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.
1
TIPS AND TOOLS
This icon denotes a helpful hint that provides useful information you can find throughout this guide and online at www.agilent.com/chem.
VIDEO
This icon denotes a video that is available to view on our website.
Just visit www.agilent.com/chem/techsupport to view how-to videos and obtain more information.
2 Gas Management
3 Gas Types
4 Contaminants & Purities
4 Gas Purification Systems
12 Regulators
13 Tubing
14 Leak Detection
15 Flow Rates
18 Sample Introduction
Consumables & GC Inlets
Sample Introduction
19 Vials
21 Syringes
Inlet Types
26 Packed-Column
28 Split/Splitless
31 Cool On-Column
34 Programmed Temperature
Vaporizer PTV
Inlet Accessories
36 Septa
42 Ferrules
47 Liners
52 Flip Top Inlet Sealing System
54 Parts & Supplies
56 Columns
57 Column Maintenance
57 Column Selection
58 Column Installation/Setup
& Conditioning
59 Column Performance
63 Columns Types and
Characteristics
68 Detectors
69 Flame Ionization Detector (FID)
Thermal Conductivity Detector
(TCD)
72 Electron-Capture Detector
(ECD)
74 Thermal Conductivity Detector
(TCD)
76 Flame Photometric Detector
(FPD)
78 Nitrogen-Phosphorus Detector
(NPD)
82 GC/MS Systems
83 Maintaining Mass Selective
Detectors (MSDs)
87 Mass Spectrometer Symptoms
88 Ion Source
93 Vacuum Systems & Pumps
96 Electron Multipliers &
Replacement Horn
97 Maintaining the MS Engine
99 Ion Source Parts & Supplies
100 General GC/MS Supplies
101 Test & Performance Samples
104 Services & Support
105 Expert Service, Training
& Support
Don’t Miss…
GC Maintenance Schedule (inside back cover) www.agilent.com/chem • 800 227 9770
www.agilent.com/chem • 800 227 9770
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.
“Gas management is more than just selecting the highest quality carrier gas available. It’s about selecting the appropriate carrier gas for your needs, and taking steps to prevent system contamination. Agilent understands this and provides products that make gas management easy to implement in your lab.”
Kenji Yamaguchi
Applications Support Manager
CATALOG
For a complete selection of gas management supplies, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
2
The most frequently used carrier gases are helium and hydrogen, although nitrogen and argon can be used. Purity is essential for these gases since they sweep the sample through the column where it is separated into its component parts and then through the detector for component quantification. Carrier gas purity is also critical to prevent degradation of chromatographic hardware.
Contaminants in carrier gases can have a significant effect on column life and subsequent analyte detection. Harmful effects of impure gases include contaminant peaks and elevated column bleed, along with column and/or detector damage. The following sections describe the gases and purities that are necessary for gas chromatography carrier gases, as well as other support gases.
Support gases may be specific for detectors or for applications. These gases include fuels, oxidants, coolants, detector gases, and pneumatic gases. The degree of purity required for support gases is dependent on how that gas is being used, and whether or not it will make contact with the sample. Coolant gases (carbon dioxide) and pneumatic gases (air or nitrogen) generally do not come in contact with the sample or detector. Therefore, these non-contact gases do not have to be the highest purity available.
Fuels, oxidants and detector gases, in most cases, do come in contact with the sample and detector, and require higher purity gases. Unfortunately, gas nomenclature as it relates to purity is not consistent across specialty gas suppliers. It is important to recognize the impurities in your gas supplier’s products, and to utilize the appropriate Agilent gas purification products (see next section).
Gas Type
Air
Nitrogen
Function
Pneumatics
Pneumatics
Sample
Contact
No
No
Purity Required*
Low Grade
Low Grade
Limit of Detection required:
1-1000 ppm 1000 ppm-1% Trace (0-1 ppm)
Hydrogen
Hydrogen/Helium Mix
Methane/Argon or Nitrogen
Air
Carrier or fuel gas for detector
Fuel gas for detector
Carrier or make-up for ECD
Oxidant for detector
Yes
Yes
Yes
No
Research
Research
Research
Ultra-Pure
Ultra-Pure
Ultra-Pure
Research
Ultra-Pure
Nitrogen, Helium, or Argon
Carrier or make-up gas Yes Research Ultra-Pure
*Purities of gases depend upon the type of detector that is used. Use this table as a general guide only and refer to your detector manual for specific gas purities that are needed.
Low Grade = Specialty or industrial gases (
≤
99.998%)
UHP/Zero Grade (99.999%)
Ultra-Pure Grade (99.9995%)
Research Grade (99.9999%)
Ultra-Pure
Ultra-Pure
Research
UHP/Zero
Ultra-Pure
1%-100%
UHP/Zero
UHP/Zero
N/A
UHP/Zero
UHP/Zero
3 www.agilent.com/chem • 800 227 9770
Contaminants in gases are major contributors to capillary column degradation and detector noise, and can interfere with chromatographic results. Concentration of these contaminants vary by the grade of gas.
Analytical gases are available in many grades of quality, from high purity
(99.995%) to chromatography grade purity
(99.9995+%). The higher the purity, the higher the cost.
To make a proper purity choice it is helpful to understand the contaminants most common in GC gases and how they can affect your analysis. Common contaminants are:
Hydrocarbons and Halocarbons
• decrease detector sensitivity by increasing detector background noise
• can also cause baseline drift or wander, contaminant peaks, and noisy or high offsets of baselines
• can be introduced by improper handling and/or installation of plumbing
• a common cause of column stationary phase degradation
• can damage instrument
• most common contaminant
• a common cause of column stationary phase and inlet liner degradation
• can cause decomposition of labile analytes
• opportunity for introduction at every fitting present in the gas line or during use of gas permeable tubing.
In some cases it may be difficult to determine which contaminant presents the biggest problem in a given analysis. If unsure, a call to your gas supplier may be helpful. Once the problem contaminants have been identified and a general contaminant level is determined, the next step is to choose a gas purity level that comes closest to these requirements.
Keep in mind that higher grades of gas generally cost more. The greatest cost savings can be achieved by using the lowest purity gas which will neither interfere with the analysis nor damage your equipment. Using the proper gas purification equipment to remove common contaminants and achieve the desired purity level is essential.
Agilent brings the highest performance and largest variety of gas purifiers (traps) to gas chromatographers. Purifiers are available in a variety of sizes and configurations to remove common contaminants like oxygen, moisture, and hydrocarbons. In-line gas purifiers, including refillable, indicating, S-shaped, and metal body types, are made to remove specific contaminants. Agilent also offers gas purification systems with removable cartridges. These systems provide the ability to design the right combination of filters needed for your application to achieve the proper gas purity.
The illustration on the next page shows the most common gas purification configurations used in gas chromatography.
Regardless of which purification system is employed, proper installation and maintenance is required to achieve optimal performance from the purification system(s). A purifier that is not maintained will eventually expire and become ineffective, or worse, a source of contamination.
• determine desired purity level
• keep number of fittings in gas line to a minimum
• install purifiers in a convenient location close to the GC
• purifier log books are useful for determining maintenance schedule
• use indicating traps closest to the GC so you can determine when to change the traps that are upstream www.agilent.com/chem • 800 227 9770 4
In-Line Gas Purifiers
Gas supply
-OR-
Gas Purification System
Gas supply
-OR-
Vent
Combination Trap
Key:
1 = Moisture Trap
2 = Hydrocarbon Trap
3 = Oxygen Trap
4 = Indicating Oxygen Trap
5 = Gas Purification System
6 = Combination Trap for moisture, oxygen, and hydrocarbon removal
Detector Gas Purification
FID make-up, air, and H
2
ECD make-up
ELCD reaction gas
MS carrier gas
Gas supply = cylinder, in-house line, or gas generator
Regulator = Brass dual stage regulator
The purpose of gas traps is to remove detrimental impurities from the carrier and detector gases. Moisture (water), oxygen and hydrocarbon traps are the most common traps used with GC systems. A few combination traps are available which remove moisture, oxygen and/or organics with a single trap. The effectiveness of the traps depends on the initial quality of the gas. Little enhancement by traps to the GC system is obtained by traps when using very high purity gases (e.g., ultra-high purity or similar grades) while obvious improvement is obtained with lower grades of gas.
Constant exposure of capillary columns to oxygen and moisture, especially at high temperatures, results in rapid and severe column damage. The use of oxygen and moisture traps for the carrier gas may extend column life and protect the instrument. Traps may provide some protection if there is a leak at or around the gas cylinder. Any moisture or oxygen introduced into the gas stream due to the leak will be removed by the trap until it expires. This creates an opportunity to detect and fix the leak before column or instrument damage occurs.
5
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.
www.agilent.com/chem • 800 227 9770
There are several different adsorbents and indicating materials used in moisture traps. Moisture traps can be easily refilled.
Adsorbent refills are typically 1/4 to 1/2 the cost of a new trap making refilling a more economical (and less wasteful) option.
Indicating moisture traps are available in plastic and glass bodies.
Glass body traps are used when potential contaminants from plastic trap bodies are a concern. Glass traps are normally encased in a protective, plastic shrink wrap or a high impact plastic shield (outer trap body). Glass and plastic bodied traps are usually pressure tested at 150 psi, thus they are safe for use at the typical pressures required by the GC.
Refillable Glass Moisture Trap
Description
Size
(cc)
H
2
O Removal Maximum Effluent H
2
Capacity (g) Concentration (ppb)
O 1/8 in.
Part No.
1/4 in.
Part No.
Molecular Sieve 13X and Indicating 4Å – Economy, with plastic Lexan body (other packings available, see Agilent catalog)
Refillable Moisture Trap
Adsorbent Refill (1 pint) for MT Series
200 36 18 MT200-2
MSR-1
Glass Indicating Moisture Traps (larger size is available, see Agilent catalog)
Glass Indicating Moisture Traps 100
Molecular Sieve Refill for GMT Series 250
16.3
6 GMT-2-HP
GMSR
MT200-4
MSR-1
GMT-4-HP
GMSR
Moisture Removal S-Trap – can be reconditioned in the GC oven
Moisture S-Trap – preconditioned
Big Moisture Traps – for the Ultimate Moisture Capacity
Big Moisture Trap
Refill for BMT Series (2 refills)
750
5060-9084
BMT-2
BMSR-1
BMT-4
BMSR-1
Price
$226
$235
$ 58
$104
$ 55
$119
$ 63
Refillable Moisture Trap www.agilent.com/chem • 800 227 9770
Moisture S-Trap Big Moisture Trap
6
Indicating Oxygen Trap
Big Oxygen Trap
Oxygen traps usually include a metalcontaining inert support reagent. Most oxygen traps reduce the oxygen concentration to below 15-20 ppb. The capacity of a standard oxygen trap is approximately 30mg of oxygen per 100cc of trap volume. Oxygen traps can also remove some small organic and sulfur compounds from gas streams, but this is not their primary application.
Metal (usually aluminum) trap bodies are recommended for GC analyses. Some
Description Size (cc)
1/8 in.
Part No.
Indicating Oxygen Traps – glass body with plastic safety shield
1/4 in.
Part No.
Price
Indicating Oxygen Trap 30 IOT-2-HP IOT-4-HP
Big Oxygen Traps – non-indicating, for the Ultimate Oxygen Capacity (smaller size available, see Agilent catalog)
Big Oxygen Trap 750 BOT-2 BOT-4
$143
$235 plastics are permeable to air and contain contaminants that can degrade gas quality.
In addition, many of the metal bodied oxygen traps can withstand high pressures
(up to 2000 psi). Some oxygen traps also remove moisture from the gas stream without affecting the oxygen removal capability.
Indicating oxygen traps change color when oxygen is present in the gas at harmful levels. Indicating traps are not intended to be the primary oxygen removal trap, but should be used in conjunction with a high
capacity non-indicating oxygen trap. They are installed after the high capacity oxygen trap in the gas line to indicate when the high capacity trap has expired and needs to be changed. Expired oxygen traps need to be immediately changed since they can contaminate the gas, in addition to failing to remove oxygen.
7
Description Size (cc)
1/8 in.
1/4 in.
Part No.
Part No.
Price
Hydrocarbon Traps – General Purpose
Refillable Hydrocarbon Trap
Adsorbent Refill (1 pint, 2 refills)
200 HT200-2
ACR
Big Hydrocarbon Traps – for the Ultimate Hydrocarbon Capacity
HT200-4
ACR
$106
$ 63
Big Hydrocarbon Trap
Refill for Big Hydrocarbon Trap (2 refills)
750 BHT-2
BACR
BHT-4
BACR
$235
$ 52
Hydrocarbon Removal S-Trap – can be reconditioned in the GC oven
Hydrocarbon S-Trap 5060-9096
Capillary Grade Hydrocarbon Traps – for crucial capillary applications
Capillary Grade Hydrocarbon Trap
Adsorbent Refill (1 pint, 3 refills)
100 HT3-2
ACR
HT3-4
ACR
$232
$ 98
$ 63
Hydrocarbon traps remove organics, such as hydrocarbons and halocarbons, from the gas stream. The adsorbent is usually activated carbon or an impregnated carbon filter media. Carbon removes organic solvents from the gas stream, including the typical solvents used in nearly every lab.
Hydrocarbon-moisture combination traps are also available which remove water in
Hydrocarbon Trap www.agilent.com/chem • 800 227 9770
addition to organics as described in the next section. Capillary grade hydrocarbon traps are purged with ultra-high purity helium and packed with a very efficient activated carbon material. Metal trap bodies are used to prevent any contaminants in plastic trap bodies from contaminating the carbon adsorbent. Most hydrocarbon traps can be refilled by the end user.
Big Hydrocarbon Trap
Hydrocarbon S-Trap
Agilent carries several Combination Traps that provide multiple contaminant removal in a single trap. These traps offer:
• Optimized adsorbents for maximum surface area and capacity
• Leak-free, one-piece design to eliminate potential leaks from using multiple traps
• Efficient design which prevents channeling and promotes efficient scrubbing
• The ultimate in purification with a single trap (Big Universal Trap)
Description
Oxygen/Moisture Traps
Size (cc)
1/8 in.
Part No.
1/4 in.
Part No.
Price
Agilent OT3 Trap
Hydrocarbon/Moisture Traps
100 OT3-2 OT3-4 $104
Refillable Hydro-Moisture Trap
Refill for Hydrocarbon/
Moisture Trap (1 pint, 2 refills)
200 HMT200-2
HCRMS
HMT200-4
HCRMS
$ 98
$ 63
Big Universal Traps – for the Ultimate in Gas Purification, removes oxygen, moisture, hydrocarbons, CO, and CO
2
Big Universal Trap – Helium purged (also recommended for GC Mass Spec) 750 RMSH-2 RMSH-4 $261
Big Universal Trap – Hydrogen purged 750
Big Universal Trap – Nitrogen purged 750
Big Mounting Clip for mounting Big Traps 2/pk
RMSHY-2
RMSN-2
UMC-5-2
RMSHY-4
RMSN-4
UMC-5-2
$261
$261
$ 21
Agilent OT3 Trap
Big Universal Trap
Hydrocarbon Moisture Trap www.agilent.com/chem • 800 227 9770 8
9
Three Cartridge
High Capacity
Gas Purification
System
Description Part No.
Three Cartridge System–Includes manifold for wall or bench mount and 3 cartridges
(H
2
O/hydrocarbon, oxygen, and indicating O
2
)
With 1/8 in. fittings 5183-1907
With 1/4 in. fittings
Replacement Cartridge Kit–
Includes all three cartridges for above system
5182-9776
5182-9780
Single Cartridge System–Includes single cartridge manifold brackets for wall or bench mount, and a triple combination cartridge
(H
2
O/hydrocarbon, and O
2
)
With 1/8 in. fittings 5183-4598
5183-4599 With 1/4 in. fittings
Triple combination replacement cartridge for single cartridge system 5183-4600
• Agilent’s highest capacity and most economical gas purification system.
• Provides low-cost gas contaminant removal for up to 18 cylinders of carrier gas.
• Includes a manifold with cartridge mounts and three replaceable cartridges: 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.
• Contains a triple-combination cartridge that offers the same highly efficient contaminant removal properties from eight cylinders of carrier gas but without the visual indicator.
• Other cartridges are also available for detector gas supplies and as individual filters for specialized requirements.
Price
$239
$255
$136
$612
$567
$393 www.agilent.com/chem • 800 227 9770
The QC+ Point of Operation Panel contains purifier cartridges that can be quickly changed. The cartridges are removed from the panel without interruption of gas flow to the system, drastically minimizing costly instrument downtime.
Filter cartridges are of all metal or glass construction, eliminating infusion and resultant signal noise associated with filters constructed from plastics. Cartridges are quickly installed via a simple knurled retaining nut, with no wrenches needed.
As many as four cartridges can be replaced in a matter of seconds, and because there is low dead volume, a minimal amount of gas system purge is required after installation.
Fitting (in.) Part No.
Description
4-Head
O
2
, indicating O
2
, HC, H
2
O 1/8 RQC-P
Price
$1604
Description
High capacity oxygen
High capacity moisture
Indicating moisture
Hydrocarbon
Indicating oxygen
Part No.
GC-1
GC-2
GC-2-I
GC-3
GC-4
Price
$ 64
$ 64
$106
$ 64
$155
RQC-P
www.agilent.com/chem • 800 227 9770
EASY ONLINE ORDERING
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
10
11
Super-Clean gas filter systems are designed to provide the utmost in convenience and contamination reduction. The system is tested for leak-tightness and the glass and metal construction of the cartridges eliminates diffusion of contaminants into the gas stream. During cartridge replacement, check valves and close off the system to the atmosphere, further minimizing the entry of contaminants.
Available with 1/8" fittings only
Description
Carrier Gas Purification System: Single position system perfect for GC/MS,
ECD and NPD detectors. Includes the triple filter cartridge.
Super-Clean Gas Purification System:
For your most demanding GC application, includes four position baseplate manifold with four filter cartridges: oxygen, moisture (both with indicator), and two hydrocarbon cartridges.
Replacement Filter Cartridges
Triple Filter Cartridge: A single carrier gas filter now with hydrocarbon, moisture, and oxygen trapping capability. Includes moisture and oxygen indicator so you know exactly when to replace the cartridge.
Filter cartridge bundle of 4 (oxygen, moisture, and 2 hydrocarbon)
Part No.
5182-9704
5182-0816
5182-9705
5183-4770
Price
$ 398
$1291
$ 186
$ 530
Description
Universal/external split vent trap with 3 cartridges
(1/8 in. Swagelok fitting)
Replacement cartridges (3/pk)
Part No.
RDT-1020
RDT-1023
Price
$ 94
$ 45
Split vent traps stop environmental pollution. The split vent trap was designed to protect the lab environment from the contaminants released by split injection systems, which can vent up to 500 times the amount of sample reaching the detector into the laboratory's air. A replaceable, impregnated carbon filter media traps and eliminates a broad range of contaminants. The traps are also easy to change and come with three packs of replacement cartridges each. Replace approximately every six months.
Split Vent Trap and Cartridges www.agilent.com/chem • 800 227 9770
Pressure regulators are an integral component in any gas handling system.
Their function is to reduce the pressure from a high pressure source, such as a cylinder, to a suitable use pressure.
Although regulators are very good at controlling pressure, they do not control flow. They have a maximum flow rate which is dictated by the design. Basically, the flow is determined by the pressure drop across the regulator.
There are primarily two types of regulators: single stage and dual (or two) stage.
The difference is that a dual stage regulator is actually two regulators connected in a series.
Dual stage regulators provide more precise and consistent pressure control than single stage regulators. The reason is that in a single stage regulator, as the gas cylinder empties and the inlet pressure to the regulator decreases (inlet decay), the pressure on the diaphragm is reduced.
Without proper adjustment, the outlet pressure might slowly rise.
A dual stage regulator overcomes this problem by connecting two regulators together. The first stage regulates the pressure to the second stage, thus creating a constant pressure and allowing minimal inlet decay. Agilent recommends using two-stage regulators with our GC Systems to provide the proper pressure control for optimal use.
Regulators are usually constructed of brass or stainless steel. The choice of material follows the same guidelines as the choice of tubing. Generally, it is not recommended that the materials be interchanged. If stainless steel tubing were chosen due to purity considerations, then a stainless steel regulator should be chosen for the same reasons. Steel regulators are more expensive, which is why Agilent offers brass regulators for less demanding applications.
No matter which material is chosen for the regulator body, be sure to specify one with stainless steel diaphragms for critical applications such as use on carrier, fuel or detector gases. Agilent recommends using our economical brass body, dual stainless
Brass Body Regulator steel diaphragm regulators for most GC applications. These regulators, combined with the proper gas purification system, provide proper gas pressure control and purity for gas chromatography.
When ordering a regulator, be sure to specify the proper connections. In the
US, most gas manufacturers follow CGA connection guidelines. In Europe, there are a number of organizations designating cylinder connections that are specific to individual countries. It is best to contact your local supplier for the proper connection designation.
Description Part No.
Brass Body, Dual Stainless Steel Diaphragms (1/8 in.)*
CGA 346, 125 psig max (8.6 bar), Air
CGA 350, 125 psig max (8.6 bar), H
2
, Ar/Me
CGA 540, 125 psig max (8.6 bar), O
2
CGA 580, 125 psig max (8.6 bar), He, Ar, N
2
CGA 590, 125 psig max (8.6 bar), Air
*For 1/4 in. tubing, purchase a 1/4 in. adapter listed below
5183-4641
5183-4642
5183-4643
5183-4644
5183-4645
Regulator Outlet Adapters – Female NPT to Swagelok-style
1/4 in. to 1/8 in. brass
(included with brass regulators)
1/4 in. to 1/4 in. brass**
** Required for plumbing 1/4 in. tubing to regulators above
0100-0118
0100-0119
Price
$ 14
$ 15
$275
$275
$275
$275
$275
TIPS AND TOOLS
Always depressurize a regulator before closing by adjusting knob and removing the regulator from the cylinder.
www.agilent.com/chem • 800 227 9770 12
13
Spectra-Link Tubing Connecting System on a two-stage regulator
Tubing Type Diameter
(inches)
Recommended
Max. Length (feet)
Copper
Copper
1/8 *
1/4*
50
300
*Recommended when multiple instruments are connected to the same source
Pressure Drop
(psig)
2
0.5
When constructing or maintaining a gas delivery system for GC, choosing the proper tubing material is very important and will help to eliminate potential problems and improve the overall quality of the gas system. Although there are many common tubing materials available, some pose safety or cleanliness problems.
Non-metallic types of tubing such as polyethylene and Teflon are not recommended for GC applications due to their gas permeability and difficulty in cleaning. This type of tubing can be used for non-critical applications, such
Parameters: 2000sccm (4.2 scfh); Temperature: 70˚F; Pressure 30 psig as pressurizing pneumatic lines; however, be aware of its pressure limitations.
In view of these problems, the list of appropriate tubing materials has been narrowed down to two: copper and stainless steel. Agilent recommends using copper tubing for most applications, since it is easy to bend and plumb and is less expensive than stainless steel. Use stainless steel tubing only for crucial applications that require very high purity, or where building codes mandate its use.
Before any tubing is placed into service, or if it becomes contaminated with use, it is essential that it be properly cleaned.
Unclean or improperly cleaned tubing can lead to contamination of the system with disastrous results.
Cleaning tubing requires the use of suitable detergents and solvents along with nitrogen and a purgeable oven for drying. This may be done easily for small lengths of tubing, but in larger systems the cleaning procedure sometimes becomes unwieldy, leaving behind a large quantity of solvent requiring proper disposal.
Fortunately, Agilent provides clean, high quality GC grade tubing for large systems as an economical alternative.
Description Part No.
Price
Copper tubing, 1/8 in., 50 ft.
Copper tubing, 1/8 in., 12 ft.
5180-4196
5021-7107
$56
$28
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.
www.agilent.com/chem • 800 227 9770
• Stainless Steel: no outgassing or permeation through polymeric materials
• Quick Connection: prevents air from entering gas lines during tank changeover
• Tested: each system has leak rates lower than 1x10 -5 cc/sec
Description
Spectra-Link with 1/8 in. fittings and 36 in. SS tubing
Spectra-Link with 1/4 in. fittings and 36 in. SS tubing
Part No.
