Agilent 3000 Micro Gas Chromatograph

User Information

 Agilent Technologies 2001, 2002 All Rights Reserved. Reproduction, adaptation, or translation without permission is prohibited, except as allowed under the copyright laws. Part number G2801-90118 First Edition, December 2002 Replaces part number G2801-90117, April 2002 and part number G2801-90110, July 2001. Made in USA Teflon is a registered trademark of E.I. du Pont de Nemours Inc. Swagelok is a registered trademark of Crawford Fitting Company. Stabilwax is a registered trademark of Restek Corporation. Software Licenses Portions of the software included with this product are covered by various free software licenses, including the GNU General Public License. Copies of these licenses are included in the \Licenses subdirectory on the enclosed CD-ROM. Software listed in the file public.txt is covered by one or more free software licenses. The specific license or licenses applying to a program or library is listed either at the head of the source modules for that program or library, or in a file named COPYING in the source distribution for that program or library. Software listed in the file agilent.txt is NOT covered by a free software license. Copyright notices for free software packages that require explicit acknowledgement are located in the \Copyrights subdirectory on the CD-ROM. For more information on licenses and copyrights applicable to the software used in this instrument, refer to file public.html in the root directory of the enclosed CD-ROM. Source code for the free portions of the included programs is available from Agilent for four years from the original date of purchase. Send a written request to the address below.

Safety Information The Agilent Technologies Micro Gas Chromatographs meet the following IEC (International Electro-technical Commission) classifications: Safety Class III, Transient Overvoltage Category II, Pollution Degree 2. This unit has been designed and tested in accordance with recognized safety standards and is designed for use indoors. If the instrument is used in a manner not specified by the manufacturer, the protection provided by the instrument may be impaired. Whenever the safety protection of the Micro Gas Chromatograph has been compromised, disconnect the unit from all power sources and secure the unit against unintended operation. Refer servicing to qualified service personnel. Substituting parts or performing any unauthorized modification to the instrument may result in a safety hazard. Hot Surfaces Should be Avoided The Micro Gas Chromatograph has heated inlets which are maintained at 110C. Contacting the inlets once they are at operating temperatures can result in injury. Extreme care should be taken to avoid these surfaces. Do Not Operate in an Explosive Atmosphere Do not operate the instrument in the presence of flammable gases or fumes. Operation of any electrical instrument in such an environment constitutes a definite safety hazard. Use Only Supplied Power Source Use of any other power supply could result in catastrophic failure of the electrical system leading to personal injury. Cleaning To clean the unit, disconnect the power and wipe down with a damp, lint-free cloth. Recycling the Product For recycling, send the product to: Agilent Technologies, Inc. 2850 Centerville Road Wilmington, DE 19808-1610 or Agilent Technologies Deutschland GmbH Hewlett-Packard Strasse 8 76337 Waldbronn Germany

Safety Symbols Warnings in the manual or on the instrument must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions violates safety standards of design and the intended use of the instrument. Agilent Technologies assumes no liability for the customers failure to comply with these requirements. WARNING A warning calls attention to a condition or possible situation that could cause injury to the user. CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the users work. See accompanying instructions for more information Indicates a hot surface. Indicates hazardous voltages. Indicates earth (ground) terminal. Indicates explosion hazard.

Agilent Technologies, Inc. 2850 Centerville Road Wilmington, DE 19808-1610 USA

Electromagnetic compatibility This device complies with the requirements of CISPR 11 and EN 61326. Operation is subject to the following two conditions: 1 This device may not cause harmful interference. 2 This device must accept any interference received, including interference that may cause undesired operation. If this equipment does cause harmful interference to radio or television reception, which can be determined by turning the equipment off and on, the user is encouraged to try one or more of the following measures: 1 Relocate the radio or television antenna. 2 Move the device away from the radio or television. 3 Plug the device into a different electrical outlet, so that the device and the radio or television are on separate electrical circuits. 4 Make sure that all peripheral devices are also certified. 5 Make sure that appropriate cables are used to connect the device to peripheral equipment. 6 Consult your equipment dealer, Agilent Technologies, or an experienced technician for assistance. 7 Changes or modifications not expressly approved by Agilent Technologies could void the users authority to operate the equipment. 8 This ISM device complies with Canadian ICES-001. Cet appareil ISM est conforme a la norme NMB001 du Canada.

Sound Emission Certification for Federal Republic of Germany Sound pressure Lp <65 dB(A) During normal operation At the operator position According to ISO 7779 (Type Test) Schallemission Schalldruckpegel LP < 65 dB (A) Am Arbeitsplatz Normaler Betrieb Nach DIN 45635 T. 19 (Typprufng)

Contents
Introduction
About your instrument ......................................................................................... 8 Serial numbering ................................................................................................... 9 Safety information ............................................................................................... 11 Contacting Agilent ............................................................................................... 12

Installation
Remove any caps and connect your gases ....................................................... 13 Set gas source pressures and check for leaks ................................................. 17 Connect all cables ................................................................................................ 18 Turn on the GC .................................................................................................... 19 Set IP address ....................................................................................................... 19 Verify gas configuration set to helium .............................................................. 21 Install Agilent Cerity Networked Data System for Chemical QA/QC software ................................................................................................................. 23 Install external inlet filter .................................................................................. 23 Connect checkout gas cylinder to instrument ................................................. 24 Set method. Start run. Verify chromatographic peaks. .................................. 25 Finish up ............................................................................................................... 25 Connecting to a LAN .................................................................................... 26

Understanding the GC
The GC module ..................................................................................................... 30 Injection ......................................................................................................... 30 Separation ..................................................................................................... 30 Detection ....................................................................................................... 31 Electronic Pressure Control (EPC) ................................................................... 31 The Remote connector ........................................................................................ 31 Selecting a control mode ............................................................................. 31 How the GC and Cerity Chemical respond to and signal remote events ............................................................................................................. 33

Operation
Getting started ...................................................................................................... 35 Learning the control software .................................................................... 35 How to connect a sample to the instrument ............................................ 35 Overview of operation ......................................................................................... 35 Creating a method ............................................................................................... 36 What is a method? ........................................................................................ 36 Method parameters ...................................................................................... 36 Installing a sample filter or conditioner .......................................................... 37 Preparing the sample .......................................................................................... 38 Assemble the sample vessel ........................................................................ 38 Collect the sample ........................................................................................ 39

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Agilent 3000 Micro GC User Information

Prepare the sample vessel for connection to the GC .............................. 40 Running a low pressure, clean gas sample ...................................................... 41 Running a low pressure gas sample containing entrained liquids/particles ................................................................................................... 42 Running a high pressure gas sample without entrained liquids/particles ................................................................................................... 43 Running a high pressure gas sample containing entrained liquids/particles ................................................................................................... 44 Running a high pressure gas sample containing C5+ components .............. 45 Using a sample vessel .................................................................................. 45 Using a transfer line or other continuous sample source ...................... 46 Running a high pressure liquefied petroleum gas (LPG) sample ................. 48 The 3000 Micro GC Portable .............................................................................. 50 General information and cautions ............................................................ 50 Battery usage information .......................................................................... 50 To view the battery status .......................................................................... 51 Charging the battery .................................................................................... 51 The internal carrier gas supply .................................................................. 51 Filling the internal carrier gas cylinder .................................................... 52 Before turning off the carrier gas .............................................................. 55 Shutting down the GC ......................................................................................... 55 References ............................................................................................................. 56

Checkout
The checkout sample ........................................................................................... 57 Connecting the checkout sample to the GC ............................................. 57 Sample composition .................................................................................... 58 Create the checkout method .............................................................................. 59 Run the checkout sample .................................................................................... 60 Checkout method parameters and typical results .......................................... 61 OV-1 columns, fixed injector ...................................................................... 61 OV-1 columns, variable injector ................................................................. 63 OV-1701 columns .......................................................................................... 65 MolSieve 5A PLOT columns ........................................................................ 67 Alumina PLOT columns .............................................................................. 69 PLOT Q columns ........................................................................................... 71 PLOT U columns ........................................................................................... 73 Stabilwax DB columns ................................................................................ 75 0.4 L Backflush injector with Alumina PLOT 10 m 0.32 mm column and Alumina PLOT 1 m 0.32 mm pre-column ........................ 77 1.0 L Backflush injector with MolSieve 5A 10 m 0.32 mm column and PLOT U 3 m 0.32 mm pre-column ..................................... 79 1.0 L Backflush injector with PLOT U 8 m 0.32 mm column and PLOT Q 1 m 0.32 mm pre-column ........................................................... 81 NGA Calibration Gas Standard .......................................................................... 83 RGA Calibration Gas Standard .......................................................................... 86

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Agilent 3000 Micro GC User Information

Troubleshooting Tables
Common chromatographic problems ............................................................... 90 Temperature readout problems ......................................................................... 92 Pressure readout problems ................................................................................ 92 Pneumatic problems ............................................................................................ 93 Output problems .................................................................................................. 94 Communication problems .................................................................................. 94

Troubleshooting
How to determine GC configuration ................................................................. 95 Using the LAN connection .......................................................................... 95 Manually determining hardware configuration ...................................... 99 Hardware/software problems .......................................................................... 100 Verify power ............................................................................................... 100 Verify communications ............................................................................. 101 Verify Cerity Chemical program settings ............................................... 103 Verify GC modules ..................................................................................... 104 Download method ...................................................................................... 104 Test flows .................................................................................................... 106 Inspect tubing ............................................................................................. 106 Test carrier in ............................................................................................. 107 Chromatographic problems .............................................................................. 107 Baseline symptoms .................................................................................... 107 Retention time symptoms ......................................................................... 109 Peak symptoms ........................................................................................... 110 Deformed peaks .......................................................................................... 111 Method problems ............................................................................................... 113 Column and detector bakeout .................................................................. 113 Correcting instrument parameter settings ............................................. 114 Checking the vacuum system ................................................................... 115

Replacement and Service Procedures

Prepare the GC and control software for servicing ...................................... 116 Tools required for any replacement procedure ............................................ 116 Remove the covers ............................................................................................. 116 Remove and replace a GC module ................................................................... 117 Update the instrument firmware ............................................................. 117 Types of replacement modules ................................................................ 117 Decommission the old GC module ........................................................... 118 Remove the old GC module ...................................................................... 121 Install the new GC module ....................................................................... 127 Commission the new module ................................................................... 131 Enable the instrument in Cerity Chemical ............................................. 132 Confirm or update Cerity Chemical methods ........................................ 133 To set the carrier gas type ................................................................................ 133 To change the instruments IP address .......................................................... 136 To restore a lost or unknown IP address ....................................................... 140
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Replacing the Micro GC Portable battery ....................................................... 142 Replacing the Micro GC Portable battery cable fuse .................................... 143 Accessory replacement procedures ................................................................ 144 Replacing the external 10-micron particle filter ................................... 144 Replacing the 2-micron filter in the G2819A heated vaporizer .......... 145 Replacing the 7-micron filter in the G2818A heated regulator ........... 145

Replacement Parts
Power cables and converters ........................................................................... 147 GC modules ......................................................................................................... 148 Accessories and filters ..................................................................................... 151 Cables ................................................................................................................. 152 Plumbing supplies ............................................................................................ 152 Calibration samples ........................................................................................... 153

Site Preparation
Tools and items needed for installation ......................................................... 154 Hardware ..................................................................................................... 154 Other items .................................................................................................. 154 Ventilation requirements .................................................................................. 154 Carrier gases ....................................................................................................... 155 Gas plumbing ...................................................................................................... 155 Compressed gas cylinder safety ............................................................... 155 Installation .................................................................................................. 156 Ensuring gas purity ................................................................................... 157 Connections to the GC ............................................................................... 157 Swagelok connections ....................................................................................... 158

Specifications
Technical specifications .................................................................................... 160 Environmental conditions ................................................................................ 160

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Agilent 3000 Micro GC User Information

Introduction
This document describes the use and maintenance of the Agilent 3000 Micro Gas Chromatograph (GC). The Micro GC is a 1- to 4-channel instrument that performs analyses in seconds rather than minutes or hours. It can be used to analyze natural gas, refinery gases, vent gas, landfill gas, water and soil headspace samples, mine gas, and furnace gas. Additional applications include custody transfer, well logging, environmental screening, storage tank analysis, scrubber analyses, lead detection and monitoring volatile organic compounds (VOC) in waste water. These analyzers are used in combination with the powerful Agilent Cerity Networked Data System for Chemical QA/QC data handling and instrument control software. The complete package is a comprehensive, easy to use gas analysis system.

About your instrument

The instrument uses self-contained GC modules, each consisting of an injector, columns, flow control valving, and a thermal conductivity detector (TCD). Routine replacement of parts such as septa, ferrules, or columns is not required. This eliminates the need for frequent leak testing. Samples are introduced through a 1/16-inch Swagelok connection to the inlet(s) on the front panel. This design eliminates the need for traditional hypodermic syringe injection through septa. The inlet pressure can be nearly atmospheric since an internal vacuum pump connected to the column exit eliminates column back pressure. See Table 1 for a summary of external connections.

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Introduction Serial numbering

Table 1.
Connection

Summary of Connections
Notes 1/16-inch Swagelok 0 to 210 kPa (0 to 30 psi) 35 to 69 kPa (5 to 10 psi) External 10-micron particle trap standard. (not used with accessories G2816A, G2817A, G2818A, G2819A, G2845A, or G2846A) Cerity Chemical for 3000 Micro GC (G2801A/G2805A option 601) BTU/Calorific Report (G2801A/G2805A option 602, G2814AA) Refinery Gas Report (G2802A option 603, G2815AA) 1/8-inch Swagelok 1/8-inch Luer-lock

Input fitting(s) Input pressure Range Recommended Sample filtration

Instrument control

Carrier gas inlet fitting Vent gas fitting

Due to the micromachined construction of the GC module components, introduce only clean gases or vapors; and avoid aerosols, condensable vapors, liquids and solid particles. Install an appropriate sample filter or conditioner. An external 10-micron filter is shipped with the instrument from the factory, and must be used unless replaced by another filter or sample conditioner. Contact your local Agilent Technologies sales representative for details on available accessories. You control the Micro GC through a standard LAN connection, either directly from a computer using a cross-over cable or through a local LAN. The Agilent 3000 control software handles all experimental settings, data collection, and data analysis.

