due to the
by traps to the GC system is obtained by leak will be removed by the trap until it
traps when using very high purity gases expires. This creates an opportunity to
(e.g., ultra-high purity or similar grades) detect and fix the leak before column or
while obvious improvement is obtained instrument damage occurs.
NEED MORE HELP? with lower grades of gas.
Tap Agilent’s GC knowledge
over the phone, on-line, in the
classroom, even at your site.
See pages 56-58 for more
information about our expert
training, service and support.
6 www.agilent.com/chem
GAS MANAGEMENT
Size H2O Removal Maximum Effluent H2O 1/8 in. 1/4 in.
Description (cc) Capacity (g) Concentration (ppb) Part No. Part No.
Molecular Sieve 13X and Indicating 4Å – Economy, with plastic Lexan body (other packings available, see Agilent catalog)
Glass Indicating Moisture Traps (larger size is available, see Agilent catalog)
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 7
GAS MANAGEMENT
Oxygen Traps
Oxygen traps usually contain a metal- plastics are permeable to air and contain
containing inert support reagent. Most contaminants that can degrade gas quality.
Indicating Oxygen Trap oxygen traps reduce the oxygen In addition, many of the metal bodied
concentration to below 15-20 ppb. The oxygen traps can withstand high pressures
capacity of a standard oxygen trap is (up to 2000 psi). Some oxygen traps also
approximately 30mg of oxygen per 100cc remove moisture from the gas stream
of trap volume. Oxygen traps can remove without affecting the oxygen removal
some small organics and sulfur compounds capability.
from gas streams.
Big Oxygen Trap Indicating oxygen traps change color when
Metal (usually aluminum) trap bodies are oxygen is present in the gas at harmful
recommended for GC analyses. Some levels. Indicating traps are not intended to
Oxygen Traps be the primary oxygen removal trap, but
should be used in conjunction with a high
1/8 in. 1/4 in.
capacity non-indicating oxygen trap. They
Description Size (cc) Part No. Part No.
are installed after the high capacity oxygen
Indicating Oxygen Traps – glass body with plastic safety shield
trap in the gas line to indicate when the
high capacity trap is expired and needs to
Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP be changed. Expired oxygen traps need to
be immediately changed since they can
Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller size contaminate the gas, in addition to failing
available, see Agilent catalog) to remove oxygen.
Big Oxygen Trap 750 BOT-2 BOT-4
Capillary Grade Hydrocarbon Traps – for crucial capillary applications Hydrocarbon Trap
8 www.agilent.com/chem
GAS MANAGEMENT
Hydrocarbon S-Trap
Combination Traps
Agilent carries several Combination Traps ● Leak-free, one-piece design to eliminate
that provide multiple contaminant removal potential leaks from using multiple traps
in a single trap. These traps offer: ● Efficient design which prevents
● Optimized adsorbents for maximum channeling and promotes efficient
surface area and capacity scrubbing
● The ultimate in purification with a single
trap (Big Universal Trap)
Oxygen/Moisture Traps
Big Universal Traps – for the Ultimate in Gas Purification, removes oxygen, moisture,
hydrocarbons, CO, and CO2 Big Universal Trap
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 9
GAS MANAGEMENT
10 www.agilent.com/chem
GAS MANAGEMENT
4-Head
Replacement Cartridges
NEED MORE HELP?
Description Part No. Tap Agilent’s GC knowledge
over the phone, on-line, in the
High capacity oxygen GC-1
classroom, even at your site.
High capacity moisture GC-2 See pages 56-58 for more
information about our expert
Indicating moisture GC-2-I training, service and support.
Hydrocarbon GC-3
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
www.agilent.com/chem Gas Purifier Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 11
GAS MANAGEMENT
Only a small sampling of gas purifiers are shown here. For a complete selection of gas purifiers, see the
12 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 empties and the inlet pressure to the
component in any gas handling system. regulator decreases (inlet decay), the
Their function is to reduce the pressure pressure on the diaphragm is reduced.
from a high pressure source, such as a Without proper adjustment, the outlet
cylinder, to a suitable use pressure. pressure might slowly rise. Brass Body Regulator
Although regulators are very good at
A dual stage regulator overcomes this
controlling pressure, they do not control
problem by connecting two regulators
flow. They have a maximum flow rate
together. The first stage regulates the to purity considerations, then a stainless
which is dictated by the design. Basically,
pressure to the second stage thus creating steel regulator should be chosen for the
the flow is determined by the pressure
a constant pressure and allowing minimal same reasons. Unfortunately, use of high
drop across the regulator.
inlet decay. Agilent recommends using purity stainless steel regulators is often
two-stage regulators with our GC Systems cost-prohibitive.
Types of Regulators to provide the proper pressure control for
optimal use. No matter which material is chosen for the
There are primarily two types of
regulator body, be sure to specify one with
regulators: single stage and dual (or two)
stainless steel diaphragms for critical
stage. The difference is that a dual stage Regulator Materials applications such as use on carrier, fuel or
regulator is actually two regulators
Regulators are usually constructed of brass detector gases. Agilent recommends using
connected in a series.
or stainless steel. The choice of material our economical brass body, dual stainless
Dual stage regulators provide more precise follows the same guidelines as the choice steel diaphragm regulators for most GC
and consistent pressure control than single of tubing. Generally, it is not recommended applications. These regulators, combined
stage regulators. The reason is that in a that the materials be interchanged. If with the proper gas purification system,
single stage regulator, as the gas cylinder stainless steel tubing were chosen due provide proper gas pressure control and
purity for gas chromatography.
