Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
At Agilent Technologies, we understand that many of today’s labs face the challenge
of operating with a reduced staff. That’s why we’re committed to bringing you the
world’s best GC and GC/MS systems — plus the critical information you need to keep
them running properly.
In this newly updated Maintenance Guide, we share everything from essential service
schedules … to invaluable troubleshooting tips and problem-solving methods.
We’ve even included easy guides to help you order Agilent parts and supplies —
which have 40 years of high quality and technical experience built right in. So you can
keep your downtime to a minimum, and get the results you need.
Don’t Miss…
GC Maintenance Schedule (inside back cover)
1 www.agilent.com/chem
Gas Management
The use of quality carrier gases is essential
for consistent and accurate GC analyses.
Proper gas management is key to achieving
this goal. Agilent provides a diverse line of
high quality gas management products —
gas purifiers, regulators, leak detectors
and flowmeters — all designed to prevent
column damage, improve detector life, and
improve the quality and consistency of your
GC separations. This section explains how
common contaminants like oxygen, moisture
and hydrocarbons can damage your GC
column, and helps you understand how to
prevent it. Also, look for practical information
about regulators, the importance of clean
GC-tubing, and minimizing the likelihood
of GC system contamination.
CATALOG
www.agilent.com/chem 2
GAS MANAGEMENT
Gas Types
Carrier Gases
The most frequently used carrier gases are bleed, along with column and/or detector dioxide) and pneumatic gases (air or
helium and hydrogen, although nitrogen damage. The following sections describe nitrogen) generally do not come in contact
and argon can be used. Purity is essential the gases and purities that are necessary with the sample or detector. Therefore,
for these gases since they sweep the for gas chromatography carrier gases, as these non-contact gases do not have to
sample through the column where it is well as other support gases. be the highest purity available.
separated into its component parts and
Support Gases Fuels, oxidants and detector gases, in most
then through the detector for component
Support gases may be specific for cases, do come in contact with the sample
quantification. Carrier gas purity is also
detectors or for applications. These gases and detector, and require higher purity
critical to prevent degradation of
include fuels, oxidants, coolants, detector gases. Unfortunately, gas nomenclature as
chromatographic hardware.
gases, and pneumatic gases. The degree it relates to purity is not consistent across
Contaminants in carrier gases can have of purity required for support gases is specialty gas suppliers. It is important to
a significant effect on column life and dependent on how that gas is being used, recognize the impurities in your gas
subsequent analyte detection. Harmful and whether or not it will make contact supplier’s products, and to utilize the
effects of impure gases include with the sample. Coolant gases (carbon appropriate Agilent gas purification
contaminant peaks and elevated column products (see next section).
Sample
Gas Type Function Contact Purity Required*
Hydrogen/Helium Mix Fuel gas for detector Yes Research Ultra-Pure Ultra-Pure UHP/Zero
3 www.agilent.com/chem
GAS MANAGEMENT
www.agilent.com/chem 4
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 introduced into the gas stream due to the
enhancement by traps to the GC system is leak will be removed by the trap until it
obtained by traps when using very high expires. This creates an opportunity to
purity gases (e.g., ultra-high purity or detect and fix the leak before column or
similar grades) while obvious improvement instrument damage occurs.
is obtained with lower grades of gas.
5 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)
www.agilent.com/chem 6
GAS MANAGEMENT
Oxygen Traps
Oxygen traps usually include a metal- plastics are permeable to air and contain
containing inert support reagent. Most contaminants that can degrade gas quality.
oxygen traps reduce the oxygen In addition, many of the metal bodied
concentration to below 15-20 ppb. The oxygen traps can withstand high pressures
Indicating Oxygen Trap
capacity of a standard oxygen trap is (up to 2000 psi). Some oxygen traps also
approximately 30mg of oxygen per 100cc remove moisture from the gas stream
of trap volume. Oxygen traps can also without affecting the oxygen removal
remove some small organic and sulfur capability.
compounds from gas streams, but this is
Indicating oxygen traps change color when
not their primary application.
oxygen is present in the gas at harmful
Big Oxygen Trap
Metal (usually aluminum) trap bodies are levels. Indicating traps are not intended to
recommended for GC analyses. Some be the primary oxygen removal trap, but
Oxygen Traps should be used in conjunction with a high
capacity non-indicating oxygen trap. They
1/8 in. 1/4 in. are installed after the high capacity oxygen
Description Size (cc) Part No. Part No. trap in the gas line to indicate when the
high capacity trap has expired and needs
Indicating Oxygen Traps – glass body with plastic safety shield to be changed. Expired oxygen traps need
to be immediately changed since they can
Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP
contaminate the gas, in addition to failing
Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller size to remove oxygen.
available, see Agilent catalog)
Hydrocarbon Traps
Hydrocarbon Traps
Hydrocarbon traps remove organics, such
1/8 in. 1/4 in.
as hydrocarbons and halocarbons, from
Description Size (cc) Part No. Part No.
the gas stream. The adsorbent is usually
Hydrocarbon Traps – General Purpose activated carbon or an impregnated carbon
filter media. Carbon removes organic
Refillable Hydrocarbon Trap 200 HT200-2 HT200-4 solvents from the gas stream, including the
typical solvents used in nearly every lab.
Adsorbent Refill (1 pint, 2 refills) ACR ACR Hydrocarbon-moisture combination traps
Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity
are also available which remove water in
7 www.agilent.com/chem
GAS MANAGEMENT
Hydrocarbon S-Trap
Combination Traps
Agilent carries several Combination Traps • Efficient design which prevents
that provide multiple contaminant removal channeling and promotes efficient
in a single trap. These traps offer: scrubbing
• Optimized adsorbents for maximum • The ultimate in purification with a single
surface area and capacity trap (Big Universal Trap)
• Leak-free, one-piece design to eliminate
potential leaks from using multiple traps
Oxygen/Moisture Traps
Hydrocarbon/Moisture Traps
Big Universal Traps – for the Ultimate in Gas Purification, removes oxygen, moisture,
hydrocarbons, CO, and CO2 Big Universal Trap
www.agilent.com/chem 8
GAS MANAGEMENT
High Capacity
Gas Purification System
Three Cartridge System Single-Cartridge System
• Agilent’s highest capacity and most • Contains a triple-combination cartridge
economical gas purification system. that offers the same highly efficient
Three Cartridge
High Capacity contaminant removal properties from
• Provides low-cost gas contaminant
Gas Purification eight cylinders of carrier gas but without
System
removal for up to 18 cylinders of
the visual indicator.
carrier gas.
• Other cartridges are also available for
• Includes a manifold with cartridge
detector gas supplies and as individual
mounts and three replaceable cartridges:
filters for specialized requirements.
one moisture/hydrocarbon cartridge; one
oxygen cartridge; and one oxygen
indicating cartridge.
• Consists of a permanent all-welded
stainless steel manifold to minimize
the potential for leaks.
• Suitable for bench or wall mounting.
9 www.agilent.com/chem
GAS MANAGEMENT
4-Head
Replacement Cartridges
Hydrocarbon GC-3
From oxygen traps to purification systems, you can find all your
gas management supplies … all in one place.
Just visit www.agilent.com/chem/4ecatalog
www.agilent.com/chem 10
GAS MANAGEMENT
11 www.agilent.com/chem
GAS MANAGEMENT
Regulators
Pressure regulators are an integral A dual stage regulator overcomes this
component in any gas handling system. problem by connecting two regulators
Their function is to reduce the pressure together. The first stage regulates the
from a high pressure source, such as a pressure to the second stage, thus creating
cylinder, to a suitable use pressure. a constant pressure and allowing minimal
Brass Body Regulator
Although regulators are very good at inlet decay. Agilent recommends using
controlling pressure, they do not control two-stage regulators with our GC Systems
flow. They have a maximum flow rate to provide the proper pressure control for steel diaphragm regulators for most GC
which is dictated by the design. Basically, optimal use. applications. These regulators, combined
the flow is determined by the pressure with the proper gas purification system,
drop across the regulator. Regulator Materials provide proper gas pressure control and
Regulators are usually constructed of brass purity for gas chromatography.
Types of Regulators or stainless steel. The choice of material
There are primarily two types of regulators: follows the same guidelines as the choice When ordering a regulator, be sure to
single stage and dual (or two) stage. of tubing. Generally, it is not recommended specify the proper connections. In the
The difference is that a dual stage that the materials be interchanged. If US, most gas manufacturers follow CGA
regulator is actually two regulators stainless steel tubing were chosen due connection guidelines. In Europe, there
connected in a series. to purity considerations, then a stainless are a number of organizations designating
steel regulator should be chosen for the cylinder connections that are specific to
Dual stage regulators provide more precise individual countries. It is best to contact
same reasons. Steel regulators are more
and consistent pressure control than single your local supplier for the proper
expensive, which is why Agilent offers
stage regulators. The reason is that in a connection designation.
brass regulators for less demanding
single stage regulator, as the gas cylinder
applications.
empties and the inlet pressure to the
regulator decreases (inlet decay), the No matter which material is chosen for the
pressure on the diaphragm is reduced. regulator body, be sure to specify one with
Without proper adjustment, the outlet stainless steel diaphragms for critical
pressure might slowly rise. applications such as use on carrier, fuel or
detector gases. Agilent recommends using
our economical brass body, dual stainless
CGA 350, 125 psig max (8.6 bar), H2, Ar/Me 5183-4642
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 12
GAS MANAGEMENT
Tubing
When constructing or maintaining a gas as pressurizing pneumatic lines; however,
delivery system for GC, choosing the be aware of its pressure limitations.
proper tubing material is very important
In view of these problems, the list of
and will help to eliminate potential
appropriate tubing materials has been
problems and improve the overall quality of
narrowed down to two: copper and
the gas system. Although there are many
stainless steel. Agilent recommends using
common tubing materials available, some
copper tubing for most applications, since
pose safety or cleanliness problems.
it is easy to bend and plumb and is less
Non-metallic types of tubing such as expensive than stainless steel. Use
polyethylene and Teflon are not stainless steel tubing only for crucial
recommended for GC applications due applications that require very high purity,
Spectra-Link Tubing Connecting System to their gas permeability and difficulty or where building codes mandate its use.
on a two-stage regulator in cleaning. This type of tubing can be
used for non-critical applications, such Cleaning Tubing
Before any tubing is placed into service,
or if it becomes contaminated with use,
Determining Tubing Length it is essential that it be properly cleaned.