The Agilent 3000 Micro GC Portable

High-speed gas analysis is possible in the field with the Agilent 3000 Micro GC Portable. The Micro GC Portable is a completely self-contained, miniaturized gas chromatograph designed specifically for fast, accurate analysis. Each Micro GC Portable contains one or two GC modules and an internal carrier gas cylinder. Rechargeable battery packs and automobile power cables are also available for power sourcing in the field.

Serial numbering
Agilent applies serial numbers to the instrument and to each GC module inside it. These serial numbers may be requested whenever you contact Agilent for service or repair.
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Introduction Serial numbering

The instruments serial and model numbers are located on a label on the back panel of the Micro GC and the GC module identification are on another label located on top of the GC module. See Figure 1. For a complete listing of GC module types and part numbers, see GC modules on page 148.

OUT Channel A Reference Analyical Channel B

Sample

LAN
Made in U. S. A.

2-channel
CARRIER
2 1

GC model number and serial number

RS-232

IN

REMOTE

19-24 70 VA

Channel D

Channel C

Channel B

Channel A LAN

Reference Analyical

Reference Analyical

Reference Analyical

Reference Analyical SAMPLE OUT RS 232

4-channel

COLUMN VENTS

REMOTE

19-24 125 VA

CARRIER IN
Made in U. S. A.

OUT
CARRIER FILL 1800 PSI MAX Sample CARRIER OUT Reference Analytical
G2805A

Channel A

LAN
Channel B

Made in U. S. A.

Portable
DANGER - EXPLOSION HAZARD. DO NOT FILL TANK WITH HYDROGEN. 2

RS 232
CARRIER

REMOTE 1 IN

15 Vdc 130 VA

GC Module identification

Top view of a G2801A GC, with top cover removed. Others are similar.

Figure 1.

Serial and model number locations

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Introduction Safety information

Safety information
A gas chromatograph can be hazardous. The following general warnings apply to the instrument as a whole. Specific warnings are provided throughout this document when a possibly hazardous operation is discussed.

WARNING

Shock hazard. To avoid injuries, always disconnect the power cable before replacing or touching any components.

WARNING

Hot surfaces. Many parts of the GC operate at temperatures high enough to cause serious burns. These parts include, but are not limited to: The inlet port The inlet manifold The GC module The column nuts attaching the module to an inlet or a vent

Extreme care should be taken to avoid these heated surfaces. Column temperatures can be maintained as high as 180C. Do not operate the instrument with the GC module disassembled.

WARNING

Hydrogen (H2) gas can present an explosion hazard when not handled properly. Leaks, when confined in an enclosed space, may create a fire or explosion hazard. In any application using hydrogen, leak test all plumbing connections before operating the instrument. Always turn off the hydrogen supply at its source before working on the instrument. Do not turn on hydrogen carrier flow with a GC module disassembled. Hydrogen is flammable. Vent exhaust gases safely.

WARNING

Never fill the 3000 Micro GC Portable internal gas cylinder with hydrogen. A high-pressure hydrogen leak inside the instrument can cause an explosion hazard.

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Introduction Contacting Agilent

WARNING

If pressure in the Micro GC Portable internal carrier gas tank exceeds 12,405 kPa (1800 psi) during filling, you will hear a relief valve on the Cylinder Recharging Kit open. A loud startling noise continues until the supply tank pressure is at 12,405 kPa (1800 psi). The 3000 Micro GC Portable is equipped with a refillable carrier gas cylinder. This cylinder is United States Department of Transportation rated at 1800 psig (12,405 kPa) maximum with a 5 year Hydrostat approval.

WARNING

Electrostatic discharge is a threat to electronics. Electrostatic discharge (ESD) can damage the printed circuit boards in the GC. If you must handle a board, wear a grounded wrist strap and handle the board only by its edges.

Contacting Agilent
To contact Agilent, call your local sales representative, or visit us on the web at www.agilent.com/chem, or call us at 1.800.227.9770 (U.S. or Canada).

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Installation
Before starting, prepare the site for installation and prepare the carrier gas supplies as described in Site Preparation on page 154.

Remove any caps and connect your gases

At the factory, your instrument was configured to use helium as the carrier gas in order to run the checkout method. If you choose to use another carrier gas, first install the instrument and verify performance as described here, then reconfigure your instrument according to the instructions in To set the carrier gas type on page 133.

To use a benchtop carrier gas:

1. Remove any caps.

Analytical column vents Reference column vents

OUT

Sample gas vents

Channel A Sample Reference Analyical Channel B

2-channel Micro GC (Micro GC Portable is similar)

CARRIER

Carrier inlets

IN

REMOTE

Analytical column vent

Channel D Channel C Channel B Channel A

Reference column vent

Reference Analyical Reference Analyical Reference Analyical Reference Analyical SAMPLE OUT R COLUMN VENTS

Sample gas vents

2 1 REMOTE 19-2 1 CARRIER IN

Carrier inlets 4-channel Micro GC

Figure 2.

Gas connections
Agilent 3000 Micro GC User Information 13

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Installation Remove any caps and connect your gases

2.

If you are using a Micro GC Portable, make sure the carrier valve on the front panel is set to OFF. Disconnect the carrier jumper tube from the CARRIER 1 input fitting.
Front

ON

Carrier valve

200

1800 2000

OFF
REFILL

CARRIER

CARRIER

3000 Micro GC

Back

OUT
CARRIER FILL 1800 PSI MAX Sample CARRIER OUT Reference Analytical
G2805A

Channel A

LAN
Channel B

Made in U. S. A.

RS 232

Carrier jumper tube

CARRIER DANGER - EXPLOSION HAZARD. DO NOT FILL TANK WITH HYDROGEN. 2 IN 1

REMOTE

15 Vdc 130 VA

Figure 3.

Micro GC Portable front/back

3. Install one carrier gas filter (3150-0602) on the supply tubing for each carrier gas used. See Figure 4. Install the carrier gas filter near the GC fitting to maximize its effectiveness. Agilent recommends using a cutoff valve (not provided) as shown below for ease of maintenance.

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Installation Remove any caps and connect your gases

For details on making Swagelok connections, see Swagelok connections on page 158. Use the carrier gas filter only for low pressure (< 690 kPa/100 psi) gases.
Cutoff valve (not provided)

3150-0602 Arrow points to GC < 15 cm (6 in.) preferred

Figure 4.

Installing the carrier gas filter on the supply tubing

WARNING

Vent noxious gases safely. 4. 5. Purge supply lines. Connect your gases. Vent noxious gases safely. The fittings labeled Analytical Out and Sample Out vent the sample gas. The checkout method requires helium as the carrier gas.

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Installation Remove any caps and connect your gases

To use the internal carrier gas cylinder (Micro GC Portable):

1. Remove any caps.

Analytical column vents Reference column vents Sample column vents

OUT
CARRIER FILL 1800 PSI MAX Sample CARRIER OUT Reference Analytical
G2805A

Channel A

LAN
Channel B

Made in U. S. A.

Internal carrier gas cylinder output Carrier jumper tube

RS 232
CARRIER DANGER - EXPLOSION HAZARD. DO NOT FILL TANK WITH HYDROGEN. 2 IN 1

REMOTE

15 Vdc 130 VA

Carrier in

Figure 5.

Gas connections (Micro GC Portable)

Note

See Filling the internal carrier gas cylinder on page 52 for information on how to fill the internal cylinder. 2. 3. Make sure the carrier switch on the front of the GC is set to OFF. Connect the CARRIER OUT port to the CARRIER IN port with the supplied carrier jumper tube as shown in Figure 5. Use CARRIER IN port 1 if your Micro GC Portable has 2 ports available. Set the carrier switch on the front of the GC to ON. Connect your sample gases. Vent noxious gases safely. The fittings labeled Analytical Out and Sample Out vent the sample gas. The checkout method requires helium as the carrier gas.

4. 5.

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Installation Set gas source pressures and check for leaks

Set gas source pressures and check for leaks

Check all external connections for leaks.
Carrier gas Helium* Hydrogen** Argon Nitrogen Required delivery pressure 552 14 kPa (80 2 psi) 552 14 kPa (80 2 psi) 552 14 kPa (80 2 psi) 552 14 kPa (80 2 psi)

* Required for checkout ** Never fill the Micro GC Portable internal carrier gas cylinder with hydrogen

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Installation Connect all cables

Connect all cables

1. Connect the crossover cable (part number 5183-4649) between the PC and GC.

Power and communications

Channel A

Sample

Reference

Analyical Channel B

LAN RS-232

OUT

Carrier

Carrier

B
IN

REMOTE

19-24 70 VA

Power cord and converter

Crossover cable 5183-4649

Standalone installation

Remote start/stop cable G2801-60618

Crossover cable 5183-4649

Figure 6.

Cable connections (2-channel unit shown. Others are similar.)

2. If available, connect the remote start stop cable (G2801-60618) to the GC. 3. For details on the remote start stop connector, see The Remote connector on page 31.

Connect the power cord and converter to the GC.

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Installation Turn on the GC

Turn on the GC
Channel B inlet Channel A inlet

On/off switch

3000A Micro GC

Figure 7.

Agilent 3000 Micro GC (2-channel, two inlet unit shown)

The instrument will beep once at power on, then beep twice after it has successfully passed its internal tests.

Set IP address
The GC can be connected directly to the PC using a crossover cable, or used on a LAN. In either case, you must first connect the GC to the PC using a crossover cable. You will need to change your PCs current IP address to do this. After establishing communication and performing the checkout test(s), you can either continue to use the GC and PC as set-up, or reset the GC and PC IP addresses to conform to your LAN. Set the PC IP address as follows: 1. Windows 2000: Select Start / Settings / Network and Dialup Connections. Select the Properties of the local area connection, then get the properties of Internet Protocol (TCP/IP). Windows XP: Select Start / Control Panel. From the Control Panel's category view, select Network and Internet Connections / Network Connections / Local Area Connector. Select the General tab and click Properties. Highlight Internet Protocol (TCP/IP) and select Properties.

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Installation Set IP address

Figure 8.
2. 3.

Setting your computer IP address for initial communication

If you intend to install the GC on a LAN, record all of your PCs current IP address settings so that you can reconnect it to your LAN. For the first use, set your computers IP address and Subnet Mask to the settings shown in Table 2 below. Change them if needed. You must use these addresses to connect to the instrument for the first time. The gateway and DNS server entries are not used for direct connection.

Table 2.

Default Computer and GC Address Settings

Computer GC 10.1.1.101 255.255.255.0

IP Address Subnet mask Gateway DNS Server

10.1.1.100 255.255.255.0

4.

Select OK and reboot your computer if prompted.

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Installation Verify gas configuration set to helium

Once the computers IP address is set, verify the GCs IP address. Open the Command Prompt [C:\>] and enter ping 10.1.1.101. You should see a reply similar to Figure 9 below.

Figure 9.

Ping reply from 10.1.1.101

If the GC does not reply, see Verify communications on page 101. If using the GC with this direct connection, the GCs IP address is set.

Verify gas configuration set to helium

The checkout method requires helium as the carrier gas. Verify that your instrument is configured for helium carrier gas as follows: 1. Start a web browser and enter the current GC IP address (10.1.1.101) into the address line. Your browser will connect to the GC.

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Installation Verify gas configuration set to helium

Figure 10. Agilent 3000 web page

2. Select tab Gas Type. You will get a screen similar to that shown in Figure 11 below. The current gas configuration for installed modules is shown. (Note that in the Used By column, m1 and m2 represent channels A and B respectively. Entries m3 and m4 represent channels C and D, if installed.)

Figure 11. Representative screen for current gas configuration

3. If the current gas type shown for each GC module is not helium, change the carrier gas type to helium as described in To set the carrier gas type on page 133.

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Installation Install Agilent Cerity Networked Data System for Chemical QA/QC software

Install Agilent Cerity Networked Data System for Chemical QA/QC software
Refer to the instructions included on the program CD-ROM. After installing the program and any applications, configure the 3000 GC in the ConnectAdmin Utility and enable it for use by Cerity Chemical.

Install external inlet filter

1. Inspect the external filter assembly and verify that the filter disk is in place. If not, place a filter disk (part no. 5183-4652) in part A and assemble the filter halves. (See page 144 for more information.) Install the filter assembly on the GC inlet with the double-sided ferrule placed between the filter body and the GC inlet. Use a 5/16-inch wrench on part A of the filter to tighten it 1/4-turn past finger-tight.

2.

Inlet filter assembly

Figure 12. Inlet filter assembly installed on Agilent 3000 Micro GC

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Installation Connect checkout gas cylinder to instrument

Connect checkout gas cylinder to instrument

WARNING Caution
The calibration sample contains flammable gases. Vent safely. Do not overtighten the external filter onto the GC. Use a second wrench to secure the external filter when installing the sample line. 1. Connect the checkout gas cylinder to the external filter assembly on the instrument. For details, see Connecting the checkout sample to the GC on page 57.
Pressure regulator 1/4-inch NPT fitting

Purge the sample line for 2 minutes before assembling to the GC.
1/16-inch Swagelok fitting and inlet filter assembly

Checkout sample

1/16-inch Swagelok nut and ferrule set Filter assembly Dual-end ferrule

Figure 13.

Connect checkout sample (2-channel GC shown)

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Installation Set method. Start run. Verify chromatographic peaks.

Set method. Start run. Verify chromatographic peaks.

1. 2. Set the checkout method conditions. See Create the checkout method on page 59. Using the Agilent control software, run the checkout sample. 3. If your micro GC has two inlets, run the checkout method separately for each. Refer to the control softwares help and tutorials for details on its use.