When ordering a regulator, be sure to
specify the proper connections. In the
Description Part No.
US, most gas manufacturers follow CGA
connection guidelines. In Europe, there
Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*
are a number of organizations designating
CGA 346, 125 psig max (8.6 bar), Air 5183-4641 cylinder connections that are specific to
individual countries. It is best to contact
CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642 your local supplier for the proper
connection designation.
CGA 540, 125 psig max (8.6 bar), O2 5183-4643
CGA 580, 125 psig max (8.6 bar), He, Ar, N2 5183-4644
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
www.agilent.com/chem 13
GAS MANAGEMENT
Tubing
When constructing or maintaining a gas used for non-critical applications, such as
delivery system for GC, choosing the proper pressurizing pneumatic lines; however, be
tubing material is very important and will aware of its pressure limitations.
help to eliminate potential problems and
In view of these problems, the list of
improve the overall quality of the gas
appropriate tubing materials has been
system. Although there are many common
narrowed down to two: copper and
tubing materials available, some pose
stainless steel. Agilent recommends using
safety or cleanliness problems.
copper tubing for most applications, since
Non-metallic types of tubing such as it is easy to bend and plumb and is less
polyethylene and Teflon are not expensive than stainless steel. Use
Spectra-Link Tubing Connecting System
recommended for GC applications due stainless steel tubing only for crucial
on a two-stage regulator to their gas permeability and difficulty applications that require very high purity.
in cleaning. This type of tubing can be
Cleaning Tubing
Determining Tubing Length Before any tubing is placed into service,
or if it becomes contaminated with use,
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig
it is essential that it be properly cleaned.
Tubing Type Diameter Recommended Pressure Drop
Unclean or improperly cleaned tubing can
(inches) Max. Length (feet) (psig)
lead to contamination of the system with
disastrous results.
Copper 1/8* 50 2
Cleaning tubing requires the use of suitable
Copper 1/4* 300 0.5 detergents and solvents along with
nitrogen and a purgeable oven for drying.
*Recommended when multiple instruments are connected to the same source This may be done easily for small lengths
of tubing but in larger systems, the
cleaning procedure becomes unwieldy
sometimes, leaving behind a large quantity
of solvent requiring proper disposal.
Fortunately, Agilent provides clean high
Tubing—Precleaned quality GC grade tubing for large systems
as an economical alternative.
Description Part No.
14 www.agilent.com/chem
GAS MANAGEMENT
Cylinder Bracket
Leak Detection
Leaks allow oxygen and other and easy detection and measurement of
contaminants to enter the gas stream. gas leaks for 12 common gases. Based on a
Therefore, GC instrument maintenance dual cell micro volume thermal conductivity
should include checking fittings and system, this unit provides very high
connections with a gas leak detector. sensitivity and eliminates contamination
Agilent’s Gas Leak Detector enables quick caused by soap solution methods.
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).
www.agilent.com/chem 15
GAS MANAGEMENT
Flow Rates
Setting and maintaining GC flow rates Selecting a Flowmeter
greatly affect the instrument accuracy Agilent manufactures the largest selection
and sensitivity. During maintenance, of volumetric and mass flowmeters for
verify carrier and support gas flows chromatography. We have developed
with the proper flowmeter. Choosing a flowmeters for measuring capillary column
flowmeter for your application depends flows, calibrating air pumps and flow
upon measurement speed, ease of use, controllers, and verifying instrument gas
accuracy, and flow rate range. flows. All flowmeters are calibrated to
NIST-traceable standards.
16 www.agilent.com/chem
GAS MANAGEMENT
Flowmeters
Electronic Mass Flowmeter – dedicated mass flowmeter, very accurate for specific gases*
Veri-Flow 500 He, H2, Ar/CH4 Rechargeable Battery
(110 V) 5.0 500 N2, Air ±3 or 110 VAC Yes HVF-500
Veri-Flow 500
Optiflow 420
Only a small sampling of flowmeters are shown here. For a complete selection of flowmeters, see the
www.agilent.com/chem Flowmeter Selection Guide in the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 17
There’s More!
Agilent offers a series of free
Maintenance Guides for your GC System.
Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes, see the
www.agilent.com/chem Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 19
SAMPLE INTRODUCTION & INLETS
Sample Introduction
Vial Options
Glass—for general purpose Silanized—for use with Polypropylene—for use Amber Vials—for use with Microvolume Inserts— High Recovery Vials—
use and for use with acids samples that bind to glass, with alcohols and aqueous light-sensitive samples for use with very small for use with limited sample
and for trace analyses solvents sample volumes volumes
1 mL 50 µL
3.6 mm*
100 µL vial
*Needle position based on standard sampling depth.
20 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
Vials
Teflon/Silicone/Teflon
● Used in trace analysis applications Description Quantity Part No.