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig Unclean or improperly cleaned tubing can
lead to contamination of the system with
Tubing Type Diameter Recommended Pressure Drop disastrous results.
(inches) Max. Length (feet) (psig)
Cleaning tubing requires the use of
Copper 1/8* 50 2 suitable detergents and solvents along
with nitrogen and a purgeable oven for
Copper 1/4* 300 0.5 drying. This may be done easily for small
lengths of tubing, but in larger systems the
*Recommended when multiple instruments are connected to the same source
cleaning procedure sometimes becomes
unwieldy, leaving behind a large quantity
of solvent requiring proper disposal.
Fortunately, Agilent provides clean, high
Tubing–Precleaned quality GC grade tubing for large systems
as an economical alternative.
Description Part No.
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
Cylinder Bracket
Leak Detection
Leaks allow oxygen and other gas leaks for 12 common gases. Based on a
contaminants to enter the gas stream. dual cell micro volume thermal conductivity
Therefore, GC instrument maintenance system, this unit provides very high
should include checking fittings and sensitivity and eliminates contamination
connections with a gas leak detector. caused by soap solution methods.
Agilent’s Gas Leak Detector enables quick
and easy detection and measurement of
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 14
GAS MANAGEMENT
Flow Rates
Setting and maintaining GC flow rates Selecting a Flowmeter
greatly affect the instrument accuracy Agilent manufactures the largest selection
and sensitivity. During maintenance, of volumetric and mass flowmeters for
verify carrier and support gas flows chromatography. We have developed
with the proper flowmeter. Choosing a flowmeters for measuring capillary column
flowmeter for your application depends flows, calibrating air pumps and flow
upon measurement speed, ease of use, controllers, and verifying instrument gas
accuracy, and flow rate range. flows. All flowmeters are calibrated to
NIST-traceable standards.
15 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
www.agilent.com/chem 16
You asked … we listened!
CATALOG
www.agilent.com/chem 18
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Sample Introduction
Vials Vial Filling
Agilent’s wide opening vials are designed When filling sample vials, keep in mind:
specifically for analyzing samples with your
• if you need to test a large amount of
GC. They have specially designed vial neck
sample over repeated injections, divide
angles, bottom design and height to ensure
the sample among several vials to obtain
compatibility with Agilent autosamplers
reliable results
with rotating or robotic arm trays. Agilent
offers a large variety of autosampler vials • when sample volume in the vial is low,
in different closures, cap colors, septa contaminants from the previous sample
choices and package options. Agilent also injection or solvent washes may have a
offers convenience packs with 500 vials greater impact on the sample.
and caps in a reusable blue storage box.
The airspace in the vial is necessary to
For small sample sizes, Agilent offers a avoid forming a vacuum when sample
variety of options. You can use microvolume is withdrawn. This could affect
inserts with the wide opening vials or, for reproducibility.
added convenience, use vials with small
volume capacity.
Vial Options
Glass–for general purpose Silanized–for use with Polypropylene –for use Amber Vials–for use with Microvolume Inserts–for High Recovery Vials–
use and for use with acids samples that bind to glass, with alcohols and aqueous light-sensitive samples use with very small sample for use with limited sample
and for trace analyses solvents volumes volumes
1 mL 50 µL
3.6 mm*
100 µL vial
*Needle position based on standard sampling depth.
19 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Red Rubber/Teflon
• Routine analysis Determining Your Quantity Needs
• Moderate resealing
To determine potential septa ordering
• Excellent chemical inertness
quantities, consider:
• Not recommended for multiple
• the number of samples run during a
injections or storage of samples
day/week
• Least expensive Unattended autosampler
• if samples are run in small or large
runs require a precise fit for
www.agilent.com/chem 20
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Packed, split or
splitless (including PTV) 23 gauge or 23/26 gauge tapered any
Needle tips
Sharp tip Cone tip
Tapered needle
For best results, use the Agilent Cone Tip (HP Point Style) with
Agilent’s Centerguide Septa, page 38.
21 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
www.agilent.com/chem 22
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Syringe Tips
• Make sure to input the proper syringe • Remove a gas-tight plunger from the • To maximize the lifetime of standard
size when setting up the injection section syringe for long-term storage to keep the plungers, rinse the syringe and wipe
of your data handling device. Teflon tip leak-free. If a gas-tight plunger the plunger with solvent (isopropanol
does not fit properly, place it in hot water or acetone) and a lint-free wipe, as
• Rinse syringes and clean their plungers
for about 10 minutes then press the tip specified in the syringe cleaning
before use to maximize syringe lifetime.
uniformly on a clean, hard surface and let procedure included with each syringe.
• Rinse the syringe 5-8 times between cool to room temperature. The plunger
injections to minimize sample carryover. should reseal correctly to provide 10-25%
more injections.
• Pump sample in and out of the syringe at
least 5 times to remove any air bubbles,
and for maximum reproducibility and
accuracy.
• A 26-gauge syringe can be used for
on-column injections into a 0.53mm id
column. Always check that on-column
syringe needles fit inside the capillary
column before installing the column
and syringe in the GC.
• For on-column injections, always use
the proper septum nut and stainless steel
insert for the column dimension you are
using. Use a septum with a molded
through-hole with injections onto 0.32mm
and 0.25mm columns.
• The more polar the solvent, the more
likely it is to contain water. Trace
amounts of water, especially when
combined with water-extractable
materials from samples, can accelerate
syringe wear dramatically. With these
types of samples, use a Teflon tipped
syringe plunger. Even better, proactively
replace syringes, since plunger bends
may be inevitable.
VIDEO
23 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Bent plungers or stuck syringes • Particles such as dust, leftover samples, salts, • If the plunger’s movement feels “gritty,”
metal, or glass can fill the narrow gap between remove the plunger from the barrel, flush the
the plunger shaft and the inside wall of the shaft with solvent, and wipe it dry with a lint-
barrel. free cloth. Then, carefully insert the plunger
back into the barrel. Finally, submerge the tip
of the needle into a container of solvent, and
cycle the plunger to pull the solvent into and
out of the barrel.
• Never cycle the plunger in a dry syringe.
• Do not “mix & match” plungers and barrels.
• Always clean syringes after use.
Bent needles • Improper needle alignment. • Use only Agilent autosamplers. They are
• Narrow-gauge needles (26 gauge) bend more precision-designed to ensure proper
easily than larger (23 gauge) needles. alignment with the syringe needle.
• Needles tend to bend when inserted into the • Use 23 to 26-gauge tapered needles to get
sample vial – not the inlet port. This can be the combined benefits of greater septa life
caused by septa that are too “tough.” and fewer bent needles.
• If the needle has been slightly bent when • Only use Agilent vials and septa.
mounted in the autosampler – or when the
syringe is installed into the autosampler – then
it is more likely to bend further when it pushes
through the septa on the sample vial caps.
Blocked needles • Sample material or contaminants may be • Remove the plunger and use a second
trapped inside the needle. syringe to fill the blocked syringe with
• The needle may not have been properly cleaned. solvent. Then, insert the plunger and gently
push solvent through needle. Important: Try
to use a cleaning agent that is appropriate for
the contaminant. Common choices are
methanol, methylene chloride, acetonitrile,
and acetone.
Rust • During normal use, the shaft rubs against the • To slow this process, remove the water from
Note: even minor rust can cause the plunger glass walls of the barrel. This gradually wears the syringe at the end of each day.
to become stuck in the barrel. away the rust-resistant metal on the shaft’s 1. Rinse the syringe several times with a “dry”
surface. solvent, such as acetone.
• Rusting happens most rapidly when using water 2. Remove the syringe from the autosampler,
or solvents that may contain (or absorb) water. and wipe the plunger dry with a lint-free
cloth
3. Let syringe and plunger air dry.
“Ring around the neck” (A dark ring between • Skin oils and other organic material. • Never touch the plunger shaft with your
the top of the barrel and the end of the • Fine metal and glass particles from the syringe fingers.
volume scale.) plunger and barrel may be rubbing together. • If build-up appears when water is the
Once this happens, the plunger may bend if solvent: rinse syringe with acetone and wipe
used further. the plunger clean at the end of each day.
Loose plungers – accompanied by syringe • The syringe is nearing the end of its useful life. • Replace the syringe.
leaks and area count reproducibility problems. Note: Plungers normally feel “loose” when
non-polar solvents (like hexane and toluene)
are used.
www.agilent.com/chem 24
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
25 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Packed-Column Inlets
Packed-column direct inlets are very
popular. Packed-column analysis is
frequently done when high efficiency Packed-Column Inlet Procedures/Practices
separations are not needed or when gases
are analyzed by gas-solid chromatography. Parameter Selection/Setting Rationale
Packed-column inlets are simple in both
Inlet temperature BP of solvent +50˚C Ensures flash vaporization
design and use. Few parameters need to
BP of major solute(s) Use for neat samples
be set, and all carrier gas flow flushes
through the inlet into the column in the Insert type 1/8-inch stainless steel Use for ss column only
standard configuration. 1/4-inch stainless steel Inserts permit connection of
columns up to 1/4-inch od.