Verify chromatographic peaks. Refer to the checkout chromatogram for your checkout sample type and column type:
For column option... OV-1 OV-1701 MolSieve 5A PLOT Alumina PLOT PLOT Q PLOT U Stabilwax DB Alumina PLOT, 10 m 0.32 mm Alumina PLOT, 1 m 0.32 mm MolSieve 5A PLOT, 10 m 0.32 mm PLOT U, 3 m 0.32 mm PLOT U, 8 m 0.32 mm PLOT Q, 1 m 0.32 mm and Injector type... Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable 0.4 L Backflush 1.0 L Backflush 1.0 L Backflush See page 61 page 65 page 67 page 69 page 71 page 73 page 75 page 77 page 79 page 81

4.

Repeat steps 1 through 3 for each inlet fitting in your instrument.

Finish up
If necessary, remove the external 10-micron sample filter and install the appropriate Agilent sample conditioner for your application. See Table 1. If you want to use a carrier gas other than helium, configure your instrument to use that gas as described in To set the carrier gas type on page 133.
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Installation Finish up

Connecting to a LAN
To use the system on a LAN, first obtain the IP address, Subnet mask, and default Gateway for the GC from your local LAN administrator to avoid conflicts with other devices on the network (including printers). The LAN administrator may also add DNS (Domain Name System) and WINS (Windows Internet System) addresses if desired. They are used to access the web or to browse a network that uses DHCP (Dynamic Host Control Protocol). If using DHCP, the GCs must be assigned fixed IP addresses. 1. 2. Start a web browser, and enter the current GC IP address into the address line. Your browser will connect to the GC. See Figure 10. Select the IP Config tab. The screen displays the current IP communication settings for the GC.

Figure 14. Typical screen displaying current IP settings

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Installation Finish up

3.

Select Make changes... When prompted, enter ipconfig as the user name, and ipconfig as the password. You will get a screen similar to Figure 15.

Figure 15. Example screen for changing IP settings

4. Enter the new Host Name, Domain Name, IP address, Subnet Mask, Gateway Address, and DNS server information. 5. Print this screen using the web browser to make a record of this information. Keep the printout in a safe, convenient place.

Select Submit. An information screen appears.

Caution

Do not turn off the GC yet. The changes can be lost. After selecting the Shutdown or Restart button, it takes 3 minutes for the GC to complete the changes.

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Installation Finish up

6.

Select Shutdown. The GC will respond that it is shutting down. Wait 3 full minutes. (Note: new links are shown on screen but will not work until you complete the next steps.)

7. 8. 9.

Turn off the GC. Reconfigure your PCs IP address for LAN use. Disconnect the crossover cable and connect the GC and the PC to the LAN using standard LAN cables (part no. G1530-61485).

LAN hub (customer provided)

LAN cables G1530-61485 Simple LAN installation

Figure 16. A typical LAN cabling setup

10. Reboot the PC and turn on the GC. 11. After approximately 3 minutes, the GC will beep. Reconnect to the GC using the new IP address. Open the Command Prompt [C:\>], and use the ping command to verify the connection. For example, if your new GC IP address is 10.1.1.111, enter ping 10.1.1.111.

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Installation Finish up

You should see a reply similar to that shown in Figure 9. If the GC does not reply, see Verify communications on page 101. 12. Once communication is established, open the Cerity Chemical ConnectAdmin Utility and update the instruments entry to the new IP address. After enabling the instrument in ConnectAdmin, it should appear online in Cerity Chemicals Instrument View.

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Understanding the GC
The Agilent Micro GC 3000 is a compact and efficient analytical tool, using well established chemical separation and detection principles.

The GC module
The heart of the instrument is the GC module. It includes a heated injector, sample column, reference column, thermal conductivity detector (TCD), electronic pressure control (EPC) hardware, gas flow solenoids, and control board. Operation can be better understood by examining what takes place during an analysis. The major steps include: 1. 2. 3. Injection Separation Detection

Injection
The gaseous sample enters the Micro GC heated manifold. The manifold regulates the samples temperature and directs it into the injector. The injector then drives the sample onto the column, while a vacuum pump helps draw the sample through the system.

Separation
After passing through the injector, the sample gas enters the column, which separates it into its component gases in typically less than 180 seconds. Gas chromatography works because different volatile molecules have unique partitioning characteristics between the column substrate and the carrier gas. These differences allow for component separation and eventual detection. In practice, achieving quality separations involves understanding and optimizing the effect of many variables including: Choice and thickness of column coating Column length and diameter Choice of carrier gas and flow rate Oven temperature

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Understanding the GC Electronic Pressure Control (EPC)

Detection
After separation on the column, the sample gas flows through a TCD. Carrier and sample gases separately feed this detector, each passing over different hot filaments. The varying thermal conductivity of sample molecules causes a change in the electrical resistance of the sample filaments when compared to the reference or carrier filaments.

Electronic Pressure Control (EPC)

The instrument precisely controls the temperature, pressure, and flow electronically during the run and between runs, without operator intervention.

The Remote connector

Normally, using Cerity Chemical control, runs begin and end automatically depending on the GCs Work List status (started, stopped, or paused) and GC readiness. To have an external device start or cancel a run: 1. 2. 3. Install the Digital I/O module accessory, G2847A, if needed. (It is installed if the GC has a REMOTE connector.) Determine which control mode is appropriate for your installation and implement it. See Selecting a control mode on page 31. In Cerity Chemical, enable Wait for Instrument Start for each sample requiring remote start/cancel functionality.

Selecting a control mode

There are three equivalent cabling circuits which can be used to implement remote start/cancel functionality. There are two identical input and output circuits. Figure 17 shows each of them alongside the GCs internal remote

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Understanding the GC The Remote connector

start/cancel circuitry. (See Figure 18 on page 33 for the connector pin functions.)
Input 1 or 9 316 5 VDC

2 or 10

162 3 or 11

4 or 12 Logic input Normally open Normally closed 121 GC remote circuity

Possible customer cabling circuity from connecting controller Output 5 or 6

7 or 8 For logic out

10 k

5 VDC

For logic out

14 or 15

13

Possible customer cabling circuitry from GC remote

GC remote circuitry

Figure 17.

Remote start cancel circuitry

Logic input This option requires a logic signal of 35 VDC across pins 2 and 3 to provide 520 mA of current to start a run. A similar signal across pins 10 and 11 provides a CANCEL input.

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Understanding the GC The Remote connector

Normally open This option uses the GCs internal 5 VDC signal and one jumper. To start a run, close the switch across pins 3 and 4. To cancel a run, close the switch across pins 10 and 11. Normally closed This option uses the GCs internal 5 VDC signal and two jumpers. To start a run, open the switch across pins 2 and 3. To cancel a run, open the switch across pins 10 and 11. Figure 18 lists the connectors pin functions.

Pin

Function Provides 5 milliamps for remote input REMOTE_START input REMOTE_START input Variable GND Provides 5 V pull up for logic output Provides 5 V pull up for logic output Contact closure output FAULT_OUT* Contact closure output READY_OUT Provides 5 milliamps for remote input REMOTE_CANCEL input REMOTE_CANCEL input Variable GND GND Contact closure output FAULT_OUT*

Wire color, cable G2801-60618 Black Brown Red Green Orange Blue White/black Red/black Green/black Orange/black Blue/black Black/white Red/white Green/white

15

1 2 3 4 5 6

7 8 9 10 11 12 13 14

* Not implemented

Figure 18.

Remote start/cancel connector pin outputs

How the GC and Cerity Chemical respond to and signal remote events
The 3000 Micro GCs remote start/cancel behavior depends heavily on the use of Cerity Chemical. Table 3 lists how the GC and Cerity Chemical respond to remote start, remote cancel, and Cerity commands. It also lists the output response available across the READY_OUT connector pins. Note this table assumes the user adds all Cerity Chemical samples to the GCs Work List with Wait for Instrument Start enabled. If a sample does

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Understanding the GC The Remote connector

not require Wait for Instrument Start, the remote start/cancel functionality is not enabled.

Table 3.
Remote start

Summary of Remote Start and Cancel Events and Behaviors

State or Response Cerity Chemical status No samples in Work List Sample(s) added to Work List, no run in progress Sample(s) in Work List, no run in progress Sample(s) in Work List, no run in progress Sample(s) in Work List, user pauses/ aborts Work List Running a sample, collects data User aborts current sample User pauses Work List GC state or action Cerity Chemical response Waits for instrument Data collection starts Pauses Work List Work list paused GC Output READY_OUT signal circuit Is Open Closes Remote cancel

Remote Input to GC*

Before a run has started No No Idle Prepares for run, then waits for remote start Starts run Becomes idle Becomes idle

Yes No No

No Yes No

Opens Opens Opens

After a run has started No Running a sample After current sample, becomes idle Completes current sample, then becomes idle Sample aborted, Work List pauses Pauses Work List after current sample Opens Opens

Opens

* A dash () indicates the signal input is ignored during the given GC state.

Note: When running a Cerity Chemical sample with Wait for Instrument Start enabled, the GC monitors the REMOTE connector. A 5 ms contact closure in the REMOTE_START circuit starts the GC run and Cerity Chemical begins data acquisition. When the GC is ready to begin a run but a start signal has not been received, the READY_OUT contacts are closed. They remain closed until the runs starts or the run is cancelled/aborted. If the user aborts the instruments Work List in Cerity Chemical, the GC opens the READY_OUT relay to signal the connected device(s) that the run was terminated. The current sample will be aborted and the Work List pauses.

For complete information about Cerity Chemicals run control (the Work List, aborting a sample, etc.) refer to its online help system.

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Operation
Getting started
Learning the control software
Before making your first run, learn how to use your Agilent control software. The software contains an extensive help system and self-directed tutorials to teach you the fundamentals. Because the software controls all GC functions and performs all analyses, understanding its use is essential.

How to connect a sample to the instrument

Sample delivery methods include high- and low-pressure vessels and transfer lines connected directly to either the filter on the micro GCs front input fitting or to the input fitting of an installed accessory. Because the GC draws samples at different times to purge the internal flow paths or perform the run, do not use gas-tight syringes. Use containers that can supply sample on demand. If using a sample vessel, see Preparing the sample on page 38 for information about how to prepare and store the sample. If using a transfer line or other delivery method, see Table 5 for the sample types and input pressure for each filter or accessory.

You will need to provide appropriate mounting hardware to connect the sample to the GC or accessory.

Overview of operation
The following steps describe the basic tasks required to run a sample. 1. 2. 3. 4. Create the method. See Creating a method on page 36. Install either the external filter or accessory appropriate for the sample type to test. See Installing a sample filter or conditioner on page 37. Prepare the sample for use. See Preparing the sample on page 38. Micro GC Portable: slowly turn the Carrier knob on the front panel to On.

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Operation Creating a method

5.

Connect the sample to the instrument/accessory and run it. Instructions vary depending on the type of accessory, if any, installed. Refer to Table 4:

Table 4.
Sample type Clean

Filters and Accessories for Sample Input

Pressure Low Low Accessory required None. Use external filter. G2817A See Running a low pressure, clean gas sample on page 41 Running a low pressure gas sample containing entrained liquids/particles on page 42 Running a high pressure gas sample without entrained liquids/particles on page 43 Running a high pressure gas sample containing entrained liquids/particles on page 44 Running a high pressure gas sample containing C5+ components on page 45 Running a high pressure liquefied petroleum gas (LPG) sample on page 48

Entrained liquids/particles Clean

High

G2815A

Entrained liquids/particles Clean

High

G2816A

High

G2818A (1, 2-channel GC) G2845A (3, 4-channel GC) G2857A (Micro GC Portable) G2819A (1, 2-channel GC) G2846A (3, 4-channel GC) G2858A (Micro GC Portable)

Liquefied petroleum gas (LPG)

High

Creating a method
What is a method?
A method is the set of control and analysis parameters that define your experiment, data analysis, and reporting functions. All methods are created and stored in the Agilent 3000 control software.

Method parameters
To create a method, define the parameters listed below in the control software. Define each channel. These parameters will vary based on your GC module configuration. Sample Inlet Temperature Injector Temperature, Sampling Time, Inject Time, and Backflush Time Column Temperature and Pressure Run Time

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Operation Installing a sample filter or conditioner

Post Run Time and Pressure Pressure Equilibration Time Detector Data Rate The detector can capture data at four data rates: 20 Hz, 50 Hz, 100 Hz, and 200 Hz. Use lower rates to characterize broad peaks and higher rates to define sharp peaks. Detector Sensitivity

Refer to the Agilent control software for descriptions of each parameter, and Create the checkout method section of this document for more details.

Installing a sample filter or conditioner

Because contaminantsespecially particulates and condensing aerosolscan damage your instrument, Agilent recommends using an appropriate filter or sample conditioner at all times. Table 5 lists the typical usage and filtration capabilities of the standard filter and available accessories.

Table 5.

Sample and Filter/Conditioner Options

Input pressure to accessory 0 to 210 kPa (0 to 30 psi) 70 to 345 kPa (10 to 50 psi) 345 to 6900 kPa (50 to 1000 psig) < 3450 kPa (< 500 psig) Sample container/ delivery Any Any Any Any Particle filtration (microns) 10

Type Standard external filter Gas-liquid separator Pressure reducer Gas-liquid separator and pressure reducer Heated regulator for sampling Heated vaporizer for LPG sampling

Sample condition Relatively clean and dry Entrained liquids and particles C5+ components < 0.5 mole % Entrained liquids and particles, C5 + components < 0.5 mole % C5 + components > 0.5 mole %

Part number G2801-60980 (Figure 72) G2817A (Figure 24) G2815A (Figure 25) G2816A (Figure 26)

< 3450 kPa (< 500 psig)

Transfer line or high-pressure vessel High-pressure vessel

G2818A, G2845A or G2857A (Figure 27) G2819A, G2846A or G2858A (Figure 29)

1380 to 5500 kPa (200 to 800 psig)

Liquefied petroleum gas (LPG)

Refer to Accessories and filters on page 151 for replacement filter information.

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Operation Preparing the sample

Preparing the sample

Follow the procedures below if using a sample vessel to store the sample for use. Note that sample vessels used for Agilent Accessories G2818A/G2845A/ G2857A, heated regulator, and G2819A/G2846A/G2858A, heated vaporizer, require special preparation.