SL-8
SL-4
Price
$496
$496
Description
Cylinder wall bracket with strap and chain
(cylinder size up to 14 in., 35 cm)
Part No.
5183-1941
Price
$ 60
Leaks allow oxygen and other contaminants to enter the gas stream.
Therefore, GC instrument maintenance should include checking fittings and connections with a gas leak detector.
Agilent’s Gas Leak Detector enables quick and easy detection and measurement of gas leaks for 12 common gases. Based on a dual cell micro volume thermal conductivity system, this unit provides very high sensitivity and eliminates contamination caused by soap solution methods.
Description Part No.
Price
Leak detector includes probe, extended flexible probe, range extension nozzle, probe clip and template, cable, AC power adapter/battery charger, battery, user manual, cleaning wipe, and carrying case (available in 115 V or 220 V).
Gas leak detector, 115 V
Gas leak detector, 220 V
5182-9646
5182-9648
$1915
$1915
Cylinder Wall Bracket
Gas Leak Detector www.agilent.com/chem • 800 227 9770 14
Setting and maintaining GC flow rates greatly affect the instrument accuracy and sensitivity. During maintenance, verify carrier and support gas flows with the proper flowmeter. Choosing a flowmeter for your application depends upon measurement speed, ease of use, accuracy, and flow rate range.
Agilent manufactures the largest selection of volumetric and mass flowmeters for chromatography. We have developed flowmeters for measuring capillary column flows, calibrating air pumps and flow controllers, and verifying instrument gas flows. All flowmeters are calibrated to
NIST-traceable standards.
15
FlowTracker 2000
ADM 1000
Description Part No.
Price
FlowTracker 1000 Flowmeter
FlowTracker 2000 Flowmeter and
Leak Detector
5183-4779
5183-4780
FlowTracker Universal AC Adapter (optional, not supplied with FlowTracker units) 5183-4781
$ 816
$1143
$ 43
• Accuracy ± 3%
• Operating temperature range–
0 to 45ºC for the instrument, -70 to
135ºC for the tubing
• Calibration–traceable to NIST primary standards
• Real time, split ratio measurement
• CE mark certified
• Measures flow rates from 0.5 to
1000 mL/min
• Split ratios–compare the ratio from one gas measurement to another
(i.e., injection port split ratios)
In addition to the features of the ADM
1000, the ADM 2000 includes:
• Mass flow measurements–measure flow rate, independent of atmospheric pressure and temperature (calculated)
• Data output through RS-232 port
• 9V battery and AC power adapter
(120 or 220 VAC)
ADM 2000 www.agilent.com/chem • 800 227 9770
Description
Flow Rate (mL/min)
Low High
Gases
Measured
Accuracy
(%)
Power
Supply
RS-232 Data
Output
ADM1000
ADM2000
ADM2000E
0.5
0.5
0.5
1000
1000
1000
All
All
All
± 3
± 3
± 3
9V Battery
Battery or 120 VAC
Battery or 220 VAC
None
Yes
Yes
Veri-Flow 500
(110 V)
Veri-Flow 500
(220 V)
5.0
5.0
500
500
He, H
2
, Ar/CH
4
N
2
, Air
He, H
2
, Ar/CH
4
N
2
, Air
± 3
± 3
Rechargeable Battery or 110 VAC
Rechargeable Battery or 220 VAC
Yes
Yes
Optiflow 420 0.1
50 All +/- 3 9V Battery
Optiflow 570
Optiflow 650
0.5
5.0
700
5,000
*non-corrosive gases only
**non-corrosive and mildly corrosive gases only
All
All
+/- 3
+/- 2
9V Battery
9V Battery
None
None
None
Part No.
220-1170
220-1171-U
220-1171-E
HVF-500
HVF-500-2
HFM-420
HFM-570
HFM-650
Price
$620
$725
$725
$681
$681
$573
$573
$677
Veri-Flow 500 www.agilent.com/chem • 800 227 9770
Optiflow 420
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.
16
You asked … we listened!
Based on customer feedback, we’ve rebuilt our site navigation and layout to help you more quickly find the information you need about Agilent products and services.
screen resolution and optimizes the page size for less scrolling.
product literature, technical support, education, events, and news.
pricing, order status, quotes, and local sales information.
keep your instruments running in top condition.
for consistent and accurate GC analyses.
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 • 800 227 9770
“Good sample introduction helps ensure good reproducibility, optimal peak shape, and accurate sample delivery. Agilent’s commitment to offering the highest quality supplies means accurate, reliable results.
Time after time.”
Bryan Bente, Ph.D.
Technology Development Manager
CATALOG
For a complete selection of vials, syringes, and inlets, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
18
Agilent’s wide opening vials are designed specifically for analyzing samples with your
GC. They have specially designed vial neck angles, bottom design and height to ensure compatibility with Agilent autosamplers with rotating or robotic arm trays. Agilent offers a large variety of autosampler vials in different closures, cap colors, septa choices and package options. Agilent also offers convenience packs with 500 vials and caps in a reusable blue storage box.
For small sample sizes, Agilent offers a variety of options. You can use microvolume inserts with the wide opening vials or, for added convenience, use vials with small volume capacity.
When filling sample vials, keep in mind:
• if you need to test a large amount of sample over repeated injections, divide the sample among several vials to obtain reliable results
• when sample volume in the vial is low, contaminants from the previous sample injection or solvent washes may have a greater impact on the sample.
The airspace in the vial is necessary to avoid forming a vacuum when sample is withdrawn. This could affect reproducibility.
Glass –for general purpose use and for use with acids
Silanized –for use with samples that bind to glass, and for trace analyses
Polypropylene –for use with alcohols and aqueous solvents
Amber Vials –for use with light-sensitive samples
Microvolume Inserts –for use with very small sample volumes
High Recovery Vials – for use with limited sample volumes
19
TIPS AND TOOLS
Do not inject air into the vials to prevent the vacuum.
This often damages the cap seal.
1 mL
3.6 mm*
*Needle position based on standard sampling depth.
50 µL
100 µL vial www.agilent.com/chem • 800 227 9770
Vial cap septa are critically important to optimal analysis. Each septum complements the overall system and enhances chemical performance.
Agilent’s vial cap septa are specifically formulated and constructed for optimum system performance, with minimal coring and superior chemical inertness.
• Routine analysis
• Moderate resealing
• Excellent chemical inertness
• Not recommended for multiple injections or storage of samples
• Least expensive
• Excellent resealing
• Resists coring
• Good for multiple injections
• Used in trace analysis applications
• Above average resealing
• Most resistant to coring
• Least evaporation
• Use with large diameter, blunt tip syringe needles
• Good for MS and ECD analysis
• Good for large-volume injections
• Chemically inert
• No resealing
• Single injection
• No long-term sampling storage
• Chlorinated solvents
• Organic acids
• Limited resealing
• Not suitable for 32 gauge syringe
To determine potential septa ordering quantities, consider:
• the number of samples run during a day/week
• if samples are run in small or large batches
• if samples are run manually or with an autosampler
• if samples are run overnight, unattended
Unattended autosampler runs require a precise fit for uninterrupted operation.
Typically, automated sample runs use a higher quality and quantity of vials.
Description Quantity Part No.
Vials
2 mL Crimp top vial convenience pack with silver AI caps with
Teflon/Red rubber septa
2 mL Screw top vial convenience pack with blue screw caps and
Teflon/Red rubber septa
2 mL Snap top vial convenience pack with clear polypropylene snap caps and Teflon/Red rubber septa
100 µL Insert for wide opening vials
500/pk
500/pk
5181-3400
5182-0732
30 µL reservoir volume, High recovery vial, crimp top
500/pk
100/pk
5182-0547
5181-1270
250 µL Polypropylene flat bottom inserts 500/pk 5183-2087
100 µL Glass lined polypropylene vials 100/pk 9301-0977
Less than 5 µL dead volume,
Micro-V vial, clear crimp top 100/pk 5184-3551
100/pk 5182-3454
Price
$115
$183
$154
$ 88
$ 57
$158
$ 69
$109 www.agilent.com/chem • 800 227 9770 20
Syringe type and design are important for chromatography to ensure reproducible sample injections for consistent results.
The Agilent line of syringes include a variety of plunger and needle choices to use with your autosamplers.
Agilent syringes are designed:
• for reproducible sample volume delivery
• specifically for the Agilent inlet or autosampler
• to maximize inlet septum lifetime
1. Select the syringe type based on the inlet (injection port) you are using and the volume of sample you want to inject.
2. Select a syringe. Refer to your automatic liquid sampler operating documentation for available syringe sizes and corresponding injection volumes.
3. Select the appropriate syringe needle gauge.
Sharp tip
Inlet
Packed, split or splitless (including PTV)
Cool on-column
Cool on-column
Cool on-column
Needle Gauge Column Type
23 gauge or 23/26 gauge tapered any
23/26 gauge tapered or 26 gauge 530 µm
26/32 gauge tapered
26/32 gauge tapered
320 µm
250 µm
Needle tips
Cone tip
Tapered needle
Use syringe needles with an Agilent dualtaper needle or a conical tip. Sharp-tipped needles tend to tear the inlet septum and cause leaks. Also, a sharp-tipped needle tends to leave residual amounts of sample on the septum as it exits, resulting in a large solvent tail on the chromatogram.
21
TIPS AND TOOLS
For best results, use the Agilent Cone Tip (HP Point Style) with
Agilent’s Centerguide Septa, page 38. www.agilent.com/chem • 800 227 9770
Syringe
5 µL, fitted plunger
Advantage Limitations Recommended Use
• Most accurate syringe for 1µL injection
• Thinnest plunger, • 1 µL injections can bend more easily
• Clean samples
• Routine analysis
• No hardware • Not ideal for higher modification needed viscosity samples for 0.5 µL injection • Plunger not replaceable
10 µL, fitted • Most economical plunger • Most reliable fitted plunger syringe
• Less bending
• Better for high viscosity samples
• Most accurate only • General purpose for 1 µL and larger syringe injections • Clean samples
• Plunger not replaceable
• Routine analysis
10 µL, gas-tight
• Replaceable plunger • More expensive • Dirty samples for reduced repair cost than fitted plunger • Gases and volatile
• Not available in samples
• Reactive samples • Less plunger binding 5 µL size than fitted plunger
• Tight seal between plunger and barrel
The stainless steel needles used for
250-µm and 320-µm injections must be inserted into a glass syringe barrel.
Select the correct size needle for the column you plan to use.
To insert a needle into a syringe barrel:
1. Unscrew the syringe barrel cap and remove the spring.
2. Make sure the needle has the Teflon disk. If the syringe barrel does not have the Teflon disk, use the instructions in the syringe box to wrap the needle yourself.
3. Slide the spring and the cap down over the needle.
4. Insert the needle into the syringe barrel.
5. Screw the cap back on the syringe barrel.
TIPS AND TOOLS
Failure to use an on-column syringe when injecting into an on-column inlet could damage the injector, syringe and column.
www.agilent.com/chem • 800 227 9770 22
• Make sure to input the proper syringe size when setting up the injection section of your data handling device.
• Rinse syringes and clean their plungers before use to maximize syringe lifetime.
• Rinse the syringe 5-8 times between injections to minimize sample carryover.
• Pump sample in and out of the syringe at least 5 times to remove any air bubbles, and for maximum reproducibility and accuracy.
• 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.
• Remove a gas-tight plunger from the syringe for long-term storage to keep the
Teflon tip leak-free. If a gas-tight plunger does not fit properly, place it in hot water for about 10 minutes then press the tip uniformly on a clean, hard surface and let cool to room temperature. The plunger should reseal correctly to provide 10-25% more injections.
• To maximize the lifetime of standard plungers, rinse the syringe and wipe the plunger with solvent (isopropanol or acetone) and a lint-free wipe, as specified in the syringe cleaning procedure included with each syringe.
see page 25
23
VIDEO
To view a video on syringe installation, visit www.agilent.com/chem/techsupport. www.agilent.com/chem • 800 227 9770
Proper care, cleaning, and handling of each syringe will help ensure correct performance and long life. When cleaning your syringe, it is best to use solvents that effectively dissolve the sample you are working with. Try to avoid cleaning agents that are alkaline, contain phosphates, or are strongly acidic.
Problem
Bent plungers or stuck syringes
Possible Cause(s)
• Particles such as dust, leftover samples, salts, metal, or glass can fill the narrow gap between the plunger shaft and the inside wall of the barrel.
Suggested Action(s)
• If the plunger’s movement feels “gritty,” remove the plunger from the barrel, flush the shaft with solvent, and wipe it dry with a lintfree 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
Blocked needles
• Improper needle alignment.
• Narrow-gauge needles (26 gauge) bend more easily than larger (23 gauge) needles.
• Needles tend to bend when inserted into the sample vial – not the inlet port. This can be caused by septa that are too “tough.”
• If the needle has been slightly bent when 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.
• Use only Agilent autosamplers. They are precision-designed to ensure proper alignment with the syringe needle.
• Use 23 to 26-gauge tapered needles to get the combined benefits of greater septa life and fewer bent needles.
• Only use Agilent vials and septa.
• Sample material or contaminants may be trapped inside the needle.
• The needle may not have been properly cleaned.
• Remove the plunger and use a second syringe to fill the blocked syringe with 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
Note: even minor rust can cause the plunger to become stuck in the barrel.
“Ring around the neck” (A dark ring between the top of the barrel and the end of the volume scale.)
• During normal use, the shaft rubs against the glass walls of the barrel. This gradually wears away the rust-resistant metal on the shaft’s surface.
• Rusting happens most rapidly when using water or solvents that may contain (or absorb) water.
• To slow this process, remove the water from the syringe at the end of each day.
1. Rinse the syringe several times with a “dry” solvent, such as acetone.
2. Remove the syringe from the autosampler, and wipe the plunger dry with a lint-free cloth
3. Let syringe and plunger air dry.
• Skin oils and other organic material.
• Fine metal and glass particles from the syringe plunger and barrel may be rubbing together.
Once this happens, the plunger may bend if used further.
Loose plungers – accompanied by syringe leaks and area count reproducibility problems.
• The syringe is nearing the end of its useful life.
• Never touch the plunger shaft with your fingers.
• If build-up appears when water is the solvent: rinse syringe with acetone and wipe the plunger clean at the end of each day.
• Replace the syringe.
Note: Plungers normally feel “loose” when non-polar solvents (like hexane and toluene) are used. www.agilent.com/chem • 800 227 9770 24
25
Description Gauge/Length Quantity
Tapered Needle Syringes
(use for split/splitless or on-column injections with 0.53 mm id columns)
10 µL
5 µL
Tapered
Tapered
Fixed Needle
Fixed Needle
23-26s/42
23-26s/42
Straight Needle Syringes
(use with Merlin Microseal)
10 µL
5 µL
Straight
Straight
Fixed Needle
Fixed Needle
23/42
23/42
6/pk
6/pk
6/pk
6/pk
Part No.
5181-3360
5181-8810
9301-0725
5182-0875
Price
$198
$303
$191
$292
Description Unit Part No.
Miscellaneous Autosampler Supplies
4 mL Clear screw top wash vials with screw caps (no Septa)
Septa for 4 mL vial
Diffusion caps for 4 mL vials
4 mL wash vial with fill marking, caps
Screw for mounting syringe
Quadrant kit (4 tray sections)
7673/83 Basic Supply Kit contains:
10 mL syringes (6/ea), 23/26 gauge needles, 4 mL vials with diffusion caps
(144/pk), 2 mL automatic sampler vials with screw caps (1,000/pk),
GC septa (25/pk), Vial racks (5/pk)
144/pk
144/pk
9301 0723
9301-1031
12/pk 07673-40180
25/pk 5182-0551
07673-20570
18596-40015
07673-60840
Price
$755
$ 64
$ 21
$ 19
$ 26
$ 13
$ 75
Lot Numbers ensure certified performance to all specifications
Gold protective cap prevents chipping of the glass syringe barrel as it contacts the septum retainer nut
Black ink and gold illuminating backdrop for easier viewing of the volume scale
Individually sealed packaging for contaminant-free use www.agilent.com/chem • 800 227 9770
Packed-column direct inlets are very popular. Packed-column analysis is frequently done when high efficiency separations are not needed or when gases are analyzed by gas-solid chromatography.
Packed-column inlets are simple in both design and use. Few parameters need to be set, and all carrier gas flow flushes through the inlet into the column in the standard configuration.
Parameter Selection/Setting Rationale
Inlet temperature BP of solvent +50˚C
BP of major solute(s)
Ensures flash vaporization
Use for neat samples
Insert type 1/8-inch stainless steel
1/4-inch stainless steel
Use for ss column only
Inserts permit connection of columns up to 1/4-inch od.
Liner
Initial column temperature
Column type
Carrier gas flow
Glass Use to lower activity
(replaceable) temperature programming Sharpens peaks and reduces run time
1/8-inch packed stainless Will not break
1/4-inch packed glass Better for polar or labile compounds
20-40 mL/min
30-60 mL/min
Use with N
2 carrier gas
Use with He or
H
2 carrier gas
Most problems with packed-column inlets involve sample decomposition, flashback, or leaks.
Since packed-column inlets are active, especially if glass liners are not used, polar sample components will often tail or degrade in the inlet. Sample decomposition caused by the inlet is easily diagnosed; the decomposition products will have peaks at the same retention times as standards for the decomposition product.
When inlet-caused decomposition is suspected, try intracolumn direct injection, deactivated glass liners, or lower inlet temperatures, and remove any column packing in the inlet zone.
The inherent activity of packed-column inlets is somewhat mediated by the fact that they usually have low internal volume.
When this is coupled with the relatively fast flow rates used with packed columns, the residence time of sample in the inlet is short and decomposition is reduced in comparison to the decomposition that occurs with some capillary inlets (for example, splitless inlets).
The negative side of low inlet volume, however, means that excessively large sample injections will easily exceed the capacity of the liner and will flash back into gas supply lines and onto the septum. This can cause several maladies, including ghost peaks, sample losses, irreproducible peak areas, and decomposition.
Since packed-column inlets are usually flow-controlled, septum and column leaks will have a direct impact on retention times and peak areas. Sample can be lost through the leak holes, and air can diffuse back into the inlet to cause column degradation. Change the septum on a regular basis and check column connections at the first stage of problems.
To prevent stationary phase decomposition, make sure that the oven and inlet are at room temperature when not in use and when changing the septum.
www.agilent.com/chem • 800 227 9770 26
27
Item Description Unit Part No.
Price
1
2
3
4
5
9
10
11
Septum nut
Septa Bleed temperature, optimized, 11 mm
Top insert weldment
Viton O-rings
50/pk
12/pk
Glass liner, disposable 25/pk
Glass liner, disposable/deactivated 5/pk
6
7
Vespel/graphite ferrules, 1/4 in. id 10/pk
Tubing nut, 1/4 in. brass 10/pk
Adapters with glass liners
8 0.53 mm column adapter
1/8 in. column adapter
1/4 in. column adapter
Upper insulation
Nut warmer cup with insulation
Column nut for 0.53 mm column 2/pk
18740-60835
5183-4757
19243-80570
5080-8898
5080-8732
5181-3382
5080-8774
5180-4105
19244-80540
19243-80530
19243-80540
19243-00067
19234-60720
5181-8830
$ 37
$119
$ 99
$141
$ 5
$ 54
$ 25
For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
* For Model 6890/6850 only
$ 67
$132
$ 12
$ 37
$ 14
$ 42
$ 13
Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site.
See pages 104-115 for more information about our services and support.
Description Unit
Nonpurging septum nut assembly for manual flow control only, not EPC
Adapters without glass liners
1/8 in. column adapter
1/4 in. column adapter
Universal Packed-Column Inlet (non-purged)
Septum retainer nut for headspace sampling, nonpurging
Brass nut, 1/4 in.
10/pk
9
10
11
5
6
7
8
1
2
3
4
Liner
Part No.
1/4 in. Vespel/ graphite ferrule
Price
19243-60570 $100
19243-80510
19243-80520
$ 88
$128
19243-60505
5180-4105
$ 70
$ 13 www.agilent.com/chem • 800 227 9770
The combined “split/splitless” inlet is the most popular inlet for capillary column gas chromatography. Because it can be used in either split or splitless mode, it provides a very effective combination that can cover most analysis requirements.
Split injection is an effective way to introduce small amounts of sample without overloading the column. Split injection is required for samples that:
• cannot be diluted for analysis (for example, solvents)
• 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 injection is also good for screening samples of which little is known or for those that have widely differing concentrations, since the split ratio can be adjusted easily. Split inlets are also a good choice for dirty samples.
Split inlets are spared from most bandbroadening phenomena, since narrow peaks are generated as part of the splitting process. Therefore, any peak broadening or tailing observed with split injection is usually due to improper column installation, low split flow, (<20 mL/min on 6890) or low inlet temperature. If you suspect that the inlet temperature may be too low, increase it by 50˚C and compare the results to the lower temperature analysis. Repeat if results are positive until no further improvement is seen.
A majority of the problems encountered with split inlets are related to discrimination and decomposition. Both analytical accuracy and reproducibility decrease with the increases in discrimination and decomposition. Split inlets suffer from both needle discrimination and inlet discrimination.
Parameter Selection/Setting Rationale
Inlet temperature Try 250˚C or BP of last eluting compound
Inlet liner Large volume, deactivated
Ensures flash vaporization
Minimizes inlet discrimination
Minimizes flashback
Minimizes degradation
Inlet packing
Injection volume
Silanized glass wool
Glass beads or frit
None
0.5-3 µL liquid
0.10-10 mL gas
Injection technique Fast autoinjection
Split ratio
Hot-needle fast manual injection
50:1 to 500:1
Retains non-volatiles
Minimizes inlet discrimination
Less active than wool
Least active
Split easily adjusted
Split adjusted accordingly
Less needle discrimination
Reproducible discrimination
Not critical
Depends on sample and injection volume, and column ID
Narrow initial peaks Initial column temperatures
Septum purge 2-3 mL/min Minimizes ghosting
For fast and easy liner changes, check out Agilent’s new Flip Top Inlet Sealing System on page 52.
www.agilent.com/chem • 800 227 9770 28
29
Inlet temperature
Inlet liner
Inlet packing
Just above highest boiling point of solutes (+20˚C)
Large volume >0.8mL
Small volume <0.2mL
None
Silanized glass wool
Ensures flash vaporization
Reduce if degradation occurs
Use higher for dirty samples and higher-boiling solutes
Use with autoinjector
Use only for slow manual injections, and gas injections
Use only with slow injection
Decreases degradation
Use for fast autoinjection
& dirty samples
Injection volume 0.5-2 µL liquid Depends on solvent, liner,
& conditions
Injection technique Fast autoinjection Most reproducible
Less needle discrimination
Hot-needle slow manual Inject 1-2µL.sec if narrow liner is used and >1µL injection
Hot-needle fast manual Use for <1µL injections
Purge flow
Purge delay time
20-50 mL/min
20-80 sec
Higher if using constant flow
Adjust according to column flow rate/liner type
& sample conditions
Oven temperature 10-25˚C below solvent BP Necessary for solvent focusing
Column flow >2mL/min when possible Clears inlet fast
Reduces backflash and decomposition
Septum purge
Quantification
2-3mL/min
Internal standard
Standard addition
Reduces ghosting
Maximizes reproducibility
Use only with constant injection volume
Retention gap 1-3m, deactivated
(1-2m per µL injected)
Reduces peak distortion
Promotes solvent and stationary phase focusing
For splitless injection, a conventional split injector is operated in a nonsplitting mode by closing the split valve during injection.
The sample is flash-vaporized in the liner, and sample vapors are carried into the column by the carrier gas where they are recondensed at temperatures below the boiling point of the solvent. After most of the sample has been transferred into the column, vapors remaining in the liner are cleared by opening the split vent which remains open for the duration of the run.
The most important benefit of splitless injection is that a majority of the injected sample is introduced into the column. This results in much higher sensitivity than that achieved using split injection.
One requirement of splitless injections is that the initial column temperature should be kept at least 10˚C below the boiling point of the sample solvent. This allows the sample solvent to condense at the front of the column trapping the solvent molecules into a tight, narrow band.