Liner Glass Use to lower activity
(replaceable)
Initial column temperature programming Sharpens peaks and
temperature reduces run time
Column type 1/8-inch packed stainless Will not break
1/4-inch packed glass Better for polar or labile
compounds
Carrier gas flow 20-40 mL/min Use with N2 carrier gas
30-60 mL/min Use with He or
H2 carrier gas
Troubleshooting
Most problems with packed-column inlets The inherent activity of packed-column Leaks
involve sample decomposition, flashback, inlets is somewhat mediated by the fact Since packed-column inlets are usually
or leaks. that they usually have low internal volume. flow-controlled, septum and column leaks
When this is coupled with the relatively will have a direct impact on retention times
Decomposition fast flow rates used with packed columns, and peak areas. Sample can be lost
Since packed-column inlets are active, the residence time of sample in the inlet is through the leak holes, and air can diffuse
especially if glass liners are not used, polar short and decomposition is reduced in back into the inlet to cause column
sample components will often tail or comparison to the decomposition that degradation. Change the septum on a
degrade in the inlet. Sample decomposition occurs with some capillary inlets (for regular basis and check column
caused by the inlet is easily diagnosed; the example, splitless inlets). connections at the first stage of problems.
decomposition products will have peaks at To prevent stationary phase decomposition,
the same retention times as standards for Flashback make sure that the oven and inlet are at
the decomposition product. The negative side of low inlet volume, room temperature when not in use and
however, means that excessively large when changing the septum.
When inlet-caused decomposition is
sample injections will easily exceed the
suspected, try intracolumn direct injection,
capacity of the liner and will flash back into
deactivated glass liners, or lower inlet
gas supply lines and onto the septum. This
temperatures, and remove any column
can cause several maladies, including
packing in the inlet zone.
ghost peaks, sample losses, irreproducible
peak areas, and decomposition.
www.agilent.com/chem 26
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
11
27 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Split/Splitless Inlets
The combined “split/splitless” inlet is the Troubleshooting
most popular inlet for capillary column gas Split inlets are spared from most band- A majority of the problems encountered
chromatography. Because it can be used in broadening phenomena, since narrow with split inlets are related to discrimination
either split or splitless mode, it provides a peaks are generated as part of the splitting and decomposition. Both analytical
very effective combination that can cover process. Therefore, any peak broadening accuracy and reproducibility decrease
most analysis requirements. or tailing observed with split injection is with the increases in discrimination
usually due to improper column and decomposition. Split inlets suffer
Split Mode installation, low split flow, (<20 mL/min from both needle discrimination and
Split injection is an effective way to on 6890) or low inlet temperature. If you inlet discrimination.
introduce small amounts of sample without suspect that the inlet temperature may be
overloading the column. Split injection is too low, increase it by 50˚C and compare
required for samples that: the results to the lower temperature
• cannot be diluted for analysis (for analysis. Repeat if results are positive
example, solvents) until no further improvement is seen.
• are gases that cannot be focused, or
that have long injection times (valve
injections)
• have important minor peaks eluting
directly before the solvent peak (as in
solvent analysis) Split Mode Variables, Practices, and Rationales
For fast and easy liner changes, check out Agilent’s new Flip Top Inlet Sealing System on page 52.
www.agilent.com/chem 28
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
VIDEO
29 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Troubleshooting
Most problems encountered with splitless Decomposition
injection are related to incorrect purge Loss of peak area or generation of new
time, degradation, improper focusing, and peaks, can sometimes be dramatically
flashback. reduced by changing liner type or by
deactivating the liner and inlet with
Appropriate initial column temperature is
silanizing reagents. Removing or reducing
critical. Sample vapors can be lost through
the amount of liner packing can also
the septum purge line if the insert is
decrease inlet activity.
overfilled with sample vapor (either too
large injection volume or too small liner
volume), leading to irreproducibility and
nonlinearity of peak areas. Match inlet
temperature, liner volume, and injection
volume carefully to avoid backflash.
www.agilent.com/chem 30
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Initial inlet temperature = or 3˚C above column oven temperature Ensures sample focusing in solvent front
Initial inlet temperature ramp Same as oven (oven track) Faster than oven Simple and effective
Narrows initial peak width
Injection volume 0.1-2.0 µL liquid Use smaller injections for small id columns;
Depends on column capacity
Injection technique Fast autoinjection Projects droplets away from syringe tip
Fused silica needle Use for manual injection into small id columns
Oven temperature Inlet temperature or slightly lower Prevents backflash
Column flow 50-80cm/sec Use for H2 carrier gas
30-50cm/sec Use for He carrier gas
Septum purge 12-15mL/min Use if installed to prevent ghosting
Quantification All methods Inherently reproducible technique
Lack of discrimination
Retention gap requirements 1-3m, deactivated Corrects peak distortion
Protects column from non-volatile components
Permits autoinjection with narrow-bore columns
Since the sample is directly deposited into the column, nonvolatile sample components
can accumulate at the head of the column and will degrade efficiency and/or interact with
subsequent injections.
31 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
VIDEO
www.agilent.com/chem 32
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
33 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
VIDEO
www.agilent.com/chem 34
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
0.53 mm 5182-9762 7
8
9 Ferrules for 0.20 mm 10/pk 5182-9756 9
10
Graphpak inlet 0.25 mm 10/pk 5182-9768
0.32 mm 10/pk 5182-9769
0.53 mm 10/pk 5182-9770
10 Split nut for inlet adapters 5062-3525 11
PTV Liners
35 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Septa
One of the key components of sample What is the Function
introduction is the inlet septum. All The septum isolates the sample flow path
columns must have carrier gas head from the outside world. It must provide a
pressure to establish flow through the barrier that is readily penetrated by the
column. Septa maintain the leak-free seal injector needle while maintaining internal
and exclude air from the inlet. They come pressure without contaminating the
in many different sizes and are made from analysis. They are generally made of
many different types of material specific special high-temperature, low-bleed
to inlet type and analysis needs. silicone rubber formulations.
Septa are usually available according to Why Replace
their recommended upper temperature Septa should be replaced regularly to avoid:
limits. Lower temperature septa are • leaks
usually softer, seal better, and can • decomposition Agilent Introduces Innovative
withstand more punctures (injections) • sample loss
than their high-temperature counterparts.
Packaging for Inlet Septa
• reduced column or split vent flow
If used above their recommended • ghost peaks Agilent has recently introduced a new
temperatures, however, they can leak or • column degradation and innovative packaging design for
decompose. This causes sample losses, inlet septa. This new packaging is a
lower column flow, decreased column life How to Minimize Problems tri-fold blister pack that provides
and ghosting. Avoid problems by: cleanliness, convenience, and
• using within the recommended consistency for our complete line
temperature range of 11 mm and 9.5 mm septa.
• changing regularly
• installing “hand tight” Your 50th Septum will be
• using septum purge when available as Clean as Your 1st!
• using autoinjectors
• using sharp syringe needles The primary benefit behind the new
packaging is that each septum is
individually packaged for the ultimate
cleanliness. Each septum is easily
dispensed one at a time by pushing it
through the back foil, as is commonly
done with pharmaceutical capsules and
tablets. No longer do you need to reach
into a jar and wonder how clean the
septa are or if you are contaminating
other septa.
In addition, the new packaging delivers
the following features and added value:
• No more clumping or sticking: Septa
don’t stick to each or the jar
• Easy to see exactly how many are
left: Know exactly when to reorder
• Compact storage size: Fits easily into
drawers
• Convenient quantities: All septa are
packaged in either 50 or 100 packs
• High quality PET packaging: Tested by
GC-FID, GC/MS, and GC-ECD to
ensure the absence of interfering
background peaks
www.agilent.com/chem 36
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Septa Troubleshooting
Extra Peaks/Humps Septum bleed. Turn off injector heater. If extra peaks
disappear, clean the inlet and change the
liner. If cored septa particles are present,
use a centerguide septa and a 23-26 gauge
tapered syringe. Important: always use the
septum specified for higher temperature or
analyze at lower inlet temperature.
Normal Problem
Baseline Change After Large Peak Large leak at septum during injection and Replace septum and use smaller diameter
for a short time thereafter (common with needles.
large diameter needles).
Retention Times Prolonged Carrier gas leaks at septum or column Check for leaks. Replace septum or tighten
connection. connections if necessary.
MAINTENANCE MINDER
37 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Other suppliers coat their septa with powder to prevent sticking. However, this
coating can accumulate inside split vent lines and interfere with the analysis of
active analytes.
Agilent’s plasma-treated non-stick septa But Agilent’s new non-stick septa are plasma coated, which eliminates chemical
bleed and contamination from foreign substances. So your GC system will maintain
its integrity, stay cleaner and require less maintenance.
www.agilent.com/chem 38
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Agilent’s premium GC inlet septa are not garden-variety septa Figure 1. Comparison of Coring, With and Without CenterGuide
(30x magnification)
stamped out in large sheets, creating variations in geometry. Rather,
each Agilent premium septum is molded to a perfectly uniform size High-Temperature Septa Without CenterGuide: Major Coring Before 1
and shape. 00 Autoinjections
TEMPERATURE
SEPTUM TYPE BLEED LIFETIME LIMIT
39 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Agilent Bleed and Temperature Agilent Long-Life Non-Stick Septa Agilent Advance Green
Optimized Non-Stick Septa (BTO) • Pre-pierced for extended life and Non-Stick Septa
• Extended temperature range, low-bleed reduced coring • True Long-Life, High Temperature
• Maximum Injection Port Temperature • The preferred Septum for Autosamplers Green Septum
400ºC • Ideal for Overnight Runs • More Injections per Septum
• Virtually eliminates injection-port • Up to 400 Injections Per Septum injection • Reduced Injection Port Sticking
sticking • Maximum Injection Port Temperature
• Maximum Injection Port Temperature
• Pre-conditioned; packaged in glass 350ºC 350ºC
to prevent contamination • Packaged in glass vials for high purity
• Soft, 45 Durometer, Easy On
• Ideal for use with low-bleed, Autosampler Needles • Economical alternative to competitor’s
“Mass Spec” capillary columns “Green” Septa
www.agilent.com/chem 40
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Part No.