Caution

The sample must be clean and dry. While the accessorys filter will remove many particulate contaminants, samples containing aerosols, excessive amounts of particulate matter, high concentrations of water, and other contaminants can damage your instrument. The sample is stored at high pressure. Do not expose the sample vessel to excessive heat or flame. Vent the high and low pressure exhausts to a safe environment, such as a fume hood or dedicated exhaust.

WARNING

Assemble the sample vessel

For GC input fitting, external filter, and Accessories G2815A (pressure reducer), G2816A (gas-liquid separator and pressure reducer) and G2817A (gas-liquid separator) Set up the sample vessel with appropriate hardware to mate with the GC or accessory input fitting:
GC or Accessory GC input fitting or external filter assembly G2815A pressure reducer G2816A gas-liquid separator and pressure reducer G2817A gas-liquid separator Fitting 1/16-inch Swagelok 1/8-inch Swagelok 1/8-inch NPT (male) 1/16-inch stainless steel tubing

For Accessory G2818A/G2845A/G2857A, heated regulator Set up the sample vessel with ball valve stopcocks as shown in Figure 19. The heated regulator requires a Swagelok QC4 stem connection. Use the stem assembly provided with your accessory. This stem assembly accepts a 7/16-inch threaded male connector.

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Operation Preparing the sample

Sample vessel (user-supplied) Ball valve stop-cocks (user-supplied)

7/16-inch male threaded fitting to mate with Swagelok QC4 quick disconnect stem assembly provided with your accessory

Figure 19. Typical sample vessel setup for G2818A/G2845A/G2857A

For accessory G2819A/G2846A/G2858A, heated vaporizer Set up the sample vessel with ball valve stopcocks as shown in Figure 19. Use a 7/16-inch female threaded fitting to mate with the filter disconnect assembly.

Sample vessel (user-supplied) Ball valve stop-cocks (user-supplied)

7/16-inch female threaded fitting to mate with filter disconnect assembly

Figure 20. Typical sample vessel setup for G2819A/G2846A/G2858A

Collect the sample

For accessory G2818A/G2845A/G2857A, heated regulator a. b. Collect natural gas samples per Gas Processors Association (GPA) Standard 2166-861. Store at < 3450 kPa (< 500 psig) in the sample vessel.

For accessory G2819A/G2846A/G2858A, heated vaporizer a. b. Collect LPG samples per Gas Processors Association (GPA) Standard 2140-972. Store at 1380 to 5500 kPa (200 to 800 psig) in the sample vessel.

For other accessories/fittings Collect and store the sample at a pressure compatible with the accessory or GC fitting. See Table 5 on page 37 for values.

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Operation Preparing the sample

Prepare the sample vessel for connection to the GC

Accessory G2818A/G2845A/G2857A, heated regulator a. If desired, create a short transfer line using stainless steel tubing. The transfer line requires a male 7/16-inch threaded fitting to mate with the Swagelok QC4 stem assembly provided with your accessory. Install the stem assembly onto the sample vessel or transfer line. See Figure 21.
Stainless steel tubing Accepts 1/4 male NPT fitting on heated regulator quick disconnect

b.

Transfer line assembly (user-supplied)

Figure 21. Transfer line installed on sample vessel

Accessory G2819A/G2846A/G2858A heated vaporizer Install the filter disconnect assembly onto the sample vessel. See Figure 22. Use only the filter trap provided in the disconnect assembly. Agilent recommends that you avoid installing any other scrubbers, traps, or devices in-line from the sample vessel to the heated vaporizer.

Filter disconnect assembly

Figure 22. Filter disconnect assembly installed

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Operation Running a low pressure, clean gas sample

Running a low pressure, clean gas sample

For clean, low pressure samples, Agilent recommends using the standard 10-micron filter assembly for filtration. 1. 2. 3. Turn on the GC. Check that the carrier gas supply is sufficient to run all of your samples. If using a sample vessel, prepare the sample. See Preparing the sample on page 38. 4. If not installed, install the external filter assembly. For sample source pressures above 210 kPa (30 psi), install a pressure regulator as shown below. Connect the sample container or gas source to the GC.

Set input pressure to 0 to 210 kPa (0 to 30 psi) Preferred pressure: 35 to 70 kPa (5 to 10 psi)

Safety stand for gas cylinder

Dual-end ferrule

External filter assembly G2801-60900

Figure 23.

Example sample connection

5. 6. Open the sample vessel valve. 7. 8. Adjust the input pressure to < 210 kPa (< 30 psi). Refer to the programs help system for method and run information. Use the control software to load the method and perform the analysis.

When the analysis is complete, close the sample vessel valve and disconnect the vessel from the instrument. Repeat steps 3 to 7 to run the next sample.

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Operation Running a low pressure gas sample containing entrained liquids/particles

Running a low pressure gas sample containing entrained liquids/particles

1. Check that Accessory G2817A, gas-liquid separator, is installed.

To GC

Vent tubing Sample input tubing

(Mounting bracket not shown)

Figure 24. The G2817A gas-liquid separator

2. 3. 4. 5. Turn on the GC. Check that the carrier gas supply is sufficient to run all of your samples. If using a sample vessel, prepare the sample. See Preparing the sample on page 38. Connect the sample container or gas source to the GC. For sample source pressures above 345 kPa (50 psi), install a pressure regulator between the sample source and the gasliquid separator. Adjust the input pressure to between 70 to 210 kPa (10 to 30 psi). Refer to the programs help system for method and run information.

6. 7.

Open the sample vessel valve. Use the control software to load the method and perform the analysis.

8. 9.

When the analysis is complete, close the sample vessel valve and disconnect the vessel from the instrument. Repeat steps 4 to 8 to run the next sample.

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Operation Running a high pressure gas sample without entrained liquids/particles

Running a high pressure gas sample without entrained liquids/particles

1. Verify that Accessory G2815A, pressure reducer, is installed.

Adjustment knob

Sample in

To input fitting on GC

Vent

(Mounting bracket not shown)

Figure 25. The G2815A pressure reducer

2. 3. 4. 5. 6. 7. Turn on the GC. Check that the carrier gas supply is sufficient to run all of your samples. If using a sample vessel, prepare the sample. See Preparing the sample on page 38. Connect the sample container or gas source to the sample fitting on the pressure reducer accessory. See Figure 25. Open the sample vessel valve. Use the control software to load the method and perform the analysis. 8. 9. Refer to the programs help system for method and run information.

When the analysis is complete, close the sample vessel valve and disconnect the vessel from the instrument. Repeat steps 4 to 8 to run the next sample.

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Operation Running a high pressure gas sample containing entrained liquids/particles

Running a high pressure gas sample containing entrained liquids/particles

1. Check that Accessory G2816A, gas-liquid separator, is installed.

Adjustment knob

To input fitting on GC

Sample input fitting

Figure 26. G2816A Gas-liquid separator and pressure reducer

2. 3. 4. 5. 6. 7. Turn on the GC. Check that the carrier gas supply is sufficient to run all of your samples. If using a sample vessel, prepare the sample. See Preparing the sample on page 38. Connect the sample container or gas source to the sample input fitting on the gasliquid separator. See Figure 26. Open the sample vessel valve. Use the control software to load the method and perform the analysis. 8. 9. Refer to the programs help system for method and run information.

When the analysis is complete, close the sample vessel valve and disconnect the vessel from the instrument. Repeat steps 4 to 8 to run the next sample.

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Operation Running a high pressure gas sample containing C5+ components

Running a high pressure gas sample containing C5+ components

This procedure applies to samples from transfer lines or high pressure sample vessels using an Agilent heated regulator accessory:
3000 GC type 1 or 2-channel GC 3 or 4-channel GC Micro GC Portable Accessory G2818A G2845A G2857A

The accessories are the same except for their mounting brackets.

Using a sample vessel

1. Verify the heated regulator accessory is installed.
Stainless steel tubing (user supplied)

Sample vessel stopcock Quick disconnect fitting Sample vessel Low pressure vent tubing to vent

Relief valve

High pressure vent tubing to vent

Figure 27. Sample vessel connected to G2818A heated regulator and 2-channel Micro GC via quick disconnect fitting
2. 3. 4. Turn on the GC and the heated regulator accessory and allow approximately 30 minutes for it to stabilize at operating temperature. Check that the carrier gas supply is sufficient to run all of your samples. Prepare the sample vessel. See Preparing the sample on page 38.

Caution

Make sure that the sample vessel stopcock is closed and the relief valve is turned fully to Sample (closed).
Agilent 3000 Micro GC User Information 45

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Operation Running a high pressure gas sample containing C5+ components

5. 6. 7.

Connect the sample vessel to the quick disconnect. You may need to apply significant pressure. See Figure 27. Open the stopcock on the sample vessel. Smoothly turn the relief valve toward Vent until a small but steady flow is vented, and allow the sample to purge the line for approximately 30 seconds. Turn the relief valve to Sample and allow the system to purge for several minutes. Use the control software to load the method and perform the analysis. Refer to the programs help system for method and run information.

8. 9.

10. When the analysis is complete, close the stopcock on the sample vessel. 11. Turn the relief valve toward Vent to release the back pressure in the system, then close the valve. 12. Remove the sample vessel from the quick disconnect. 13. Repeat steps 4 to 12 to run the next sample.

Using a transfer line or other continuous sample source

1. Verify the heated regulator accessory is installed.

Caution

Agilent recommends using a heated separator and an in-line filter between the sample source and the GC. These devices will eliminate liquids and most particulates from the gas stream. Liquids and particulates can damage the GC. The transfer line should be heated from the sample source to the heated regulator at a temperature of at least 60C, depending upon sample composition and pressure. Shut off the sample stream through your transfer line before connecting it to the GC. Vent the high and low pressure exhausts to a safe environment, such as a fume hood or dedicated exhaust. If you are using the instrument in a vehicle, vent the high and low pressure exhausts outside of the vehicle and away from any sources of ignition. 2. 3. 4. If the sample transfer line is not connected to the heated regulator, shut off any gas flow through it. If needed, purge the transfer line. Prepare the GC for operation and turn it on.

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Operation Running a high pressure gas sample containing C5+ components

5. 6.

Turn on the heated regulator and allow approximately 30 minutes for it to stabilize at operating temperature. If not connected, connect the transfer line to the quick disconnect on the heated regulator. See Figure 28.

Heated transfer line (user supplied)

Quick disconnect fitting on heated regulator Low pressure tubing to vent Relief valve High pressure tubing to vent

Figure 28. Typical setup using a transfer line (2-channel GC shown)

7. 8. Start flow through the transfer line to the instrument when ready. Smoothly turn the relief valve to Vent until a small but steady flow is vented. Vent long enough to allow the sample to adequately purge the transfer line and heated regulator. 9. The purge time required depends on the length of transfer line you are using.

Turn the relief valve to Sample. Refer to the programs help system for method and run information.

10. Use the control software to load the method and perform the analysis.

11. When the analysis is complete, stop flow through the transfer line. 12. Turn the relief valve toward Vent to release the back pressure in the system, then close the valve. 13. Disconnect the transfer line. 14. Repeat steps 2 to 13 to run the next sample.

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Operation Running a high pressure liquefied petroleum gas (LPG) sample

Running a high pressure liquefied petroleum gas (LPG) sample

This procedure applies to high pressure LPG samples using an Agilent heated vaporizer accessory:
3000 GC type 1 or 2-channel GC 3 or 4-channel GC Micro GC Portable Accessory G2819A G2846A G2858A

The accessories are the same except for their mounting brackets. 1. Verify the heated vaporizer for LPG sampling accessory is installed.

WARNING

The LPG sample is stored at high pressure. Do not expose the sample vessel to excessive heat or flame. Vent the high and low pressure exhausts to a safe environment, such as a fume hood or dedicated exhaust

Caution

The sample to the GC must be relatively clean and dry. While the 2-micron filter will remove many particulate contaminants, samples containing aerosols, excessive amounts of particulate matter, high concentrations of water, and other contaminants can damage your instrument. 2. 3. 4. 5. Prepare the GC for operation and turn it on. Turn on the heated vaporizer and allow approximately 20 minutes for it to stabilize at operating temperature. Make sure that the sample vessel stopcock is closed and the relief valve is turned fully to Sample (closed). Connect the sample vessel to the filter disconnect assembly on the heated vaporizer. See Figure 29.

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Operation Running a high pressure liquefied petroleum gas (LPG) sample

Sample vessel

Sample vessel stopcock

Filter disconnect assembly

Quick disconnect fitting Heated vaporizer Low pressure tubing to vent Relief valve

High pressure tubing to vent

Figure 29. Sample vessel installed on G2819A heated vaporizer (2-channel GC shown)
6. 7. Open the stopcock on the sample vessel. Slowly turn the relief valve toward Vent until a small but steady flow is vented and allow the sample to purge the line for approximately 30 seconds. Turn the relief valve to Sample. Use the control software to load the method and perform the analysis. Refer to the programs help system for method and run information.

8. 9.

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Operation The 3000 Micro GC Portable

10. When the analysis is complete, close the stopcock on the sample vessel. 11. Turn the relief valve toward Vent to release the back pressure in the system, then close the valve. 12. Remove the sample vessel from the filter disconnect assembly. 13. Repeat steps 4 to 12 for the next analysis.

The 3000 Micro GC Portable

Because of its internal carrier gas cylinder and battery, the Micro GC Portable requires a few special handling procedures and precautions.

General information and cautions

Never fill the internal carrier gas cylinder with hydrogen gas. Leakage into the enclosed GC can create an explosive mixture. Never operate the Micro GC Portable while standing vertically (on the feet that surround the back panel). The pneumatic valves may not function correctly.