Additionally, use a solvent that is similar in polarity to the column stationary phase, and avoid mixed solvents. Breaking these rules may result in split peaks.
Splitless injection is routinely used in areas such as:
• environmental analysis
• pesticide monitoring of foods
• drug screening
In these applications, sample preparation requirements are significant, and it is not always possible or economically justifiable to clean up a sample extensively. So column protection becomes as important as sensitivity. Also, samples with trace quantities of important solutes that elute on the solvent tail may be focused by the solvent to yield more sensitive analyses.
VIDEO
To view a video on liner and gold seal replacement, visit
www.agilent.com/chem/techsupport.
www.agilent.com/chem • 800 227 9770
Most problems encountered with splitless injection are related to incorrect purge time, degradation, improper focusing, and flashback.
Appropriate initial column temperature is critical. Sample vapors can be lost through the septum purge line if the insert is overfilled with sample vapor (either too large injection volume or too small liner volume), leading to irreproducibility and nonlinearity of peak areas. Match inlet temperature, liner volume, and injection volume carefully to avoid backflash.
Loss of peak area or generation of new peaks, can sometimes be dramatically reduced by changing liner type or by deactivating the liner and inlet with silanizing reagents. Removing or reducing the amount of liner packing can also decrease inlet activity.
6
7
8
9
10
4
5
1
2
3
Item Description Unit Part No.
Price
6
7
4
5
1
2
3
8
9
10
11
12
13
14
Septum retainer nut
Septa
Insert Weldment
Liner O-ring
Liner
Split vent trap assembly (6890/6850 only)
Retaining nut (6890/6850 only)
Retaining nut (5890 only)
SS seal
Gold-plated seal
Washer, 0.375 in. od
Reducing nut
Insulation (requires 3)
Lower insulation cover
Ferrule
Column nut (6890/5890 only)
Column nut (6850 only)
12/pk
2/pk
2/pk
Angled wrench for split/splitless inlet
18740-60835
See page 36
G1544-60575
See page 52
See page 47
G1544-80550
G1544-20590
19251-20620
18740-20880
18740-20885
5061-5869
18740-20800
19243-00067
19243-00070
5181-8830
5183-4732
19251-00100
$ 39
$216
$128
$ 26
$ 31
$ 26
$ 33
$ 8
$ 34
$ 5
$ 15
$ 26
$ 47
$ 29
* For a complete parts breakdown, see the 6890/6850 Series GC Instrument User and/or Service Manuals.
11
12
13
14 www.agilent.com/chem • 800 227 9770
TIPS AND TOOLS
A guard column or retention gap is often beneficial for splitless injections, improving peak shape and extending column life when analyzing dirty samples.
(See page 61).
30
Cool on-column injection is superior in many ways to other sample introduction techniques.
• elimination of sample discrimination
• elimination of sample alteration
• solvent focusing of early eluting solutes
• high analytical precision
If done properly, cool on-column injection provides the most accurate and precise results of the available inlets. Syringe discrimination is completely eliminated.
Moreover, inlet-related discrimination does not occur, since the liquid is introduced directly into the column. Automated oncolumn injection provides even higher analytical precision. Add to this the elimination of thermal decomposition and rearrangement reactions, and it becomes apparent that cool on-column injection should be considered whenever high precision and accurate results are required.
• maximum sample volumes are smaller compared with other inlets (0.5 µL to 2.0 µL)
• solute peaks eluting just before the solvent cannot be focused and are difficult to determine
• capillary columns (especially those with a large phase ratio or small inner diameter) can be easily overloaded with sample
• parameters such as initial column temperature, solvent nature, and injection rate must often be optimized
Parameter Selection/Setting Rationale
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
Injection volume 0.1-2.0 µL liquid
Simple and effective
Narrows initial peak width
Use smaller injections for small id columns;
Depends on column capacity
Injection technique
Oven temperature
Column flow
Septum purge
Quantification
Fast autoinjection
Fused silica needle
Inlet temperature or slightly lower
50-80cm/sec
30-50cm/sec
12-15mL/min
All methods
Projects droplets away from syringe tip
Use for manual injection into small id columns
Prevents backflash
Use for H
2 carrier gas
Use for He carrier gas
Use if installed to prevent ghosting
Retention gap requirements 1-3m, deactivated
Inherently reproducible technique
Lack of discrimination
Corrects peak distortion
Protects column from non-volatile components
Permits autoinjection with narrow-bore columns
31
TIPS AND TOOLS
Since the sample is directly deposited into the column, nonvolatile sample components can accumulate at the head of the column and will degrade efficiency and/or interact with subsequent injections.
www.agilent.com/chem • 800 227 9770
Sample preparation is important for on-column injection because of:
• the potential for column overload, column contamination,
• the incompatibility of some solvents with the stationary phase,
• dependence of the initial column temperature on the boiling point of the solvent.
Many of the problems associated with these variables can be resolved by using a retention gap ahead of the analytical column.
The major problems found with cool oncolumn injection are associated with column overload, solvent/stationary phase incompatibility, and column contamination.
If the flooded zone after injection is too long (large injections, poor wettability), peaks will be broad or split. A retention gap usually will resolve this problem. Loss of column efficiency with on-column injection usually is caused by contamination or degradation of the stationary phase at the head of the column. Only columns with an immobilized stationary phase should be used with cool on-column injection to prevent displacement of the stationary phase by solvents.
Immobilized stationary phases can be washed to remove contaminants and renew performance. If column performance does not improve after washing, cut 0.5m
off the inlet side of the column. If that does not return column performance, the column must be replaced and a retention gap should be used for all further injections of dirty samples.
Description
Column nut
250 µm graphite/Vespel ferrule
320 µm 0.5 mm graphite/Vespel ferrule
250 µm retention gap (one 5 m piece)
320 µm retention gap (one 5 m piece)
530 µm retention gap (one 5 m piece)
Quartz deactivated column connector fits 0.18-0.53 mm
Unit
2/pk
10/pk
10/pk
5/pk
Part No.
5181-8830
5181-3323
5062-3514
160-2255-5
160-2325-5
160-2535-5
5181-3396
Price
$ 26
$ 55
$ 51
$ 39
$ 42
$ 59
$ 94
TIPS AND TOOLS
Sample degradation can occur with cool on-column injection if column or retention gap activity is high. Use only well-deactivated retention gaps and high quality capillary columns from Agilent.
www.agilent.com/chem • 800 227 9770
VIDEO
To view a video on cool on-column installation and septum replacement, visit www.agilent.com/chem/techsupport.
32
33
Item Description
Manual injection
1c Cooling tower assembly
1d Duckbill septum
Fused silica syringe needles
Syringe barrel for use with fused-silica needles,10 µL
Common Supplies
3 Spring
Unit
10/pk
6/pk
Part No.
19320-80625
19245-40050
19091-63000
9301-0658
Price
$175
$ 29
$ 41
$ 90
19245-60760 $ 9
4 Inserts for capillary columns
For 200 µm columns (one ring)
For 250 µm columns (six rings)
For 320 µm columns (five rings)
For 530 µm columns (no rings)
19245-20510 $ 89
19245-20515 $114
19245-20525 $ 78
19245-20580 $ 55
For 530 µm Al clad columns (four rings) 19245-20780 $ 54
5 Ferrule 5080-8853
6 Column nut 2/pk 5181-8830
$ 47
$ 26
6890 Series GC Cool On-Column Inlet Supplies
Automatic Injection
1a Septum nut base for 320 mm assembly 19245-80521 $ 62
1b Septum nut base for 530 mm assembly
2 Advanced green 5 mm through hole septa
BTO 5 mm through hole septa
50/pk
50/pk
G1545-80520
5183-4760
5183-4758
$ 63
$ 62
$ 72
5890 Series Cool On-Column Inlet Supplies
Automatic Injection
1a Septum nut (5890 Series II GC)
1b Needle guide (for 7673A only)
19245-80520
19245-20670
$ 91
$ 35
* For a complete parts breakdown, see the 6890 Series GC Instrument User and/or Service Manuals.
1a
1b
1d
1c
2
3
4
5
6 www.agilent.com/chem • 800 227 9770
PTV inlets combine the benefits of split, splitless and on-column inlets. The sample is usually injected into a cool liner, so syringe needle discrimination does not occur. Then the inlet temperature is increased to vaporize the sample. The user programs vent times and temperature to achieve the equivalent of split or splitless transfer of sample vapors to the column. PTV injection is considered the most universal sample introduction system because of its flexibility.
• no syringe-needle discrimination
• minimal inlet discrimination
• no special syringe needed
• use of large injection volumes
• removal of solvent and low boiling components
• trapping of nonvolatile components in liner
• split or splitless operation
• retention time and area reproducibility approaching cool on-column injection
PTV inlets are actively cooled before and during injection by Peltier devices or by forced gases (air, liquid N
2
, or liquid CO
2
).
Cryogenic cooling of the inlet can reduce inlet temperature enough to thermally focus gas injections from other sampling devices in the liner. This is a distinct advantage of using PTV inlets in comparison to conventional inlets for coupling auxiliary sampling devices to capillary columns.
Post-injection, PTV inlets are heated using electrical heaters or preheated compressed air. Depending on design, inlet temperature ramps are either ballistic (i.e., ramped to the maximum temperature at an uncontrolled maximum rate) or programmable.
Parameter Selection/Setting Rationale
Injection mode Cold split
Cold splitless
For general use and sample screening
For trace analysis
Inlet temperature ramp rate
Adjustable (i.e., 2˚C/sec to 12˚C/sec)
Ballistic
Use slower ramp rates for labile, complex, or large volume samples
Use faster ramp rates for most samples
Use faster ramp rates to shorten splitless purge delay time
Simpler, less expensive instrumentation
Inlet liner
Injection volume
Sample Injection technique
Oven temperature
Straight with silanized wool For general use
Baffled For labile samples
Packed with an adsorbent For focusing gaseous injections from auxiliary sampling devices
0.1-1.5µL Use lower volumes for volatile solvents and fast ramp rates
Use volumes larger than
1.5µL only in solvent- elimination mode
Autosampler or manual, fast or slow
Not critical for cold split
& splitless modes
10-25˚C below solvent BP
Column flow
Sample dependent
30-50 cm/sec
For proper solvent effect in splitless mode
For split mode
Clears inlet faster
Less backflash
Septum purge
Quantification
Retention gap
1-5mL/min
Any method
1-3m, deactivated
Minimizes ghosting
Inherently reproducible
Low discrimination in cold injection modes
Compensates for extended flooded zone and solventcolumn incompatibility
VIDEO
To view a video on PTV column installation, liner installation and silver seal replacement, visit www.agilent.com/chem/techsupport.
www.agilent.com/chem • 800 227 9770 34
35
Item Description
3
4
5
1
2
6
7
8
9
10
11
Septumless head
Septum head
Septum nut
PTV inlet assy
PTV LCO
2 cooling jacket
PTV LN
2 cooling jacket
Silver seal
Column ID Unit Part No.
G2617-60507
G2618-80500
18740-60835
G2617-60506
G2617-60508
G2619-60501
5182-9763
Ferrules for
Graphpak inlet
5/pk
Graphpak inlet adapter 0.20 mm
0.25-0.33 mm
0.53 mm
5182-9754
5182-9761
5182-9762
0.20 mm 10/pk 5182-9756
0.25 mm 10/pk 5182-9768
0.32 mm 10/pk 5182-9769
Split nut for inlet adapters
0.53 mm 10/pk 5182-9770
5062-3525
PTV insulation block
PTV cryo insulator (not shown)
G2617-20510
G2617-60510
Teflon ferrule (needle seal)
Kalrez seal
Valve body
Pressure spring
Viton seal
Sealing element
CO
2
Cryo inline filter
Service kit for septumless head contains Kalrez seal, valve body, and pressure spring
Graphpak 3D ferrules
Installation tool for 3D ferrules
5/pk
5182-9748
5182-9759
5182-9757
5182-9758
5182-9775
5182-9760
3150-0602
5182-9747
5182-9749
G2617-80540
Price
$ 166
$ 146
$ 159
$ 61
$ 53
$ 137
$ 110
$ 91
$ 6
$ 24
$ 73
$ 137
$ 224
$2661
$1078
$ 39
$4850
$ 544
$ 473
$ 62
$ 173
$ 152
$ 146
$ 158
$ 166
$ 143
$ 208
1
3
2
4
5, 6
7
8
9
10
11
There are few choices in liner design for PTV inlets.
However, liner volume and activity are still key issues to be considered when selecting among the few available PTV liners. PTV liners require packing or a modified surface to hold the liquid sample in place before and during the vaporizing process.
Description
PTV Liner Single Baffle, 2 mm id 180 µL volume, deactivated, glasswool
PTV Liner Single Baffle, 2 mm id 200 µL volume, deactivated
PTV Liner Multi Baffle, 1.5 mm id 150 µL volume, deactivated
PTV Liner Fritted Glass, 1.5 mm id 150 µL volume, deactivated
Part No.
5183-2038
5183-2036
5183-2037
5183-2041
Price
$ 25
$ 20
$ 29
$ 55 www.agilent.com/chem • 800 227 9770
One of the key components of sample introduction is the inlet septum. All columns must have carrier gas head pressure to establish flow through the column. Septa maintain the leak-free seal and exclude air from the inlet. They come in many different sizes and are made from many different types of material specific to inlet type and analysis needs.
Septa are usually available according to their recommended upper temperature limits. Lower temperature septa are usually softer, seal better, and can withstand more punctures (injections) than their high-temperature counterparts.
If used above their recommended temperatures, however, they can leak or decompose. This causes sample losses, lower column flow, decreased column life and ghosting.
The septum isolates the sample flow path from the outside world. It must provide a barrier that is readily penetrated by the injector needle while maintaining internal pressure without contaminating the analysis. They are generally made of special high-temperature, low-bleed silicone rubber formulations.
Septa should be replaced regularly to avoid:
• leaks
• decomposition
• sample loss
• reduced column or split vent flow
• ghost peaks
• column degradation
Avoid problems by:
• using within the recommended temperature range
• changing regularly
• installing “hand tight”
• using septum purge when available
• using autoinjectors
• using sharp syringe needles
Agilent has recently introduced a new and innovative packaging design for inlet septa. This new packaging is a tri-fold blister pack that provides cleanliness, convenience, and consistency for our complete line of 11 mm and 9.5 mm septa.
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 • 800 227 9770 36
37
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
Large leak at septum during injection and for a short time thereafter (common with large diameter needles).
Replace septum and use smaller diameter needles.
Normal Problem Problem
(flow increase) (flow decrease)
Carrier gas leaks at septum or column connection.
Check for leaks. Replace septum or tighten connections if necessary.
Normal Problem Problem
MAINTENANCE MINDER
After repeated injections, septa can become prone to leakage.
To maintain system integrity, change septa regularly. www.agilent.com/chem • 800 227 9770
Our premium non-stick septa have a recess on the injection side, to guide the syringe needle to the same point with every injection.
• Proprietary plasma treatment ensures non-stick septa without the use of potentially damaging talcum powder
• Center point guides the needle for easy penetration and less coring
• Reduce needle bending
• Precision molding assures accurate fit in the inlet
• Each batch tested on an Agilent 6890 GC-FID for bleed
Agilent’s plasma-treated non-stick septa
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.
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.
Available in Bleed Optimized, Long-Life, and Advance Green.
Competitor “non-stick” septa www.agilent.com/chem • 800 227 9770 38
39
Agilent’s premium GC inlet septa are not garden-variety septa stamped out in large sheets, creating variations in geometry. Rather, each Agilent premium septum is molded to a perfectly uniform size and shape.
Individual molding lets us put a dimple in the center of each septum to guide the syringe needle into the inlet.
With the dimpled CenterGuide, the syringe needle enters the septum at precisely the same spot each time.
The result: minimal coring (see Figure 1).
• Less chance that a cone of material will be punched out of the bottom during the first few injections
• Virtually no septa material falling into the inlet liner, improving chromatographic quality
• Up to 1,000 autoinjections under optimal conditions before failure with HP Point syringes. The HP Point syringe yields optimal performance and reliability and reduces coring by parting, not cutting, the septum.
Agilent septa are made of highly durable, high-temperature tested silicone rubber.
Each lot is tested to ensure low bleed at high temperatures.
Figure 1. Comparison of Coring, With and Without CenterGuide
(30x magnification)
High-Temperature Septa Without CenterGuide: Major Coring Before 1
00 Autoinjections
1 autoinjection 100 autoinjections 700 autoinjections
Agilent BTO Septa With CenterGuide: Very Little Coring Even After
700 Autoinjections
SEPTUM TYPE
BTO
(Bleed and
Optimized)
Long Life
Advanced Green
✔✔✔ = best
BLEED
✔✔✔
(optimized for
LIFETIME
✔
TEMPERATURE
LIMIT to 400ºC
✔
✔✔
✔✔✔
✔✔
✔✔ = very good ✔ = good to 350ºC to 350ºC www.agilent.com/chem • 800 227 9770
p/n 5183-4757
• Extended temperature range, low-bleed
• Maximum Injection Port Temperature
400ºC
• Virtually eliminates injection-port sticking
• Pre-conditioned; packaged in glass to prevent contamination
• Ideal for use with low-bleed,
“Mass Spec” capillary columns p/n 5183-4761
• Pre-pierced for extended life and reduced coring
• The preferred Septum for Autosamplers
• Ideal for Overnight Runs
• Up to 400 Injections Per Septum injection
• Maximum Injection Port Temperature
350ºC
• Soft, 45 Durometer, Easy On
Autosampler Needles p/n 5183-4759
• True Long-Life, High Temperature
Green Septum
• More Injections per Septum
• Reduced Injection Port Sticking
• Maximum Injection Port Temperature
350ºC
• Packaged in glass vials for high purity
• Economical alternative to competitor’s
“Green” Septa
Agilent’s General Purpose Septa are made from an enhanced injection-molded silicone rubber material. The septa material, dark red or gray in color, is specified to withstand over 200 automatic injections at an injection port temperature of
350ºC. You can have confidence in your chromatographic results knowing that each lot of septa is placed through a demanding QC test to ensure that only the highest quality product is delivered to your laboratory.
• Low bleed for reduced instrument maintenance downtime and increased laboratory productivity
• Less frequent replacement for long lifetime and the ability to withstand more than 200 autosampler injections at maximum injection port temperatures
• While general purpose septa do not have the centerguide of premium septa, they are made of durable material to minimize the risk of contamination and the need for reconditioning
• Convenient blister packs of 50 or 100 septa minimize risk of contamination and need for reconditioning www.agilent.com/chem • 800 227 9770 40
Premium Non-Stick Septa
Agilent Bleed and Temperature Optimized Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
Agilent Advanced Green Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
Agilent Long-Life Non-Stick Septa
11 mm septa for 4890, 5890, 6850 and 6890 GCs (50/pk)
11 mm septa for 4890, 5890, 6850 and 6890 GCs (100/pk)
5 mm septa through-hole for on-column in glass jar (50/pk)
General Purpose Septa
Gray Septa
11 mm for 5880, 5890, 6850 and 6890 GCs (50/pk)
11 mm for 5880, 5890, 6850 and 6890 GCs (100/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)
Red Septa
11 mm solid for 5880, 5890, 6850 and 6890 GCs (50/pk)
11 mm solid for 5880, 5890, 6850 and 6890 GCs (100 pk)
11 mm with partial through-hole for 5880, 5890, (50/pk)
6850 and 6890 GCs
11 mm with partial through-hole for 5880, 5890, (100/pk)
6850 and 6890 GCs
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (50/pk)
9.5 mm (3/8 in.) for 5700 series and 5830/40 GCs (100/pk)
5 mm through-hole for on-column inlets, (25/pk) automatic or manual injections*
5 mm solid for high column backpressure, on-column inlets* (25/pk)
* 5 mm septa are packaged in glass jars
41
EASY ONLINE ORDERING
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
Part No.
5183-4757
5183-4757-100
5183-4758
5183-4759
5183-4759-100
5183-4760
5183-4761
5183-4761-100
5183-4762
5080-8896-50
5080-8894-100
$52
$93
5080-8728-50 $52
5080-8728-100 $93
5181-1263-50
5181-1263-100
$52
$93
5181-3383-50 $52
5181-3383-100 $93
5181-1283-50
5181-1283-100
$52
$93
5181-1260 $29
5181-1261 $29
Price
$72
$134
$72
$62
$107
$62
$84
$150
$84 www.agilent.com/chem • 800 227 9770
Using the wrong ferrule or a worn-out ferrule to seal your column connection can result in inconsistent and unreliable chromatography. An improper ferrule can cause leaks which allow air and other contaminants to enter the instrument through the column seal, causing major interference with column and detector performance. For optimum performance, ferrules should be replaced every time the column is replaced and when performing column maintenance.
Agilent offers a comprehensive selection of ferrules made of different materials and configurations for a leak-free connection between the column and injector.
Three main types of ferrules are used with capillary GC columns: graphite, Vespel and
Vespel-graphite composites. Graphite ferrules can withstand temperatures as high as 450ºC, and Vespel and Vespelgraphite ferrules are rated to 280ºC and
350ºC, respectively.
Ferrules seal the connection of the column or liner to the system. The ideal ferrule provides a leak-free seal, accommodates various column outer diameters, seals with minimum torque, will not stick to the column or fittings, and will tolerate temperature cycling.
Signals that a ferrule is damaged include:
• background noise from oxygen diffusing into the system
• column bleed catalyzed by oxygen
• sample degradation
• loss of sample
• increase in detector signal/noise
• poor retention time reproducibility
Graphite Easy-to-use, stable seal
Higher temperature limit
Vespel or Mechanically robust
Vespel-graphite Long lifetime
Soft, easily deformed or destroyed
• possible system contamination
• not for use with GC/MS transfer-lines
Flows at elevated temperature
• must retighten frequently
• prone to leakage
Polymer bleed problematic with some detectors (NPD and ECD)
General technique for installing ferrules:
• don’t overtighten – finger-tighten column nut, then use wrench to tighten
• maintain cleanliness
• bake out ferrules prior to use (Vespel and
Vespel/Graphite only)
• avoid contamination – such as fingerprint oils
• inspect used ferrules with magnifier for cracks, chips, or other damage before reusing them
• change ferrules when new columns or injector/detector parts are installed www.agilent.com/chem • 800 227 9770 42
Normal Peaks Tailing Solvent Peaks
Normal Peaks Tailing Solvent Peaks
Wrong Peak Ratios
Wrong Peak Ratios
Correct column positioning in both injection port and FID
Column positioned incorrectly in the injection port, or possible ferrule or septum particle in the carrier gas flow path
Column positioned incorrectly in the inlet
(either too far or not far enough; verify
4-6mm installation distance)
Reusing a ferrule – or using off-brand ferrules – may be a costly mistake. That’s because you’ll increase the likelihood of dangerous leaks that can damage the GC column and sensitive detector parts.
For best results, always use new Agilent ferrules, which feature the highest quality design, and are supported by decades of technical expertise.
Two different types of Agilent column nuts can be used with these ferrules:
• The universal column nut (p/n 5181-
8830) has a hexagonal head requiring the use of a wrench to tighten it completely.
• The finger-tight column nut (p/n 5020-
8293 for 530um columns and p/n 5020-
8292 for columns 320µm or less) does not require a wrench to tighten.
It can only be used with the 100% graphite ferrules.
43
TIPS AND TOOLS
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.
www.agilent.com/chem • 800 227 9770
The combination of graphite and Vespel results in a ferrule having low oxygen diffusion rates which does not shrink to the same extent as pure Vespel. These ferrules are recommended for use with
GC/MS or other oxygen sensitive detectors, like the ECD, but are also compatible with other detectors like FID and NPDs.
In addition, the Vespel/graphite ferrules provide added confidence of leak-free connections when installed correctly.
Proper installation requires a finger-tight turn on the nut, then an additional 1/
4 –
1/
2 turn with a wrench.
These ferrules are very hard and cannot be deformed sufficiently to seal multiple column diameters. The ferrule hole must match the column OD exactly to ensure a leak-free seal. For capillary column applications, there is a specific ferrule for each column diameter. Choosing a ferrule with a larger hole than is specified for a given column dimension can result in a large leak. If left unchecked, an improper seal at the injector will result in high column bleed and a shortened column lifetime. An improper seal at the detector can result in increased detector signal/noise. In the case of the MSD it can also contribute to oxidation of the ion source which can increase the frequency of detector maintenance.