Premium Non-Stick Septa
Agilent Bleed and Temperature Optimized Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4757
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4757-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4758
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4759
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4759-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4760
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk) 5183-4761
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk) 5183-4761-100
5 mm septa through-hole for on-column in glass jar (50/pk) 5183-4762
Gray Septa
Red Septa
11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk) 5181-1263-50
11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk) 5181-1263-100
11 mm with partial through-hole for 5880, 5890, (50/pk) 5181-3383-50
6850 and 6890 GCs
11 mm with partial through-hole for 5880, 5890, (100/pk) 5181-3383-100
6850 and 6890 GCs
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk) 5181-1283-50
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk) 5181-1283-100
5 mm through-hole for on-column inlets, (25/pk) 5181-1260
automatic or manual injections*
5 mm solid for high column backpressure, on-column inlets* (25/pk) 5181-1261
* 5 mm septa are packaged in glass jars
Our online store offers every GC inlet and consumable that your system
might need – including pieces that are hard to find.
Just visit www.agilent.com/chem/4ecatalog
41 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Ferrules
Using the wrong ferrule or a worn-out
ferrule to seal your column connection
can result in inconsistent and unreliable
chromatography. An improper ferrule
can cause leaks which allow air
and other contaminants to enter the
instrument through the column seal,
causing major interference with column
and detector performance. For optimum
performance, ferrules should be replaced
every time the column is replaced and
when performing column maintenance.
Agilent offers a comprehensive selection
of ferrules made of different materials and
configurations for a leak-free connection
between the column and injector.
Three main types of ferrules are used with
capillary GC columns: graphite, Vespel and
Vespel-graphite composites. Graphite
ferrules can withstand temperatures as
Column Ferrule Types
high as 450ºC, and Vespel and Vespel- Advantages Limitations
graphite ferrules are rated to 280ºC and
350ºC, respectively. Graphite Easy-to-use, stable seal Soft, easily deformed or destroyed
www.agilent.com/chem 42
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Ferrule Troubleshooting
Correct column positioning in both Column positioned incorrectly in the Column positioned incorrectly in the inlet
injection port and FID injection port, or possible ferrule or septum (either too far or not far enough; verify
particle in the carrier gas flow path 4-6mm installation distance)
Do not use 100% graphite ferrules in GC/MS transfer lines. They will
deform and leak over time, due to the softness of the graphite.
43 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Vespel/Graphite
(85%/15%) Ferrules
The combination of graphite and Vespel
results in a ferrule having low oxygen
diffusion rates which does not shrink to
the same extent as pure Vespel. These
ferrules are recommended for use with
GC/MS or other oxygen sensitive
detectors, like the ECD, but are also
compatible with other detectors like FID
and NPDs.
In addition, the Vespel/graphite ferrules
provide added confidence of leak-free
connections when installed correctly.
Proper installation requires a finger-tight
turn on the nut, then an additional 1/4 – 1/2 Two different lengths of Vespel/graphite When using Vespel/graphite ferrules,
turn with a wrench. ferrules are available for capillary column Agilent recommends tightening the column
use. The standard sized ferrule is nut to a 1/4 turn after the first temperature
These ferrules are very hard and cannot compatible with the universal column nut. program runs. Even preconditioned ferrules
be deformed sufficiently to seal multiple The second ferrule size is slightly longer can exhibit some shrinkage after a
column diameters. The ferrule hole must and is specifically designed to fit with the temperature programmed run.
match the column OD exactly to ensure a MS interface nut used for the GC/MS
leak-free seal. For capillary column transfer line connection. The larger ferrule
applications, there is a specific ferrule for can also be used to make column
each column diameter. Choosing a ferrule connections to inlets and other detectors
with a larger hole than is specified for a but requires a specially designed column
given column dimension can result in a nut (p/n 05988-20066) to accommodate
large leak. If left unchecked, an improper the longer ferrule.
seal at the injector will result in high
column bleed and a shortened column
lifetime. An improper seal at the detector
can result in increased detector
signal/noise. In the case of the MSD it
can also contribute to oxidation of the ion Vespel/Graphite Nut & Ferrule Combinations
source which can increase the frequency
of detector maintenance.
Standard ferrule and standard nut
Universal Column Nut + Vespel/Graphite Ferrules
5181-8830 5181-3323 (0.1, 0.2, 0.25 mm ID columns)
5062-3514 (0.32 mm)
5062-3512 (0.45 and 0.53 mm)
www.agilent.com/chem 44
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
VIDEO
45 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Column Nuts
Short Nuts
Universal column nut, 1/16 in. hex 2/pk 5181-8830
Finger-tight column nut for 0.53 mm columns* 1 ea 5020-8293
Finger-tight column nut for 0.32 mm columns* and smaller 1 ea 5020-8292
Blanking plug, finger-tight style 1 ea 5020-8294
6850 Column Nut 2/pk 5183-4732
Long Nuts
MS interface column nut 1 ea 05988-20066
Column nut for GC/MS ferrules 1 ea 05921-21170
Column nut wrench, 1 /4 in. and 5 /16 in. 1 ea 8710-0510
* For use with graphite ferrules only.
Always match short nuts with short ferrules and long nuts with long ferrules.
www.agilent.com/chema 46
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liners
Agilent offers a complete selection of
GC split and splitless inlet liners that
deliver consistent quality. So you can get
consistent results.
And unlike other manufacturer’s liners,
Agilent liners are built to Agilent’s precise
inlet tolerances which helps ensure
optimal dimensional accuracy and
inertness toward demanding compounds.
Choosing the proper liner for a specific
application can be a difficult and
challenging task. The three liner
characteristics that must be considered
for each application are:
• Liner volume
• Liner treatments or deactivation
• Any liner design features that might
affect carrier gas flow through the inlet
or sample vaporization
VIDEO
47 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Discussion
of Liner
Characteristics
Liner Volume
The purpose of the injection port is to allow
the introduction of a sample into the gas
chromatograph in an accurate, reproducible
manner. The vaporized sample should be
a true representation of the liquid sample
and, unless specifically desired, should
be injected without chemical change. The
elevated temperatures used in the inlet
vaporize the liquid sample to a gas for
transfer to the head of the column. This
phase transition is accompanied by a very
significant volume change. The volume of
the resulting vapor must be small enough
to fit within the volume of the liner. If the
volume is too great for the liner, it could
result in backflash, or sample loss caused
by expansion into the septum purge or split
vent lines. Both can compromise Liner Deactivation
reproducibility and sensitivity. Backflash Active sites on inlet liners can adsorb With use, even deactivated liners can
also frequently results in sample carryover. sample components and cause peak tailing, begin to exhibit activity. When this occurs,
and potential loss of sensitivity and the liner should be replaced. Liners can be
Larger volume liners (> 800 µL) are
reproducibility. Deactivation agents are cleaned to remove particulate material or
characterized by larger inside diameters
used to cover or react with active sites on solvent rinsed to remove less volatile
(ID) and are typically used with injection
the glass surface of the liner. Agilent liners components. However, choosing the
sizes of 1 µL or more. The small volume
are deactivated using deactivation proper liner cleaning procedure can be
liners have a smaller ID and are usually
procedures that produce reproducible and difficult. Some solvents may remove the
used with small injection sizes (< 1 µL),
inert liners, with long lifetimes. For splitless deactivation layer, and tools might scratch
fast 100 µm ID columns, gas samples, or
applications or when even slightly polar the glass surface of the liner, resulting in
when using external sampling devices
compounds must be analyzed, a the generation of unwanted active sites.
like headspace and purge and trap.
deactivated liner should be used. A new liner almost always outperforms
a cleaned and re-deactivated one –
especially for trace analysis.
Agilent offers a free software tool that calculates the vapor volume of an extended list of
common solvents, based on your choice of inlet temperatures and pressures for a given
Agilent inlet liner. To download, go to www.agilent.com/chem/techsupport. Click “User
Contributed Software;” then, click “GC Pressure/Flow Calculator.”
www.agilent.com/chem 48
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
49 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liner Troubleshooting
Symptom Possible Cause Remedy
Tailing Peaks Sample components adsorbed by column, Use new, deactivated liner or clean old
inlet liner or contaminated gold inlet seal. liner and replace glass wool.
Needle hitting and breaking packing in Partially remove packing from liner or use
inlet liner. without packing.
Normal Problem Column end poorly cut Remove column. Make a clean, square
(sample absorption). cut using a reliable capillary fused silica
Broken or chipped inlet liner. cutting tool (such as a ceramic wafer or
the Agilent Column Cutter), then reinstall
column.
Inlet flow too low. Make sure total flow in inlet is above
40 mL/min.
Baseline Rise Before or After Peak Sample decomposing. Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass
wool and packing. Column/sample
residues could also be the problem.