● Above average resealing
● Most resistant to coring Vials
● Least evaporation
2 mL Crimp top vial convenience
● Use with large diameter, blunt tip
pack with silver AI caps with
syringe needles Teflon/Red rubber septa 500/pk 5181-3400
Teflon Disc 2 mL Screw top vial convenience
● Good for MS and ECD analysis pack with blue screw caps and
● Chemically inert Teflon/Red rubber septa 500/pk 5182-0732
● No resealing
2 mL Snap top vial convenience pack
● Single injection
with clear polypropylene snap caps
● No long-term sampling storage and Teflon/Red rubber septa 500/pk 5182-0547
www.agilent.com/chem 21
SAMPLE INTRODUCTION & INLETS
Packed, split or
splitless (including PTV) 23 gauge or 23/26 gauge tapered any applicable
Needle tips
Sharp tip Cone tip
Tapered needle
22 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
www.agilent.com/chem 23
SAMPLE INTRODUCTION & INLETS
Syringe Tips
● Make sure to input the proper syringe ● Remove a gas-tight plunger from the ● To maximize the lifetime of standard
size when setting up the injection section syringe for long-term storage to keep the plungers, rinse the syringe and wipe the
of your data handling device. Teflon tip leak-free. If a gas-tight plunger plunger with solvent (isopropanol or
does not fit properly, place it in hot water acetone) and a lint-free wipe, as specified
● Rinse syringes and clean their plungers
for about 10 minutes then press the tip in the syringe cleaning procedure
before use to maximize syringe lifetime.
uniformly on a clean, hard surface and let included with each syringe.
● Rinse the syringe 5-8 times between cool to room temperature. The plunger
injections to minimize sample carryover. should reseal correctly to provide 10-25%
more injections.
● Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
● A 26 gauge syringe can be used for on-
column injections into a 0.53mm id
column. Always check that on-column
syringe needles fit inside the capillary
column before installing the column and
syringe in the GC.
● For on-column injections, always use the
proper septum nut and stainless steel
insert for the column dimension you are
using. Use a septum with a molded
through-hole with injections onto 0.32mm
and 0.25mm columns.
24 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
Syringes
Only a small sampling of vials and syringes are shown here. For a complete selection of vials and syringes,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 25
SAMPLE INTRODUCTION & INLETS
Packed-Column Inlets
Packed-column direct inlets are very Packed-Column Inlet Procedures/Practices
popular. Packed-column analysis is
frequently done when high efficiency Parameter Selection/Setting Rationale
separations are not needed or when gases
are analyzed by gas-solid chromatography. Inlet temperature BP of solvent +50˚C Ensures flash vaporization
Packed column inlets are simple in both BP of major solute(s) Use for neat samples
design and use. Few parameters need to be Insert type 1/8-inch stainless steel Use for ss column only
set, and all carrier gas flow flushes through 1/4-inch stainless steel Inserts permit connection of
the inlet into the column in the standard columns up to 1/4-inch od.
configuration.
Liner Glass Use to lower activity
(replaceable)
Initial column temperature programming Sharpens peaks and
temperature reduces run time
Column type 1/8-inch packed stainless Will not break
1/4-inch packed glass Better for polar or labile
compounds
Carrier gas flow 20-40 mL/min Use with N2 carrier gas
30-60 mL/min Use with He or
H2 carrier gas
Troubleshooting
Most problems with packed-column inlets The inherent activity of packed-column Leaks
involve sample decomposition, flashback, inlets is somewhat mediated by the fact Since packed-column inlets are usually
or leaks. that they usually have low internal volume. flow-controlled, septum and column leaks
When this is coupled with the relatively will have a direct impact on retention times
Decomposition fast flow rates used with packed columns, and peak areas. Sample can be lost through
Since packed-column inlets are active, the residence time of sample in the inlet is the leak holes, and air can diffuse back into
especially if glass liners are not used, polar short and decomposition is reduced in the inlet to cause column degradation.
sample components will often tail or comparison to the decomposition that Change the septum on a regular basis and
degrade in the inlet. Sample decomposition occurs with some capillary inlets (for check column connections at the first stage
caused by the inlet is easily diagnosed; the example, splitless inlets). of problems. To prevent stationary phase
decomposition products will have peaks at decomposition, make sure that the oven
the same retention times as standards for Flashback and inlet are at room temperature when not
the decomposition product. The negative side of low inlet volume, in use and when changing the septum.
however, means that excessively large
When inlet-caused decomposition is
sample injections will easily exceed the
suspected, try intracolumn direct injection,
capacity of the liner and will flash back into
deactivated glass liners, or lower inlet
gas supply lines and onto the septum. This
temperatures, and remove any column
can cause several maladies, including
packing in the inlet zone.
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.
26 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
1
1 Septum nut 18740-60835 2
3
2 Septa Bleed temperature, 4
optimized, 11 mm** 50/pk 5183-4757
11
www.agilent.com/chem 27
SAMPLE INTRODUCTION & INLETS
Split/Splitless Inlets
The combined “split/splitless” inlet is the Troubleshooting results to the lower temperature analysis.
most popular inlet for capillary column gas Repeat if results are positive until no
Split inlets are spared from most band-
chromatography. Because it can be used in further improvement is seen.
broadening phenomena, since narrow
either split or splitless mode, it provides a
peaks are generated as part of the A majority of the problems encountered
very effective combination that can cover
splitting process. Therefore, any peak with split inlets are related to
most analysis requirements.
broadening or tailing observed with split discrimination and decomposition. Both
injection is usually due to improper analytical accuracy and reproducibility
Split Mode column installation, low split flow, or decrease with the increases in
Split injection is an effective way to low inlet temperature. If you suspect that discrimination and decomposition.
introduce small amounts of sample without the inlet temperature may be too low, Split inlets suffer from both needle
overloading the column. Split injection is increase it by 50˚C and compare the discrimination and inlet discrimination.