Battery usage information

The LED in the front panel power switch begins to flash when the battery is about 70% discharged. The battery should be recharged (see Charging the battery on page 51) as soon as possible. For longest battery life and optimal performance, observe the following: Whenever possible, operate the 3000 Micro GC Portable with the 15 VDC power supply connected to the power line. This prolongs the life of your internal battery and eliminates the need to recharge it often. When operating the Micro GC Portable, the instrument can run from the internal battery or from the charger. The internal battery provides 34 hours of power when running with moderate chromatographic conditions. When operating at high temperatures, as when "baking out" or "column conditioning," run the GC from the charger to avoid running out of power. Note that in order to protect the battery, the GC shuts down before the battery is completely drained.

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Operation The 3000 Micro GC Portable

To view the battery status

Connect to the GCs web page and select the status view. Note that the displayed battery voltage and percent charge apply only when the GC is not recharging the battery. Cerity Chemical also displays the current battery status.

Charging the battery

The power supply recharges the sealed lead-acid battery inside the 3000 Micro GC Portable whenever the AC power cord is plugged in. The battery will continue to charge while the GC is operating. When operating the Micro GC Portable from the Automobile Power Cable Adapter (part number G2751-60530), be advised that the internal battery will charge only if the input from the vehicles cigarette lighter plug is > 13.5 V. Due to variation in automobile manufacturing, make sure that your automobile can safely supply the maximum power required by the instrument. See Specifications on page 160 for GC power requirements. Also consult your automobiles documentation. An initial minimum charge time of 16 hours is recommended. The charger can be left on indefinitely without harming the battery. Plug the battery charger into the electrical outlet and then into the GC back panel at the location marked 15 VDC to charge the battery.

OUT
CARRIER FILL 1800 PSI MAX Sample CARRIER OUT Reference Analytical
G2805A

Channel A

LAN
Channel B

Made in U. S. A.

RS 232
CARRIER DANGER - EXPLOSION HAZARD. DO NOT FILL TANK WITH HYDROGEN. 2 IN 1

REMOTE

15 Vdc 130 VA

15 VDC power connector

Figure 30. Micro GC Portable back panel

The internal carrier gas supply

The internal carrier gas cylinder connects to the GCs carrier input fitting through the external jumper tube. See Figure 5. Internal pressure regulators

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Operation The 3000 Micro GC Portable

and a check valve ensure a steady 550 kPa (80 psig) carrier gas supply to the GC when the Carrier knob is turned On. The internal carrier gas cylinder requires periodic refilling. Refill the cylinder when the pressure gauge on the front panel reads < 200 psig.

Refill when pressure reads < 200 psig

Figure 31. Micro GC Portable pressure controls

Filling the internal carrier gas cylinder

The Micro GC Portable contains a refillable, high pressure carrier gas supply cylinder. The cylinder volume is 300 mL and will last 35 to 40 hours under normal operating pressure. This cylinder has been certified by the U.S. Department of Transportation (DOT) to a pressure of 1800 psig (12,405 KPa). You will need to refill this cylinder periodically.

WARNING

Never fill the Micro GC Portable internal carrier gas cylinder with hydrogen. Use an external tank to supply hydrogen. High pressure gas is an incredible source of energy and is very dangerous. Filling the tank can be done safely using the Agilent Cylinder Recharging Kit. For your safety, read the following steps before making any connections. Components Required: 1. 2. 3. Agilent 3000 Micro GC Portable Cylinder Recharging Kit (part number PNU-2058) Agilent 3000 Micro GC Portable Bulk carrier gas cylinder (1800 psi/12,405 KPa or less) with CGA-580 fittings

WARNING

Caution

Caution

Agilent Technologies is not responsible for personal injury or damage to equipment as a result of filling gas cylinders with this apparatus.

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Operation The 3000 Micro GC Portable

To avoid injury, proceed as follows: 1. Connect the Cylinder Recharging Kit to the supply tank via the CGA-580 fitting (Figure 32). To avoid leaks tighten the connections securely with an adjustable wrench. Make sure the needle valve of the Cylinder Recharging Kit is fully closed by turning the needle valve clockwise until firmly seated.
To the GC 1800 psi (12,405 KPa) carrier fill port Pressure gauge

2.

Needle valve CGA 580 fitting Supply tank valve

Overpressure vent Supply tank

Transfer line with Swagelok fittings

Figure 32.

Cylinder Recharging Kit setup

3. Partially open the valve on the supply tank. No gas should flow at this point.

OUT

Carrier fill port

CARRIER FILL 1800 PSI MAX Sample CARRIER OUT Reference Analytical

Channel A

LAN
G2805A

Channel B

Made in U. S. A.

RS 232

Carrier jumper tube Carrier in ports

CARRIER DANGER - EXPLOSION HAZARD. DO NOT FILL TANK WITH HYDROGEN. 2 IN 1

REMOTE

15 Vdc 130 VA

Figure 33.

Back of Micro GC Portable

4. Connect the 1/8-inch tube from the Cylinder Recharging Kit to the CARRIER FILL port of the Micro GC Portable back panel via the Swagelok bulkhead fitting (Figure 33). Finger tighten and then loosen 1/4-turn.

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Operation The 3000 Micro GC Portable

5.

Partially open the needle valve on the Cylinder Recharging Kit and listen for gas leaking through the loose 1/8-inch fitting on the back panel. This purges the Cylinder Recharging Kit transfer lines so that no air enters the GC. After the transfer lines have been sufficiently purged (about 15 seconds), tighten the 1/8-inch fitting on the back panel of your Micro GC Portable, then turn the needle valve on the Cylinder Recharging Kit clockwise until seated. If your GC carrier gas cylinder has not been completely emptied or you are not changing to a different carrier gas, go to step 13. Loosen the Swagelok fitting that secures the carrier jumper tube (Figure 33) to the CARRIER IN port on the back panel. This permits purging the refill kit air and optionally purging air or a different carrier gas from your Micro GC Portable carrier gas cylinder. If the Micro GC Portable carrier gas cylinder contains an unwanted carrier gas, you may empty it at this time by slowly turning the Carrier On/Off control valve on the front panel to the On position. When you no longer hear gas escaping, ensure that the Carrier On/Off control valve is set to Off. Slowly open the needle valve on the Cylinder Recharging Kit until you see an increase in pressure on the Cylinder Recharging Kit pressure gauge.

6.

7.

8.

9.

10. When you see an indication of approximately 500 psi, turn the Carrier On/Off control valve to the On position. You will hear a rush of gas escaping from the end of the carrier jumper tube. When the gauge needle returns to zero, turn the Carrier On/Off control valve to the Off position. The pressure gauge needle will begin to rise again. When the gauge needle again reaches 500 psi, repeat the process. For best results, the GC carrier gas cylinder should be purged, as described above, a minimum of three times. 11. Close the needle valve on the Cylinder Recharging Kit. 12. Tighten the Swagelok connection between the Carrier Jumper Tube (Figure 33) and the Carrier In port on the GC back panel. 13. Observe the pressure gauge in the Cylinder Recharging Kit. Partially open the needle valve on the Cylinder Recharging Kit. When the pressure on the gauge reads 1500 to 1800 psig, close the needle valve on the Cylinder Recharging Kit. Do not exceed 1800 psig (12,405 kPa).

WARNING

If pressure in the GC tank exceeds 1800 psig/12,405 KPa during filling, you will hear a relief valve on the Cylinder Recharging Kit burst. A loud startling noise continues until the supply tank pressure is at 1800 psig/12,405 KPa. 14. Completely close the valve on the supply tank and disconnect the 1/8 inch tube from the back panel of the GC.

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Operation Shutting down the GC

15. Replace the Swagelok cover fitting over the carrier fill inlet. 16. Set gas source pressures and check for leaks:
Carrier gas Helium* Argon Nitrogen * Required for checkout Required delivery pressure 552 14 kPa (80 2 psi) 552 14 kPa (80 2 psi) 552 14 kPa (80 2 psi)

Before turning off the carrier gas

The internal carrier gas cylinder carries sufficient gas for 3540 hours under typical operating conditions. Normally, leave the carrier gas On between analyses to protect the column(s) and detector(s). If you still wish to turn off the carrier gas between analyses, first download a method to the GC that will cool the column(s) and turn off the detector filament(s). Abruptly stopping carrier flow on a hot column and filament can damage them.

Shutting down the GC

In order to maintain peak operating performance, Agilent recommends that you normally leave the instrument on with carrier gas flowing through the system.

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Operation References

To shut down the Micro GC: 1. Create a method that: 2. 3. Turns off the detector filament Maintains a small carrier gas purge flow through the system Lowers the column temperature

Load the method. Turn off the power and unplug any accessory power cord.

These procedures help prevent column contamination and degradation.

References
1. 2. Gas Processors Association (GPA) Standard 216686, Obtaining Natural Gas Samples for Analysis by Gas Chromatography Gas Processors Association (GPA) Standard 214097, Liquefied Petroleum Gas Specifications and Test Methods.

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Checkout The checkout sample

Checkout
Run the Agilent Calibration Gas Standard to verify that the overall system is fully operational.

The checkout sample

Agilent calibration samples are high purity and contain no aerosols, particles, or molecules that could plug or condense in an appropriately heated GC. Each is supplied in a canister under high pressure (1600 kPa/ 240 psi). If using an Agilent sample kit, the kit contains a single-stage regulator and a short stainless steel transfer line. See Calibration samples on page 153 for ordering information.

WARNING

The checkout sample is a flammable gas stored under pressure. Keep away from heat and flame. Secure the compressed gas sample cylinder to an immovable structure or use an approved cylinder stand. Store and handle compressed gases in accordance with relevant safety codes.

Connecting the checkout sample to the GC

1. 2. Clean the threads on the sample cylinder. Install the pressure regulator and stainless steel tubing as shown in Figure 34.

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Checkout The checkout sample

Pressure regulator 1/4-inch NPT fitting

1/16-inch Swagelok fitting and inlet filter assembly

Checkout sample

1/16-inch Swagelok nut and ferrule set Filter assembly Dual-end ferrule

Figure 34. Caution

Checkout sample canister connection to Micro GC

Vent noxious gases safely. 3. Purge the tubing for approximately 5 seconds. The pressure gauge will read approximately 240 psi for a new cylinder. If using the Agilent regulator, its output pressure is fixed. It delivers the sample at approximately 4 kPa (0.5 psig), with a backpressure maximum of 138 kPa (20 psig). If using a variable regulator, set it to deliver the sample gas at 35 to 70 kPa (5 to 10 psi).

4. 5.

Connect the stainless steel tubing to the GC inlet to be tested. Check for leaks.

Sample composition
Use the Universal Calibration Gas for checking the performance of any GC module. See Table 6 for its composition.

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Checkout Create the checkout method

Table 6.

The Universal Gas Calibration Standard

Concentration 0.10% 0.05% 0.10% 0.05% 0.10% Balance, 99.05% 0.05% 0.05% 0.05% 0.10% 0.05% 0.05% 0.05% 0.05% 0.05% 0.05%

Components Helium Neon Hydrogen Oxygen Nitrogen Methane Ethane Ethylene Carbon dioxide Carbon monoxide Acetylene Propane Methyl acetylene n-Butane n-Hexane n-Heptane

Create the checkout method

You can use one method to check all installed GC modules. If your instrument configuration includes GC modules with different sample inlet temperatures for checkout, use either value for all GC modules. 1. Determine your instrument configuration. In Cerity Chemical, select the Instrument view, then use the Status and Configuration sub-tabs to learn the GCs installed column and injector types. Apply the following settings to the Cerity Chemical method: Select Area Percent Report as the Method Output. Agilent recommends selecting the Method Report also. Output results to a file (use html format to include both tabulated results and an image of the chromatogram) for future reference, and select the Add Date and/or Auto Increment option(s) under File Naming to prevent overwriting previous checkout data. In the Method / Acquisition / Signal Parameters view, select Save Data for all channels being tested by the method.

2.

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Checkout Run the checkout sample

3.

Turn the Detector Filament On, set Detector Sensitivity to Standard, and select Detector Data Rate 50 Hz. Turn Continuous Sampling Off.

Build the rest of each method using the acquisition parameters, integration parameters, and output settings, listed for each specific GC module type.
For Column option... OV-1 OV-1701 MolSieve 5A PLOT Alumina PLOT PLOT Q PLOT U Stabilwax DB Alumina PLOT, 10 m 0.32 mm Alumina PLOT, 1 m 0.32 mm MolSieve 5A PLOT, 10 m 0.32 mm PLOT U, 3 m 0.32 mm PLOT U, 8 m 0.32 mm PLOT Q, 1 m 0.32 mm and Injector type... Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable Fixed or variable 0.4 L Backflush 1.0 L Backflush 1.0 L Backflush See page 61 page 65 page 67 page 69 page 71 page 73 page 75 page 77 page 79 page 81

Run the checkout sample

If installed, remove any sample conditioner blocking access to the GC inlet. 1. Install the external 10-micron filter. 2. 3. 4. 5. The 10-micron filter element can collect contaminants. Replace it periodically.

Connect the sample to the input fitting. Using the Agilent control software, perform the analysis using the appropriate checkout method. Make 10 runs, and use the results for the last run. Examine the results. The chromatographic output should be comparable to the chromatograms and typical data shown for the column type. See Checkout method parameters and typical results on page 61. If the data shows a problem, see Troubleshooting Tables on page 90. Repeat steps 2 through 5 for each input fitting.

6.

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Checkout Checkout method parameters and typical results

Checkout method parameters and typical results

OV-1 columns, fixed injector
Method conditions The tables and figure below show typical conditions and results for new GC modules using an OV-1 column with a fixed injector. Use it as a general indicator of the performance of your Micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 7.