Baseline Change After Large Peak Column and inlet liner misaligned. Check installation of column end and inlet
See also”Septum Troubleshooting,” liner; adjust if necessary.
page 37
Unresolved Peaks Column or inlet liner contaminated or Use a guard column to prolong column life.
column deteriorating. Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass
wool and packing. Trim the front end of the
column a minimum of 6 inches.
www.agilent.com/chem 50
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Agilent Liners
Our engineering and testing efforts focus on these parameters when designing liners for Agilent inlet systems. Intensive liner
development and testing have resulted in a set of liners that we recommend whenever new methods are being developed, when
methods are being optimized, or when problems with existing methods are encountered. These liners are:
Direct injection:
Straight liner without glass wool,
deactivated, Agilent Part No. 5181-8818
(use only for gas samples, headspace, or
purge and trap applications).
Direct Connect
Direct Connect liners are ideal for
customers running highly sensitive
compounds, or for users who require
maximum inertness performance and
minimal inlet discrimination for trace GC
and GC/MS applications. Direct Connect
liners also eliminate sample exposure to
metal parts, minimizing inlet-related
degradation. These liners are included in
our new 8270 EPA Applications kit
designed specifically for optimizing a
6890/5973 GC/MSD to this method.
The liners are deactivated, come in either
a single or double taper, and utilize a press
fit connection to the column. In addition,
there is a small, drilled hole in the side of
the liner whose size and placement was
Split injection: optimized by Agilent R&D engineers to
Agilent low-pressure-drop split liner with allow them to work with EPC.
glass wool, bottom taper, glass bead for Focus Liner
easy positioning, and deactivated, Agilent Improve reproducibility, improve results.
Part No. 5183-4647 (with extraordinarily The Focus Liner traps a precisely controlled
tight dimensional control for optimum amount of glass wool in the ideal position
split performance). in the injection port liner. At the point of
Splitless injection: injection, the glass wool provides extra
Single tapered liner without glass wool, surface area for vaporization, traps
deactivated, Agilent Part No. 5181-3316EN. nonvolatile sample residue, and wipes
any residual sample from the sample
Note: For pesticide analysis – especially needle – reproducibility is the result.
DDT and Endrin, where breakdown is a
problem – we recommend Agilent Part In addition to these liners we offer a
Nos. 5181-3316EN and 5181-3315EN. broad selection of liners for your specific
application needs.
General purpose split/
splitless injection: Liner O-Rings
Similar design to Agilent Part No. 5183- Liners are sealed in the inlet with O-rings
4647, but with an outer diameter that or graphite seals. O-ring seals are easier to
compromises for both split and splitless remove and to replace than graphite that
injections, Agilent Part No. 5183-4711. deforms and flakes apart. The graphite
seals should be used when inlet
temperatures exceed 350ºC.
51 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
VIDEO
Description Part No.
To view videos on the Flip Top Inlet Sealing System,
Flip Top Inlet Sealing System 5188-2717 visit www.agilent.com/chem/fliptop2
Liner O-rings (10/pk) 5188-2741
www.agilent.com/chem 52
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Liner, splitless, single-taper, For splitless injection 900 5181-3316 5183-4695 5183-4696
no glass wool, deactivated
Liner, direct, 2 mm ID, For direct injection 250 5181-8818 5183-4703 5183-4704
deactivated (use for gas samples,
headspace, or purge
and trap applications)
Liner, splitless, double-taper, no glass wool, deactivated 800 5181-3315 5183-4705 5183-4706
Split Inlet Liners For Manual Injection 800 18740-80190 5183-4699 5183-4700
Liner, split, with cup, no glass wool
Liner, split, with cup, glass wool, and packing 800 18740-60840 5183-4697 5183-4698
[not recommended for use with electronic pressure
control (EPC)], for manual injection
Focus Liners
ID Wool Dimensions Part No.
Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4004-5
Focus liner 4.0 mm Yes 6.3 mm X 78.5 mm 210-4022-5
53 www.agilent.com/chem
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Heater-Sensor Assembly
Part No. G1544-61140
www.agilent.com/chem 54
SAMPLE INTRODUCTION CONSUMABLES & GC INLETS
Part No.
Agilent Gold Seals are micromachined to minimize surface area and potential inlet activity. Other manufacturers’ seals are not
machined, and may compromise your results.
Top
Bottom
Gold-plated seal p/n 18740-20885 Gold-plated seal with cross p/n 5182-9652
Use when inlet flow exceeds 400 ml/min.
55 www.agilent.com/chem
Columns
Choosing the right GC column and
following Agilent’s simple column care
recommendations will maximize GC column
performance and lifetime. In this section our
experts offer practical advice on how to
select, install and store your GC column,
plus give helpful hints about avoiding thermal
and oxygen degradation. Because GC column
contamination is the primary cause of
shortened column lifetime, we’ve also
included a detailed discussion about the
prevention of non-volatile and semi-volatile
contamination, as well as appropriate
recovery measures.
CATALOG
www.agilent.com/chem 56
COLUMNS
Column Maintenance
While GC column maintenance is predefined timetable of maintenance items, installation/system setup, and avoiding
simple, the frequency and type of the main focus should be how to obtain the primary factors that cause column
column maintenance that is required the highest performance and lifetime performance degradation (breakage,
varies due to many system and sample from a capillary column. This depends on thermal damage, oxygen damage, chemical
factors. Instead of simply following a choosing the right column, correct damage and contamination).
57 www.agilent.com/chem
COLUMNS
www.agilent.com/chem 58
COLUMNS
59 www.agilent.com/chem
COLUMNS
www.agilent.com/chem 60
COLUMNS
Prevention
• Perform sample preparation to remove
inorganic acids and bases from the
sample
• Install guard column and trim frequently
• If acids or bases must be used choose an Guard Column
organic alternative or HCl or NH4OH INJECTOR DETECTOR
Recovery
• Remove 0.5 to 1 meter from the front
of the column
• Severe cases may require the removal
of 5 or more meters Guard Column Column
Column Contamination
Column contamination is the most
common problem encountered in capillary Union
GC. Unfortunately, it mimics most other
chromatographic problems and is often
misdiagnosed. A contaminated column Guard column installation instructions are available at www.agilent.com/chem.
is usually not damaged, but it may be Click on “Technical Support,” then “GC Reference Library.” The procedure can be
rendered unusable. There are two basic found under “General Information.”
types of contaminants: nonvolatile and
semivolatile.
61 www.agilent.com/chem
COLUMNS
Nonvolatile Contaminants
Nonvolatile contaminants or residues do Description Part No.
not elute and accumulate in the column
(most often confined to the first few Split/Splitless Inlet liner: glass wool,
meters). The column becomes coated with taper, deactivated (5/pk) 5183-4712
these residues which interfere with the
proper partitioning of solutes in and out Splitless Inlet liner: single-taper,
of the stationary phase. Also, the residues no glass wool, deactivated (5/pk) 5183-4695
may interact with active solutes resulting
in peak adsorption problems (evident as Quartz deactivated column
peak tailing or loss of peak size). Active connector (5/pk) 5181-3396
solutes are those containing a hydroxyl
Polyimide sealing resin (5 grams) 500-1200
(-OH) or amine (-NH) group, and some
thiols (-SH) and aldehydes. Deactivated Fused silica,
10m, 0.53mm i.d. 160-2535-10
Prevention
• Perform sample cleanup to remove Deactivated Fused silica,
nonvolatile materials from the sample 10m, 0.25mm i.d. 160-2255-10
• Use injection port liners packed with
glass wool (may not be feasible when Capillary column rinse kit 430-3000
analyzing active compounds)
• Install a guard column and trim regularly
Recovery
• Do not bakeout the column
• Front End Maintenance: Prevention Column Storage
• Perform sample cleanup to remove Capillary columns should be stored in their
– Clean or change the injection port liner
semi-volatile materials from the sample original box when removed from the GC.
– Clean out the injector • Increase the final temperature of the Place GC septa over the ends to prevent
GC run (not to exceed the temperature debris from entering the tubing. Upon
– Cut off typically 0.5 to 1 meter of the
limit of the column) reinstallation of the column, the column
front of the column
ends need to be trimmed by 2-4 cm to
• Change septa regularly ensure that a small piece of septa is not
• Turn the column around (install detector
end into injector). Not recommended for Recovery lodged in the column.
sensitive ECD, NPD, and MS detectors. • Bakeout the column: limit 1-2 hours If a column is left in a heated GC, there
• Solvent rinse the column (excess baking may polymerize some should always be carrier gas flow through
contamination and reduce column the column. The carrier gas flow can be
• Cut the column in half and use the back
lifetime) turned off only if the oven, injector,
half (detector side)
• Solvent rinse the column detector and transfer lines are turned off
Semivolatile Contaminants (i.e., not heated). Without carrier gas flow,
Semivolatile contaminants or residues Does Your Sample Have Residues? damage to the heated portion of the
accumulate in the column, but eventually Perform this simple test. column occurs.
elute. Hours to days may elapse before 1. Place 20-30 µL of the sample onto a
they completely leave the column. Like microscope slide.
nonvolatile residues, they may cause peak
shape and size problems and, in addition, 2. Put the slide over the heated GC inlet
are usually responsible for many baseline for 20 minutes.
problems (instability, wander, drift, ghost 3. Hold the slide up to the light.
peaks, etc.).
If you can see anything where the drop
was, your sample has residues.
www.agilent.com/chem 62
COLUMNS
63 www.agilent.com/chem
COLUMNS
www.agilent.com/chem 64
COLUMNS
65 www.agilent.com/chem
COLUMNS
www.agilent.com/chem 66
COLUMNS
67 www.agilent.com/chem
Detectors
Most detectors require simple but periodic
cleaning to maintain peak performance.
This is especially true for highly sensitive
GC detectors. Without routine detector
maintenance, GC system performance will
deteriorate and can cause detector failure.