Two different lengths of Vespel/graphite ferrules are available for capillary column use. The standard sized ferrule is compatible with the universal column nut.
The second ferrule size is slightly longer and is specifically designed to fit with the
MS interface nut used for the GC/MS transfer line connection. The larger ferrule can also be used to make column connections to inlets and other detectors but requires a specially designed column nut (p/n 05988-20066) to accommodate the longer ferrule.
When using Vespel/graphite ferrules,
Agilent recommends tightening the column nut to a 1/
4 turn after the first temperature program runs. Even preconditioned ferrules can exhibit some shrinkage after a temperature programmed run.
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)
Longer ferrule with MS interface nut
MS Interface Column Nut + Vespel/Graphite Ferrules
05988-20066 5062-3508 (0.1, 0.2, and 0.25 mm ID columns)
5062-3506 (0.32 mm)
5062-3538 (0.45 and 0.53 mm) www.agilent.com/chem • 800 227 9770 44
Vespel is a high-temperature polyimide based material which is very hard. This material has the lowest permeability to oxygen, making it an excellent sealing material when making metal or glass connections. These ferrules do not deform easily. So, it is important to match the ferrule hole size to the proper column diameter.
The main disadvantage of 100% Vespel ferrules is the shrinkage of the material when exposed to temperature cycling conditions. 100% Vespel ferrules should only be used for isothermal applications.
VIDEO
To view a video on ferrules, visit www.agilent.com/chem/techsupport.
45
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Graphite 450ºC General purpose Not for MS or
(100%) for capillary columns.
Suitable for FID and NPD. oxygen sensitive detectors.
Recommended for high temperature and cool on-column applications.
Can be removed easily.
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Vespel/Graphite 350ºC General purpose for Not reusable.
(85%/15%) capillary columns.
Recommended for leak-free connection.
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Vespel
(100%)
280ºC
MS or oxygen sensitive detectors. Most reliable
Isothermal operation.
Leaks after temperature cycle.
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
SilTite N/A Use only with SilTite Nut Kits Not Reusable
(100% metal) www.agilent.com/chem • 800 227 9770
Ferrule Id
(mm)
General Purpose Graphite Ferrules (Short Ferrules)
0.5
1.0
0.4
0.8
Column Id
(mm)
Quantity
0.1, 0.2, 0.25, 0.32
10/pk
0.53
0.05-0.25
0.45, 0.53
10/pk
10/pk
10/pk
85% Vespel, 15% Graphite Ferrules (Short Ferrules)
0.80.3
0.80.4
0.80.5
0.80.8
0.1, 0.2
0.1, 0.2, 0.25
0.32
0.45, 0.53
Preconditioned 85% Vespel, 15% Graphite Ferrules (Long Ferrules)
0.3
0.4
0.5
0.8
0.1
0.1, 0.2, 0.25
0.32
0.53
These ferrules are recommended for use with GC/MS.
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
100% Vespel High-Performance Ferrules (Short Ferrules)
0.4
0.5
0.8
These ferrules are recommended for use in isothermal analysis only.
Specialty Ferrules, 85% Vespel, 15% Graphite
Two Hole 0.4 ID holes
0.5 ID holes
No Hole
SilTite Metal Ferrules
For use with 0.20-0.25 mm ID capillary columns. Includes 2 column nuts
For use with 0.32 mm ID capillary columns. Includes 2 column nuts
For use with 1/16 in. od
SS tubing. Includes 2 column nuts
For use with 0.53 mm ID capillary columns.
Includes 2 nuts
Column Nuts
Short Nuts
Universal column nut, 1/16 in. hex
Finger-tight column nut for 0.53 mm columns*
Finger-tight column nut for 0.32 mm columns* and smaller
Blanking plug, finger-tight style
6850 Column Nut
Long Nuts
MS interface column nut
Column nut for GC/MS ferrules
Column nut wrench, 1 /4 in. and 5 /16 in.
* For use with graphite ferrules only.
Always match short nuts with short ferrules and long nuts with long ferrules.
0.1, 0.2, 0.25
0.32
0.45, 0.53
0.1, 0.2, 0.25
0.32
0.4
0.5
0.8
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
10/pk
2/pk
1 ea
1 ea
1 ea
2/pk
1 ea
1 ea
1 ea www.agilent.com/chem • 800 227 9770a
Part No.
5080-8853
5080-8773
500-2114
500-2118
5062-3516
5181-3323
5062-3514
5062-3512
5062-3507
5062-3508
5062-3506
5062-3538
5181-3322
5062-3513
5062-3511
5062-3580
5062-3581
5181-3308
5184-3569
5184-3570
5184-3571
5188-2789
5181-8830
5020-8293
5020-8292
5020-8294
5183-4732
05988-20066
05921-21170
8710-0510
Price
$ 47
$ 38
$ 26
$ 26
$ 51
$ 55
$ 51
$ 53
$ 62
$ 62
$ 56
$ 48
$ 55
$ 51
$ 51
$ 79
$ 79
$ 47
$ 87
$ 87
$ 85
$135
$ 26
$ 18
$ 18
$ 12
$ 47
$ 13
$ 16
$ 24
46
47
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
Liners are the centerpiece of the inlet system in which the sample is evaporated and brought into the gas phase.
These problems will occur if the liner is not changed on a regular basis or if the correct liner is not used:
• peak shape degradation
• solute discrimination
• poor reproducibility
• sample decomposition
• ghost peaks
• reduced column life
Change liners on a regular basis determined by:
• previous use pattern
• sample cleanliness
• chromatographic abnormalities such as:
– peak shape changes
– peak discrimination
– poor reproducibility
– sample pyrolysis
– active analyte response loss or decomposition
VIDEO
To view a video on Liners, visit www.agilent.com/chem/techsupport.
www.agilent.com/chem • 800 227 9770
The purpose of the injection port is to allow the introduction of a sample into the gas chromatograph in an accurate, reproducible manner. The vaporized sample should be a true representation of the liquid sample and, unless specifically desired, should be injected without chemical change. The elevated temperatures used in the inlet vaporize the liquid sample to a gas for transfer to the head of the column. This phase transition is accompanied by a very significant volume change. The volume of the resulting vapor must be small enough to fit within the volume of the liner. If the volume is too great for the liner, it could result in backflash, or sample loss caused by expansion into the septum purge or split vent lines. Both can compromise reproducibility and sensitivity. Backflash also frequently results in sample carryover.
Larger volume liners (> 800 µL) are characterized by larger inside diameters
(ID) and are typically used with injection sizes of 1 µL or more. The small volume liners have a smaller ID and are usually used with small injection sizes (< 1 µL), fast 100 µm ID columns, gas samples, or when using external sampling devices like headspace and purge and trap.
Active sites on inlet liners can adsorb sample components and cause peak tailing, and potential loss of sensitivity and reproducibility. Deactivation agents are used to cover or react with active sites on the glass surface of the liner. Agilent liners are deactivated using deactivation procedures that produce reproducible and inert liners, with long lifetimes. For splitless applications or when even slightly polar compounds must be analyzed, a deactivated liner should be used.
With use, even deactivated liners can begin to exhibit activity. When this occurs, the liner should be replaced. Liners can be cleaned to remove particulate material or solvent rinsed to remove less volatile components. However, choosing the proper liner cleaning procedure can be difficult. Some solvents may remove the deactivation layer, and tools might scratch the glass surface of the liner, resulting in the generation of unwanted active sites.
A new liner almost always outperforms a cleaned and re-deactivated one – especially for trace analysis.
www.agilent.com/chem • 800 227 9770
TIPS AND TOOLS
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.”
48
49
• The outside diameter (OD) of the liner determines if the liner is more effectively used in split or splitless mode
• Larger OD liners are designed for splitless operation, fit tightly and limit sample contact with metal parts of the inlet
• Larger OD liners improve analyte recovery by retaining more sample inside the liner
• Agilent splitless liners are all designed with exacting dimensional tolerances to fit tightly in the inlet and minimize sample contact with metal surfaces
• Smaller OD liners are designed for split injection because they produce less resistance to carrier and split flow through the inlet
• Large volume liners are used for split injections with enforced dimensional stability for a wide range of split ratios
Tapering or narrowing the liner internal diameter (ID) is done for a number of purposes:
• Bottom taper focuses sample onto the head of the column
• Bottom taper minimizes contact with metal parts of the inlet
• Center taper positions glass wool correctly
• Top taper minimizes sample backflash
To operate properly, the column must be installed correctly in the injection port with the tip of the column ideally located about halfway into the taper, or about 4-6 mm from the column tip to the top of the ferrule
(See Figure 1). Some applications will work better with different column installation depths. Therefore, you should check the instrument manual for proper installation distances and determine which distance is appropriate for your application.
Reproducible positioning is important for repeatable quantitative results.
Many liner designs use deactivated glass wool packing. The glass wool is positioned or held in place near the center of the liner to:
• Provide additional surface area for complete volatilization of the sample to minimize thermal discrimination
• Trap non-volatile components and septum particles before they reach the column
• Wipe any sample from the syringe needle, thereby increasing reproducibility and preventing sample residue build-up at the septum
Glass wool liners that have glass wool near the center of the liner, such as Agilent Part
Nos. 5183-4647 and 5183-4711, are recommended for automatic injections.
If glass wool is positioned at the bottom of the liner, its main purpose is simply to trap non-volatile components. Glass wool is generally not recommended for the following analytes:
• phenols
• organic acids
• pesticides
• amines
• drugs of abuse
• reactive polar compounds
• thermally labile compounds
Another design feature used to help volatilize the sample and provide good mixing is the incorporation of a glass cup inside the liner. Glass cup liners are also available with additional glass wool and inert packing to increase reproducibility and limit sample discrimination. Not recommended for use with Electronic
Pressure Control Inlets on 6890 or 6850 GCs.
Figure 1.
www.agilent.com/chem • 800 227 9770
Tailing Peaks
Normal Problem
Baseline Rise Before or After Peak
Sample components adsorbed by column, inlet liner or contaminated gold inlet seal.
Needle hitting and breaking packing in inlet liner.
Column end poorly cut
(sample absorption).
Broken or chipped inlet liner.
Inlet flow too low.
Sample decomposing.
Use new, deactivated liner or clean old liner and replace glass wool.
Partially remove packing from liner or use without packing.
Remove column. Make a clean, square cut using a reliable capillary fused silica cutting tool (such as a ceramic wafer or the Agilent Column Cutter), then reinstall column.
Make sure total flow in inlet is above
40 mL/min.
Remove inlet liner and check cleanliness.
Use new, deactivated liner or replace glass wool and packing. Column/sample residues could also be the problem.
Normal Problem Problem
Baseline Change After Large Peak Column and inlet liner misaligned.
See also”Septum Troubleshooting,” page 37
Check installation of column end and inlet liner; adjust if necessary.
Normal Problem Problem
Unresolved Peaks Column or inlet liner contaminated or column deteriorating.
Use a guard column to prolong column life.
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.
Normal Problem Problem www.agilent.com/chem • 800 227 9770 50
51
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:
Agilent low-pressure-drop split liner with glass wool, bottom taper, glass bead for easy positioning, and deactivated, Agilent
Part No. 5183-4647 (with extraordinarily tight dimensional control for optimum split performance).
Single tapered liner without glass wool, deactivated, Agilent Part No. 5181-3316EN.
Note: For pesticide analysis – especially
DDT and Endrin, where breakdown is a problem – we recommend Agilent Part
Nos. 5181-3316EN and 5181-3315EN.
Similar design to Agilent Part No. 5183-
4647, but with an outer diameter that compromises for both split and splitless injections, Agilent Part No. 5183-4711.
Straight liner without glass wool, deactivated, Agilent Part No. 5181-8818
(use only for gas samples, headspace, or purge and trap applications).
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 optimized by Agilent R&D engineers to allow them to work with EPC.
Improve reproducibility, improve results.
The Focus Liner traps a precisely controlled amount of glass wool in the ideal position in the injection port liner. At the point of injection, the glass wool provides extra surface area for vaporization, traps nonvolatile sample residue, and wipes any residual sample from the sample needle – reproducibility is the result.
In addition to these liners we offer a broad selection of liners for your specific application needs.
Liners are sealed in the inlet with O-rings or graphite seals. O-ring seals are easier to remove and to replace than graphite that deforms and flakes apart. The graphite seals should be used when inlet temperatures exceed 350ºC.
www.agilent.com/chem • 800 227 9770
• Cuts liner replacement time to as little as 30 seconds
• No more frustrating searches for special wrenches or tools
• Improved inlet ergonomics – no more handling of heated parts, no more burns or scrape
• Decreased downtime = increased productivity
• Minimizes exposure to ambient air extending column life
• Installs easily in 15 minutes (customer installable)
1. Do you change liners more than 2-3 times per week?
2. How long does it take you to change a liner (total downtime)?
3. Do you want to increase your productivity and column life?
4. Have you ever burned your fingers or scraped your knuckles trying to open a hot inlet?
One of the most frequent maintenance tasks customers face when running a GC or GC/MS system is changing the inlet liners. A hot inlet may have to be opened on each system every
24 to 48 hours to change a dirty inlet liner. The special wrench used for this operation is often misplaced, bent at an odd angle, too thin, or simply awkward to use. In addition, the inlet nut is usually too hot to handle so it must be turned several times with the wrench before it will release the top assembly of the injection port.
Once the dirty liner is replaced, the inlet nut must be replaced on the injection port and occasionally the wrench slips off the nut leading to scrapes, burns, and cuts. It can take at least 5 minutes of wrestling with this hot injection port nut and wrench combination just to take out the old liner and put in a new one. By the time the operator finishes the procedure and re-equilibrates, it can result in 15 minutes of downtime!
Of course, doing this with a GC/MS causes even more problems as ambient air is drawn into the capillary column, through the hot MS interface, and into the heated source resulting in multiple problems for the operator including shortened column life and air background in the MS.
Agilent’s new Flip Top Inlet Sealing System is a device designed to allow the user to safely and reliably change an inlet liner in as little as 30 seconds without tools in a consistent leakfree manner. No longer will you have to contend with frustrating searches for wrenches or burning your fingers on hot inlets.
Available exclusively from Agilent, the Flip Top has a levered arm that attaches to any
6890/6850/5890 insert weldment and locks to the injection port using an adapter ring screwed onto the inlet. Once installed, the user simply lifts the arm of the Flip Top which releases the insert weldment from the injection port, and allows instant access to the liner.
The process is simply reversed to re-seal the weldment to the port.
Flip Top Inlet Sealing System
Liner O-rings (10/pk) www.agilent.com/chem • 800 227 9770
5188-2717
5188-2741
$514
$19
VIDEO
To view videos on the Flip Top Inlet Sealing System, visit www.agilent.com/chem/fliptop2
52
Application Liner Single
Volume(µl) Liner
Agilent Choice Liners
Liner, split, low press. drop, glass wool, taper, deactivated
Liner, splitless, single-taper, no glass wool, deactivated
NEW! Liner, Splitless,
Single-taper, no glass wool, polymerically deactivated
For split injection
For splitless injection
For trace pesticide analysis
Liner, direct, 2 mm ID, deactivated
Liner, general purpose split/splitless, glass wool, taper, deactivated
For direct injection
(use for gas samples, headspace, or purge and trap applications)
For split/splitless injection
Splitless Inlet Liners
Liner, splitless, single-taper, glass wool, deactivated
Liner, splitless, double-taper, no glass wool, deactivated
NEW! Liner, Splitless, double-taper, no glass wool, polymerically deactivated
For trace pesticide analysis
Direct Inlet Liners
Liner, direct, 2 mm ID, non-deactivated, quartz
870
900
900
250
870
900
800
800
250
5183-4647
$35
5183-4701
$157
5181-3316
$29
5181-3316EN
$32
5183-4695
$124
5181-8818
$24
5183-4711
$27
5183-4703
$95
5183-4712
$112
5062-3587
$30
5181-3315
$36
5181-3315EN
$43
5183-4693
$129
5183-4705
$163
Liner, direct, 1.5 mm ID, non-deactivated
[use for gas samples, headspace, or purge and trap applications]
Liner, straight, splitless 4.0 mm ID
140
18740-80220 5183-4707
$28 $124
18740-80200 5183-4709
$17 $73
Split Inlet Liner
Liner, split, glass wool, non-deactivated
Split Inlet Liners For Manual Injection
Liner, split, with cup, no glass wool
Liner, split, with cup, glass wool, and packing
[not recommended for use with electronic pressure control (EPC)], for manual injection
Direct Connect Liners
Single taper direct connect liner, 4 mm ID, deactivated
Dual taper direct connect liner, 4 mm ID, deactivated
Focus Liners
Focus liner
Focus liner
ID
4.0 mm
4.0 mm
Wool
Yes
Yes
Dimensions
6.3 mm X 78.5 mm
6.3 mm X 78.5 mm
Liner O-Rings
Fluorocarbon O-ring (12/pk)
Graphite O-ring for splitless liner (10/pk)
Graphite O-ring for split liner (10/pk)
Inlet Liner O-rings for use with the Flip Top Inlet Sealing System (10/pk)
990
800
800
990
$19
210-3003
$84
19251-60540 5183-4691
$19 $78
18740-80190 5183-4699
$40 $179
18740-60840 5183-4697
$43 $191
Part No.
G1544-80730
G1544-80700
Part No.
210-4004-5
210-4022-5
Part No.
5180-4182
5180-4173
5180-4168
Price
$62
$62
5183-4702
$700
5183-4696
$533
5183-4704
$414
5183-4713
$476
5183-4694
$560
5183-4706
$751
5183-4708
$533
5183-4710
$308
210-3003-5
5183-4692
$336
5183-4700
$784
5183-4698
$840
Price
$98
$108
Price
$13
$52
$52
5188-2741 $19
53 www.agilent.com/chem • 800 227 9770
When it comes to inlet replacement parts for your Agilent GCs, don’t settle for imitations; choose only genuine Agilent parts.
Our inlets are backed by the same 40 years of design experience that you’ve come to expect from our instruments. So you get optimal performance, plus the reproducible results that your lab demands.
What’s more, Agilent supplies every replacement part that your system might need – not just a few select pieces. So you can get all your consumables, all in one place.
Septum Nut
Part No. 18740-60835
Septum See page 36
Split/Splitless Inlet Weldment
Part No. G1544-60575, for 6890 GC with EPC
Viton O-Ring
Part No. 5180-4182, 12/pk
Liners See page 47
Heater-Sensor Assembly
Part No. G1544-61140
For a complete parts breakdown, see the
5890, 6890, and 6850 series GC Instrument
User and/or Service Manuals, or visit
www.agilent.com/chem.
Retaining Nut
Part No. G1544-20590
Washer
Part No. 5061-5869, 12/pk
Reducing Nut
Part No. 18740-20800,
1 each www.agilent.com/chem • 800 227 9770
Gold-Plated Seal (Splitless)
See page 55
Ferrules (85% Vespel, 15% Graphite)
– Part No. 5062-3516, 0.37 mm I.D., for 100-200 µm Columns, 10/pk
– Part No. 5181-3323, 0.40 mm I.D., for 250 µm Columns, 10/pk
– Part No. 5062-3514, 0.50 mm I.D., for 320 µm Columns, 10/pk
– Part No. 5062-3512, 0.74 mm I.D., for 530 µm Columns, 10/pk
Column Nut for 6890 GC
Part No. 5181-8830, 2/pk
54
55
Part No.
6890/6850 Split/Splitless Insert Assemblies
Standard manual pneumatics
Original standard EPC using 1/4" split vent filter.
Similar to G1544-60575 except allowed insertion for 1/4" chemical filters to clean carrier gas for ECD operation.
S/SL insert weldment. Used with large charcoal canister type filter for 6890/6850.
Similar to G1544-60575 except carrier lines separated for interface to valved systems of a G1540A instrument.
S/SL insert assembly for G1540A with valved system option. This insert assembly uses the large charcoal canister split vent filter for 6890/6850.
19251-60575
G1544-60575
G1544-80580
G1544-60585
G1580-60575
G1580-60585
5890 Split/Splitless Multimode Inlet Supplies
Septum retainer nut
Retainer nut for headspace sampling
Retaining nut
18740-60835
18740-60830
19251-20620
Reducing nut 18740-20800
For a complete parts breakdown, see the 5890, 6890 and 6850 series GC Instrument User and/or Service Manuals.
Liner Seals and Washers
Stainless steel
Gold-plated seal
Gold-plated seal with cross
Washers (12 pk)
18740-20880
18740-20885
5182-9652
5061-5869
$39
$106
$31
$35
$26
$33
$40
$8
Price
$230
$216
$73
$330
$261
$236
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
Gold-plated seal p/n 18740-20885
Bottom
Gold-plated seal with cross p/n 5182-9652
Use when inlet flow exceeds 400 ml/min.
www.agilent.com/chem • 800 227 9770
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 • 800 227 9770
“Agilent lets you choose from over 1,000 different columns. It’s no wonder that, for nearly 40 years, customers have built products – and entire businesses – around the results they get from our DB- and HPcapillary GC columns.”
Phil Stremple,
GC Columns Program Manager
CATALOG
For a complete selection of GC columns and parts, see Agilent’s 2005-
2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
56
While GC column maintenance is simple, the frequency and type of column maintenance that is required varies due to many system and sample factors. Instead of simply following a predefined timetable of maintenance items, the main focus should be how to obtain the highest performance and lifetime from a capillary column. This depends on choosing the right column, correct installation/system setup, and avoiding the primary factors that cause column performance degradation (breakage, thermal damage, oxygen damage, chemical damage and contamination).
57
All phases can be used with conventional
GC systems, and most stationary phases can be used with a GC/MS system.
However, it is a good idea to choose a phase for your application that has the lowest amount of column bleed as possible. Column bleed is the natural degradation of the stationary phase that occurs at higher temperatures, which appears as an elevated baseline as the temperature rises to the column’s upper thermal limit. Column bleed will deposit in the MSD ion source, which can decrease
MSD performance. By minimizing the amount of column bleed, you will help reduce the frequency of required ion source maintenance.
Primary
“Quantion” is hidden
Primary
“Quantion” is enhanced
There are a few simple rules for choosing columns with lower bleed levels:
• Choose a low-bleed phase for your application – Agilent has developed several low-bleed versions of the most popular phases. These are chemically designed to possess minimal levels of column bleed possible and often have the benefit of an increased uppertemperature limit.
• If a low-bleed column is not available, choose a low-polarity column with a moderate film thickness. The amount of bleed will rise with increases in polarity, film thickness, and length.
• Use more polar phases when difficult 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)
All dimensions can be used with conventional GC systems. Many types of GC column phases can be used with the MSD, but there are some dimensional considerations. The maximum allowable flow rate and optimal sensitivity flow rates will vary depending upon the type of pump.
In general, the column flow should be
1mL/min (2mL/min for Performance Turbo
Pumps). Therefore, column length and internal diameter combinations are restricted to provide the appropriate flow to the GC/MS.
• Narrow-bore columns (0.25mm i.d. and smaller) can be installed directly into the
GC interface.
www.agilent.com/chem • 800 227 9770
• Wide-bore columns (0.32mm i.d.) that are
30m or longer can be installed directly into the 5973 GC interface (other MSDs may require 50m or longer). If using a wide-bore column with a shorter length, an effluent splitter or jet separator should be utilized.
• Columns with internal diameters greater than 0.32mm should not be directly interfaced into the GC interface. For these columns, an effluent splitter or jet separator should be installed.
DB-1ms, 0.25mm i.d., 30m, 0.25µm
HP-5ms, 0.25mm i.d., 30m, 0.25µm
DB-XLB, 0.25mm i.d., 30m, 0.25µm
DB-35ms, 0.25mm i.d., 30m, 0.25µm
HP-INNOWax, 0.25mm i.d.,
30m, 0.25µm
122-0132
19091S-433
122-1232
122-3832
$483
$483
$483
$483
19091N-133 $413
The first step in obtaining optimal column performance and lifetime is proper installation:
• Choose the appropriate size and material ferrule for the column, injector and detector type.
• Avoid re-using ferrules.