required for samples that:
● cannot be diluted for analysis (for
example, solvents)
● are gases that cannot be focused, or
that have long injection times (valve
injections)
● have important minor peaks eluting Split Mode Procedures/Practices
directly before the solvent peak (as in
solvent analysis) Parameter Selection/Setting Rationale
Split injection is also good for screening Inlet temperature BP last eluting compound Ensures flash vaporization
samples of which little is known or for Minimizes inlet discrimination
those that have widely differing Inlet liner Large volume, deactivated Minimizes flashback
concentrations, since the split ratio Minimizes degradation
can be adjusted easily. Split inlets are
also a good choice for dirty samples. Inlet packing Silanized glass wool Retains non-volatiles
Stops flow of droplets
Glass beads or frit Less active than wool
None Least active
Injection volume 0.5-3 µL liquid Split easily adjusted
0.10-10 mL gas Split adjusted accordingly
Injection technique Fast autoinjection Less needle discrimination
Hot-needle fast manual Reproducible discrimination
injection
Split ratio 50:1 to 500:1 Depends on sample and
injection volume
Initial column Not critical Narrow initial peaks
temperatures
Septum purge 2-3 mL/min Minimizes ghosting
28 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
www.agilent.com/chem 29
SAMPLE INTRODUCTION & INLETS
Splitless injection is routinely used in on the solvent tail may be focused by the volume), leading to irreproducibility and
areas such as: solvent to yield more sensitive analyses. nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
● environmental analysis
Troubleshooting volume carefully to avoid backflash.
● pesticide monitoring of foods
Most problems encountered with splitless Decomposition
● drug screening injection are related to incorrect purge Loss of peak area or generation of new
In these applications, sample preparation time, degradation, improper focusing, and peaks, can sometimes be dramatically
requirements are significant, and it is not flashback. reduced by changing liner type or by
always possible or economically justifiable Appropriate initial column temperature is deactivating the liner and inlet with
to clean up a sample extensively. So critical. Sample vapors can be lost through silanizing reagents. Removing or reducing
column protection becomes as important the septum purge line if the insert is the amount of liner packing can also
as sensitivity. Also, samples with trace overfilled with sample vapor (either too decrease inlet activity.
quantities of important solutes that elute large injection volume or too small liner
1
1 Septum retainer nut 18740-60835
2
2 Septa**
3
4
3 Insert Weldment**
6
5
4 Liner O-ring**
5 Liner**
8 SS seal 18740-20880
Gold-plated seal 18740-20885
30 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
Initial inlet Same as oven (oven track) Simple and effective Sample Considerations
temperature ramp Faster than oven Narrows initial peak width
Sample preparation is important for
Injection volume 0.1-2.0 µL liquid Use smaller injections for on-column injection because of:
small id columns;
Depends on column capacity ● the potential for column overload,
column contamination,
Injection technique Fast autoinjection Projects droplets away from
syringe tip
● the incompatibility of some solvents
Fused silica needle Use for manual injection into with the stationary phase,
small id columns ● dependence of the initial column
temperature on the boiling point of
Oven temperature Inlet temperature or Prevents backflash
the solvent.
slightly lower
Many of the problems associated
Column flow 50-80cm/sec Use for H2 carrier gas
with these variables can be resolved
30-50cm/sec Use for He carrier gas
by using a retention gap ahead of the
Septum purge 12-15mL/min Use if installed to prevent analytical column.
ghosting
Quantification All methods Inherently reproducible
technique
Lack of discrimination
Retention gap 1-3m, deactivated Corrects peak distortion
requirements Protects column from non-
volatile components
Permits autoinjection with
narrow-bore columns
HELPFUL HINT: Since the sample is directly deposited into the column, nonvolatile sample
To view a video on cool on-column installation and
components can accumulate at the head of the column and will degrade efficiency and/or septum replacement, visit www.agilent.com/chem/supplies,
interact with subsequent injections. click on “How-to Video” under the Reference Library.
www.agilent.com/chem 31
SAMPLE INTRODUCTION & INLETS
Troubleshooting
The major problems found with cool on- prevent displacement of the stationary
column injection are associated with phase by solvents.
column overload, solvent/stationary phase
Immobilized stationary phases can be
incompatibility, and column contamination.
washed to remove contaminants and
If the flooded zone after injection is too renew performance. If column performance
long (large injections, poor wettability), does not improve after washing, cut 0.5m
peaks will be broad or split. A retention gap off the inlet side of the column. If that does
usually will resolve this problem. Loss of not return column performance, the column
column efficiency with on-column injection must be replaced and a retention gap
usually is caused by contamination or should be used for all further injections of
degradation of the stationary phase at the dirty samples.
head of the column. Only columns with an
immobilized stationary phase should be
used with cool on-column injection to
32 www.agilent.com/chem
SAMPLE INTRODUCTION & INLETS
*For a complete parts breakdown, see the 6890/5890 Series GC Instrument User and/or Service Manuals.