Detailed procedures on how to clean,
maintain and replace common detectors,
including FID, TCD, NPD, ECD, and FPD are
summarized in this section. Also included
are special handling techniques and specific
recommendations to maximize specific
detector operations. For example, learn how
to resolve flame ignition problems associated
with your flame photometric detector and
test electron capture detectors for
radioactivity leaks.
CATALOG
www.agilent.com/chem 68
DETECTORS
Hardware Problems
If the flame goes out or will not light:
• Check the column flow rate. It may FID Ferrules
be too high. Decrease the flow rate or
pressure. Switch to a more restrictive
column (longer or with a smaller id).
If you must use a large id column, first
cool the GC oven to below 50˚C, then turn
off the carrier flow long enough to allow
the FID to light. Check for partially or
Cleaning & Replacement
Even with normal use, deposits develop in
completely plugged jet.
the jet and detector (usually white silica
• Check that the right type of jet is installed from column bleed or black carbonaceous
for the column you are using. soot). These deposits reduce sensitivity
• Injecting large volumes of aromatic and cause chromatographic noise and
solvent or water can cause the flame to spikes. Although you can clean the jet, it is
go out. Switch to a nonaromatic solvent usually more practical to replace dirty jets
or inject less solvent. with new ones. If you do clean the jet, be FID Cleaning Kit, P/N 9301-0985
• The lit offset value may be too low or too careful not to scratch the jet internally;
high. Adjust the value. scratches will ruin the jet
VIDEO
69 www.agilent.com/chem
DETECTORS
5. Remove the jet from the bath and rinse it FID retainer nut wrench 19301-00150
thoroughly, first with hot tap water and (5880, 5890, 6890)
then with a small amount of GC-grade 1/4 in. Nut Driver for FID jet-drilled shaft 8710-1561
methanol. FID supplies kit-Includes: 5182-3450
6. Blow the jet dry with a burst of Jet, packed standard 3 each 18710-20119
compressed air or nitrogen, and then FID performance evaluation sample kit 2 each 18710-60170
place the jet on a paper towel and allow Ignitor glow plug assembly 2 each 19231-60680
it to air dry. Jet, cap. series 530 µm 3 each 19244-80560
FID flow measuring insert 2 each 19301-60660
Cleaning wires for 0.03 in. ID jet 5180-4150
Cleaning wires: 0.018 in. ID/530 µm jet 1/pk 5180-4152
Wire, jet cleaning, 5 each 19301-20720
Capillary inlet cleaning wires 5180-4153
Detector cleaning kit 9301-0985
**Not included in assembly.
*Hastelloy components may be used when analyzing highly corrosive materials.
1 Does not include Hastelloy component.
www.agilent.com/chem 70
DETECTORS
FID Jets
3
FID Consumables
4
8 5
Description Unit Part No.
6
FID flow measuring insert 19301-60660
7
FID ignitor cable G1531-60680
FID Performance evaluation sample kit, 0.03% C14, 18710-60170 6
C15, and C16 normal alkanes in hexane
O-rings 12/pk 5080-4978
Cleaning wire 19301-20720
Jet cleaning wire for 0.03 in. ID jet 5/pk 5180-4150
Jet cleaning wire for Series 530 mm and 0.018 in. ID jet 5/pk 5180-4152
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
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
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
www.agilent.com/chem 74
DETECTORS
75 www.agilent.com/chem
DETECTORS
www.agilent.com/chem 76
DETECTORS
12 Coupling, SS 19256-20550 20
21
14 Screw, M3 x 12 (4 required) 0515-0911
15 Clamp 19256-00090
16 O-ring, inner window 12/pk 5061-5886
17 Window, second heat shield 19256-80060
18 O-ring, outer window 12/pk 5061-5891
19 Flange adapter 19256-20510
20 Flange ring 19256-00200
21 O-ring, Viton, 1.239 in. id 12/pk 5061-5890
Adapter weldment, 1/8 in. columns 19256-80590
Adapter weldment, capillary 19256-80570
Start-up kit (5890 only) 19256-60500
FPD O-ring (5890 only) 12/pk 5061-5867
Liner/ferrule kit 19256-60590
Sulfur filter 19256-80000
Phosphorus filter 19256-80010
Kalrez O-ring, size 2-002 0905-1609 Install the correct optical
MAINTENANCE MINDER
77 www.agilent.com/chem
DETECTORS
www.agilent.com/chem 78
DETECTORS
6890/5890 Adaptable
79 www.agilent.com/chem
DETECTORS
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 a longer lifetime.
www.agilent.com/chem 80
You asked … we listened!
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
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 Agilent’s new Flip Top Inlet
Sealing System, you don’t have to check or
change liners. So you save time and effort.
See page 52 for ordering information.
Every week
Check the foreline pump oil level and
diffusion pump fluid. Change the injection
port liners and O-rings. Gas ballast the
foreline pump.
Every month
Clean the split/splitless inlet vent line
trap. Check for leaks (inlet and column
connections).
Every three months
Replace gas cylinders (when below
500 psig).
TASK EVERY EVERY EVERY AS
WEEK 6 MONTHS YEAR NEEDED Every six months
Replace the foreline pump oil. Check,
and if necessary, refill the calibration vial.
Tune the MSD •
Change injection port liners •* Every year
Check the foreline pump oil level • Replace the diffusion pump fluid.
Gas ballast the foreline pump • Recondition or replace internal and external
Check the calibration vial • traps and chemical filters on the GC.
Replace the foreline pump oil • As needed
Check the diffusion pump fluid • Tune the MSD. Clean the ion source.
Replace the diffusion pump fluid • Replace the carrier gas trap. Replace
Replace the traps and filters • worn-out parts (filaments, EM, etc.).
Clean the ion source • Replace the column. Lubricate seals.
Change the carrier gas trap(s) and purifier • Monitor
Replace the worn out parts • Record all tune values such as electron
Lubricate seals (where appropriate) • multiplier and ion source parameters in
Replace column • a log book to monitor instrument
performance. In addition note the high
vacuum and foreline vacuum pressures.
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.
www.agilent.com/chem 84
GC/MS SYSTEMS
Corrective Action
• Check interface nut for tightness.
Replace if necessary.
• Check leak/test the GC injection port.
Fingerprints
Fingerprints contain hydrocarbons that can Corrective Action
appear in mass spectra. Hydrocarbon • Reclean using clean, nylon gloves and
contamination is characterized by a series proper cleaning techniques.
of mass peaks 14 amu apart. The
abundances of these peaks decrease as
peak mass increases. Fingerprint
contamination is usually caused by the
Description Part No.
failure to wear lint-free, nylon gloves during
ion source cleaning, GC inlet maintenance, Nylon gloves, lint-free, Large 8650-0030
or from installing the column. Use special Nylon gloves, lint-free, Small 8650-0029
care to avoid recontamination of parts after
you clean them. This typically occurs after
some maintenance or part replacement.
85 www.agilent.com/chem
GC/MS SYSTEMS
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
18, 28, 32, 44 or 14, 16 H2O, N2, O2, CO2 or N, O Residual air and water, air leaks, outgassing from
Vespel™ ferrules
31, 51, 69, 100, 119, 131, 169, PFTBA and related ions PFTBA (tuning compound)
181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614
31 Methanol Cleaning solvent
43, 58 Acetone Cleaning solvent
78 Benzene Cleaning solvent
91, 92 Toluene or xylene Cleaning solvent
105, 106 Xylene Cleaning solvent
151, 153 Trichloroethane Cleaning solvent
69 Foreline pump fluid or Foreline pump oil vapor or calibration valve leak
PFTBA
73, 147, 207, 221, 281, Dimethylpolysiloxane Septum bleed or methyl silicone column coating
295, 355, 429
77, 94, 115, 141, 168, 170, Diffusion pump fluid Diffusion pump fluid and related ions
262, 354, 446
149 Plasticizer (phthalates) Vacuum seals (O-rings) damaged by high temperatures,
use of vinyl or plastic gloves
Peaks spaced 14 amu apart Hydrocarbons Fingerprints, foreline pump oil
www.agilent.com/chem 86
GC/MS SYSTEMS
Repeatability
Symptoms Corrective Action
87 www.agilent.com/chem
GC/MS SYSTEMS
Ion Source
The ion source operates by electron cules, ionizing and fragmenting them. The
ionization (EI) or chemical ionization (CI). positive voltage on the repeller pushes the
The sample enters the ion source from the positive ions into the lens stack, where
GC/MSD interface. Electrons emitted by a they pass through several electrostatic
filament enter the ionization chamber, lenses. These lenses concentrate the ions
guided by a magnetic field. The high-energy into a tight beam, which is directed into the
electrons interact with the sample mole- mass filter.
www.agilent.com/chem 88
GC/MS SYSTEMS
89 www.agilent.com/chem
GC/MS SYSTEMS
www.agilent.com/chem 90
GC/MS SYSTEMS
B
A
H
D F
TIPS AND TOOLS
C
E
B I It is good practice to replace scratched lenses and other ion source parts.
Scratched source parts lead to poor performance.
G
05972-60226
Transfer line tip, gold-plated 5972/5971 Part No. GCD Part No.
05971-20305 G1800-20305
Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates
below for flow limitations.