• Use an appropriate column cutting tool such as a ceramic wafer or diamond tipped scribe.
• Make sure column ends are cleanly cut and free of particulate matter before installing into the injector and detector.
• Install the column the appropriate distance into the injector and detector as specified by the GC manufacturer.
• The column should be placed on a column hanger and no portion of the capillary tubing should touch the oven walls.
• Verify that all fittings are leak-free and the carrier gas is oxygen-free before heating the oven.
• Briefly conditioning a column before installing it into the GC/MS interface is recommended. When the column and inlet are first heated, volatile materials within the flow-path and a small portion of the column stationary phase move into the gas phase. These materials are then carried by the carrier gas into the MSD and can deposit in the MSD ion source.
This can decrease MSD performance.
Conditioning the column briefly prior to installation into the MSD will minimize the contamination brought into the ion source.
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.
www.agilent.com/chem • 800 227 9770 58
59
Column Installation & Setup continued
Bad
Good
Example of column cuts
• Check the installation and set the linear velocity by injecting a non-retained compound.
• Condition the column as specified in the literature provided with each column.
Description
Ceramic wafer (4/pk)
20x Magnifier
General Purpose Graphite ferrule
(0.5mm ID, for column IDs
≤
0.32mm)
10/pk
General Purpose Graphite ferrule
(1.0mm ID, for 0.45-0.53mm
ID columns) 10/pk
Gas leak detector 115V
Gas leak detector 220V
Part No.
5181-8836
430-1020
5080-8853
5080-8773
5182-9646
5182-9648
Price
$ 15
$ 42
$ 47
$ 38
$1859
$1859
Fused silica columns can break wherever there are small scratches or abrasions in the protective polyimide coating.
Continuous heating and cooling of the oven, vibrations caused by the oven fan as well as being wound on a circular cage all place stress on the tubing.
While under these stresses, flaws will propagate until breakage occurs.
NOTE: Larger diameter columns
(0.45- 0.53mm id) are more prone to breakage.
• Avoid scratches and abrasions by not exposing the column to sharp edges such as column hangers and tags, metal edges in the GC oven, column cutters and other miscellaneous items on the lab bench.
• Avoid winding or bending the column too tightly.
• If a broken column has been heated, damage to the stationary phase is very likely. Discard the back of the column
(the column half without carrier gas).
Trim 6 inches off the end of the column and reinstall.
• If the broken column has not been heated, connect the two pieces with a low volume union. No more than
2-3 unions should be installed for one column.
Description Part No.
Price
Fused Silica Union,
Universal 2-way
(5/pk) 705-0905 $ 50
Quartz deactivated column connector
(5/pk) 5181-3396 $ 94
Polyimide Sealing resin (5 grams) 500-1200 $ 24 www.agilent.com/chem • 800 227 9770
Exceeding a column’s upper temperature limit results in accelerated degradation of the stationary phase and tubing surface.
This results in the premature onset of excessive column bleed, peak tailing for active compounds and/or loss of efficiency
(resolution).
• Do not exceed the columns specified upper temperature limits:
– Isothermal limit: temperature that the column can be held at for an indefinite time
– Programmed limit: maximum column temperature; column should only be held there for about 5-10 minutes
• Set the GC maximum oven temperature function at or a few degrees above the temperature limit of the column. With two columns in the oven be sure to set the maximum temperature to the temperature limit of the column with the lowest value.
• Disconnect column from detector
• Heat the column 8-16 hours at the isothermal limit
• Remove 10-15 cm from the column end
• Reinstall into the detector and condition as usual
NOTE: Thermal damage cannot be reversed.
The column usually does not return to its original performance; however, it is often still functional. The life of the column will be reduced after thermal damage.
Oxygen is an enemy to all capillary GC columns. Constant exposure to oxygen does not damage the column at or near ambient temperatures; however, severe damage occurs as the column temperature increases. A leak in the carrier gas flow path (e.g., gas lines, fittings, injector, septa) is the most common source of oxygen exposure. As the column is heated, very rapid degradation of the stationary phase occurs. This results in the premature onset of excessive column bleed, peak tailing for active compounds and/or loss of efficiency (resolution).
NOTE: Momentary exposure to oxygen such as an injection of air or removing the septum nut for a short period of time is not a problem.
Maintain an oxygen and leak-free system by:
• performing periodic leak checks
• changing septa regularly
• using high quality carrier gases
• installing and maintaining oxygen traps
• changing gas cylinders before they are completely empty
Perform column “bakeout” as described under thermal damage recovery.
NOTE: Oxygen damage occurs very rapidly.
In less severe cases, the column may still be functional but at a reduced performance level. In more severe cases, the column is irreversibly damaged.
Description Part No.
FlowTracker 2000 Flowmeter and Leak Detector 5183-4780
Big Oxygen Trap (750 cc, 1/8" fitting) BOT-2
BMT-2 Big Moisture Trap (750 cc, 1/8" fitting)
Big Universal Trap (Combination Trap)
(750cc, 1/8" fitting, He)
Advanced Green Septa (11mm, 50/pk)
RMSH-2
5183-4759
Price
$1143
$ 235
$ 235
$ 261
$ 62
TIPS AND TOOLS
Install a moisture trap upstream of the oxygen trap to increase the oxygen trap lifetime.
www.agilent.com/chem • 800 227 9770 60
61
Inorganic or mineral acids and bases are the primary sources of chemical damage to stationary phases. Most of these acids and bases have low volatility and accumulate at the front of the column.
If allowed to remain, the acids or bases damage the stationary phase. The only organic compounds that have been reported to chemically damage stationary phases are perfluoroacids and these need to be present at high levels (e.g., 1% or higher). This results in the premature onset of excessive column bleed, peak tailing for active compounds and/or loss of efficiency (resolution).
NOTE: Hydrochloric acid and ammonium hydroxide are the least harmful of the group as both tend to follow any water that is present in the sample. Thus, if HCl or NH
4
OH are present in a sample, minimizing water retention will render these compounds relatively harmless to the column.
• Perform sample preparation to remove inorganic acids and bases from the sample
• Install guard column and trim frequently
• If acids or bases must be used choose an organic alternative or HCl or NH
4
OH
• Remove 0.5 to 1 meter from the front of the column
• Severe cases may require the removal of 5 or more meters
Column contamination is the most common problem encountered in capillary
GC. Unfortunately, it mimics most other chromatographic problems and is often misdiagnosed. A contaminated column is usually not damaged, but it may be rendered unusable. There are two basic types of contaminants: nonvolatile and semivolatile.
A guard column is a piece of fused silica tubing attached with a union to the front of the analytical column with the following characteristics:
• Material should be deactivated fused silica tubing to minimize solute interactions.
• Length should be from 1-10 meters. Typical lengths of 5-10 meters allow substantial trimming before the entire guard column has to replaced.
• Internal diameter are generally the same as the column. Guard columns with larger ids can be used for additional residue capacity.
• A low volume union should be used to attach the tubing to the column.
Glass pressfit unions are inexpensive and easy to install. DuraGuard columns offer the guard column built into the analytical column as a single piece of fused silica, eliminating the need for unions.
Guard columns are used to minimize the effect of non-volatile residues on the analysis. The non-volatile residues deposit in the guard column and not in the analytical column. This greatly reduces the interaction between the residues and the sample. Periodic cutting or trimming of the guard column is usually required upon a build-up of residues. The onset of peak shape problems is the usual indicator that the guard column needs trimming or changing.
INJECTOR
DETECTOR
Guard Column
Column
Union
Guard column installation instructions are available at www.agilent.com/chem.
Click on “Technical Support,” then “GC Reference Library.” The procedure can be found under “General Information.” www.agilent.com/chem • 800 227 9770
Nonvolatile contaminants or residues do not elute and accumulate in the column
(most often confined to the first few meters). The column becomes coated with these residues which interfere with the proper partitioning of solutes in and out of the stationary phase. Also, the residues may interact with active solutes resulting in peak adsorption problems (evident as peak tailing or loss of peak size). Active solutes are those containing a hydroxyl
(-OH) or amine (-NH) group, and some thiols (-SH) and aldehydes.
• Perform sample cleanup to remove nonvolatile materials from the sample
• Use injection port liners packed with glass wool (may not be feasible when analyzing active compounds)
• Install a guard column and trim regularly
• Do not bakeout the column
• Front End Maintenance:
– Clean or change the injection port liner
– Clean out the injector
– Cut off typically 0.5 to 1 meter of the front of the column
• Turn the column around (install detector end into injector). Not recommended for sensitive ECD, NPD, and MS detectors.
• Solvent rinse the column
• Cut the column in half and use the back half (detector side)
Semivolatile contaminants or residues accumulate in the column, but eventually elute. Hours to days may elapse before they completely leave the column. Like nonvolatile residues, they may cause peak shape and size problems and, in addition, are usually responsible for many baseline problems (instability, wander, drift, ghost peaks, etc.).
Description
Split/Splitless Inlet liner: glass wool, taper, deactivated (5/pk)
Splitless Inlet liner: single-taper, no glass wool, deactivated (5/pk)
Quartz deactivated column connector (5/pk)
Polyimide sealing resin (5 grams)
Deactivated Fused silica,
10m, 0.53mm i.d.
Deactivated Fused silica,
10m, 0.25mm i.d.
Capillary column rinse kit
• Perform sample cleanup to remove semi-volatile materials from the sample
• Increase the final temperature of the
GC run (not to exceed the temperature limit of the column)
• Change septa regularly
• Bakeout the column: limit 1-2 hours
(excess baking may polymerize some contamination and reduce column lifetime)
• Solvent rinse the column
Perform this simple test.
1. Place 20-30 µL of the sample onto a microscope slide.
2. Put the slide over the heated GC inlet for 20 minutes.
3. Hold the slide up to the light.
If you can see anything where the drop was, your sample has residues.
Part No.
5183-4712
5183-4695
5181-3396
500-1200
160-2535-10
160-2255-10
430-3000
Price
$112
$124
$ 94
$ 24
$110
$ 73
$ 78
Capillary columns should be stored in their original box when removed from the GC.
Place GC septa over the ends to prevent debris from entering the tubing. Upon reinstallation of the column, the column ends need to be trimmed by 2-4 cm to ensure that a small piece of septa is not lodged in the column.
If a column is left in a heated GC, there should always be carrier gas flow through the column. The carrier gas flow can be turned off only if the oven, injector, detector and transfer lines are turned off
(i.e., not heated). Without carrier gas flow, damage to the heated portion of the column occurs. www.agilent.com/chem • 800 227 9770 62
63
• 100% Dimethylpolysiloxane
• Identical selectivity to DB-1
• Nonpolar
• Very low bleed characteristics
• Improved acid performance compared to standard 100% Dimethylpolysiloxane columns
• Improved signal-to-noise ratio for better sensitivity and mass spectral integrity
• Excellent general purpose column
• Bonded and cross-linked
• Solvent rinsable
I.D.
Length Film Part No.
0.25
0.25
0.25
0.32
0.32
0.32
0.10
0.10
0.10
0.10
0.20
0.20
HP-1ms, Rtx-1ms, CP-Sil 5CB
30
30
60
30
30
60
10
10
20
20
12
25
0.10
0.25
0.25
0.10
0.25
0.25
0.10
0.40
0.10
0.40
0.33
0.33
Price
127-0112
127-0113
127-0122
127-0123
128-0112
128-0122
122-0131
122-0132
122-0162
123-0131
123-0132
123-0162
General purpose: Amines, hydrocarbons, pesticides, PCBs, phenols, sulfur compounds, flavors and fragrances.
$483
$483
$823
$521
$521
$896
$343
$343
$495
$495
$261
$400 www.agilent.com/chem • 800 227 9770
• Phenyl Arylene polymer equivalent to a
(5%-Phenyl)-methylpolysiloxane
• Nonpolar
• Very low bleed characteristics
• Excellent inertness for active compounds
• Improved signal-to-noise ratio for better sensitivity and mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Certified for MS
• Exact replacement of HP-5TA
• Close equivalent to USP Phase G27
I.D.
Length Film
0.18
0.18
0.20
0.20
0.32
0.32
0.32
0.32
0.32
0.32
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
Rtx-5ms, HP-5ms, PTE-5, CP-Sil 8CBms,
BPX-5
50
60
60
30
30
30
30
50
60
60
25
25
30
30
20
40
25
50
0.18
0.18
0.33
0.33
0.10
0.25
0.50
0.25
0.10
0.25
0.25
0.40
0.10
0.25
0.50
0.25
0.10
0.25
Part No.
Price
121-5522
121-5542
128-5522
128-5552
122-5522
122-552A
122-5531
122-5532
122-5536
122-5552
122-5561
122-5562
123-5531
123-5532
123-5536
123-5552
123-5561
123-5562
Semivolatiles, alkaloids, drugs, FAMEs, halogenated compounds, pesticides, herbicides
$412
$740
$400
$674
$521
$521
$521
$804
$896
$896
$421
$421
$483
$483
$483
$753
$823
$823
• (5%-Phenyl)-methylpolysiloxane
• Nonpolar
• Very low bleed characteristics
• Excellent inertness for active compounds
• Improved signal-to-noise ratio for better sensitivity and mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Certified for MS
• Equivalent to USP Phase G27
Rtx-5ms, DB-5ms, PTE-5, CP-Sil 8CBms,
BPX-5, Rtx-5 Amine
Semivolatiles, alkaloids, drugs, FAMEs, halogenated compounds, pesticides, herbicides
I.D.
Length Film Part No.
0.20
0.20
0.20
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.32
0.32
0.32
0.32
0.32
0.32
0.32
* This column is shipped with the 5973 MSD.
30
30
30
60
60
15
15
15
12
25
50
30
60
60
15
25
30
30
0.33
0.33
0.33
0.10
0.25
1.00
0.10
0.25
0.50
0.10
0.25
1.00
0.52
0.10
0.25
0.50
0.10
0.25
19091S-101
19091S-102
19091S-105
19091S-331
19091S-431
19091S-231
19091S-333
19091S-433*
19091S-133
19091S-336
19091S-436
19091S-211
19091S-112
19091S-313
19091S-413
19091S-113
19091S-316
19091S-416
Price
$261
$400
$674
$295
$295
$295
$483
$483
$483
$823
$823
$319
$448
$521
$521
$521
$896
$896 www.agilent.com/chem • 800 227 9770 64
65
• Exceptionally low bleed
• Low polarity
• Extended temperature limit of 360°C
• Unique selectivity
• Excellent inertness for active compounds
• Ideal for confirmational analyses
• Excellent for pesticides, herbicides, PCBs and PAHs
• Certified for MS
• Bonded and cross-linked
• Solvent rinsable
0.18
0.18
0.20
0.20
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.25
0.32
0.32
0.32
0.32
MDN-12
I.D.
Length Film Part No.
30
30
30
30
60
15
15
15
30
30
30
60
20
30
12
25
0.18
0.18
0.33
0.33
0.10
0.25
1.00
0.10
0.25
0.50
1.00
0.25
0.10
0.25
0.50
0.25
Price
121-1222
121-1232
128-1212
128-1222
122-1211
122-1212
122-1213
122-1231
122-1232
122-1236
122-1233
122-1262
123-1231
123-1232
123-1236
123-1262
PCB congeners, pesticides, chlorinated herbicides, phenoxy acid methyl esters, haloacetic acids
$412
$579
$261
$400
$295
$295
$295
$483
$483
$483
$483
$823
$521
$521
$521
$896
• Equivalent to a (35%-Phenyl)methylpolysiloxane
• Midpolarity
• Very low bleed characteristics
• Extended temperature limit of 360°C
• Excellent inertness for active compounds
• Certified for MS
• Ideal for confirmational analyses
• Bonded and cross-linked
• Solvent rinsable
• Replaces HP-35ms
• Close equivalent to USP Phase G42
I.D.
0.20
0.20
0.25
0.25
0.25
0.25
0.32
0.32
Length
15
25
15
30
30
60
30
60
Film
0.33
0.33
0.25
0.15
0.25
0.25
0.25
0.25
Part No.
128-3812
128-3822
122-3812
122-3831
122-3832
122-3862
123-3832
123-3862
Rtx-35, SPB-35, AT-35, Sup-Herb
Price
$261
$400
$295
$483
$483
$823
$521
$896
Aroclors, PCBs, amines, pesticides, chlorinated herbicides, haloacetic acids, pharmaceuticals, drugs of abuse www.agilent.com/chem • 800 227 9770
• Equivalent to (50%-Phenyl)methylpolysiloxane
• 320/340°C Upper temperature limit
• Very low bleed midpolarity column
• Excellent inertness for active compounds
• Enhanced mass spectral integrity
• Bonded and cross-linked
• Solvent rinsable
• Best column for CLP pesticides
I.D.
Length Film Part No.
0.18
0.25
0.25
0.25
0.25
0.25
0.32
0.32
20
15
15
30
30
60
30
30
0.18
0.15
0.25
0.15
0.25
0.25
0.15
0.25
121-4722
122-4711
122-4712
122-4731
122-4732
122-4762
123-4731
123-4732
DB-17, HP-50+, Rtx-50, 007-17, SP-2250,
SPB-50, BPX-50, SPB-17
Drugs, glycols, pesticides, steroids
Price
$412
$295
$295
$483
$483
$823
$521
$521
• Equivalent to (50%-Cyanopropylphenyl)methylpolysiloxane
• Mid/high polarity
• Excellent for separations of cis- and trans-fatty acid methyl esters (FAMEs)
• Low bleed
• Bonded and cross-linked
• Solvent rinsable
• Close equivalent to USP Phase G7
I.D.
Length Film Part No.
0.25
0.25
0.25
0.32
15
30
60
30
0.25
0.25
0.25
0.25
122-2912
122-2932
122-2962
123-2932
HP-225, SP-2330, CP-Sil 43CB, RSL-500,
Rtx-225, BP-225, CB-225, OV-225, 007-225
Price
$295
$483
$823
$521
Alditol acetates, FAMEs, neutral sterols www.agilent.com/chem • 800 227 9770
EASY ONLINE ORDERING
Need a column that’s custom-designed for your lab?
Just visit www.agilent.com/chem/4ecatalog
66
67
• Polyethylene glycol (PEG)
• High polarity
• Highest upper-temperature limits of the bonded PEG phases
• Column-to-column repeatability
• Bonded and cross-linked
• Solvent rinsable
• Close equivalent to USP Phase G16
I.D.
Length Film Part No.
Price
0.20
0.20
0.20
0.20
0.25
0.25
0.25
0.25
0.25
0.25
0.32
0.32
0.32
0.32
0.32
0.32
60
60
60
30
30
30
25
25
50
50
30
30
30
60
60
60
0.20
0.40
0.20
0.40
0.15
0.25
0.50
0.15
0.25
0.50
0.15
0.25
0.50
0.15
0.25
0.50
19091N-102
19091N-202
19091N-105
19091N-205
19091N-033
19091N-133
19091N-233
19091N-036
19091N-136
19091N-236
19091N-013
19091N-113
19091N-213
19091N-016
19091N-116
19091N-216
$379
$379
$636
$636
$413
$413
$413
$737
$737
$737
$447
$447
$447
$816
$816
$816
HP-20M, SUPELCOWAX 10, CP-WAX 52CB,
SUPEROX II, CB-WAX, Stabilwax, BP-20,
007-CW, Carbowax, DB-WAXetr
Alcohols, aromatics, essential oils, solvents
• Unique bonded PLOT column technology
• Excellent choice for light hydrocarbons and sulfur gases
• Retention stability not affected by water
• Separates CO and CO2 on a single column
• Ideal PLOT column for GC/MS – no particles
I.D.
0.32
0.32
Length
30
60
Part No.
113-4332
113-4362
CP-Silica PLOT
Price
$627
$942
C1 to C12 hydrocarbons, CO2, trace-level sulfurs, hydride gases, inorganic gases, halocarbons, SF6, oxygen/nitrogen separation at -80°C.
www.agilent.com/chem • 800 227 9770
Most detectors require simple but periodic cleaning to maintain peak performance.
This is especially true for highly sensitive
GC detectors. Without routine detector maintenance, GC system performance will deteriorate and can cause detector failure.
Detailed procedures on how to clean, maintain and replace common detectors, including FID, TCD, NPD, ECD, and FPD are summarized in this section. Also included are special handling techniques and specific recommendations to maximize specific detector operations. For example, learn how to resolve flame ignition problems associated with your flame photometric detector and test electron capture detectors for radioactivity leaks. www.agilent.com/chem • 800 227 9770
“GC detectors are highly sensitive systems that are often compromised by various types of contamination. By implementing some recommended detector maintenance routines, you can minimize instrument downtime and keep your GC system working at peak efficiency.”
Bernhard Rothweiler
Applications Chemist
CATALOG
For a complete selection of Detector supplies, see Agilent’s 2005-2006
Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
68
Flame Ionization Detectors require little maintenance to keep them performing at satisfactory levels. The primary task is to occasionally measure hydrogen, air and makeup gas flows. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be independently measured to obtain the most accurate values.
Since the FID combustion process results in water formation, the detector temperature must be kept above 100˚C to prevent condensation. Such condensation, especially when combined with chlorinated solvents or samples, causes corrosion and sensitivity loss.
If the flame goes out or will not light:
• Check the column flow rate. It may be too high. Decrease the flow rate or pressure. Switch to a more restrictive column (longer or with a smaller id).
If you must use a large id column, first cool the GC oven to below 50˚C, then turn off the carrier flow long enough to allow the FID to light. Check for partially or completely plugged jet.
• Check that the right type of jet is installed for the column you are using.
• Injecting large volumes of aromatic solvent or water can cause the flame to go out. Switch to a nonaromatic solvent or inject less solvent.
• The lit offset value may be too low or too high. Adjust the value.
Even with normal use, deposits develop in the jet and detector (usually white silica from column bleed or black carbonaceous soot). These deposits reduce sensitivity and cause chromatographic noise and spikes. Although you can clean the jet, it is usually more practical to replace dirty jets with new ones. If you do clean the jet, be careful not to scratch the jet internally; scratches will ruin the jet
Igniter Glow Plug Assembly
Collector Assembly
Collector Body
FID Jets
FID Ferrules
FID Cleaning Kit, P/N 9301-0985, $41
69
To view a video on FID column installation, jet replacement, collector maintenance, or ignitor replacement, visit
www.agilent.com/chem/techsupport.
www.agilent.com/chem • 800 227 9770
(using Agilent’s FID Cleaning Kit #9301-0985)
1. Run a cleaning wire through the top of the jet. Run it back and forth a few times until it moves smoothly. Be careful not to scratch the jet. (Do not force too large a wire or probe into the jet opening or the opening will become distorted. A loss of sensitivity, poor peak shape and/or lighting difficulties may result if the opening is deformed.)
2. Fill an ultrasonic cleaning bath with aqueous detergent, and place the jet in the bath. Sonicate for five minutes.
3. Use a jet reamer to clean the inside of the jet.
4. Sonicate again for five minutes.
NOTE: From this point on, handle the parts only with forceps!
5. Remove the jet from the bath and rinse it thoroughly, first with hot tap water and then with a small amount of GC-grade methanol.
6. Blow the jet dry with a burst of compressed air or nitrogen, and then place the jet on a paper towel and allow it to air dry.
Item Description Unit Part No.
Price
1 PTFE chimney (optional)**
2 Collector nut
3 Spring washer
4 Ignitor castle
Optional Hastelloy Ignitor Castle*
5 Ignitor glow plug assembly
6 Collector insulator
7 Collector body
Hastelloy Collector Body
10/pk
19231-21050
19231-20940
5181-3311
19231-20910
19231-21060
19231-60680
G1531-20700
G1531-20690
61531-21090
9 FID collector assembly 1
Detector insulation assembly
FID collector cleaning brush
Collector Housing
2/pk
G1531-60690
G1531-20700
8710-1346
G1531-20740
$194
$ 17
$ 8
$175
FID retainer nut wrench
(5880, 5890, 6890)
1/4 in. Nut Driver for FID jet-drilled shaft
19301-00150 $ 8
8710-1561 $ 13
FID supplies kit-Includes: 5182-3450
Jet, packed standard 3 each 18710-20119
FID performance evaluation sample kit 2 each 18710-60170
Ignitor glow plug assembly
Jet, cap. series 530 µm
FID flow measuring insert
Cleaning wires for 0.03 in. ID jet
2 each
3 each
2 each
19231-60680
19244-80560
19301-60660
5180-4150
Cleaning wires: 0.018 in. ID/530 µm jet 1/pk
Wire, jet cleaning, 5 each
5180-4152
19301-20720
Capillary inlet cleaning wires
Detector cleaning kit
5180-4153
9301-0985
**Not included in assembly.
*Hastelloy components may be used when analyzing highly corrosive materials.