Checkout Conditions for OV-1 (0.15 mm) Columns and Fixed Injector
4 1.2 45 50 50 10 30 90 60 0 103 (15) 103 (15) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.185 0.185 8 1.2 45 50 50 10 30 210 60 0 138 (20) 138 (20) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.500 0.500 6 2 75 75 80 10 30 120 80 0 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.180 0.180 8 2 80 85 90 10 30 120 30 60 172 (25) 228 (33) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.380 0.380 10 2 80 85 90 10 30 150 30 60 172 (25) 228 (33) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.600 0.600 14 2 80 95 100 10 30 180 30 15 240 (35) 276 (40) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.800 0.800

Length, m Thickness, m Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

0.000 1.500 0.000 40000

0.000 3.500 0.000 40000

0.000 1.500 0.000 50000

0.000 1.500 0.000 50000

0.000 2.500 0.000 50000

0.000 3.000 0.000 20000

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Checkout Checkout method parameters and typical results

Checkout results for OV-1 columns with fixed injector

1 2 3

Peak

Length, m Thickness, m

4 1.2

8 1.2

6 2

8 2

10 2

14 2

Typical retention times 1 2 3 n-Butane n-Hexane n-Heptane 0.197 0.557 1.162 0.525 1.437 2.952 0.196 0.466 0.851 0.405 0.852 1.448 0.642 1.309 2.208 0.847 1.557 2.462

Minimum areas (V s) 1 2 3 n-Butane n-Hexane n-Heptane 1000 1300 1500 1300 1500 1600 700 900 1000 1000 1300 1400 1100 1500 1500 1400 1700 1600

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Checkout Checkout method parameters and typical results

OV-1 columns, variable injector

Method conditions The tables and figure below show typical conditions and results for new GC modules using an OV-1 column with a variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 8.

Checkout Conditions for OV-1 (0.15 mm) Columns and Variable Injectors
4 1.2 45 50 50 10 30 90 60 0 103 (15) 103 (15) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.185 0.185 8 1.2 45 50 50 10 30 210 60 0 138 (20) 138 (20) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.450 0.450 6 2 80 85 90 10 30 120 30 60 172 (25) 228 (33) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.180 0.180 8 2 80 85 90 10 30 120 30 60 172 (25) 228 (33) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.380 0.380 14 2 80 95 100 10 30 180 60 0 241 (35) 241 (35) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.840 0.840

Length, m Thickness, m Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

0.000 1.500 0.000 40000

0.000 3.500 0.000 10000

0.000 1.000 0.000 50000

0.000 1.500 0.000 50000

0.000 3.000 0.000 20000

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Checkout Checkout method parameters and typical results

Checkout results for OV-1 Columns with variable injector

1 2 3

Peak

Length, m Thickness, m

4 1.2

8 1.2

6 2

8 2

14 2

Typical retention times 1 2 3 n-Butane n-Hexane n-Heptane 0.195 0.537 1.108 0.500 1.398 2.905 0.188 0.392 0.667 0.408 0.855 1.449 0.870 1.701 2.756

Minimum areas (V s) 1 2 3 n-Butane n-Hexane n-Heptane 600 800 800 450 600 600 600 800 900 400 500 600 500 700 700

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Checkout Checkout method parameters and typical results

OV-1701 columns
Method conditions The tables and figure below show typical conditions and results for new GC modules using an OV-1701 column with either a fixed or variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 9.

Checkout Conditions for OV-1701 (8 m 0.1 mm 0.5 m) Columns

Injector Fixed 45 50 50 10 30 120 30 60 240 (35) 240 (35) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.600 0.600 Variable 45 50 50 10 30 120 30 60 240 (35) 240 (35) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.600 0.600

Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

0.000 2.000 0.000 70000

0.000 2.000 0.000 30000

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Checkout Checkout method parameters and typical results

Checkout results for OV-1701 (8 m 0.1 mm 0.5 m) columns

Peak

Compound

Fixed injector

Variable injector

Typical retention times (min.) 1 2 n-Hexane n-Heptane 0.863 1.531 0.839 1.493

Minimum areas (V s) 1 2 n-Hexane n-Heptane 1800 2000 800 900

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Checkout Checkout method parameters and typical results

MolSieve 5A PLOT columns

Method conditions The tables and figure below show typical conditions and results for new GC modules using an MolSieve 5A PLOT column. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 10.

Checkout Conditions for MolSieve 5A PLOT, 10 m 0.32 mm Columns

Fixed Variable

Injector Method Analysis Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events: Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

95 95 100 10 30 180 120 15 207 (30) 276 (40) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.400 0.400

45 95 100 10 30 180 120 15 207 (30) 276 (40) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.400 0.400

0.000 1.500 0.000 20000

0.000 1.500 0.000 20000

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Checkout Checkout method parameters and typical results

Checkout results for MolSieve 5A columns

Peak

Compound

Fixed injector

Variable injector

Typical retention times (min.) 1 2 3 4 5 Neon + H2 Oxygen Nitrogen Methane Carbon monoxide 0.441 0.588 0.760 0.934 1.431 0.434 0.546 0.678 0.779 1.196

Minimum areas (V s) 1 2 3 4 5 Neon + H2 Oxygen Nitrogen Methane Carbon monoxide 100 300 900 400000 400 300 600 1700 883000 1000

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Checkout Checkout method parameters and typical results

Alumina PLOT columns

Method conditions The tables and figure below show typical conditions and results for new GC modules using an Alumina PLOT column with either a fixed or variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 11.

Checkout Conditions for Alumina PLOT (10 m 0.32 mm) Columns

Fixed Variable

Injector Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

45 75 80 10 30 90 30 60 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.400 0.400 0.495

45 75 80 10 30 90 30 60 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.400 0.400 0.445

0.000 1.500 0.000 10000

0.000 1.500 0.000 80000

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Checkout Checkout method parameters and typical results

Checkout results for Alumina PLOT (10 m 0.32 mm) columns

4 5 6

Peak

Compound

Fixed injector

Variable injector

Typical retention times (min.) 1 2 3 4 5 6 Methane air Ethane Ethylene Propane Acetylene n-Butane 0.456 0.503 0.538 0.653 1.146 1.222 0.418 0.465 0.494 0.596 0.982 1.080

Minimum areas (V s) 1 2 3 4 5 6 Methane air Ethane Ethylene Propane Acetylene n-Butane 454500 300 300 400 200 400 1410000 900 800 1300 700 1300

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Checkout Checkout method parameters and typical results

PLOT Q columns
Method conditions The tables and figure below show typical conditions and results for new GC modules using a PLOT Q column with either a fixed or variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 12.

Checkout Conditions for PLOT Q (8 m 0.32 mm) Columns

Fixed Variable

Injector Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

45 55 60 10 30 240 30 60 138 (20) 138 (20) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.460 0.460

45 55 60 10 30 240 30 60 138 (20) 138 (20) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.440 0.440

0.000 1.000 -800 10000

0.000 1.000 -800 30000

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Checkout Checkout method parameters and typical results

Checkout results for PLOT Q columns

1 2

3 4

Peak

Compound

Fixed injector

Variable injector

Typical retention times (min.) 1 2 3 4 Nitrogen Methane Carbon dioxide Ethane 0.495 0.522 0.630 0.960 0.484 0.497 0.611 0.919

Minimum areas (V s) 1 2 3 4 Nitrogen Methane Carbon dioxide Ethane 3900 411800 300 300 4500 1480000 7700 1000

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Checkout Checkout method parameters and typical results

PLOT U columns
Method conditions The tables and figure below show typical conditions and results for new GC modules using a PLOT U column with either a fixed or variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 13.

Checkout Conditions for PLOT U (0.32 mm) Columns

Length, m injector 4 fixed 6 fixed 8 fixed 4 variable 6 variable 8 variable

Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

65 70 70 10 30 60 60 60 103 (15) 172 (25) 0 He 10000 0.002 1.000 1.000 OFF OFF 0.000 0.440 0.440

65 70 70 10 30 90 60 60 103 (15) 172 (25) 0 He 10000 0.002 1.000 1.000 OFF OFF 0.000 0.700 0.700

65 70 70 10 30 120 60 60 103 (15) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.800 0.800

65 70 70 10 30 60 60 60 103 (15) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.430 0.430

65 70 70 10 30 90 60 60 103 (15) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.660 0.660

65 70 70 10 30 120 60 60 103 (15) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.800 0.800

0.000 1.000 0.000 10000

0.000 1.500 0.000 10000

0.000 2.000 0.000 20000

0.000 1.000 0.000 30000

0.000 1.500 0.000 30000

0.000 2.000 0.000 30000

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Checkout Checkout method parameters and typical results

Checkout results for PLOT U columns

Peak

Compound

4m fixed

6m fixed

8m fixed

4m variable

6m variable

8m variable

Typical retention times (min.) 1 2 3 4 Carbon dioxide Ethylene Ethane Acetylene 0.466 0.519 0.568 0.730 0.723 0.809 0.889 1.155 0.962 1.051 1.138 1.492 0.449 0.496 0.541 0.699 0.701 0.781 0.856 1.105 0.927 1.026 1.119 1.452

Minimum areas (V s) 1 2 3 4 Carbon dioxide Ethylene Ethane Acetylene 400 400 400 300 300 300 400 300 400 400 500 300 700 700 800 600 800 800 900 700 900 1000 1100 700

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Checkout Checkout method parameters and typical results

Stabilwax DB columns
Method conditions The tables and figure below show typical conditions and results for new GC modules using a Stabilwax DB column with either a fixed or variable injector. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 14.

Checkout Conditions for Stabilwax DB (10 m 0.5 mm) Columns

Fixed Variable

Injector Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Graphic Options Time Range Low High Response Range Low High

45 60 60 10 30 60 30 60 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.440 0.440 0.575

45 60 60 10 30 60 30 60 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.410 0.410 0.530

0.200 1.000 0.000 30000

0.000 1.000 0.000 60000

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Checkout Checkout method parameters and typical results

Checkout results for Stabilwax DB columns

Peak

Compound

Fixed injector

Variable injector

Typical retention times (min.) 1 n-Heptane 0.585 0.561

Minimum areas (V s) 1 n-Heptane 600 1300

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Checkout Checkout method parameters and typical results

0.4 L Backflush injector with Alumina PLOT 10 m 0.32 mm column and Alumina PLOT 1 m 0.32 mm pre-column
Method conditions The tables and figure below show typical conditions and results for new GC modules using a 0.4 L backflush injector with an Alumina PLOT 10 m 0.32 mm column and Alumina PLOT 1 m 0.32 mm pre-column. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 15.

Checkout Conditions for 0.4 L Backflush Injector with Alumina PLOT 10 m 0.32 mm Column and Alumina PLOT 1 m 0.32 mm Pre-column
Setpoint 100 100 140 10 0 150 10 10 210 (32) 210 (32) 0 6.5 He 2000 0.005 10.000 1.000 OFF OFF 0.000 0.260 0.280 0.380 0.440

Parameter Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Backflush Time (s) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Tail Tangent Skim ON at time (min.) Baseline Now at time (min.) Baseline Now at time (min.)

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Checkout Checkout method parameters and typical results

Parameter Graphic Options Time Range Low High Response Range Low High

Setpoint

0.000 2.500 0.000 500

Checkout results for a 0.4 L backflush injector with Alumina PLOT 10 m 0.32 mm column and Alumina PLOT 1 m 0.32 mm pre-column

1 2 3 4 5

Peak 1 2 3 4 5

Compound Propane Acetylene n-Butane Methyl acetylene n-Hexane

Typical retention times (min.) 0.544 0.678 0.690 1.271 2.217

Minimum areas (V s) 100 60 100 80 100

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Checkout Checkout method parameters and typical results

1.0 L Backflush injector with MolSieve 5A 10 m 0.32 mm column and PLOT U 3 m 0.32 mm pre-column
Method conditions The tables and figure below show typical conditions and results for new GC modules using a 1.0 L backflush injector with a MolSieve 5A 10 m 0.32 mm column and PLOT U 3 m 0.32 mm pre-column. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 16.

Checkout Conditions for1.0 L Backflush Injector with MolSieve 5A 10 m 0.32 mm Column and PLOT U 3 m 0.32 mm Pre-Column
Setpoint 100 100 110 10 10 150 10 10 276 (40) 276 (40) 0 9.5 Ar 5000 0.010 1.000 1.000 OFF OFF 0.000 0.550 0.550 0.650 0.750 0.850 1.000

Parameter Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Backflush Time (s) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events

Integration OFF at time (min.) Integration ON at time (min.) Negative Peak ON at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Baseline Now at time (min.)

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Checkout Checkout method parameters and typical results

Parameter Graphic Options Time Range Low High Response Range Low High

Setpoint

0.000 1.500 2000 0

Checkout results for a 1.0 L backflush injector with MolSieve 5A 10 m 0.32 mm column and PLOT U 3 m 0.32 mm pre-column

2 1 3 4

Peak 1 2 3 4 5 6

Compound Neon Hydrogen Oxygen Nitrogen Methane Carbon monoxide

Typical retention times (min.) 0.667 0.691 0.788 0.887 1.045 1.232

Minimum areas (V s) 700 1100 70 300 210000 70

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Checkout Checkout method parameters and typical results

1.0 L Backflush injector with PLOT U 8 m 0.32 mm column and PLOT Q 1 m 0.32 mm pre-column
Method conditions The tables and figure below show typical conditions and results for new GC modules using a 1.0 L backflush injector with a PLOT U 8 m 0.32 mm column and PLOT Q 1 m 0.32 mm pre-column. Use it as a general indicator of the performance of your micro GC. A new instrument should show similar performance; performance for older instruments will vary.

Table 17.

Checkout Conditions for 1.0 L Backflush Injector with PLOT U 8 m 0.32 mm Column and PLOT Q 1 m 0.32 mm Columns
Setpoint 100 100 100 10 20 150 10 10 210 (32) 210 (32) 0 4.0 He 5000 0.010 1.000 1.000 OFF OFF

Parameter Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Backflush Time (s) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events

Integration OFF at time (min.) Integration ON at time (min.) Tail Tangent Skim ON at time (min.) Baseline Now at time (min.)

0.000 0.250 0.280 0.290

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Checkout Checkout method parameters and typical results

Parameter Graphic Options Time Range Low High Response Range Low High

Setpoint

0.000 1.500 0.000 5000

Checkout results for a 1.0 L backflush injector with PLOT U 8 m 0.32 mm column and PLOT Q 1 m 0.32 mm columns

12

4 5 6

Peak 1 2 3 4 5 6

Compound Carbon dioxide Ethylene Ethane Acetylene Propane Methyl acetylene

Typical retention times (min.) 0.430 0.461 0.485 0.546 0.937 1.414

Minimum areas (V s) 3000 1900 1800 600 800 400

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Checkout NGA Calibration Gas Standard

NGA Calibration Gas Standard

If using a dedicated natural gas analyzer (NGA), a calibration standard is available for use. Table 18 lists its composition.