Min Max Diff Pump Max Turbo Pump Tuning Max
5973 0.1 2.0 4.0 2.0
5972 0.1 2.0 NA 2.0
5971 0.1 1.5 NA 1.0
GCD 0.1 1.0 NA 1.0
91 www.agilent.com/chem
GC/MS SYSTEMS
Filaments
Two filaments are located on opposite
sides outside of the ion source. The active
filament carries an adjustable ac emission
current. The emission current heats the
filament, causing it to emit electrons; these
electrons ionize the sample molecules. In
addition, for the 5973 and 5972, both
filaments have an adjustable dc bias
voltage. The bias voltage determines the
energy on the electrons, usually -70 eV.
www.agilent.com/chem 92
GC/MS SYSTEMS
MAINTENANCE MINDER
MAINTENANCE MINDER
93 www.agilent.com/chem
GC/MS SYSTEMS
Pressure Symptoms
This section describes unusual pressure These pressures can vary widely from The vacuum manifold pressures can only be
readings and their possible causes. The instrument to instrument so it is important measured if your system is equipped with
symptoms in this section are based on that you are familiar with the pressures the optional gauge controller.
typical pressures. At typical column flow that are typical for your instrument at a
rates (0.5 – 2.0 ml/minute), the foreline given carrier gas flow and oven
pressure will be approximately 20 to 100 temperature.
mTorr. The vacuum manifold pressure will
be approximately 1 x 10-6 to 1.4 x 10-4 Torr. The foreline pressures listed can only be
measured on diffusion pump-equipped
systems. Turbomolecular pumps are
controlled according to their speed and
do not have foreline pressure gauges.
Symptom • Pressure is above 100 mTorr. Symptom • Pressure is above 1.4 x 10-4 Torr.
• Pressure for a given column flow has • Pressure for a given column flow has
increased over time. increased over time.
Possible Cause • Column (carrier gas) flow is too high Possible Cause • Column (carrier gas) flow is too high
• Wrong carrier gas • Wrong carrier gas
• Air leak (normally at transferline interface) • Air leak
• Foreline pump oil level is low or oil is • Foreline pump is not working correctly
contaminated • Diffusion pump fluid level is low or fluid is
• Foreline hose is constricted contaminated
• Foreline gauge is not working correctly • Foreline pump is not working correctly
• Foreline pump is not working correctly • Defective gauge controller
• Faulty ion gauge tube
Symptom • Pressure is below 20 mTorr. Symptom • Pressure is below 1.4 x 10-6 Torr.
Possible Cause • Column (carrier gas) flow is too low Possible Cause • Column (carrier gas) flow is too low
• Wrong carrier gas • Wrong carrier gas
• Column plugged or crushed by an • Column plugged or crushed by an
overtightened nut overtightened nut
• Empty or insufficient carrier gas supply* • Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing* • Bent or pinched carrier gas tubing*
• Foreline gauge is not working correctly • Defective gauge controller
• Faulty ion gauge tube
* These could create a fault condition in the
GC that would prevent the GC from operating. * These could create a fault condition in the
GC that would prevent the GC from operating.
www.agilent.com/chem 94
GC/MS SYSTEMS
Diffusion Pump
It is not necessary to change the diffusion How to Check the Fluid Level 6a. Use a metal ruler to determine the
pump fluid more than once a year, unless 1. If it is not vented already, shut down and depth of the fluid. A pump that has
you observe symptoms that suggest a vent the MSD according to instrument been in operation should have a pool
problem with the diffusion pump fluid. The manual. 9 mm plus or minus 1 mm deep. Fluid
MSD must be vented in order to check the in freshly charged pumps will be 12
2. Unplug the MSD power cord.
diffusion pump fluid (except for the 5973). mm deep. It is normal that up to 2 ml
Therefore, the best time to check the fluid 3. Remove the pump and cover the top of oil may be in the rear portion of the
is when the instrument is already vented with aluminum foil. vacuum manifold. The recommended
for other maintenance. 4. After heating the pump in a GC oven total fluid charge for the 5971/5972 is
at 60°C for 15 minutes to make the 18 ml (plus or minus 2 ml).
Importance of the Fluid Level fluid flow down into the reservoir at 6b. For the 5973 use the sight glass
The amount of fluid in the pump affects the bottom, remove the stack parts. to determine the depth of the fluid.
the amount of vapor and the temperature The recommended total fluid charge
of the base plate. Too little fluid will cause 5. Inspect the pump fluid, if the fluid
is discolored or contains particulate is approximately 37 ml.
the pump to run at a higher temperature
because there is less fluid to carry away the material, the fluid must be changed.
heat resulting in fluid cracking or degradation
and loss of high vacuum. It will also lower
the pumping speed because there is less
fluid vapor available to pump away gases
which can especially affect operation in
CI Mode due to higher flow rates.
Foreline Pump
The oil in the foreline or rough pump Avoid contact with the pump oil. The
should be replaced on average once every residue from some samples may be toxic.
six months, but can vary depending upon Dispose of used oil properly.
applications. After oil replacement, if the
foreline trap is present, the molecular
sieves should be replaced.
95 www.agilent.com/chem
GC/MS SYSTEMS
General Instructions on How to Replace the 8. Reconnect the MSD power cord.
Pump Oil 9. Start up and pump down the MSD
1. Shutdown and vent the MSD. according to the Instrument Manual
2. Place a container under the drain plug on the procedure.
foreline pump.
3. Remove the fill cap from the top of the pump to
expose the fill hole.
4. Remove the drain plug from the pump.
5. Reconnect the MSD to its power source. Switch TIPS AND TOOLS
on for 2 or 3 seconds, and then switch it off
again. This displaces old oil from the internal
pump cavities. Disconnect the power cord again. Use chemical-resistant gloves and safety glasses when replacing pump
fluid. Avoid contact with the fluid. Always dispose of used oil properly.
6. Reinstall the drain plug and pour pump oil into
the fill hole.
7. Reinstall the fill cap.
Symptom
Description Part No. • Voltage is over 2500 volts
• Poor vacuum
Electron multiplier replacement horn 05971-80103
(5973, 5972, 5971/GCD) Corrective Action
High energy dynode (5973 only) G1099-80001 • Replace electron multiplier
Electron multiplier kit (5972, 5971/GCD only) 05971-80102
Use only Agilent replacement multipliers and horns for Agilent MSDs.
Other manufacturers’ products can increase noise, while reducing
sensitivity and linearity.
www.agilent.com/chem 96
GC/MS SYSTEMS
97 www.agilent.com/chem
GC/MS SYSTEMS
We strongly recommend keeping a log of all system performance and routine maintenance
operations. That way, problems that might impact performance can be identified and
resolved quickly.
The most common maintenance tasks are listed in the table below.
www.agilent.com/chem 98
GC/MS SYSTEMS
C
A
D
5989 Lens Stack
99 www.agilent.com/chem
GC/MS SYSTEMS
Contents:
• Start-Up Guide, pub. No. 5988-3073EN • Pre-tested column, 30m x 250um x 0.5um
• Application Note, “Improvements in the HP-5 MS, part no. 19091S – 139
Agilent 6890/5973 GC/MSD System for • Single-taper splitless liner, 4mm i.d.,
use with USEPA Method 8270”, pub. no. deactivated, part no. 5181-3316
5988-3072EN • Direct Connect Liner, single taper, 4mm
• Ultra Ion Source Chamber i.d., deactivated, part no. G1544-80730
• Ultra Repeller • Direct Connect Liner, dual taper, 4mm
• Ultra Large Aperture Drawout Plate i.d., deactivated, part no. G1544-80700
• Floppy Disk with tuning macros
LIBRARY
There are many ways to perform semi-volatile analysis. For another option that
also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem
and do a library search for 5989-1510EN.
www.agilent.com/chem0 100
GC/MS SYSTEMS
EI CI Negative Positive
MSD Tune Tune EI Mode CI Mode CI Semi-Volatile Volatile
5973 PFTBA PFDTD OFN 1 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL DFTPP BFB
5972 PFTBA PFTBA HCB 10 pg/µL NA Benzophenone 100 pg/µL DFTPP BFB
5971 PFTBA PFTBA HCB 10 pg/µL NA Benzophenone 100 pg/µL DFTPP BFB
MS Engine
5989A PFTBA PFTBA HCB 50 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL DFTPP BFB
5989B PFTBA PFTBA HCB 20 pg/µL OFN 500 fg/µL Benzophenone 100 pg/µL DFTPP BFB
101 www.agilent.com/chem
GC/MS SYSTEMS
PFDTD 10 g 8500-8130
www.agilent.com/chem 102
You asked … we listened!
www.agilent.com/chem 104
SERVICES & SUPPORT
105 www.agilent.com/chem
SERVICES & SUPPORT
Telephone Service • Telephone access to skilled Agilent service • Fast identification and resolution
professionals. of hardware problems.
Software Service • Telephone access to trained technical • Fast identification and resolution
professionals. of software problems.
Onsite Instrument Repair • Hardware telephone support with access • A fixed annual cost for parts makes
to skilled, factory-trained Agilent service budget management more predictable.
professionals.
• You can choose the response
• Travel expenses and labor. method that fits your business
needs and budget.
• Optional coverage for consumables
used during repair.
Offsite Instrument Repair • Option 1: Replacement with an identical • Less expensive than onsite repair.
For selected Agilent analysis instruments instrument (your fastest choice).
• Fast and easy.
• Option 2: Return to Agilent for repair.
• Includes extensive diagnostics and
testing that are not feasible with onsite
maintenance or repair.
www.agilent.com/chem 106
SERVICES & SUPPORT
Installation Qualification (IQ) • Qualification and documentation of • Supplies the evidence you need to
shipment completeness. satisfy regulatory agencies.
• Comprehensive system and application • Helps fulfill the master validation plan –
software verification tests. and change-control SOP requirements –
for the IQ phase.
• Delivered by professionals with training
certification.
Operational Qualification/Performance • Verification and documentation of an • Supplies the evidence you need to
Verification (OQ/PV) instrument’s ability to meet specified satisfy regulatory agencies.