1 Does not include Hastelloy component.
$556
$ 49
$ 44
$ 42
$ 56
$ 53
$ 23
$ 23
$ 12
$ 8
$ 41
$ 14
$ 35
$ 9
$ 57
$184
$ 42
$ 17
$ 60
$260 www.agilent.com/chem • 800 227 9770
Plugged FID jet
EASY ONLINE ORDERING
Here’s another time-saving reason to place your order through our website: you can instantly view and edit the items in your shopping cart
– while keeping track of your total order price.
Just visit www.agilent.com/chem/4ecatalog
70
Description
Jets for capillary dedicated FID
Capillary jet (0.011 in./0.29 mm ID tip)
High-temperature jet (SimDIS 0.018 in. ID tip)
Adaptable FID
Capillary 0.53 mm jet (0.011 in. ID tip)
Packed (0.018 in. ID tip)
Packed (0.030 in. ID tip)
0.53 mm high temp (0.018 in. ID tip) for SimDIS
Length(mm) Part No.
48
48
61.5
63.5
63.5
61.5
G1531-80560
G1531-80620
19244-80560
18710-20119
18789-80070
19244-80620
Price
$43
$54
$56
$49
$55
$37
Description Unit Part No.
Price
FID flow measuring insert
FID ignitor cable
19301-60660 $53
G1531-60680 $41
FID Performance evaluation sample kit, 0.03% C14,
C15, and C16 normal alkanes in hexane
O-rings
18710-60170 $44
Cleaning wire
Jet cleaning wire for 0.03 in. ID jet
Jet cleaning wire for Series 530 mm and 0.018 in. ID jet
12/pk 5080-4978
5/pk
5/pk
$ 7
19301-20720 $12
5180-4150 $23
5180-4152 $23
Agilent FID Jets (from top to bottom): Dedicated capillary, Adaptable capillary, Adaptable packed
1
8
4
6
7
2
3
6
5
71
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.
6890 Series GC FID Detector
Collector Body, P/N G1531-20690 www.agilent.com/chem • 800 227 9770
www.agilent.com/chem • 800 227 9770
Agilent provides two types of electron capture detectors. The regular detector
(ECD) has a larger internal volume
(approximately 10 times) than the microcell detector (µ-ECD). These two types can be distinguished by the top cover of the detector – the ECD has a solid cover and the µ-ECD has a perforated cover.
If your baseline is noisy or the output value is abnormally high and you have determined that these problems are not being caused by leaks in the GC system, you may have contamination in the detector from column bleed and sample residues. To remove contamination, you should perform a thermal cleaning
(bakeout) of the detector.
Warning: Detector disassembly and/or cleaning procedures other than thermal should be performed only by personnel trained and licensed appropriately to handle radioactive materials. Trace amounts of radioactive 63 Ni may be removed during other procedures, causing possible hazardous exposure to ß and x-radiation.
Electron capture detectors must be tested for radioactive leakage at least every six months. Records of tests and results must be maintained for possible inspection by the Nuclear Regulatory Commission and/or the responsible local agency. More frequent tests may be conducted when necessary.
The procedure used is a “wipe test.” A wipe test kit is supplied with each new detector. Refer to the information card supplied in the Wipe Test Kit for instructions on performing the test.
For successful EC detection, it’s important that the carrier and purge gases are very clean and dry (99.9995%). Moisture, oxygen, or other contaminants can improve sensitivity, but at a cost of linear range.
Always precondition the column before connection to the detector.
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.
72
1
2
3
6890 Series GC ECD Detector
Item Description Part No.
Price
1 ECD makeup gas adapter*
2, 3 Nut warmer cup with insulation
ECD adapter replacement liner, fused silica
ECD end cap
G1533-80565
19234-60720
19233-20625
19233-20755
$198
$ 58
$ 15
$ 32
ECD chemical sample kit, 3 ampoules solution of 33 pg/mL (0.033 ppm) each of lindane and aldrin in isooctane
ECD wipe test kit
18713-60040 $ 46
18713-60050 $ 31
*Includes one each of P/N 19233-20625 and P/N 19233-20755
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
TIPS AND TOOLS
Tap Agilent’s GC knowledge over the phone, online, in the classroom, even at your site. See pages 104-115 for more information about our services and support.
www.agilent.com/chem • 800 227 9770
The TCD compares the thermal conductivities of two gas flows – pure carrier gas (also called the reference gas) and carrier gas plus sample components
(also called column effluent).
The primary maintenance for a TCD involves the filament. Most procedures involve improving filament life or keeping the filament from becoming damaged or contaminated.
A constant presence of oxygen can permanently damage filaments through oxidative processes. The most common source of oxygen is a leak(s) near the detector – or in the carrier or makeup gas line fittings. Oxygen traps are recommended for the carrier and makeup gases to reduce oxygen levels. Proper column installation techniques and regular leak checks (especially after column installation) help to keep leak problems to a minimum.
The damage caused by oxygen is more severe at high filament currents.
Chemically active sample components such as acids and halogenated compounds may attack and damage the filaments.
Avoiding these compounds when possible increases filament life. Turning off or substantially reducing the filament current when the TCD is not in use also prolongs filament life.
Increased filament lifetime will result if the following startup process is used:
1. Purge the detector with carrier and makeup gas for 10-15 minutes before turning on the filaments. This prevents oxidation of the filaments due to the presence of oxygen that has diffused into the cell under no flow conditions.
2. Turn on the filaments at the lowest possible current setting, then increase the filament current in several increments to the desired value. This reduces the power surge upon current introduction and prolongs filament lifetime.
Description Unit
Cell contamination is a problem when a lower detector temperature is used to improve sensitivity. Also, low filament currents promote contamination since the filament is maintained at a lower temperature at lower currents. If the cell becomes contaminated, a solvent flush of the detector may help to remove the condensed material.
Part No.
6890/6850/5890 Common TCD Supplies
TCD replacement cell (6890/6850 only)
TCD cap column adapter seal
TCD cap column adapter
10/pk
Graphite ferrules, 1.0 mm id
Graphite ferrules, 0.5 mm id
Capillary column nut, for 6890
Capillary column nut, for 6850
10/pk
10/pk
2/pk
2/pk
TCD packed column adapter (6890/6850 only)
G1532-60675
18740-20950
18740-20960
5080-8773
5080-8853
5181-8830
5183-4732
G1532-20710
TCD chemical sample kit, 3 ampoules,
0.5 mL, 5 solution of 0.3% C14, C15, and C16, normal alkanes in hexane 18711-60060
5890 TCD Supplies
Makeup gas adapter, TCD
TCD column adapter, 1/8 to 1/4 in. glass
TCD replacement cartridge
19232-80550
19302-80020
19232-60676
Price
$ 45
$ 126
$ 138
$1625
$1030
$ 18
$ 33
$ 38
$ 47
$ 26
$ 47
$ 44 www.agilent.com/chem • 800 227 9770 74
75
1. Cool the cell to room temperature and remove the column.
2. Place a septum in a nut or fitting assembly that fits onto the detector entrance.
3. Place the nut or assembly on the detector fitting and tighten. Verify the presence of makeup gas flow.
4. Inject 20-100 µL volumes of toluene or benzene into the detector through the septum. Inject a total volume of at least 1mL of solvent. Do not inject halogenated solvents such as methylene chloride and chloroform into the detector.
5. After the final injection, allow makeup gas to flow for 10 minutes or more.
Slowly raise the temperature of the cell to 20-30˚C above the normal operating temperature.
6. After 30 minutes, decrease the temperature to the normal value and install the column as usual.
The TCD can become contaminated with deposits from such things as column bleed or dirty samples. A wandering baseline, increased noise level, or changes in response on a checkout chromatogram all indicate contamination. Thermal cleaning, or bakeout (heating the detector block to evaporate the contaminant), should be performed only after you have confirmed that the carrier gas and the flow system components are leak-free and contaminant-free.
Watch out for decreased sensitivity caused by samples that react with the filament, originating from oxygen-contaminated carrier gas, leaks in plumbing, or column bleeding. Samples with active components, such as acids and halogenated compounds can chemically attack the filament as well. Also, sample condensation will contaminate the detector cell if the temperature is too low.
Some types of contaminants can be removed by temperature bakeout. Also, in non-modulated designs, wandering baselines due to temperature variation can be corrected by making sure the detector temperature remains constant.
www.agilent.com/chem • 800 227 9770
Flame Photometric Detectors require minimal maintenance to keep them performing at satisfactory levels. The hydrogen, air and makeup gas flows should be measured occasionally. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be measured independently to obtain the most accurate values.
The FPD requires periodic cleaning. In most cases, this only involves the jet, and less frequently, the filter. Agilent provides brushes and wires that simplify the cleaning of all detector parts (see FPD
Supplies on page 77). The brushes are used to dislodge particulates clinging to the metal surfaces. A fine wire is used to clean the jet opening of particulates. Do not force too large a wire or probe into the jet opening or the opening may become distorted. A loss of sensitivity, poor peak shape, and/or lighting difficulties may result if the opening is deformed. The filter or any of the window parts should be handled gently. Scratches or other surface deformities reduce the amount of light passing through the filter, thus reducing response. The filter and related parts should be clean and free from fingerprints.
The Photo Multiplier Tube (PMT) needs periodic replacement. The PMT is defective and needs to be rebuilt or replaced if:
• high voltage is on and the flame is lit
• low or no signal and/or noise not attributed to any other source such as bad cables are observed
• light leaks occur
• high temperatures are used
• defective signal boards are present
High detector temperatures reduce the
PMT life. When not in use, turn off the
PMT to maximize its usable lifetime. Some
PMTs may have a shelf life and should not be stored for prolonged periods before use.
Column bleed and/or effluent can contaminate the first quartz window (heat shield) nearest the detector module. Dust, fingerprints, and atmospheric contaminants can dirty both quartz windows, the filter, and/or the photomultiplier tube window.
Contamination anywhere along the light path between flame and PMT can reduce detector sensitivity.
If a response problem is encountered
(sensitivity, noise, selectivity) the FPD jet should be inspected for deposits and, if necessary, cleaned or replaced. To properly service the jet, the detector module should be removed from the instrument, and followed by appropriate service (see jet cleaning procedure on page 70).
Occasionally, the transfer line fused silica liner between the column and FPD module must be inspected, cleaned and/or replaced.
If the FPD flame won’t light or stay lit:
• Be sure there is a problem. Ignition is best confirmed by holding a mirror or shiny surface near the aluminum exhaust tube, with the rubber drip tube removed, and observe condensation if the flame is lit.
• Check Lit Offset. If it is zero, autoignition is turned off. If it is too large, the GC will not know that the flame is lit and will shut down the detector.
• Increase the air supply pressure to the pneumatics module. This makes the flame easier to light but does not affect the air flow rate setpoint.
• If the flame doesn’t light at all, check the glow plug circuit. Observe the visual display, which will momentarily go to greater than 65500 counts when the flame lights. If the display doesn’t change, check the pin connections at the printed circuit board, the lead connection on the glow plug and the appropriate 5A fuse on the GC main circuit board.
• The flame is easier to light at higher detector temperatures.
• Under some operating conditions, the flame may be more easily lit with the rubber drip tube removed. After lighting the flame, reinstall the drip tube.
• If the flame still won’t light, there could be a large leak in the system. This results in measured flow rates being different from actual flow rates, causing non-ideal ignition conditions. Thoroughly leak check the whole system.
The flame conditions are critical to successful operation. Since the detection zone is above the flame, the gas flows and jet diameter must be optimized so that components burned (activated) in the flame will emit in the detection zone.
Gas flows are also critical for optimized selectivity and sensitivity. The most critical parameters are the hydrogen/air or hydrogen/oxygen ratio, and the total gas flow, which effects flame temperature.
www.agilent.com/chem • 800 227 9770 76
77
Item Description Unit Part No.
1 Exit tube assembly
2 Nut, brass, 1/4 in.
4 Weldment, block
5 O-ring, ignitor, Kalrez
6 Spacer, ignitor
7 FPD Ignitor Replacement Kit
8 Ignitor cable assembly (6890 only)
9 Gasket, heat shield
10 Window, first heat shield
11 Disk, heat shield
12 Coupling, SS
10/pk
14 Screw, M3 x 12 (4 required)
15 Clamp
16 O-ring, inner window
17 Window, second heat shield
18 O-ring, outer window
19 Flange adapter
12/pk
12/pk
20 Flange ring
21 O-ring, Viton, 1.239 in. id
Adapter weldment, 1/8 in. columns
12/pk
Adapter weldment, capillary
Start-up kit (5890 only)
FPD O-ring (5890 only)
Liner/ferrule kit
19256-80570
19256-60500
12/pk 5061-5867
19256-60590
19256-80000
19256-80010
Sulfur filter
Phosphorus filter
Kalrez O-ring, size 2-002
Kalrez O-ring, size 2-011
Fluorocarbon Elastomer O-ring, brown, 0.926 in. id 12/pk
FPD Performance Evaluation Sample: Solution of
20 ng/mL (20 ppm) dodecanethiol and tributylphosphate in isooctane, 3 ampoules
0905-1609
0905-1608
5061-5889
19305-60580
19256-60700
5180-4105
19256-80560
0905-1610
19256-20590
19256-60800
G1535-60600
19256-80045
19256-80030
19256-20580
19256-20550
0515-0911
19256-00090
5061-5886
19256-80060
5061-5891
19256-20510
19256-00200
5061-5890
19256-80590
Price
$ 19
$ 40
$ 22
$ 21
$141
$114
$434
$ 17
$ 89
$378
$378
$ 42
$ 42
$ 1
$ 59
$ 24
$ 40
$ 24
$131
$ 68
$ 22
$ 83
$ 38
$ 80
$165
$ 72
$ 13
$536
$ 42
$ 15
8
7
6
5
1
4
3
2
16
17
18
19
20
9
10
11
12
13
14
15
21
Install the correct optical filter, depending on the choice of Sulfur or
Phosphorus mode.
For Sulfur Mode, use the 393 nanometer filter.
For Phosphorus Mode, use the 525 nanometer filter.
www.agilent.com/chem • 800 227 9770
NPDs are temperamental and require frequent maintenance. Small changes in any of a number of parameters can significantly change the performance characteristics of an NPD. The bead requires the most maintenance. It needs to be changed frequently, thus a spare is a necessity.
To extend the life of the bead:
• Use the lowest practical adjust offset or bead voltage.
• Run clean samples and keep the inlet/liner clean to minimize contamination.
• Turn off the bead when not in use.
The beads have to be kept dry which limits their storage life to about six months. When a new bead is installed, slowly raise the detector temperature and bead current.
Rapid heating can crack or break the bead especially if it has been stored under humid conditions. It has been observed that higher hydrogen flows and bead currents decrease bead life. If the NPD is not in use, the hydrogen flow and bead current should be reduced or turned off to increase bead life.
Make sure there is some type of gas flow in a heated detector or when there is current to the bead.
• Keep the detector temperature high
(320 – 335˚C).
• Turn off the hydrogen flow during solvent peaks and between runs.
• If the NPD is off for an extended period of time in a high humidity environment, water may accumulate in the detector.
To evaporate this water, set the detector temperature to 100˚C and maintain it for 30 minutes. Then set the detector temperature to 150˚C and maintain it for another 30 minutes.
The hydrogen, air and makeup gas flows should be measured frequently. They can drift over time or be changed unintentionally without knowledge of it occurring. Each gas flow should be measured independently to obtain the most accurate values. NPDs are very sensitive to changes in the gas flows and consistent flows are necessary to maintain performance levels.
Because of its high sensitivity, the NPD requires very pure gases (99.999% or better).
We strongly recommend that moisture and hydrocarbon traps be used on the carrier gas and all detector gases, including the detector hydrogen, air, and makeup gases.
Dirty gases will not only give poor chromatographic performance, but will shorten the bead life as well.
www.agilent.com/chem • 800 227 9770 78
79
The NPD requires periodic cleaning. In most cases, this only involves the collector and the jet. Agilent provides brushes and wires that simplify the cleaning of all detector parts (see NPD Supplies on page 79). The brushes are used to dislodge particulates clinging to the metal surfaces. A fine wire is used to clean the jet opening of particulates.
Do not force too large a wire or probe into the jet opening or the opening will become distorted. A loss of sensitivity or poor peak shape may result if the opening is deformed.
The various parts can be ultrasonicated after cleaning with a brush. Eventually the jet needs to be replaced, so it is strongly recommended to have spare jets on hand.
Over time, residue from the bead or sample can build up in the collector and cause baseline problems. You should clean the collector after you have changed the bead two or three times.
The metal C-rings wear slightly with each assembly and disassembly. After several assemblies and disassemblies (five or more), the rings may not seal effectively, causing an erratic baseline. A ceramic insulator and seal kit is available. Always cool the detector to near-ambient when changing seals and insulators.
Because there is no flame in the NPD, the jet does not collect silica and soot as does the FID jet. Although you can clean the jet, it is usually more practical to simply replace dirty jets with new ones. If you do clean the jet, use the cleaning wire, taking care not to damage the inside of the jet. You can also use a sonicator bath to clean the jet.
Description
Some chemical problems can also arise when using the NPD. Because it is a trace detector, be careful not to contaminate the analytical system.
Glassware must be very clean. Phosphate detergents should be avoided, so acid washing of glassware followed by distilled water and solvent rinsing is recommended.
Solvents should be checked for purity.
Chlorinated solvents and silanizing reagents can decrease the useful lifetime of the alkali source; excess reagent should be removed prior to injection, if possible.
Phosphate-containing leak detectors, phosphoric acid-treated columns or glass wool, polyimide-coated columns, or nitrogen-containing liquid phases can add noise to the system and should be avoided.
Capillary jet (0.011 in./0.29 mm id tip)
(6890 only, dedicated)
6890/5890 Adaptable
Capillary 0.53 mm jet (0.011 in. id tip)
Packed (0.018 in. id tip)
Length (mm) Part No.
48
61.5
63.5
G1531-80560
19244-80560
18710-20119
Price
$ 43
$ 56
$ 49 www.agilent.com/chem • 800 227 9770
Item Description Part No.
12
13
14
15
8
9
10
11
6
7
6890 NPD Supplies
1 Screws, M3 x 0.5 x 8 mm (Pozidriv)
2 NPD white ceramic bead assembly*
NPD black ceramic bead assembly**
3
4
5
Lid weldment
Metal C-ring, top
Alumina insulator, upper
Collector funnel
Alumina insulator, lower
Metal C-ring bottom and top
Screw, M4 x 10 mm
J-Clamp
Screw, M4 x 10 mm
NPD interconnect assembly
Mounting pallet
Jets (see page 79)
Base weldment, Capillary NPD
Base Weldment, Packed NPD
16
17
18
Lid stop
NPD Ceramic Insulator Kit includes items 4, 5, 7, and 8
Column adapters for packed NPD
Nut warmer cup with insulation
5890 NPD Supplies
NPD collector (NPD bead)
Recoating kit, sufficient for 10 collectors
Detector Trap Replacement Kit
G1534-80500
G1534-80540
G1534-20590
5182-9722
19234-60720
19234-60540
5080-8872
19231-60790
*This bead is more sensitive, but exhibits some tailing for phosphorous compounds.
Quantity discounts available.
**The black bead is potentially a little less sensitive, but does not exhibit peak tailing and typically has a longer lifetime.
0515-0655
G1534-60570
5183-2007
G1534-80510
0905-2580
G1534-40020
G1534-20530
G1534-40030
0905-1284
0515-2495
1400-0015
0515-2495
G1534-60610
G1531-40020
Price
$ 58
$289
$216
$284
$ 64
$ 42
$ 53
$ 1
$ 1
$ 1
$ 1
$368
$379
$160
$ 53
$ 72
$160
$ 29
$501
$532
$ 36
$175
13
14
16
15
17
18
2
1
3
6
5
4
8 7
9
10
12
11
www.agilent.com/chem • 800 227 9770 80
You asked … we listened!
We’ve streamlined our online store to complement the design and content of our
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.
www.agilent.com/chem • 800 227 9770
“We offer intelligent, creative solutions to help our customers maximize the performance of their GC/MS systems.”
Jim McCurry
Senior Applications Chemist
CATALOG
For a complete selection of gas management supplies, see Agilent’s
2005-2006 Essential Chromatography Catalog. Or, visit our online catalog at www.agilent.com/chem/4ecatalog.
82
Common maintenance tasks are listed in the table below. It is advisable to keep a log book of system performance, Autotune, and maintenance operations performed. This makes it easier to identify variations from normal performance and to take corrective action. Subtle differences may exist between MSD models. Consult your hardware manual for specific instruction.
TASK EVERY EVERY EVERY AS
WEEK 6 MONTHS YEAR NEEDED
•
Tune the MSD
Change injection port liners
Check the foreline pump oil level
Gas ballast the foreline pump
Check the calibration vial
Replace the foreline pump oil
Check the diffusion pump fluid
Replace the diffusion pump fluid
Replace the traps and filters
Clean the ion source
Change the carrier gas trap(s) and purifier
Replace the worn out parts
Lubricate seals (where appropriate)
Replace column
•*
•
•
•
•
•
•
•
•
•
•
•
•
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.
Check the foreline pump oil level and diffusion pump fluid. Change the injection port liners and O-rings. Gas ballast the foreline pump.
Clean the split/splitless inlet vent line trap. Check for leaks (inlet and column connections).
Replace gas cylinders (when below
500 psig).
Replace the foreline pump oil. Check, and if necessary, refill the calibration vial.
Replace the diffusion pump fluid.
Recondition or replace internal and external traps and chemical filters on the GC.
Tune the MSD. Clean the ion source.
Replace the carrier gas trap. Replace worn-out parts (filaments, EM, etc.).
Replace the column. Lubricate seals.
Record all tune values such as electron multiplier and ion source parameters in a log book to monitor instrument performance. In addition note the high vacuum and foreline vacuum pressures.
83
*For more information on inlet maintenance, see pages 26-34.
www.agilent.com/chem • 800 227 9770
Contamination is usually identified by excessive background in the mass spectra. It can come from the GC or from the MSD. The source of the contamination can sometimes be determined by identifying the contaminants. Some contaminants are much more likely to originate in the GC, others are more likely to originate in the MSD.
Contamination sources in the GC:
• column or septum bleed
• dirty injection port
• injection port liner
• contaminated syringe
• poor quality carrier gas
• dirty carrier gas tubing
• fingerprints
• air leaks
• cleaning solvents and materials
Contamination sources in the MSD:
• air leak
• cleaning solvents and materials
• diffusion pump fluid
• foreline pump oil
• fingerprints inside the manifold
The action required to remove the contamination depends on the type of contamination and the level of contamination. Minor contamination by water or solvents can usually be removed by allowing the system to pump (with a flow of clean carrier gas) overnight. Serious contamination by rough pump oil, diffusion pump fluid or fingerprints is much more difficult to remove; it may require extensive cleaning. For further details contact your Agilent
Customer Engineer (CE).
Air leaks are a problem for any instrument that requires a vacuum to operate. Leaks are generally caused by vacuum seals that are damaged or not fastened correctly.
• higher than normal vacuum manifold pressure or foreline pressure
• higher than normal background
• peaks characteristic of air (m/z 18, 28,
32, and 44 or m/z 14 and 16)
• poor sensitivity
• low relative abundance of m/z 502
(this varies with the tune program and
MSD used) www.agilent.com/chem • 800 227 9770 84
85
Leaks can occur in many more places in the MSD:
• GC/MSD interface column nut
• side/top plate O-ring (all the way around)
• vent valve O-ring
• calibration valve
• high vacuum gauge tube fitting
• cracked ion gauge tube
• front and rear end plate O-rings
• GC/MSD interface O-ring (where the interface attaches to the vacuum manifold)
• diffusion pump co-seal and/or baffle adapter O-ring
• turbomolecular pump O-ring
• new Vespel/graphite ferrules contract when heated
• Check interface nut for tightness.