Table 18.

NGA Gas Calibration Standard

Concentration 5.17% Balance, 72.24% 8.997% 1.495% 6.001% 2.999% 2.000% 0.50% 0.50% 0.10%

Components Nitrogen Methane Ethane Carbon dioxide Propane iso-Butane n-Butane Isopentane n-Pentane n-Hexane

See Typical results for a G2803A GC using the NGA calibration standard on page 85 for a typical chromatogram obtained using the NGA calibration gas standard on a G2803A GC with the method settings shown in Table 19. The G2803A natural gas analyzer consists of: Channel A: fixed volume injector, OV-1, 8 m 0.15 mm 2.0 m Channel B: fixed volume injector, PLOT U, 8 m 0.32 mm

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Checkout NGA Calibration Gas Standard

Table 19.

Example Test ConditionsNatural Gas Analyzer

Channel A Channel B

Parameter Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Integration OFF at time (min.) Graphic Options Time Range Low High Response Range Low High

90 90 95 10 30 120 80 0 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.380 0.380

90 90 70 10 30 120 80 0 172 (25) 172 (25) 0 He 15000 0.002 1.000 1.000 OFF OFF 0.000 0.500 0.500 1.000

0.000 2.000 0.000 30000

0.000 2.000 0.000 30000

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Checkout NGA Calibration Gas Standard

Typical results for a G2803A GC using the NGA calibration standard

Channel A OV-1

1 2 3

Channel B PLOT U

4 5 6

Peak 1 2 3 4 5 6 7

Compound n-Butane n-Hexane n-Heptane Carbon dioxide Ethylene Ethane Acetylene

Typical retention times (min.) 0.400 0.801 1.325 0.574 0.629 0.682 0.897

Typical areas (V s) 1940 2600 2800 470 460 530 370

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Checkout RGA Calibration Gas Standard

RGA Calibration Gas Standard

If using a dedicated refinery gas analyzer (RGA), a calibration standard 3.2is available for use. Table 20 lists its composition.

Table 20.

RGA Gas Calibration Standard

Concentration 12.0% 1.0% Balance 1.0% 3.0% 5.0% 4.0% 2.0% 1.0% 2.0% 1.0% 1.0% 0.3% 0.3% 0.3% 0.3% 0.3% 0.3% 0.3% 0.1% 0.1% 0.1% 0.1% 0.1% 0.05% 0.05%

Components Hydrogen Argon Nitrogen Carbon monoxide Carbon dioxide Methane Ethane Ethylene Acetylene Propane Propylene 1,2-Propadiene iso-Butane n-Butane 1-Butene iso-Butylene trans-2-Butene cis-2-Butene 1,3 Butadiene iso-Pentane n-Pentane 1-Pentene cis-2-Pentene trans-2-Pentene 2 methyl-2-Butene n-Hexane

The G2804A refinery gas analyzer consists of: Channel A: backflush injector, MS 5A PLOT, 10 m 0.32 mm Channel B: backflush injector, PLOT U, 8 m 0.32 mm Channel C: backflush injector, Alumina PLOT, 10 m 0.32 mm Channel D: fixed volume injector, OV-1, 10 m 0.15 mm 2.0 m

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Checkout RGA Calibration Gas Standard

Table 21.

Example Test ConditionsRefinery Gas Analyzer

Channel A Channel B Channel C Channel D

Parameter Method Acquisition Parameters Sample Inlet Temperature (C) Injector Temperature (C) Column Temperature (C) Sampling Time (s) Inject Time (ms) Run Time (s) Post Run Time (s) Pressure Equilibration Time (s) Column Pressure (kPa [psi]) Post Run Pressure (kPa [psi]) Baseline Offset (mV) Backflush Time (s) Carrier Gas Analysis/Integration Parameters Slope Sensitivity Peak Width Area Reject Height Reject Shoulders Advanced Baseline Integrator Timed Events Integration OFF at time (min.) Integration ON at time (min.) Integration ON at time (min.) Tail Tangent Skim ON at time (min.) Integration ON at time (min.) Baseline Now at time (min.) Solvent Peak OFF at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Integration ON at time (min.) Negative Peak ON at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Baseline Now at time (min.) Baseline Now at time (min.)

100 100 110 10 10 240 10 10 276 (40) 276 (40) 0 9.5 Ar 5000 0.010 1.000 1.000 OFF OFF 0.000

100 100 100 10 20 240 10 10 210 (32) 210 (32) 0 4.0 He 5000 0.010 1.000 1.000 OFF OFF 0.000 0.250 0.280 0.290

100 100 140 10 0 240 10 10 210 (32) 210 (32) 0 6.5 He 1000 0.005 1.000 1.000 OFF OFF 0.000 0.260 0.280

100 100 90 10 15 240 10 10 250 (36) 250 (36) 0 n/a He 5000 0.005 1.000 1.000 OFF OFF 0.000 0.280 0.280

0.300 0.380 0.440 0.550 0.550 0.650 0.750 0.850 1.000

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Checkout RGA Calibration Gas Standard

Parameter Graphic Options Time Range Low High Response Range Low High

Channel A

Channel B

Channel C

Channel D

0.000 1.500 2000 0

0.000 1.500 0.000 5000

0.000 2.500 0.000 500

0.000 1.000 0.000 30000

Typical results for a G2804A GC using the RGA calibration standard

Channel A MS5A 1 2 3 Channel B PLOT U 5 6 8 9 10

Channel C Alumina PLOT 11

15 16 12 13 14

17 18 19

20

21 22 23

24

Channel D OV-1

25 26

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Checkout RGA Calibration Gas Standard

Peak Channel A 1 2 3 4

Compound

Typical retention times (min.)

Typical areas (V s)

Hydrogen Nitrogen Methane Carbon monoxide

0.696 0.876 1.080 1.238

102000 49000 8900 720

Channel B 5 6 7 8 9 10 Carbon dioxide Ethylene Ethane Acetylene 1,2-Propadiene Methyl acetylene 0.431 0.461 0.483 0.546 1.132 1.403 35500 23600 50300 10100 12800 11700

Channel C 11 12 13 14 15 16 17 18 19 20 21 22 23 24 Propylene Propane n-Butane trans-2-Butene iso-Butylene 1-Butene cis-2-Butene iso-Pentane n-Pentane 1,3-Butadiene trans-2-pentene 2-Methyl-2-butene 1-Pentene cis-2-Pentene 0.544 0.607 0.690 0.828 0.855 0.892 0.926 1.032 1.090 1.213 1.404 1.498 1.552 1.661 3900 1800 730 620 660 650 650 240 353 558 230 120 250 280

Channel D 25 26 iso-Butane n-Hexane 0.388 0.811 7800 1700

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Troubleshooting Tables Common chromatographic problems

Troubleshooting Tables
These tables identify some common problems, possible causes and corrective actions. For additional information, or if your problem does not appear in the tables, see Troubleshooting on page 95.

Common chromatographic problems

Problem Poor peak separation Assembly/Part Column Comments Some separation problems are corrected by performing a column bakeout. See Column and detector bakeout on page 113. Water in sample. Damaged column. Operational parameters Carrier flow rate too fast or too slow Contaminants absorbed onto column (e.g., H2O, CO2, etc.) Old column Check that the column temperature and head pressure are suitable for the analysis. Adjust the analytical method. If the column flow is too slow, peak broadening effects in the column become significant. As a starting point, use approximately 15 psig for a 4 m column. For longer columns, add 5 psig per 2 m of additional length. First perform successive blank runs. If problem persists, perform the bakeout procedure. See Column and detector bakeout on page 113. Bake out the column. If problem persists, replace module. Expected column life (under normal use): Mol Sieve: 34 years, OV-1: 10+ years, PLOT: 34 years. Re-evaluate analytical method to change the column temperature. Check for loose connections and leaks. Do not use Snoop or other detection fluids. Check for loose connections and leaks. Do not use Snoop or other detection fluids. If problem persists call Agilent Technologies Replace GC module. Bake out the column to eliminate residues from prior injections. Sample with a 30 second sample time to clean all transfer lines. Increase time between runs to avoid carryover to next run.

Column too hot or too cold Varying peak heights Sample transfer lines Leak or bad injector Injector Ghost peaks Column contamination

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Troubleshooting Tables Common chromatographic problems

Problem Carryover

Assembly/Part Sample inlet and manifold assembly

Comments Check for leaks at the transfer lines and the manifold assembly entry. Add (or increase) delay time between injections.

Negative peaks

Carrier gas

This leak is before the carrier inlet fitting on the GC; it is external. The size of the negative peak indicates the size of the leak. Check for sources of contamination. Poor carrier gas, e.g, H2O in hydrogen. Lack of sufficient carrier gas pressure in the manifold prevents the inject valve from sealing fully, creating an air leak. Note: The inject microvalve is not defective in this case. Check for mechanical vibrations or heavy fluctuations in ambient pressure; for example, closing doors, GC in walkway area, walkie-talkies, and wind. Check if problem exists in other modules. If not, there may be a leak in the detector. Have it replaced by Agilent Technologies. Although this is rarely the cause, the control board may have to be replaced. Call Agilent Technologies. Check carrier gas setting. If method carrier gas is set for argon, sensitivity is decreased for certain compounds. Run a calibration gas injection. If you see low sensitivity with a major component peak, the sample path may be blocked. Make an overload injection of an appropriate gas. For example, perform an air injection at ambient temperature. If the N2 and O2 peaks are small (show low sensitivity) but the peaks tail (indicating that the column was overloaded with N2 and O2), then the detector is bad. If the data shows no peak tailing, the detector may be good, but the injector may have a small injection volume. Call Agilent Technologies. Check standard external inlet filter for plugging. If in doubt, replace the filter element. Check O-rings and replace if necessary. Possible pluggage. Call Agilent Technologies. If the carrier gas supply pressure drops below 78 psi, the injector microvalves may not operate properly. The pressure fed to the GC should be 78 to 82 psig. Check for a loose inlet fitting. If loose, tighten. Tighten if loose.

Carrier line into manifold is loose or leaking Noisy baseline Environment

Detector Control PCB board Low sensitivity Control PCB Sample flow path Detector

Sample inlet filter Module connecting tubes Injector Carrier gas pressure low Sample inlet fitting loose Sample tubing loose at manifold

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Troubleshooting Tables Temperature readout problems

Problem Low sensitivity Air peak on zero inject baseline

Assembly/Part O-rings in gang block Column head pressure low

Comments Check for presence and condition of the O-rings between the gang block plates. Replace if damaged or missing. Lack of sufficient carrier gas pressure in the manifold may prevent the inject valve from sealing fully, creating an air leak.

Temperature readout problems

Problem Temperature readout is different than setting Assembly/part Display Heater Comments Make sure you are monitoring the correct channel Check that the heater cable is properly seated on its connector

Pressure readout problems

Problem Pressure readings are erratic or wrong Assembly/part Display Parameters Carrier gas line into gang block is loose or O-rings missing Communication with GC Carrier gas line into manifold is loose O-rings missing or damaged Comments Make sure you are monitoring the correct channel Check your method settings. Check for the presence of undamaged O-rings inside the gang block. If there are O-rings, tighten down the plate.

Make sure that communication is active. Restart GC software, if needed. Tighten fittings.

Check for undamaged O-rings inside the gang block. If O-rings present, tighten down the block screws.

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Troubleshooting Tables Pneumatic problems

Pneumatic problems
Problem No vacuum/low vacuum Assembly/part Vacuum pump Comments Check connections. If not an obvious fitting connection call Agilent Technologies. Also see Checking the vacuum system on page 115. Call Agilent Technologies. Check flow rate at the sample vent on the back of the instrument. If there is flow, perform a zero injection and check for an air peak. If there is a leak, it will be the inject valve, the switch solenoid, or a delaminated injector. Call Agilent Technologies. Check for flow at the reference and analytical column vents. If there is no flow, call Agilent Technologies. Call Agilent Technologies. Check the fitting connections for all sample transfer and connection lines Check fittings and presence of undamaged O-rings inside gang block. Tighten down the block screws. Check remaining pressure in internal carrier gas tank. Pressure should read > 200 psig.

Control PCB High carrier gas usage or low sensitivity Leak

Column broken Solenoid valves Sample transfer lines Cannot reach column head pressure Carrier gas line into manifold is loose Portable GC: Insufficient carrier gas in internal cylinder No flow at analytical column vent No analytical column flow and no reference column flow Vacuum pump runs constantly Column broken Injector delaminated GC setup

Call Agilent Technologies. Call Agilent Technologies.

Continuous Flow mode is on.

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Troubleshooting Tables Output problems

Output problems
Problem High noise Assembly/part Detector leak Optional carrier gas Sample inlet Comments Send unit to Agilent Technologies for repair. Verify that your method matches the carrier gas in use. Make sure the inlet frit or the sample transfer lines are not plugged.

Communication problems
Problem No communication with computer Assembly/part Cable Comments Use standard LAN cable for network connections. Use crossover cable for direct GC to computer connection. See Set IP address on page 19. Check IP address. See Set IP address on page 19. Check setup of GC in Cerity (or other operative software).

Software Software

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Troubleshooting How to determine GC configuration

Troubleshooting
Although this section will provide some guidance to help you diagnose common operational problems, it cannot anticipate them all. In that case, you should consult: Agilent 3000 control software Help Agilent Technologies Service

This section is divided into four main topics: 1. 2. 3. 4. How to determine GC configuration understanding information available on the GCs internal web page, installed GC components Hardware/Software power, communications, software, and instrumental problems Chromatography common chromatographic problems and possible corrective actions Methods analytical methods and parameters

How to determine GC configuration

To learn the basic GC configuration (for example, before creating a method in Cerity Chemical), simply open Cerity Chemical to the Instrument View, then use the Status and Configuration sub-tabs to learn the installed column and injector types. For more detailed information, and to determine the configuration before contacting Agilent service, follow one of the procedures below. Always determine your complete GC configuration before contacting Agilent service.