For selected Agilent analysis instruments criteria.
• No need to write your own SOPs to
Note: We recommend Preventative • Procedures and documentation that fit the qualify Agilent instruments – or to train
Maintenance before OQ/PV. requirements of GLP, ISO 9000, and other your staff.
regulatory agencies.
• Consistent, traceable results among all
• Full automation to increase the your laboratories – and improved
qualification scope without excess time method transfer.
requirements.
• Confidence in the integrity of your
• Measuring equipment that is traceable to measurements, with traceable,
national and international standards. documented chains from sample
introduction to reporting.
Requalification (RQ) After Repair • Verification that a system is performing • Minimal system downtime after
For instruments that have their at operation specifications after repair. completion of instrument repair.
operational performance verified
by an annual OQ/PV. • Complete system operation testing. • Efficient system requalification by
performing the appropriate tests based
Note: only a subset of the Operational on the components repaired.
Qualification test is performed, based on
the type and extent of the repair. • Assurance that all instrument
subsystems are performing within
• A comprehensive test of the repaired specifications.
module using established conditions and
known sample characteristics to ensure • All procedures and documentation meet
the basic accuracy and precision of your regulatory agency requirements.
module.
107 www.agilent.com/chem
SERVICES & SUPPORT
Mass Spectrometer Ion Source Cleaning • Your staff can devote more time to
For selected Agilent analysis instruments • Onsite disassembling chemistry, not instrument maintenance.
• Testing
www.agilent.com/chem 108
SERVICES & SUPPORT
Software Backup • Telephone or onsite factory support to • Fast and easy – you simply insert a disk
facilitate restoration. … reboot … and you’ll be back in
operation in as little as two hours.
• Captures the unique system settings for all Normally, you would have to reload and
software components needed to reconfigure your software – a process
reconstruct your system including: that can take days.
- Network information
- Printers and peripherals • A complete solution – the initial
- Configurations configuration backup includes:
- User settings and operations - Simple backup software
- System registry - Ten CD-ROMs
- Application software - Ten 3.5-in. floppy disks
- Settings - A storage case
- Operating system - One full system backup
- Customizations - Installation of the backup software
- Analytical hardware and optional CD writer
- Directory structure
- Security information
109 www.agilent.com/chem
SERVICES & SUPPORT
eLearning
Agilent’s e-Learning program features a series of focused, economical and
individualized instrument training modules designed to enhance and simplify your
learning experience. From theory and operations... to common problems with your
instruments... eLearning is available when you want it, where you want it, and how
often you want it. All you need is Internet access!
You can review and register for our e-Learning offerings by visiting
www.agilent.com/chem/elearning
6890 GC Split Inlet Mode Operation Self-paced; Reviews the basic theory and operation
Four hours access of the 6890 GC split/splitless capillary
inlet when running in split mode.
6890 GC Splitless Inlet Mode Operation Self-paced; Reviews the basic theory and operation of
Four hours access the 6890 GC split/splitless capillary inlet
when running in splitless mode.
6890 GC Purged Packed Inlet Operation Self-paced; Reviews the basic theory and operation
Four hours access of the 6890 GC purged packed inlet.
www.agilent.com/chem 110
SERVICES & SUPPORT
6890 GC Keyboard Operation Self-paced; Reviews the basic operation of the 6890
Four hours access GC keyboard.
6890 GC FID Theory and Operation Self-paced; Reviews the basic theory and operation
Four hours access of the FID.
6890 GC ECD Theory and Operation Self-paced; Reviews the basic theory and operation
Four hours access of the ECD.
6890 GC TCD Theory and Operation Self-paced; Reviews the basic theory and operation
Four hours access of the TCD.
GC Automatic Liquid Sampler Operation Instructor-led; Reviews the basic operation of the 7683A
60-90 minutes automatic liquid sampler system (ALS).
111 www.agilent.com/chem
SERVICES & SUPPORT
Managing and Administering the Instructor-led; Shows you how to manage the GC/MSD
GC/MSD Security ChemStation 60-90 minutes Security ChemStation software in
to Meet FDA CFR Part 11 accordance with FDA CFR Part 11
Compliance Requirements requirements.
www.agilent.com/chem 112
SERVICES & SUPPORT
Classroom Training
Agilent’s training courses for gas also target those who want to broaden
chromatography and mass spectrometry or sharpen their troubleshooting,
help new and experienced lab maintenance, and system operation skills.
professionals learn proper and efficient
Contact Agilent today for more information
ways to use analytical instruments and
about our training and services. Or visit
software. These ISO-registered courses
www.agilent.com/chem and select
“Education.”
Technique
Introduction to Capillary GC H2615A 1 Provides an overview of capillary gas chromatography in a
lecture format.
Techniques of GC H4002A 5 Presents the fundamental concepts of gas
chromatography.
Introduction to GC-MS H2609A 1 Introduces the technique of GC-MS in a lecture format that
includes worksheet exercises.
Techniques of GC-MS H4040A 3 Reviews the key concepts of the GC-MS analysis process,
as well as qualitative and quantitative GC-MS techniques.
Hardware/Software Operation
ChemStation Operation for the 6890 GC/ALS H5926A 5 Explains how to operate the Agilent 6890 GC using GC
ChemStation software.
Operation of the GC-MSD System
Using the ChemStation for GC-MSD H4043A 5 Enhances an operator’s efficiency and productivity when
using the Agilent GC-MSD system.
Provides experience in data acquisition and analysis, library
searching, reporting, and customizing the system to meet
specific laboratory or customer needs.
GC-MSD System for Environmental Applications H4050A 5 Increases an operator’s skill in using a mass selective
detector with mass spectrometer EnviroQuant software.
113 www.agilent.com/chem
SERVICES & SUPPORT
www.agilent.com/chem 114
SERVICES & SUPPORT
Support
Tap Agilent’s GC and GC/MS • Software Downloads and Utilities Feature
expertise anytime. patches and status bulletins, tools and
utilities, firmware, and revision tables.
Just give us a call to discuss hardware,
• How-to Videos Show you how to perform
software, application concerns, or basic
common installation and maintenance
operation techniques.
procedures for Agilent products.
Visit Agilent online • Chromatogram Library A searchable
For a wealth of knowledge, tips, and collection of GC, LC, and CE
insights, go to www.agilent.com/chem. chromatograms for nearly a thousand
You’ll find: chemical compounds.
• Frequently Asked Questions about Agilent • Instrument and Software Demos Such as
instruments and supplies. product videos, 3D animations and
• Interactive Troubleshooter A step-by-step interactive software demos.
approach to help you solve common problems.
• Find a Part Includes parts information,
pricing, and availability, plus an illustrated
parts breakdown.
Have a technical GC column, method, or troubleshooting question? Agilent’s technical GC and GC/MS
experts are available to answer your questions by phone, fax or e-mail for free. With years of experience in
running samples, developing methods and troubleshooting GC systems, our chemists are promptly able to
help you consistently achieve excellent performance and high productivity in your lab.
For GC Technical Support go to www.agilent.com/chem/techsupport
and click on “Interactive Troubleshooter.”
115 www.agilent.com/chem
You asked … we listened!
Visit www.agilent.com/chem/4ecatalog
for one-click access to:
• A time-saving “quick-buy” feature
• Product pricing links (when available)
• Local sales contact information
• Online quote requests
• Order status updates
• Real-time customer support … and more
Receive a year’s worth of current chromatography insights with a
FREE subscription to Separation Times.
Best of all,
Separation Times is absolutely FREE …
and we’ll automatically e-mail it to you
seven times per year.
To reserve your subscription today, go to
www.agilent.com/chem/separationtimes
GC System Recommended Maintenance Schedule
Gas Management
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
Gas purifiers Every 6-12 months Replacement schedule is based on capacity and grade of gases.
(carrier gas & In general, replace non-indicating traps every 6-12 months or when
detector gas) indicating traps start to change color. Replace indicating traps when
indicating material is spent.
Split vent trap Every 6 months* Replace.
Flowmeter Every 1-2 years Re-calibrate electronic flowmeters – follow recommended schedule for
calibration the unit (shown on calibration certificate).
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.
Front-end Weekly – monthly* Remove 1⁄2 -1 meter from the front of the column when experiencing
Maintenance chromatographic problems (peak tailing, decreased sensitivity, retention
time changes, etc.). Replace inlet liner, septum and clean inlet as
necessary. Guard column may be useful for increasing column lifetime.
Solvent rinse As needed When chromatography degradation is due to column contamination.
Only for bonded and cross-linked phases.
Replacement As needed When trimming and/or solvent rinsing no longer return chromatographic
performance.
Ferrules Replace ferrules when changing columns and inlet/detector parts.
Detectors
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
FID/NPD Jets As needed Clean when deposits are present. Replace when they become scratched,
& Collector bent or damaged, or when having difficulty lighting FID or keeping flame lit.
NPD Bead As needed Replace when signal drifts or there is a dramatic change in sensitivity.
FID Every 6 months Measure hydrogen, air, and makeup gas flows.
TCD As needed Thermally clean by “baking-out” when a wandering baseline, increased
noise, or a change in response is present. Replace when thermal
cleaning does not resolve the problem.
ECD Every 6 months Wipe test.
As needed Thermally clean by “baking-out” when baseline is noisy, or the
output value is abnormally high. Replace when thermal cleaning
does not resolve the problem.
FPD Every 6 months Measure hydrogen, air, and makeup gas flows.
As needed Clean/replace FPD windows, and seals when detector sensitivity
is reduced.
MSD
Components require regular maintenance. For complete MSD maintenance schedule, please see page 83.
www.agilent.com/chem
www.agilent.com/chem