Replace if necessary.
• Check leak/test the GC injection port.
MS interface column nut
Column nut for GC/MS and two-hole ferrules
Universal Column Nut (2/pk)
05988-20066
05921-21170
5181-8830
TIPS AND TOOLS
The most likely point for an air leak is a seal you recently opened.
$13
$16
$26
It is common to see cleaning solvent peaks in the mass spectra shortly after the ion source is cleaned.
Corrective Action
• Dry all cleaned metal parts in the GC oven before reassembling and reinstalling them. Refer to specific cleaning procedures in your MSD Hardware
Manual.
• Use a temperature that’s just above the boiling point of the solvent.
Fingerprints contain hydrocarbons that can appear in mass spectra. Hydrocarbon contamination is characterized by a series of mass peaks 14 amu apart. The abundances of these peaks decrease as peak mass increases. Fingerprint contamination is usually caused by the failure to wear lint-free, nylon gloves during ion source cleaning, GC inlet maintenance, or from installing the column. Use special care to avoid recontamination of parts after you clean them. This typically occurs after some maintenance or part replacement.
Corrective Action
• Reclean using clean, nylon gloves and proper cleaning techniques.
Nylon gloves, lint-free, Large
Nylon gloves, lint-free, Small
8650-0030
8650-0029
$16
$16
If the diffusion pump is allowed to operate with no column (carrier gas) flow into the vacuum system, vapor from the diffusion pump fluid can drift up into the vacuum manifold. A more serious problem is when fluid is back streamed into the vacuum manifold by sudden or improper venting of the vacuum system. If a diffusion pump has back streamed, a prominent peak will often be seen at m/z 446 and the spectral baseline will exhibit increased background noise.
Corrective Action
• If m/z 446 appears please call Agilent for assistance.
www.agilent.com/chem • 800 227 9770
Foreline pump oil contamination is characterized by peaks spaced 14 amu apart (hydrocarbons). Contamination with foreline pump oil is less common than contamination with diffusion pump fluid.
Corrective Action
• Call Agilent for assistance.
The following table lists some of the more common contaminants, the ion characteristic of those contaminants, and the likely sources of those contaminants.
Ions (m/z) Compound
13,14,15,16
18, 28, 32, 44 or 14, 16
Methane
H
2
O, N
2
, O
2
, CO
2 or N, O
31, 51, 69, 100, 119, 131, 169,
181, 214, 219, 264, 376, 414,
426, 464, 502, 576, 614
31
43, 58
PFTBA and related ions
Methanol
Acetone
78 Benzene
91, 92 Toluene or xylene
105, 106
151, 153
69
Xylene
Trichloroethane
Foreline pump fluid or
PFTBA
Dimethylpolysiloxane 73, 147, 207, 221, 281,
295, 355, 429
77, 94, 115, 141, 168, 170,
262, 354, 446
149
Diffusion pump fluid
Plasticizer (phthalates)
Peaks spaced 14 amu apart Hydrocarbons
Possible Source
CI gas
Residual air and water, air leaks, outgassing from
Vespel™ ferrules
PFTBA (tuning compound)
Cleaning solvent
Cleaning solvent
Cleaning solvent
Cleaning solvent
Cleaning solvent
Foreline pump oil vapor or calibration valve leak
Septum bleed or methyl silicone column coating
Diffusion pump fluid and related ions
Vacuum seals (O-rings) damaged by high temperatures, use of vinyl or plastic gloves
Fingerprints, foreline pump oil www.agilent.com/chem • 800 227 9770 86
87
Symptoms
This section describes some of the symptoms you might observe – either in the spectra of samples or in a tune report.
Typically, these symptoms fall into two broad classes:
1. those that affect the system sensitivity.
2. those that affect the repeatability of a measurement.
Some symptoms can be corrected by following the suggested corrective actions.
Others require the services of an Agilent
Customer Engineer.
Corrective Action
Wrong retention time
Low signal
Leaking injection port
Check GC, method, application and carrier gas velocity
Check GC, tune vacuum system
Clean the injection port
Replace the injection port liner and septa
Air leak
Peak widths
Check and tighten interface nut, leak test GC injection port
Do Autotune, check flow rate and temperature stability
Interfering peaks
Excessive background
Check time parameters, coeluting peaks, column type
Do Autotune and compare to background specifications
Check time parameters
Incorrect mass assignment Retune
Abnormal spectra – excessive background contamination
Incorrect tuning
Check for contamination
Check tune file, retune, check sample
Repeller voltage is too low Raise voltage to test for response
Dirty ion source Clean source
Symptoms Corrective Action
Dirty syringe needle
Wrong syringe needle
Leaking injection port
Injection is too large
Clean or replace the syringe
Replace syringe and septa
Perform injection port maintenance
Replace the injection port liner, septa, and liner o-ring
Check method and injection volume, split ratio and/or splitless purge time
Loose column connections Tighten column nuts on injection port or transfer line
Replace column nuts and ferrule
Variations in pressure, column flow, and temperature
Ensure the MSD is located in an environment where the temperature is stable
– Keep MSD out of drafts and direct sunlight
– Check that the carrier gas is steady and well regulated
– Service the foreline pump and/or diffusion pump
Clean source Dirty ion source
Loose connections in the analyzer
Ground loops
Check internal and external analyzer wiring connections, make sure all are secure
Check main electrical lines www.agilent.com/chem • 800 227 9770
The ion source operates by electron ionization (EI) or chemical ionization (CI).
The sample enters the ion source from the
GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting them. The positive voltage on the repeller pushes the positive ions into the lens stack, where they pass through several electrostatic lenses. These lenses concentrate the ions into a tight beam, which is directed into the mass filter.
5973 Ion Source Assembly (EI)
Cleaning procedures for MSDs vary. Refer to your MSD Hardware Manual for specific ion source cleaning procedures.
Common measures of instrument performance:
• abundance of certain ions (e.g.
percentage of the 502 ion from the
Autotune report)
• shape of lens ramps and the chosen voltages, especially Repeller Ramp
• sensitivity obtainable for a given analysis
• ability to tune to a given reference compound (e.g. DFTPP)
When to Clean:
The ion source should be cleaned:
• according to a customer’s predefined schedule
• based on instrument performance (e.g.
deteriorated performance over time)
Frequency of Cleaning
The cleaning frequency is determined by:
• the number of samples run (throughput)
• the type of samples
• unique, established laboratory protocol
Selecting a Cleaning Method
The primary action of any cleaning procedure is to remove contamination from surfaces. Removing this contamination restores the electrostatic properties of the ion source lensing system. Numerous cleaning methods have been developed for restoring ion source performance. The cleaning methods include abrasive, sonic, and electropolish.
Abrasive methods offer several advantages:
• provide adequate energy to remove contamination from surfaces
• require minimal equipment
• pose minimal risks to the user
A popular material used to abrasively clean stainless steel ion source parts is aluminum oxide. It is available in either powder form or an abrasive film. After the critical surfaces have been abrasively cleaned, the loose particles must be removed. One method of removing particles is swabbing with a cotton swab or a clean cloth dipped in acetone. A clean swab should be used for each element followed by a sonication. These cleaning supplies are listed on page 89.
Preparing to Clean
Prior to cleaning, the mass spectrometer must be vented and the ion source must be removed. Before venting the system, the following conditions must be met:
• heated zones are less than 100°C
• the diffusion pump is off and cool
• the turbo pump is off and not spinning
• the rough pump is off
Always allow the automatic venting routine to run its full course. Improper venting may cause diffusion pump fluid to be deposited into the analyzer (backstreaming). It can also reduce the life of the multiplier, or other sensitive MS parts.
TIPS AND TOOLS
Agilent’s new MS Inert Ion Source improves inertness – and maintains it over multiple cleanings . For more information see page 90.
www.agilent.com/chem • 800 227 9770 88
89
Description
Cleaning and Maintenance
Nylon gloves, lint-free, Large
Nylon gloves, lint-free, Small
Lint-free industrial wipes, 100% cotton, 9 x 9 in. (300/pk)
Generic ion source cleaning kit for all GC/MS types
Includes: Cloths, lint-free (15/pk), Abrasive sheets (5/pk), Cotton swabs
(100/pk), Nylon gloves, lint-free, Alumina powder, abrasive
Cloths, lint-free (15/pk)
Abrasive Sheets, aluminum oxide green lapping paper for ion source cleaning, 600 mesh (5 sheets)
Alumina powder, abrasive
PFTBA sample, certified (10 g)
PFTBA sample kit, 1 mL
Activated alumina, absorbent pellets for Edwards rough pump traps, non-LC/MS (1 lb can)
PFTBA glass vial
Cotton swabs (100/pk)
Tools
Screwdriver, Pozidriv #1 pt, 3 in., fits no. 2 - 4 screws
Screwdriver, Pozidriv #2 pt, 4 in., fits no. 5 - 10 screws
Wrench, open-end, 1/4 x 5/16 in.
Screwdriver, TORX, T15
Screwdriver, TORX, T10
Ferrules and O-rings
Teflon 1/4 in. ferrule (back)
Teflon 1/4 in. ferrule (front)
Retainer rings (10/pk)
5973 One Year Maintenance Kit (for diffusion pump systems)
Includes: Big Universal Trap for He, Abrasive sheets (5/pk),
Cloths, lint-free (15/pk), Cotton swabs (100/pk), SantoVac Ultra,
18.5 mL (2 ea.), Rough pump oil, 1 liter, Filament assembly,
Octafluoronapthalene (OFN)
MSD Tool Kit
Includes: Small cleaning rod, Large cleaning rod, Source hold tool,
Cotton swabs (100/pk), Nylon gloves, lint-free, Abrasive sheet,
30 mm (5/pk), Tool kit (wrenches, driving tools)
Price
$ 16
$ 16
$185
$124
$ 16
$ 25
$ 24
$ 38
$ 24
$ 8
$ 8
$ 10
$657
$ 64
$ 27
$ 29
$168
$ 85
$115
$ 14
$ 10
$510
Part No.
8650-0030
8650-0029
9310-4828
5181-8863
05980-60051
5061-5896
8660-0791
8500-0656
05971-60571
8500-1233
05980-20018
5080-5400
8710-0899
8710-0900
8710-0510
8710-1622
5182-3466
0100-0160
0100-0787
5181-1258
5183-2096
05971-60561 www.agilent.com/chem • 800 227 9770
5973 MSD Ion Source Parts (EI)
Item Description
(A) Ion source body
(B) Repeller
(J) Washer, M3 (1/pk)
(K) Nut, 5.5 mm
(L) Ion Source Sensor
(M) Lens insulator, (2/pk)
Ion source assembly
Source heater assembly
Repeller assembly
Screw (for filament on the source)
5973 Part No.
G1099-20130
G1099-20132
G1099-20136
05971-20134
G1072-20008
05971-20143
05971-20126
G1099-20133
0515-1446
3050-0891
0535-0071
G1099-60104
05971-20130
G1099-60106
G1099-60177
G1099-60170
0515-1046
Price
$ 3
$ 1
$ 1
$ 200
$ 270
$ 270
$ 408
$ 481
$ 2
$ 198
$ 112
$ 29
$ 69
$ 190
$ 263
$ 105
$ 82
H
D
E
F
M
5973 Ion Source Parts (EI).
G
M
A
C
L
MS Inert Ion Source Parts
Description 5973A 5973N 5973 inert** Price
Drawout plate – 3 mm Inert
Drawout plate – 6 mm Inert** G2589-20045 G2589-20045
EI High Temp Filament
Repeller assembly, Inert source G1099-60170 G1099-60170
Screws for filament High Temp 0515-1046
Source body, Inert G1099-20130
0515-1046
G1099-20130
Source Washer, Inert
G2589-20100 $ 99
G2589-20045 $ 225
G2590-60053 $ 97
G2589-60102 $ 499
G1999-20021 $ 3
G2589-20043 $ 563
G2589-20101 $ 12
I
I
K
J
H
5973 Repeller Assembly (EI).
L
H
B
**used in G2860A and G2860B extended linearity kits www.agilent.com/chem • 800 227 9770 90
91
5972/5971/GCD Ion Source (EI)
5972/5971/GCD MSD Ion Source Parts (EI)
Description
(A) Entrance lens
(B) Lens insulator, (2/pk)
(C) Ion focus lens
(D) Drawout cylinder
(E) Drawout plate
(F) Ion source body
(G) Set screw
(H) Repeller assembly
(I) Screw (for filament on the source)
5972/5971/GCD Part No.
05971-20126
05971-20130
05971-20143
G1072-20008
05971-20134
05971-20128
0515-1446
05971-60170
0515-1046
TIPS AND TOOLS
It is good practice to replace scratched lenses and other ion source parts.
Scratched source parts lead to poor performance.
Price
$ 108
$ 278
$ 271
$ 190
$ 71
$ 531
$ 3
$ 593
$ 2
Ion source assembly
Transfer line tip, gold-plated
5972 Part No.
Price
05972-60226 $3554
5972/5971 Part No.
05971-20305
Price
$ 242
GCD Part No.
G1800-20305
Price
$259
MSD Flowrates (ml/min)
Each MSD has its own maximum flow rate requirement. Refer to the MSD Flowrates below for flow limitations.
5973
5972
5971
GCD
Min
0.1
0.1
0.1
0.1
Max Diff Pump
2.0
2.0
1.5
1.0
Max Turbo Pump
4.0
NA
NA
NA
Tuning Max
2.0
2.0
1.0
1.0
www.agilent.com/chem • 800 227 9770
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.
Maintaining the Filaments
Like the filament in an incandescent light bulb, the ion source filaments will eventually burn out. Certain practices will reduce the chance of early failure:
Tips to increase filament life
• When setting up data acquisition parameters, set the solvent delay so that the analyzer will not turn on while the solvent peak is eluting.
• When the software prompts Override
solvent delay at the beginning of a run, always select “No.”
• Higher emission current will reduce filament life.
• If you are controlling your MSD from the
Edit Parameters screen, always select
MS Off before changing any of the filament parameters.
It is very useful to switch from one filament to the other every three months so that when one filament fails, you know the other will fail soon. This will allow you to change both filaments at the same time, which helps to maximize your instrument uptime.
Filament Assembly
Description Unit
Filament, 5973 (EI)
Filament, 5973 (CI)
Filament, EI High Temperature for the 5973 inert
Filament, 5972 (EI/CI)
Filament, 5971 (EI/CI) / GCD (EI)
2/pk
Part No.
05972-60053
G1099-80053
G2590-60053
05972-60053
05971-60140
Price
$ 90
$282
$ 97
$ 90
$159
The mass filter does not require periodic maintenance. It should not be removed from the radiator or distributed in any way.
• Never put the quadrupole in an ultrasonic cleaner.
• Never change the physical orientation of the quadrupole mass filter.
• The fused-quartz quadrupole is fragile and will break if dropped or handled roughly.
• The material in the cusps of the quadrupole is very hygroscopic. If exposed to water, the quadrupole must be dried very slowly to prevent damage.
• Cleaning techniques appropriate for other manufacturers’ instruments are not suitable for Agilent MSDs – and may actually harm the mass filter.
• To save time and effort, use only Agilent
MSD mass filters, which do not require periodic cleaning or maintenance.
• In case of extreme contamination, contact a trained Agilent service representative to perform the mass filter cleaning.
www.agilent.com/chem • 800 227 9770 92
The vacuum system creates the high vacuum (low pressure) required for the
MSD to operate. Without this vacuum, the molecular mean free path is too short.
Ions cannot travel from the ion source through the mass filter to the electron multiplier (detector) without colliding with other molecules.
The major components of the vacuum system are:
• Vacuum manifold
• Foreline gauge
• Calibration valve
• Gauge controller (optional)
• Vacuum seals
• Foreline pump and/or trap
• Diffusion/turbo pump and fan
• High vacuum gauge tube
A properly maintained vacuum system will:
• Prevent premature filament failure
• Provide better sensitivity
• Require less frequent source cleaning
• Extend quadrupole lifetime
• Prevent premature EM Horn failure
Keeping a pan under the vacuum pump helps to detect and identify the origin of oil leaks.
93
Calibration
The calibration valve is an electromechanical valve with a vial that contains a tuning compound. Perfluorotribuylamine (PFTBA) is the most commonly used tuning compound. It is required for automatic tuning of the MSD in EI mode. The tuning compound is usually a liquid but can be volatile or semi-volatile solid.
How to Refill
The calibration vial can be refilled without venting the system. Fill the vial to 0.5 cm from the top. DO NOT overfill. Air is trapped in the vial when it is refilled.
PFTBA sample, certified (10 g) (EI)
PFDTD sample (10 g) (CI)
8500-0656
8500-8130
$168
$ 43
This sometimes causes an “Excess source pressure” error message during the first tune after refilling. This is more likely if the vial is overfilled. Be sure to purge the air upon refilling the vial.
If using the 5973 with a CI source, use Perfluorodimethyltrioxadodecane
(PFDTD) sample.
www.agilent.com/chem • 800 227 9770
This section describes unusual pressure readings and their possible causes. The symptoms in this section are based on typical pressures. At typical column flow rates (0.5 – 2.0 ml/minute), the foreline pressure will be approximately 20 to 100 mTorr. The vacuum manifold pressure will be approximately 1 x 10-6 to 1.4 x 10-4 Torr.
These pressures can vary widely from instrument to instrument so it is important that you are familiar with the pressures that are typical for your instrument at a given carrier gas flow and oven temperature.
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.
The vacuum manifold pressures can only be measured if your system is equipped with the optional gauge controller.
Foreline pressure is too high
Symptom • Pressure is above 100 mTorr.
• Pressure for a given column flow has increased over time.
Possible Cause • Column (carrier gas) flow is too high
• Wrong carrier gas
• Air leak (normally at transferline interface)
• Foreline pump oil level is low or oil is contaminated
• Foreline hose is constricted
• Foreline gauge is not working correctly
• Foreline pump is not working correctly
Vacuum manifold pressure is too high
Symptom • Pressure is above 1.4 x 10-4 Torr.
• Pressure for a given column flow has increased over time.
Possible Cause • Column (carrier gas) flow is too high
• Wrong carrier gas
• Air leak
• Foreline pump is not working correctly
• Diffusion pump fluid level is low or fluid is contaminated
• Foreline pump is not working correctly
• Defective gauge controller
• Faulty ion gauge tube
Foreline pressure is too low
Symptom • Pressure is below 20 mTorr.
Possible Cause • Column (carrier gas) flow is too low
• Wrong carrier gas
• Column plugged or crushed by an overtightened nut
• Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing*
• Foreline gauge is not working correctly
* These could create a fault condition in the
GC that would prevent the GC from operating.
Vacuum manifold pressure is too low
Symptom • Pressure is below 1.4 x 10-6 Torr.
Possible Cause • Column (carrier gas) flow is too low
• Wrong carrier gas
• Column plugged or crushed by an overtightened nut
• Empty or insufficient carrier gas supply*
• Bent or pinched carrier gas tubing*
• Defective gauge controller
• Faulty ion gauge tube
* These could create a fault condition in the
GC that would prevent the GC from operating.
www.agilent.com/chem • 800 227 9770 94
It is not necessary to change the diffusion pump fluid more than once a year, unless you observe symptoms that suggest a problem with the diffusion pump fluid. The
MSD must be vented in order to check the diffusion pump fluid (except for the 5973).
Therefore, the best time to check the fluid is when the instrument is already vented for other maintenance.
Importance of the Fluid Level
The amount of fluid in the pump affects the amount of vapor and the temperature of the base plate. Too little fluid will cause the pump to run at a higher temperature because there is less fluid to carry away the heat resulting in fluid cracking or degradation and loss of high vacuum. It will also lower the pumping speed because there is less fluid vapor available to pump away gases which can especially affect operation in
CI Mode due to higher flow rates.
How to Check the Fluid Level
1. If it is not vented already, shut down and vent the MSD according to instrument manual.
2. Unplug the MSD power cord.
3. Remove the pump and cover the top with aluminum foil.
4. After heating the pump in a GC oven at 60°C for 15 minutes to make the fluid flow down into the reservoir at the bottom, remove the stack parts.
5. Inspect the pump fluid, if the fluid is discolored or contains particulate material, the fluid must be changed.
6a. Use a metal ruler to determine the depth of the fluid. A pump that has been in operation should have a pool
9 mm plus or minus 1 mm deep. Fluid in freshly charged pumps will be 12 mm deep. It is normal that up to 2 ml of oil may be in the rear portion of the vacuum manifold. The recommended total fluid charge for the 5971/5972 is
18 ml (plus or minus 2 ml).
6b. For the 5973 use the sight glass to determine the depth of the fluid.
The recommended total fluid charge is approximately 37 ml.
Description
Diffusion pump fluid: SantoVac Ultra 5P,
18.5 ml (5973, 5972 or 5971/GCD)
Ion gauge controller (5973/5972A)
Ion gauge tube for measuring vacuum (5971/5972)
Triode gauge tube for measuring vacuum (5972/5973)
Part No.
Price
6040-0809
59864B
0960-0376
0960-0897
$ 82
$1399
$ 195
$ 358
95
The oil in the foreline or rough pump should be replaced on average once every six months, but can vary depending upon applications. After oil replacement, if the foreline trap is present, the molecular sieves should be replaced.
Avoid contact with the pump oil. The residue from some samples may be toxic.
Dispose of used oil properly.
Description
Rough pump oil, 1 gal Inland 45 (5973, 5972 or 5971/GCD)
Rough pump oil, 1 liter Inland 45 (5973, 5972 or 5971/GCD)
Molecular sieve (5973, 5972 or 5971/GCD)
Oil mist filter RV3/E1M18/E2M18/E2M2
Oil mist filter E2M1.5
Oil mist filter E2M18
Part No.
6040-0798
6040-0834
9301-1104
3162-1056
G1099-80037
5063-5224
Price
$122
$ 39
$ 57
$430
$173
$417 www.agilent.com/chem • 800 227 9770
General Instructions on How to Replace the
Pump Oil
1. Shutdown and vent the MSD.
2. Place a container under the drain plug on the 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 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.
6. Reinstall the drain plug and pour pump oil into the fill hole.
7. Reinstall the fill cap.
8. Reconnect the MSD power cord.
9. Start up and pump down the MSD according to the Instrument Manual procedure.
TIPS AND TOOLS
Use chemical-resistant gloves and safety glasses when replacing pump fluid. Avoid contact with the fluid. Always dispose of used oil properly.
Electron multiplier replacement horn
(5973, 5972, 5971/GCD)
High energy dynode (5973 only)
Electron multiplier kit (5972, 5971/GCD only)
05971-80103
G1099-80001
05971-80102
$1004
$2131
$1136
Maximize Lifetime
The lifetime of an EM is directly related to the current that flows through it and the extent of contamination or condensation that it experiences. To maximize electron multiplier life:
• Maintain the best possible vacuum, especially in the analyzer manifold.
• Use extreme caution and be conservative with venting, pumpdown, and all vacuum system procedures to keep pump fluid background to a minimum.
• After venting, allow four hours for pumpdown and thermal equilibration before scanning.
• Actively look for background contamination and leaks and repair them immediately.
• Don’t tune excessively. PFTBA can result in higher background over an extended period of time.
Symptom
• Voltage is over 2500 volts
• Poor vacuum
Corrective Action
• Replace electron multiplier www.agilent.com/chem • 800 227 9770
TIPS AND TOOLS
Use only Agilent replacement multipliers and horns for Agilent MSDs.
Other manufacturers’ products can increase noise, while reducing sensitivity and linearity.
96
97
• Always wear clean, lint-free, nylon gloves when handling parts which will come in contact with the sample stream. Oil from your fingers is a particularly difficult contaminant to remove.
• If you must set parts down, place them on clean, lint-free cloths or clean aluminum foil, not directly onto a laboratory bench.
• Keep parts covered so that dust does not accumulate on them.
• Do not leave the interior of the vacuum system open to the atmosphere. For example, if you are removing the ion source for cleaning, put the vacuum manifold cover back in its normal position after you have removed the source. Re-establish a low vacuum in the vacuum manifold until you need to reinstall the ion source.