Only a small sampling of inlet supplies are shown here. For a complete selection of inlet supplies,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 33
SAMPLE INTRODUCTION & INLETS
● retention time and area reproducibility Injection volume 0.1-1.5µL Use lower volumes for
approaching cool on-column injection volatile solvents and fast
ramp rates
PTV inlets are actively cooled before and Use volumes larger than
during injection by Peltier devices or by 1.5µL only in solvent-
forced gases (air, liquid N2, or liquid CO2). elimination mode
Cryogenic cooling of the inlet can reduce
inlet temperature enough to thermally Sample Injection Autosampler or manual, Not critical for cold split
focus gas injections from other sampling technique fast or slow & splitless modes
devices in the liner. This is a distinct Oven temperature 10-25˚C below solvent BP For proper solvent effect in
advantage of using PTV inlets in splitless mode
comparison to conventional inlets for Sample dependent For split mode
coupling auxiliary sampling devices to
capillary columns. Column flow 30-50 cm/sec Clears inlet faster
Less backflash
Post-injection, PTV inlets are heated
using electrical heaters or preheated Septum purge 1-5mL/min Minimizes ghosting
compressed air. Depending on design,
inlet temperature ramps are either Quantification Any method Inherently reproducible
ballistic (i.e., ramped to the maximum Low discrimination in cold
injection modes
temperature at an uncontrolled maximum
rate) or programmable. Retention gap 1-3m, deactivated Compensates for extended
flooded zone and solvent-
column incompatibility
PTV Liners
www.agilent.com/chem 35
SAMPLE INTRODUCTION & INLETS
Septa Ferrules
The septum isolates the sample flow path Ferrules seal the connection of the column Installation
from the outside world. It must provide a or liner to the system. The ideal ferrule Be sure to install ferrules correctly to avoid
barrier that is readily penetrated by the provides a leak-free seal, accommodates problems:
injector needle while maintaining internal various column outer diameters, seals with
pressure without contaminating the minimum torque, will not stick to the ● don’t overtighten – finger-tighten column
analysis. Septa are generally made of column or fittings, and will tolerate nut, then use wrench to tighten 1/4 turn
special high temperature, low-bleed temperature cycling. ● maintain cleanliness
silicone rubber formulations. Septa should
Signals that a ferrule is damaged include: ● bake out ferrules prior to use
be replaced regularly to avoid leaks,
decomposition, sample loss, reduced ● background noise from oxygen diffusing ● avoid contamination (i.e., fingerprints,
column or split vent flow, ghost peaks, into the system oils)
and column degradation. ● column bleed catalyzed by oxygen ● inspect used ferrules with magnifier for
To minimize problems: ● sample degradation cracks, chips, or other damage before
● use septa with the recommended reusing them
● loss of sample
temperature range ● change ferrules when new columns or
● change septa regularly
● increase in detector signal/noise injector/detector parts are installed
● install the retainer nut “hand tight” ● poor retention time reproducibility
● use septum purge when available
● use autoinjectors
syringe needles
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 For a complete selection of inlet
discrimination, poor reproducibility, sample supplies, refer to Agilent’s
decomposition, and ghost peaks. Change
liners on a regular basis, as determined by: GC Inlet Resource Guide.
● previous use pattern (publication # 5988-3466)
● sample cleanliness
● chromatographic abnormalities such as
peak shape changes, peak discrimination,
poor reproducibility, sample pyrolysis
36 www.agilent.com/chem
Columns
Choosing the right GC column and
following Agilent’s simple column care
recommendations will maximize GC
column performance and lifetime. In this
section our experts offer practical advice
on how to select, install and store your
GC column, plus give helpful hints about
avoiding thermal and oxygen degradation.
Because GC column contamination is
the primary cause of shortened column
lifetime, we’ve also included a detailed
discussion about the prevention of non-
volatile and semi-volatile contamination,
as well as appropriate recovery measures.
www.agilent.com/chem 37
COLUMNS
Column Maintenance
While GC column maintenance is predefined timetable of maintenance items, installation/system setup, and avoiding
simple, the frequency and type of the main focus should be how to obtain the primary factors that cause column
column maintenance that is required the highest performance and lifetime performance degradation (breakage,
varies due to many system and sample from a capillary column. This depends on thermal damage, oxygen damage, chemical
factors. Instead of simply following a choosing the right column, correct damage and contamination).
Choose the Column that offers the best DB-1ms, 0.25mm i.d., 30m, 0.25µm 122-0132
longevity:
● Use low-bleed columns whenever HP-5ms, 0.25mm i.d., 30m, 0.25µm 19091S-433
possible.
DB-XLB, 0.25mm i.d., 30m, 0.25µm 122-1232
● Choose the least polar column that
provides the best resolution for the most DB-35ms, 0.25mm i.d., 30m, 0.25µm 122-3832
difficult separation.
HP-INNOWax, 0.25mm i.d.,
● Use more polar phases when difficult 30m, 0.25µm 19091N-133
isomer separations are required. (Choose
a more polar phase when you must, but
try to make it the least polar column that
will do the job.)
● Use most favorable dimensions to enable
required separation while optimizing
temperature ranges.
38 www.agilent.com/chem
COLUMNS
This is a small sampling of the many GC columns and parts. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 39
COLUMNS
Recovery
● Disconnect column from detector
● Heat the column 8-16 hours at the
isothermal limit HELPFUL HINT: Install a moisture trap
upstream of the oxygen trap to increase
● Remove 10-15 cm from the column end
the oxygen trap lifetime.
● Reinstall into the detector and condition
as usual
Description Part No.
NOTE: Thermal damage cannot be reversed.
The column usually does not return to its
original performance; however, it is often FlowTracker 2000 Flowmeter and Leak Detector 5183-4780
still functional. The life of the column will
be reduced after thermal damage. Big Oxygen Trap (750 cc, 1/8” fitting) BOT-2
40 www.agilent.com/chem
COLUMNS
Prevention
● Perform sample preparation to remove
inorganic acids and bases from the
sample
● Install guard column and trim frequently
of 5 or more meters
Column
Guard Column
Column Contamination
Column contamination is the most common
Union
problem encountered in capillary GC.