Common maintenance tasks are listed on page 83. Performing these tasks on a regular basis can reduce overall operating costs.
Keep a record (logbook) of system performance characteristics and maintenance operations performed.
This makes it easier to detect variances from normal operation and to take corrective action.
There is not a regular interval for ion source cleaning. The ion source should be cleaned when symptoms indicate. Symptoms of a dirty ion source include poor sensitivity and inadequate abundances at high masses.
See the Troubleshooting chapter in your hardware manual for more information about these symptoms.
Balzers turbo pump lubricant, 0.25 liter
SantoVac 5, 1 liter
SantoVac 5, 128 ml
Rough pump oil, 1 gal Inland 45
Rough pump oil, 1 liter Inland 45
Particle Beam pump oil, Fomblin
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
6040-0468
6040-0370
6040-0819
6040-0798
6040-0834
6040-0730
$ 134
$2553
$ 283
$ 133
$ 40
$ 760 www.agilent.com/chem • 800 227 9770
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.
Autotune or manual tune (save results)
Clean the cabinet
Inspect hoses and cords
Vacuum the fan filter
Check mech. pump oil
Replace mech. pump oil
Replace mech. pump traps
Check diffusion pump fluid
Degas ion gauge tube
Replace ion gauge tube
Replace seals & O-rings
Clean ion source
Replace filament
Replace ion source heater
Replace mass filter heater
Replace electron multiplier horn
Refill EI calibration vial
Refill CI calibration vial
Replace interface heater
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
We recommend keeping a separate set of tools that have been thoroughly cleaned for working with the MS engine.
These tools are needed to prevent contamination when reassembling or installing clean assemblies such as the ion source.
www.agilent.com/chem • 800 227 9770 98
Many of the tools and supplies needed to service the 5989 MS Engine are included in the installation kit supplied with the instrument. The following tables list common consumable parts and supplies used in the maintenance of the MS Engine.
5989 Lens Stack
(A) Clamp insulator, ion source
(B) Entrance lens
(C) Lens insulator, ion source
(D) Plate insulator, ion source
(E) EI/CI repeller
(F) Repeller insulator
Filament block
Filament assembly
Heater cartridge
05989-20110
05989-67002
05989-20111
05989-20109
05989-20145
05989-20119
05989-20165
05985-60179
05989-60098
$108
$990
$ 62
$ 88
$318
$580
$448
$ 58
$926
5989 Repeller Assembly
99
The electron multiplier lifetime on the 5989 may be 6 to 9 months or shorter, especially with the following applications:
• Thermospray
• Particle Beam
• Purge and trap, with no jet separator
• Extensive CI
• High sensitivity work with high EM voltage
Electron multiplier kit
Electron multiplier replacement horn
Ion gauge tube, K-25 flange
Insulating ring
O-ring, detector flange (5/pk)
Diffusion pump fluid fitting fill and drain cap O-ring (12/pk)
KF 25 centering ring and O-ring
O-ring, manifold window
05989-80043
05971-80103
0960-0799
05989-20705
5181-3367
0905-1145
3162-0110
0905-1189
$2012
$1004
$ 448
$ 18
$ 47
$ 19
$ 39
$ 38 www.agilent.com/chem • 800 227 9770
• Start-Up Guide, pub. No. 5988-3073EN
• Application Note, “Improvements in the
Agilent 6890/5973 GC/MSD System for use with USEPA Method 8270”, pub. no.
5988-3072EN
• Ultra Ion Source Chamber
• Ultra Repeller
• Ultra Large Aperture Drawout Plate
• Pre-tested column, 30m x 250um x 0.5um
HP-5 MS, part no. 19091S – 139
• Single-taper splitless liner, 4mm i.d., deactivated, part no. 5181-3316
• Direct Connect Liner, single taper, 4mm i.d., deactivated, part no. G1544-80730
• Direct Connect Liner, dual taper, 4mm i.d., deactivated, part no. G1544-80700
• Floppy Disk with tuning macros
8270 Semi-Volatiles Applications Kit
G2860A
The G2860A 8270 Semi-Volatiles
Applications Kit is designed for use in
Agilent 6890/5973A and 6890/5973N
GC/MSD Systems. The kit provides modified and/or pretested components to improve system performance for USEPA
Method 8270. With the kit, system linearity is maximized and activity is minimized.
$2333
There are many ways to perform semi-volatile analysis. For another option that also features 5973 MSD Electronics upgrades, visit www.agilent.com/chem and do a library search for 5989-1510EN.
www.agilent.com/chem • 800 227 97700 100
Each GC/MS has a specific test and performance sample. Refer to the chart below for the exact sample.
5973
5972
5971
GCD
PFTBA PFDTD
PFTBA PFTBA
OFN 1 pg/µL
HCB 10 pg/µL
PFTBA PFTBA HCB 10 pg/µL
PFTBA NA Sample A (10 ng/µL)
OFN 1 pg/µL Benzophenone 100 pg/µL
NA
NA
NA
Benzophenone 100 pg/µL
Benzophenone 100 pg/µL
NA
DFTPP
DFTPP
DFTPP
DFTPP
BFB
BFB
BFB
BFB
5989A
5989B
PFTBA PFTBA HCB 50 pg/µL OFN 1 pg/µL Benzophenone 100 pg/µL
PFTBA PFTBA HCB 20 pg/µL OFN 500 fg/µL Benzophenone 100 pg/µL
DFTPP
DFTPP
BFB
BFB
101
EASY ONLINE ORDERING
Visit the Agilent website at www.agilent.com/chem/4ecatalog for one-click access to:
• Product pricing links (when available)
• Local sales contact information
• Online quote requests
• Order status updates … and more www.agilent.com/chem • 800 227 9770
Description
Contains 6 vials: 4 vials (Sample A, 10 ng/µL), 1 vial (Sample B, 100 pg/µL), and 1 vial (Sample C, 100 ng/µL) each of dodecane biphenyl, p-chlorodiphenyl, and methyl palmitate in isooctane, 1 mL ampoule
DFTPP, Benzidine, Pentachlorophenol, and p,p’-DDT 1 mg/mL in methylene chloride
HCB 50 pg/µL, HCB 20 pg/mL, Benzophenone 100 pg/µL,
OFN 1 pg/µL, mix of HCB, OFN and Benzophenone 5 ng/µL
Extended Mass Performance Sample
PFTBA certified
PFTBA Sample Kit
PFDTD
Benzophenone
Hexachlorobenzene
Hexachlorobenzene
Methyl stearate (in methanol);
PFTBA not certified
Octafluoronapthalene (OFN)
Octafluoronapthalene (OFN) p-Bromofluorobenzene (BFB)
Quantity
1 ng/µL (2 ea)
1 pg/µL,
5 ampoules
500 fg/µL
25 µg/mL
Part No.
Price
05970-60045 $ 46
8500-5995 $ 62
0.5 g, fomblin oil
1 bottle, 10 g
0.5 mL
10 g
8500-6406
8500-5500
8500-0656
05971-60571
8500-8130
100 pg/µL,
5 ampoules 8500-5440
10 pg/µL, 4 ampoules 8500-5808
1 ng/µL, 2 ampoules
20 pg/µL 8500-6405
$ 38
$141
$168
$ 85
$ 44
$ 74
$ 39
$ 32
05990-60075 $ 67
8500-5441
8500-6572
8500-5851
$ 67
$ 30
$ 39 www.agilent.com/chem • 800 227 9770 102
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Every Agilent GC and GC/MS system is backed by our nearly 40 years of experience with instrument design, lab operations, business processes, and regulatory requirements.
We stand behind our products with …
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105
Agilent service agreements operate under a yearly fixed cost, which includes preventative maintenance, compliance, telephone support, repairs, parts, and labor. No matter how many service visits or replacement parts you need, this fixed cost covers it all – at no additional charge.
If you choose, you can also consolidate instrument maintenance and repair services into multi-year agreements for administrative ease and greater cost savings.
You can rest assured that the engineer who arrives at your site will perform the requested service with optimum skill.
That’s because Agilent engineers …
• Are experts in instrument operation, maintenance, compliance, and repair.
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• Use only Agilent factory-approved replacement parts, columns, and supplies to ensure peak instrument reliability.
• Carry calibrated, traceable tools and testing equipment, as well as Agilent hardware and software qualification protocols.
What’s more, most Agilent engineers are part of the Agilent product development team. So you can be certain that ease of repair, maintenance, and compliance are built into your GC and GC/MS systems right from the start.
Our team will work with you to help your laboratory achieve …
• Maximum uptime
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Agilent Services
Telephone Service
Software Service
Features Advantages to You
• Telephone access to skilled Agilent service professionals.
• Available parts option.
• Fast identification and resolution of hardware problems.
• Low cost.
• Telephone access to trained technical professionals.
• Enhancements to the original application software purchase.
• Software bulletins that identify discovered defects and recommend workarounds.
• Fast identification and resolution of software problems.
• A fixed annual cost for software upgrades makes budget management more predictable.
• A single cost-effective source for telephone support and software updates.
• A convenient way to keep up with the latest software enhancements.
Onsite Instrument Repair • Hardware telephone support with access to skilled, factory-trained Agilent service professionals.
• Travel expenses and labor.
• Optional coverage for consumables used during repair.
• A fixed annual cost for parts makes budget management more predictable.
• You can choose the response method that fits your business needs and budget.
Offsite Instrument Repair
For selected Agilent analysis instruments
• Option 1: Replacement with an identical instrument (your fastest choice).
• Option 2: Return to Agilent for repair.
Preventative Maintenance
For selected Agilent analysis instruments
• Expert cleaning, adjustment, lubrication, and inspection of your instrument.
• Travel expenses and labor.
• Coverage for consumables used.
• Less expensive than onsite repair.
• Fast and easy.
• Includes extensive diagnostics and testing that are not feasible with onsite maintenance or repair.
• Maximum uptime.
• Extended instrument life.
• Confidence in the integrity of your measurements.
www.agilent.com/chem • 800 227 9770 106
Agilent Services
Installation Qualification (IQ)
Advantages to You
• Supplies the evidence you need to satisfy regulatory agencies.
• Helps fulfill the master validation plan – and change-control SOP requirements – for the IQ phase.
Operational Qualification/Performance
Verification (OQ/PV)
For selected Agilent analysis instruments
Note: We recommend Preventative
Maintenance before OQ/PV.
• Verification and documentation of an instrument’s ability to meet specified criteria.
• Procedures and documentation that fit the requirements of GLP, ISO 9000, and other regulatory agencies.
• Full automation to increase the qualification scope without excess time requirements.
• Measuring equipment that is traceable to national and international standards.
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• No need to write your own SOPs to qualify Agilent instruments – or to train your staff.
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• Confidence in the integrity of your measurements, with traceable, documented chains from sample introduction to reporting.
• Less risk of financial loss due to noncompliance.
• Meaningful, relevant, and understandable system tests.
Requalification (RQ) After Repair
For instruments that have their operational performance verified by an annual OQ/PV.
Features
• Qualification and documentation of shipment completeness.
• Comprehensive system and application software verification tests.
• Delivered by professionals with training certification.
• Verification that a system is performing at operation specifications after repair.
• Complete system operation testing.
Note: only a subset of the Operational
Qualification test is performed, based on the type and extent of the repair.
• A comprehensive test of the repaired module using established conditions and known sample characteristics to ensure the basic accuracy and precision of your module.
• Measuring equipment is traceable to national and international standards.
• Minimal system downtime after completion of instrument repair.
• Efficient system requalification by performing the appropriate tests based on the components repaired.
• Assurance that all instrument subsystems are performing within specifications.
• All procedures and documentation meet regulatory agency requirements.
107 www.agilent.com/chem • 800 227 9770
Agilent Services
Network Qualification
Features Advantages to You
Mass Spectrometer Ion Source Cleaning
For selected Agilent analysis instruments
• Network definition and performance testing using established Agilent Design,
Installation Qualification, and Operational
Qualification protocols.
• Documentation of the definition, integrity, supportability, and health of high-risk network segments.
• Completed protocols, created using hardware and software network testing tools. Protocols include:
- A physical and logical inventory.
- A graphical network topology map.
- A snapshot of network health, as installed.
• Network Operational Qualification testing, which monitors the network over time, and evaluates its operation over a controlled range of traffic conditions. We’ll also provide the following reports:
- Long Duration Network Characterization, which analyzes each function in its operating environment.
- Performance Predictability Analysis, which documents reserve capacity and stability over a range of operating demands.
• Significant time savings.
• Increased uptime – issues that might impact application performance are quickly identified and resolved.
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• Increased control – Agilent will verify known elements and identify unknown network contingency states that may impact application performance.
• Reduced regulatory exposure – audit-ready documentation establishes evidence of network system control.
• Onsite disassembling
• Cleaning
• Reassembling
• Testing
• Your staff can devote more time to chemistry, not instrument maintenance.
• Efficient cleaning with minimal downtime.
www.agilent.com/chem • 800 227 9770 108
Agilent Services
Software Backup
Features
• Telephone or onsite factory support to facilitate restoration.
• Captures the unique system settings for all software components needed to reconstruct your system including:
- Network information
- Printers and peripherals
- Configurations
- User settings and operations
- System registry
- Application software
- Settings
- Operating system
- Customizations
- Analytical hardware
- Directory structure
- Security information
Advantages to You
• Fast and easy – you simply insert a disk
… reboot … and you’ll be back in operation in as little as two hours.
Normally, you would have to reload and reconfigure your software – a process that can take days.
• A complete solution – the initial configuration backup includes:
- Simple backup software
- Ten CD-ROMs
- Ten 3.5-in. floppy disks
- A storage case
- One full system backup
- Installation of the backup software and optional CD writer
109
TIPS AND TOOLS
To learn more about Agilent’s complete portfolio of services, please visit www.agilent.com/chem/service.
www.agilent.com/chem • 800 227 9770
Highly trained lab professionals can boost your productivity, minimize errors and reruns, and expand your chromatography capabilities. And that’s why Agilent offers several training options that cover everything from troubleshooting and maintenance to the most advanced operational techniques. 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
Course Title
6890 GC Split Inlet Mode Operation
Duration
Self-paced;
Four hours access
6890 GC Splitless Inlet Mode Operation Self-paced;
Four hours access
6890 GC Purged Packed Inlet Operation Self-paced;
Four hours access
Description
Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in split mode.
Clarifies flow paths, so you can gain the maximum benefit from this inlet operational mode.
Discusses typical problems and routine maintenance procedures.
Reviews the basic theory and operation of the 6890 GC split/splitless capillary inlet when running in splitless mode.
Clarifies flow paths, so you can gain the maximum benefit from this inlet operational mode.
Discusses typical problems and routine maintenance procedures.
Reviews the basic theory and operation of the 6890 GC purged packed inlet.
Clarifies flow paths, so you can gain the maximum benefit from this inlet.
Discusses typical problems and routine maintenance procedures.
www.agilent.com/chem • 800 227 9770 110
Course Title
6890 GC Keyboard Operation
6890 GC FID Theory and Operation
Duration
Self-paced;
Four hours access
Self-paced;
Four hours access
6890 GC ECD Theory and Operation Self-paced;
Four hours access
6890 GC TCD Theory and Operation Self-paced;
Four hours access
GC Automatic Liquid Sampler Operation Instructor-led;
60-90 minutes
Description
Reviews the basic operation of the 6890
GC keyboard.
Thoroughly describes all keys, so you can gain the maximum benefit from your GC.
Reviews the basic theory and operation of the FID.
Covers proper column installation, keyboard setup, and flow optimization.
Discusses typical problems and routine maintenance procedures.
Reviews the basic theory and operation of the ECD.
Covers proper column installation, keyboard setup, and flow optimization.
Discusses typical problems and routine maintenance procedures.
Reviews the basic theory and operation of the TCD.
Covers proper column installation, keyboard setup, and flow optimization.
Discusses typical problems and routine maintenance procedures.
Reviews the basic operation of the 7683A automatic liquid sampler system (ALS).
Shows you how to gain maximum productivity from the ALS.
Discusses routine maintenance procedures, and how to return an ALS to Agilent for repair or exchange.
111 www.agilent.com/chem • 800 227 9770
Course Title
Logical GC Troubleshooting
Duration
Instructor-led;
60-90 minutes
Using the GC/MSD
Security ChemStation to Achieve
FDA CFR Part 11 Compliance
Managing and Administering the
GC/MSD Security ChemStation to Meet FDA CFR Part 11
Compliance Requirements
Designed for systems administrators
Instructor-led;
60-90 minutes
Instructor-led;
60-90 minutes
Description
Teaches a methodical process for troubleshooting GC system problems.
Helps you identify the source of problems quickly, making troubleshooting less daunting.
Note: This course does not discuss hardwarespecific problems or solutions.
Describes in detail how to operate the
GC/MSD Security ChemStation software in accordance with FDA CFR Part 11 requirements.
Shows you how to manage the GC/MSD
Security ChemStation software in accordance with FDA CFR Part 11 requirements.
www.agilent.com/chem • 800 227 9770 112
Classroom Training
Agilent’s training courses for gas chromatography and mass spectrometry help new and experienced lab professionals learn proper and efficient ways to use analytical instruments and software. These ISO-registered courses also target those who want to broaden or sharpen their troubleshooting, maintenance, and system operation skills.
Contact Agilent today for more information about our training and services. Or visit
www.agilent.com/chem and select
“Education.”
Course Title
Technique
Introduction to Capillary GC
Techniques of GC
Introduction to GC-MS
Techniques of GC-MS
Hardware/Software Operation
ChemStation Operation for the 6890 GC/ALS
Operation of the GC-MSD System
Using the ChemStation for GC-MSD
GC-MSD System for Environmental Applications
Course No.
No. of Days Description
H2615A
H4002A
H2609A
H4040A
H5926A
H4043A
H4050A
1
5
1
3
5
5
5
Provides an overview of capillary gas chromatography in a lecture format.
Presents the fundamental concepts of gas chromatography.
Introduces the technique of GC-MS in a lecture format that includes worksheet exercises.
Reviews the key concepts of the GC-MS analysis process, as well as qualitative and quantitative GC-MS techniques.
Explains how to operate the Agilent 6890 GC using GC
ChemStation software.
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.
Increases an operator’s skill in using a mass selective detector with mass spectrometer EnviroQuant software.
Troubleshooting and Maintenance
6890 GC Maintenance
5890 GC Maintenance
6890 GC Troubleshooting and
Preventative Maintenance
H5308A
H4001A
H5309A
4
4
1
Addresses preventative maintenance and first-level repair for the Agilent 6890 GC.
Addresses preventative maintenance and first-level repair for the Agilent 5890 GC.
Introduces troubleshooting of the Agilent 6890 GC in a lecture format.
113 www.agilent.com/chem • 800 227 9770
Course Title
Introduction to 5973 GC-MSD Troubleshooting and Preventative Maintenance
Course No.
No. of Days
H5947A 1
Description
5973 GC-MSD Troubleshooting and Preventative Maintenance H2294A 3
Demonstrates how to perform preventative maintenance and troubleshooting to keep the
Agilent 5973 GC-MSD system working properly.
Includes a discussion of typical vs. problem
Auto-Tunes.
Offers class exercises that enhance understanding of troubleshooting and maintenance principles.
Covers tuning and diagnostics, the vacuum system, the 5973 MSD ion source, the quadrupole mass filter, and the 5973 MSD.
Includes hands-on laboratory exercises to demonstrate and practice the principles conveyed.
Data Analysis and Reporting
ChemStation for GC Data Analysis and Reporting H2606A 3
Data Analysis and Reporting Using the
ChemStation for GC-MSD
Data Analysis and Reporting Using the EnviroQuant ChemStation for GC-MSD
H4076A
H4053A
3
3
Teaches the operation of the Agilent GC
ChemStation software through instructor explanations, combined with extensive hands-on and laboratory exercises.
Specifically focuses on data analysis and reporting.
Enhances skills in using the Agilent ChemStation for GC-MSD.
Makes users more efficient and productive, while expanding their ability to use ChemStation features.
Describes how to customize the software for laboratory and customer needs.
Improves proficiency in using the Agilent
EnviroQuant software.
Covers data analysis and reporting, including completion of EPA-like forms.
Describes how to customize the software for laboratory and customer needs.
www.agilent.com/chem • 800 227 9770 114
115
Just give us a call to discuss hardware, software, application concerns, or basic operation techniques.
For a wealth of knowledge, tips, and insights, go to www.agilent.com/chem.
You’ll find:
• Frequently Asked Questions about Agilent instruments and supplies.
• Interactive Troubleshooter A step-by-step approach to help you solve common problems.
• Find a Part Includes parts information, pricing, and availability, plus an illustrated parts breakdown.
• Software Downloads and Utilities Feature patches and status bulletins, tools and utilities, firmware, and revision tables.
• How-to Videos Show you how to perform common installation and maintenance procedures for Agilent products.
• Chromatogram Library A searchable collection of GC, LC, and CE chromatograms for nearly a thousand chemical compounds.
• Instrument and Software Demos Such as product videos, 3D animations and interactive software demos.
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.
GC Technical Support in the United States:
Phone: 1-800-227-9770, press #4, then #1
Fax: 1-916-608-1964
Online: go to www.agilent.com/chem/techsupport and click on “Interactive Troubleshooter.” www.agilent.com/chem • 800 227 9770
You asked … we listened!
We’ve streamlined our online store to complement the design and content of our
ITEM TYPICAL SCHEDULE
Gas purifiers
(carrier gas & detector gas)
Split vent trap
Flowmeter calibration
Every 6-12 months
Every 6 months*
Every 1-2 years
ACTIONS/COMMENTS
Replacement schedule is based on capacity and grade of gases.
In general, replace non-indicating traps every 6-12 months or when indicating traps start to change color. Replace indicating traps when indicating material is spent.
Replace.
Re-calibrate electronic flowmeters – follow recommended schedule for the unit (shown on calibration certificate).
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
Every 3 months* Syringes and/or syringe needles
Inlet liner
Liner O-rings
Inlet septum
Inlet Hardware
Weekly*
Monthly*
Daily*
Every 6 months
Every year
Replace syringe if dirt is noticeable in the syringe, if it cannot be cleaned, if the plunger doesn’t slide easily, or if clogged. Replace needle if septa wear is abnormal or the needle becomes clogged.
Check often. Replace when dirt is visible in the liner or if chromatography is degraded.
Replace with liner or with signs of wear.
Check often. Replace when signs of deterioration are visible
(gaping holes, fragments in inlet liner, poor chromatography, low column pressure, etc.).
Check for leaks and clean.
Check parts and replace when parts are worn, scratched, or broken.
ITEM
Front-end
Maintenance
Solvent rinse
Replacement
Ferrules
TYPICAL SCHEDULE
Weekly – monthly*
As needed
As needed
ACTIONS/COMMENTS
Remove
1
2
-1 meter from the front of the column when experiencing 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.
When chromatography degradation is due to column contamination.
Only for bonded and cross-linked phases.
When trimming and/or solvent rinsing no longer return chromatographic performance.
Replace ferrules when changing columns and inlet/detector parts.
ITEM TYPICAL SCHEDULE ACTIONS/COMMENTS
FID/NPD Jets
& Collector
NPD Bead
FID
As needed
As needed
Every 6 months
Clean when deposits are present. Replace when they become scratched, bent or damaged, or when having difficulty lighting FID or keeping flame lit.
Replace when signal drifts or there is a dramatic change in sensitivity.
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
As needed
Wipe test.
Thermally clean by “baking-out” when baseline is noisy, or the output value is abnormally high. Replace when thermal cleaning does not resolve the problem.
FPD Every 6 months
As needed
Measure hydrogen, air, and makeup gas flows.
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.
*Schedule is an approximation of average usage requirements.
Frequency may vary widely based upon application and sample type.
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800 227 9770
For detailed information about supplies from Agilent, please contact your local Agilent sales representative, or your authorized distributor, or visit us online.
Ask about Agilent’s other valuable resources:
• Maintaining Your Agilent 1100 Series
HPLC System
• Essential Chromatography Catalog
• Online Library and Tech Support
The information and pricing in this guide are subject to change without notice.
© Agilent Technologies, Inc. 2005
Printed in USA February 15, 2005
5989-1925ENUS