Unfortunately, it mimics most other
chromatographic problems and is often Guard column installation instructions are available at www.agilent.com/chem. Click
misdiagnosed. A contaminated column is on “Consumer Products.”
usually not damaged, but it may be
rendered unusable. There are two basic
types of contaminants: nonvolatile and
semivolatile.
This is a small sampling of the many GC columns and parts. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 41
COLUMNS
Nonvolatile Contaminants
Description Part No.
Nonvolatile contaminants or residues do
not elute and accumulate in the column
(most often confined to the first few SPE product guide Pub#5988-2685EN
meters). The column becomes coated with
Split/Splitless Inlet liner: glass wool,
these residues which interfere with the
taper, deactivated (5/pk) 5183-4712
proper partitioning of solutes in and out
of the stationary phase. Also, the residues Splitless Inlet liner: single-taper,
may interact with active solutes resulting no glass wool, deactivated (5/pk) 5183-4695
in peak adsorption problems (evident as
peak tailing or loss of peak size). Active Quartz deactivated column
solutes are those containing a hydroxyl connector (5/pk) 5181-3396
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes. Polyimide sealing resin (5 grams) 500-1200
Recovery
● Do not bakeout the column
● Front End Maintenance: are usually responsible for many baseline Column Storage
problems (instability, wander, drift, ghost
– Clean or change the injection port liner Capillary columns should be stored in their
peaks, etc.).
– Clean out the injector original box when removed from the GC.
Prevention Place GC septa over the ends to prevent
– Cut off typically 0.5 to 1 meter of the debris from entering the tubing. Upon
front of the column
● Perform sample cleanup to remove
reinstallation of the column, the column
semi-volatile materials from the sample
● Turn the column around (install detector ends need to be trimmed by 2-4 cm to
end into injector)
● Increase the final temperature of the ensure that a small piece of septa is not
GC run (not to exceed the temperature lodged in the column.
● Solvent rinse the column limit of the column)
If a column is left in a heated GC, there
● Cut the column in half and use the back ● Change septa regularly should always be carrier gas flow through
half (detector side). the column. The carrier gas flow can be
Recovery turned off only if the oven, injector, detector
Semivolatile Contaminants ● Bakeout the column: limit 1-2 hours and transfer lines are turned off (i.e., not
Semivolatile contaminants or residues (excess baking may polymerize some heated). Without carrier gas flow, damage
accumulate in the column, but eventually contamination and reduce column to the heated portion of the column occurs.
elute. Hours to days may elapse before they lifetime)
completely leave the column. Like ● Solvent rinse the column
nonvolatile residues, they may cause peak
shape and size problems and, in addition,
42 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.
Only a small sampling of FID supplies are shown here. For a complete selection of FID supplies,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 43
DETECTORS
44 www.agilent.com/chem
DETECTORS
Solvent Flush Procedure 5. After the final injection, allow makeup that the carrier gas and the flow system
gas to flow for 10 minutes or more. components are leak-free and contaminant-
1. Cool the cell to room temperature and
Slowly raise the temperature of the cell free.
remove the column.
to 20-30˚C above the normal operating
Watch out for decreased sensitivity caused
2. Place a septum in a nut or fitting temperature.
by samples that react with the filament,
assembly that fits onto the detector
6. After 30 minutes, decrease the originating from oxygen-contaminated
entrance.
temperature to the normal value and carrier gas, leaks in plumbing, or column
3. Place the nut or assembly on the install the column as usual. bleeding. Samples with active components,
detector fitting and tighten. Verify such as acids and halogenated compounds
the presence of makeup gas flow. can chemically attack the filament as
Thermal Cleaning well. Also, sample condensation will
4. Inject 20-100 µL volumes of toluene or contaminate the detector cell if the
benzene into the detector through the The TCD can become contaminated with
deposits from such things as column bleed temperature is too low.
septum. Inject a total volume of at
least 1mL of solvent. Do not inject or dirty samples. A wandering baseline, Some types of contaminants can be
halogenated solvents such as methylene increased noise level, or changes in removed by temperature bakeout. Also,
chloride and chloroform into the detector. response on a checkout chromatogram all in non-modulated designs, wandering
indicate contamination. Thermal cleaning, baselines due to temperature variation can
or bakeout (heating the detector block to be corrected by making sure the detector
evaporate the contaminant), should be temperature remains constant.
performed only after you have confirmed
Bead Maintenance higher hydrogen flows and bead currents ● Turn off the bead when not in use.
decrease bead life. If the NPD is not in use,
NPDs are temperamental and require ● Keep the detector temperature high
the hydrogen flow and bead current should
frequent maintenance. Small changes (320 – 335˚C).
be reduced or turned off to increase bead
in any of a number of parameters can
life. Make sure there is some type of gas ● Turn off the hydrogen flow during solvent
significantly change the performance
flow in a heated detector or when there is peaks and between runs.
characteristics of an NPD. The bead
current to the bead.
requires the most maintenance. It needs ● If the NPD is off for an extended period
to be changed frequently, thus a spare is of time in a high humidity environment,
a necessity. Bead Life water may accumulate in the detector.
To evaporate this water, set the detector
The beads have to be kept dry which limits To extend the life of the bead: temperature to 100˚C and maintain it
their storage life to about six months.
● Use the lowest practical adjust offset or for 30 minutes. Then set the detector
When a new bead is installed, slowly raise
bead voltage. temperature to 150˚C and maintain it
the detector temperature and bead current.
for another 30 minutes.
Rapid heating can crack or break the bead ● Run clean samples and keep the
especially if it has been stored under humid inlet/liner clean to minimize
conditions. It has been observed that contamination.
www.agilent.com/chem 45
DETECTORS
Gas Flow Cleaning & Replacement the FID jet. Although you can clean the jet,
it is usually more practical to simply replace
The hydrogen, air and makeup gas flows The NPD requires periodic cleaning. In
dirty jets with new ones. If you do clean the
should be measured frequently. They can most cases, this only involves the collector
jet, use the cleaning wire, taking care not
drift over time or be changed unintentionally and the jet. Agilent provides brushes and
to damage the inside of the jet. You can
without knowledge of it occurring. Each gas wires that simplify the cleaning of all
also use a sonicator bath to clean the jet.
flow should be measured independently to detector parts (see FID Supplies on page
obtain the most accurate values. NPDs are 53). The brushes are used to dislodge
very sensitive to changes in the gas flows particulates clinging to the metal surfaces. Contaminants
and consistent flows are necessary to A fine wire is used to clean the jet opening
maintain performance levels. of particulates. Do not force too large a Some chemical problems can also arise
wire or probe into the jet opening or the when using the NPD. Because it is a trace
opening will become distorted. A loss of detector, be careful not to contaminate the
Gas Purity sensitivity or poor peak shape may result if analytical system.
Because of its high sensitivity, the NPD the opening is deformed. The various parts
Glassware
requires very pure gases (99.999% or can be ultrasonicated after cleaning with
a brush. Eventually the jet needs to be Glassware must be very clean. Phosphate
better). We strongly recommend that
replaced, so it is strongly recommended detergents should be avoided, so acid
moisture and hydrocarbon traps be used
to have spare jets on hand. washing of glassware followed by distilled
on the carrier gas and all detector gases,
water and solvent rinsing is recommended.
including the detector hydrogen, air, and Over time, residue from the bead or sample
makeup gases. Dirty gases will not only can build up in the collector and cause Solvents
give poor chromatographic performance, baseline problems. You should clean the Solvents should be checked for purity.
but will shorten the bead life as well. collector after you have changed the bead Chlorinated solvents and silanizing
two or three times. reagents can decrease the useful lifetime
The metal C-rings wear slightly with each of the alkali source; excess reagent should
assembly and disassembly. After several be removed prior to injection, if possible.
assemblies and disassemblies (five or
more), the rings may not seal effectively, Other Contamination Sources
causing an erratic baseline. A ceramic Phosphate-containing leak detectors,
insulator and seal kit is available. Always phosphoric acid-treated columns or glass
cool the detector to near-ambient when wool, polyimide-coated columns, or
changing seals and insulators. nitrogen-containing liquid phases can add
noise to the system and should be avoided.
Because there is no flame in the NPD, the
jet does not collect silica and soot as does
NPD Jets
6890/5890 Adaptable
46 www.agilent.com/chem
DETECTORS
4 12
6 Collector funnel G1534-20530
5
7 Alumina insulator, lower G1534-40030 6
9 Screw, M4 x 10 mm 0515-2495
10 J-Clamp 1400-0015
11 Screw, M4 x 10 mm 0515-2495
*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.
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
ECD adapter fused silica liner micro ECD G2397-20540 ECD Make up Gas Adapter
www.agilent.com/chem 49
DETECTORS
50 www.agilent.com/chem
DETECTORS
12 Coupling, SS 19256-20550 20
15 Clamp 19256-00090
16 O-ring, inner window 12/pk 5061-5886
17 Window, second heat shield 19256-80060
18 O-ring, outer window 12/pk 5061-5891
19 Flange adapter 19256-20510
20 Flange ring 19256-00200
21 O-ring, Viton, 1.239 in. id 12/pk 5061-5890
Adapter weldment, 1/8 in. columns 19256-80590
Adapter weldment, capillary 19256-80570
Start-up kit (5890 only) 19256-60500
FPD O-ring (5890 only) 12/pk 5061-5867
HELPFUL HINT: Install the correct optical
Liner/ferrule kit 19256-60590 filter, depending on the choice of Sulfur or
Sulfur filter 19256-80000 Phosphorus mode. For Sulfur Mode, use
the 393 nanometer filter. For Phosphorus
Phosphorus filter 19256-80010
Mode, use the 525 nanometer filter.
Kalrez O-ring, size 2-002 0905-1101
Kalrez O-ring, size 2-011 0905-1103
Fluorocarbon Elastomer O-ring,
brown, 0.926 in. id 12/pk 5061-5889
FPD Performance Evaluation Sample: Solution of
20 ng/mL (20 ppm) dodecanethiol and
tributylphosphate in isooctane, 3 ampoules 19305-60580
www.agilent.com/chem 51
DETECTORS
Condensation
Since the FID combustion process
results in water formation, the detector
temperature must be kept above 100˚C to FID Jets
prevent condensation. Such condensation,
especially when combined with chlorinated
solvents or samples, causes corrosion and
sensitivity loss.
52 www.agilent.com/chem
DETECTORS
6. Blow the jet dry with a burst of the Ignitor castle 19231-20910
compressed air or nitrogen, and then Hastelloy Ignitor Castle 19231-21060
place the jet on a paper towel and allow
it to air dry. Ignitor glow plug assembly 19231-60680
FID collector cleaning brush 2/pk 8710-1346
FID retainer nut wrench
(5880, 5890, 6890) 19301-00150
1/4 in. Nut Driver for FID jet-drilled shaft 8710-1561
FID flow measuring insert 19301-60660
O-rings for flow measuring insert 12/pk 5080-4978
FID Performance evaluation sample kit,
0.03% C14, C15, and C16 normal
alkanes in hexane 18710-60170
Jet cleaning wire for 0.03 in. id jet 5/pk 5180-4150
Jet cleaning wire for Series 530 mm
and 0.018 in. id jet 5/pk 5180-4152
FID cleaning kit 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)
Only a small sampling of FID supplies are shown here. For a complete selection,
www.agilent.com/chem see the Agilent 2002-2003 Chromatography & Spectroscopy Supplies Reference Guide. 53
DETECTORS
FID Jets
Capillary 0.53 mm jet (0.011 in. id tip) 61.5 19244-80560 Agilent FID Jets (from top to bottom): Dedicated
capillary, Adaptable capillary, Adaptable packed
Packed (0.018 in. id tip) 63.5 18710-20119
0.53 mm high temp (0.018 in. id tip) for SimDIS 61.5 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 www.agilent.com/chem
Service & Support
Every Agilent GC system is backed by a
wealth of knowledge, all at your fingertips.
Tap our 35 years of instrument expertise
and applications knowledge by phone, in
person, in print, or on-line. Contact us for
a variety of service and repair options from
telephone support, on-site repair, even
product exchange. Take advantage
of our industry leading training courses
to help increase the overall knowledge in
your lab.
Any way you want, you get the full support
of Agilent expertise and service with every
GC system.
www.agilent.com/chem 55
SERVICE & SUPPORT
56 www.agilent.com/chem
SERVICE & SUPPORT
www.agilent.com/chem 57
SERVICE & SUPPORT
Software Support
Only Agilent can provide expert assistance
to isolate and resolve software problems.
We’ll provide telephone assistance from
highly trained experts. We’ll provide all Open inside cover for:
enhancements to the original chemical
analysis software purchased. We’ll even GC System
send you Software Bulletins to let you Recommended
know about ongoing issues and
recommended workarounds. Contact
Maintenance
Agilent today for more information about Schedule
these and other Support Services. ● Technical Support Assistance (a logical,
Hardware Support step-by-step approach to help you solve
common problems)
Agilent’s highly trained technical staff is
just a phone call away to offer you basic ● Technical Document Library (a searchable
hardware troubleshooting, operation collection of service and support
assistance, instrument and system documents)
configuration, and remote diagnostics. Call ● Chromatogram Library (a searchable
us toll-free today, or submit your question collection of GC, LC, and CE
on-line at www.agilent.com/chem. chromatograms – nearly a thousand
Stay on Top with “Separation Times” chemical compounds)
58 www.agilent.com/chem
GC System Recommended Maintenance
Gas Management
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
Gas purifiers Every 6-12 months Replacement schedule is based on capacity and grade of gases.
(carrier gas & In general, replace non-indicating traps every 6-12 months or when
detector gas) indicating traps start to change color. Replace indicating traps when
indicating material is spent.
Split vent trap Every 6 months* Replace.
Flowmeter Every 1-2 years Re-calibrate electronic flowmeters – follow recommended schedule for
calibration the unit (shown on calibration certificate).
Syringes Every 3 months* Replace syringe if dirt is noticeable in the syringe, if it cannot be
and/or syringe cleaned, if the plunger doesn’t slide easily, or if clogged. Replace
needles needle if septa wear is abnormal or the needle becomes clogged.
Inlet liner Weekly* Check often. Replace when dirt is visible in the liner or if
chromatography is degraded.
Liner O-rings Monthly* Replace with liner or with signs of wear.
Inlet septum Daily* Check often. Replace when signs of deterioration are visible
(gaping holes, fragments in inlet liner, poor chromatography,
low column pressure, etc.).
Inlet Hardware Every 6 months Check for leaks and clean.
Every year Check parts and replace when parts are worn, scratched, or broken.
Columns
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
Front-end Weekly – monthly* Remove 1⁄2 -1 meter from the front of the column when experiencing
Maintenance chromatographic problems (peak tailing, decreased sensitivity, retention
time changes, etc.). Replace inlet liner, septum and clean inlet as
necessary. Guard column may be useful for increasing column lifetime.
Solvent rinse As needed When chromatography degradation is due to column contamination.
Only for bonded and cross-linked phases.
Replacement As needed When trimming and/or solvent rinsing no longer return chromatographic
performance.
Ferrules Replace ferrules when changing columns and inlet/detector parts.
Detectors
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
FID/NPD Jets As needed Clean when deposits are present. Replace when they become scratched,
& Collector bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead As needed Replace when signal drifts or there is a dramatic change in sensitivity.
FID Every 6 months Measure hydrogen, air, and makeup gas flows.
TCD As needed Thermally clean by “baking-out” when a wandering baseline, increased
noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.
ECD Every 6 months Wipe test.
As needed Thermally clean by “baking-out” when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD Every 6 months Measure hydrogen, air, and makeup gas flows.
As needed Clean/replace FPD windows, and seals when detector sensitivity
is reduced.
www.agilent.com/chem