Using the LAN connection

If your instrument is capable of LAN communications, check its configuration as follows: 1. Open a web browser and enter the GCs IP address as the web address. For example, enter http://10.1.1.101.

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Troubleshooting How to determine GC configuration

2.

From the GC home page, select the Utilities tab.

3.

Under Configuration, select button Full System.

4.

After a moment, the instruments current configuration is displayed. Refer to the table below and to Figure 35.
Item 1 2 3 4 5 6 7 8 9 10 11 Meaning GC model GC serial number GC module communication address Channel assignment for GC module GC module part number Injector type Injector description Column type and description Sample pump used Carrier gas type Carrier gas input location

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Troubleshooting How to determine GC configuration

1 2 3 4 5

GC Type: 2801 Instrument serial number: US10000110 Module 1: Channel Assignment: A Part Number: G2801-60508 Serial Number: US10000193 Board Serial Number: STI330056114 Sample Inlet: Heater ID: m0:ThermA Pressure Sensor ID: NONE Injector: Type: Fixed . . . Description: DIE-2050 Det Die 3 Valve Fixed 1.6ul . . . Column: Type: OV1 . . . Description: Assy Col OV-1 1.2 8m Film Thickness: 1.20 m Inside Diameter: 200.00 m Length: 8 m Temperature Limits: Lower: 30 C Upper: 160 C . . . Pre-Column: NONE Sample Pump ID: m0:Pump0 Gas Supply: Type: Ar Location: carrier1 . . . Module 2: Channel Assignment: B Part Number: G2801-60506 . . .

6 7

9 10 11

Figure 35. Excerpts of example status information for a 3000 micro GC

5. To determine which sample input fitting a GC module uses, examine the GC as described in step 4 of Manually determining hardware configuration on page 100.

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Troubleshooting How to determine GC configuration

Codes for GC modules, sample pumps, and GC module layout The data displayed on the GC web pages are organized by GC module. The GC modules and sample (vacuum) pumps are labeled as shown below.

Pump m0, Pump0 m1, Pump1 GC Module m1 m2 GC Module m1 m2 m3 m4

Channel Channel A B

Channel Channel A B

Channel Channel C D

Front of 1- or 2-channel GC

Front of 3- or 4-channel GC

Figure 36.

Top view of 2- and 4-channel GCs showing labeling of GC modules

Configuration example Consider a 2-channel instrument with two sample input fittings and one carrier gas. The Full System configuration screen information might include:
Module 1: Channel Assignment: A Sample Inlet: Heater ID: m0:ThermA Injector: Type: Fixed Column: Type: OV1 Description: Assy Col OV-1 1.2 8m Sample Pump ID: m0:Pump0 Gas Supply: Type: Ar Location: carrier1 Module 2: Channel Assignment: B

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Troubleshooting How to determine GC configuration

Sample Inlet: Heater ID: m1:ThermC Injector: Type: Fixed Column: Type: PLOTU Description: Assy Col 8m Pora U Sample Pump ID: m0:Pump0 Gas Supply: Type: Ar Location: carrier1

Removing the top cover of the GC reveals the following:

Carrier gas 1 (Argon)

Sample pump: m0; Pump0

GC Module 1: Cerity Chemical Channel A OV-1 Column, 8 m

GC Module 2: Cerity Chemical Channel B PLOT U Column, 8 m

Sample input fitting 1

Sample input fitting 2

Examine GC to determine

Figure 37. Configuration diagram for a 2-channel GC with two input fittings and one carrier gas

Manually determining hardware configuration

If the instrument is not capable of communicating across the LAN, manually check the configuration as follows: 1. 2. 3. Turn off the GC and unplug the power cord. Remove the instrument top cover. See Remove the covers on page 116. Remove the manifold cover plate(s). See Remove and replace a GC module on page 117.

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Troubleshooting Hardware/software problems

4.

Examine the plumbing connections between the input fittings and each GC module to determine which input fitting supplies each GC module with sample. Examine the plumbing connections between the carrier gas external fittings and each GC module to determine which carrier gas each GC module uses. Refer to Figure 35. Any GC module connected to sample pump m0 uses carrier gas 1. Any GC module connected to sample pump m1 uses carrier gas 2. GC modules that share a carrier gas are connected to each other by stainless steel tubing between their manifold blocks.

5.

Connector tubing links carrier gas between GC modules

6.

On the top of each GC module, read the label containing GC module part number and column type information. See Figure 1 on page 10.

Hardware/software problems
If the cause of a problem is completely unknown, it can be determined by following the topics in sequence. If you suspect a particular cause, start with the appropriate topic.

Verify power
The GC Power Light is an LED, which has an extremely long life. It is very unlikely that the LED has failed.
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Troubleshooting Hardware/software problems

Is the GC Power Light on? If not, check the power supply. 1. 2. 3. 4. Verify that AC power source is active. Check the connections between the GC, the power converter (the box between the power source and the GC), and the AC power source. Make sure the GC power switch is on. If the power light still does not come on and you cant establish communications (see below), then either the power cord, the converter, or the GC is defective. If available, replace the power cord and/or converter. If the power light still does not come on, contact Agilent.

5.

Verify communications
Communication between the PC and the GC is established in one of two ways: Isolated LAN (local area network) which is not connected to other devices at the same site. Connections use a crossover cable (5183-4649). As part of a local LAN that includes other devices and users. Connections use standard cable (G1530-61485).

Check LAN communications 1. Open the Command Prompt [C:\>], and use the ping command to verify communication. For example, if the GC is set to IP address 10.1.1.101, enter ping 10.1.1.101. You should see a reply similar to the screen below.

Figure 38. Ping reply from 10.1.1.101

2. If the GC replies, it has established communication with the PC and you can go to Open web page on page 103. If the GC does not reply, see Check isolated LAN communication on page 102.

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Troubleshooting Hardware/software problems

Check isolated LAN communication 1. 2. Connect the computer directly to the instrument using a crossover cable (part 5183-4649). Set the computers IP address to the following:
Computer IP Address Subnet mask Gateway* DNS server* 192.168.1.100 255.255.255.0

* The gateway and DNS server entries are not used for direct connection.

See Set IP address on page 19 for details. 3. Open the Command Prompt [C:\>], and enter: ping 192.168.1.99 The instrument should respond as shown below.

Figure 39. Ping reply from 192.168.1.99

If communication cannot be established, contact your Agilent service representative. 4. If communication was established, the problem may be that the IP address for the GC is not correct for your installation. Change the instruments IP address as needed. For details, see To change the instruments IP address on page 136. Verify the new address as described in Check LAN communications on page 101.

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Troubleshooting Hardware/software problems

Open web page 1. 2. Open your Internet browser. Make sure the proxy server is disabled. (See browsers help for details.) Enter the GC IP address as the web address. For example, http:// 10.1.1.101. Is the web page open?

Figure 40. Representative GC web page

YesGo to Verify Cerity Chemical program settings on page 103 NoIf the web page cannot be opened, go to Check isolated LAN communication on page 102 and continue diagnostics.

Verify Cerity Chemical program settings

1. 2. 3. Go to Configure / Instruments and verify the settings for the GC. Enable the GC. Does it come online? YesGo to Pneumatics checkout on page 104. NoIs anyone else connected? YesHave them disconnect, then return to step 3 above. NoGo to Test direct connection on page 103. Test direct connection 1. 2. 3. 4. 5. Exit Cerity Chemical, shut down the computer and GC, and connect the crossover cable, Agilent part no. 5183-4649 between the PC and the GC. Turn on the GC and PC. Set the PC IP address to 192.168.1.100. Set the PC Subnet Mask to 255.255.255.0. Restart Cerity Chemical, and configure the instrument to use IP address 192.168.1.99.

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Troubleshooting Hardware/software problems

6. 7.

Enable the GC. Does the GC come online? NoContact your Agilent service representative. YesThe problem is in your local LAN configuration. Contact your local LAN administrator.

Verify GC modules
Pneumatics checkout 1. 2. In Cerity Chemical, go to Instrument / Status. Check each parameter against its setpoint. Does each parameter match its setpoint? YesGo to Test flows on page 106 NoGo to Download method on page 104.

Download method
1. 2. Download the checkout method. Does each parameter match its setpoint? If yes, go to Test flows on page 106. If not, go to Check GC module status on page 104.

Check GC module status 1. Open the browser and type in the GC IP address as the web address.

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2.

Select Status.

This battery monitor is displayed when running a 3000 Micro GC Portable

Figure 41. Representative Status screen

3. 4. Check the actual values against their setpoints. If all parameters match their setpoint values, continue with Test flows on page 106. If there are any items where the setpoint does not match the actual, is the flag = 00? YesGo to Duty cycle on page 106. NoReset the GC. Close the browser, then Power cycle the GC. After the instrument beeps twice, proceed with Check GC module status on page 104.

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Duty cycle 1. 2. Should be approximately 30 to 40% for column head pressure (CHP) and Delta P (if fixed volume). Is the Duty Cycle between 30 to 40%? YesGo to Test flows on page 106. NoIf the Duty cycle is > 50%, check the carrier gas inlet pressure. Replace the carrier gas filter (3150-0602). Recheck the Duty cycle. If it is still > 50%, contact your Agilent service representative.

Test flows
1. In Cerity Chemical, create a new method called Flow Test to: 2. 3. Set all pressures to 20 psi. Set sample time to 30 seconds. Set continuous mode to Off.

Download this method to the GC. Using a flow meter, measure the actual flow rates from the Reference and Analytical ports on the back of the GC. Typical flow rates should be: The analytical flow rate should be 1 0.5 mL/min The Reference flow rate should be 0.6 0.4 mL/min

If either flow rate is incorrect, replace the carrier gas filter (3150-0602). If the flow rate is still incorrect, then see Inspect tubing on page 106. 4. 5. 6. 7. Start a run using the Flow Test method. Measure the Sample flow rate at the sample input fitting. The sample flow rate should be between 1 and 10 mL/min. If the flow rate is correct, sufficient sample is being drawn through the instrument. If the flow rate is not correct, check if the vacuum pump is on. If the pump is on: Check inlet filters and sample conditioners. Clean or replace all used filters.

Repeat step 6.

Inspect tubing
1. 2. 3. Remove the GC cover. Examine the tubing connected to the gang block behind the GC module. Is tubing connected properly?
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YesGo to Test carrier in on page 107. NoReconnect tubing and return to Test flows on page 106.
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Test carrier in
1. 2. With carrier gas set at 80 psig, loosen the gang block retaining screw. Can you hear gas escaping? YesYou have a damaged GC module. Exchange it or return it for repair. NoThe manifold assembly is blocked. Return the entire GC to Agilent for repair.

Chromatographic problems
This section is concerned with the diagnosis of unexpected chromatographic behavior and the determination of probable cause and cure. Problems arise from many sources and include: Electronic or mechanical failure Contaminants in gas lines, injectors, columns and detectors Incorrect or inappropriate setpoints Leaks, bleed, or other chromatographic difficulties

These often interact. For example, baseline problems may arise from any of the above sources. Accordingly, this section is organized by symptoms with reference to most probable causes.

Baseline symptoms
Position Baseline position changes suddenly during a run. This can result from: Filament failure Valve failure EPC failure

Inspect configuration screens for highlighted warnings, or changed run settings. Correct problem. Rerun sample. Wander and drift Baseline wander or drift is to be expected when a flow or temperature setting is changed, but with sufficient time the problem should clear. The following cases assume that sufficient stabilization time has elapsed. 1. Baseline is erratic; moves up and down (wander).

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Suspect a leak. Check column connections. If the leak is at the detector end of the column, retention times are stable from run to run but sensitivity is reduced. If it is at the inlet end, there is reduced flow (lower linear velocity) through the column, increased retention time and reduced sensitivity.

2.

Baseline moves steadily (drift) upscale or downscale during the run: This problem can be minimized by: Thorough column conditioning. See Column and detector bakeout on page 113. Operating at a lower temperature, but this prolongs the analysis. Substitute a chromatographically equivalent column with a higher temperature limit.

Wander and drift are often accompanied by noise, discussed below. Noise Noise is rapid baseline fluctuations, broadening the baseline and giving it a hairy appearance. Noise is different from spiking; spikes are isolated events rather than almost continuous and are described later. Some noise is inevitable with any detector. At low sensitivity it may not be noticed, but it appears when the sensitivity is increased. Noise limits detector sensitivity and should be minimized. 1. Noise appears suddenly on a previously clean baseline: Consider all changes made recently to the system. Loose connections in the detector or its signal path generate noise. Detector contamination generates noise. Contaminated carrier gas: If a tank was replaced recently and the old one is still available and still has some gas in it, try the older tank to see if noise decreases. If the new gas is so badly contaminated that it saturates traps, changing to the old one may show little improvement until the traps are replaced or regenerated. This problem is most common with nitrogen carrier gas. It is a common practice for empty gas cylinders to be refilled by the gas dealer after a thorough purging procedure. Deal with a reliable gas supplier! 2. Noise increases gradually to an unacceptable level: This symptom indicates gradual buildup of the noise source, rather than an abrupt change as discussed above.
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Spiking Spikes are isolated baseline disturbances, usually as sudden (and large) upscale movements. If accompanied by noise, attack the noise problem first since spiking may disappear at the same time. If spikes appear whenever a run is in progress:, the cause is almost always electronic in origin. Loose connections are likely. Check accessible cable connections. Another possibility is external interference from local radio transmission equipment.

Retention time symptoms

Retention time drift Retention time drift is a steady increase or decrease of retention times in successive runs. Erratic times (both directions) are discussed later as retention time wander. 1. In a series of runs, retention times suddenly increase: 2. This could be due to decreased carrier flow or reduced column temperature. Check the pressure and temperature setpoints. The carrier gas tank may be nearly empty.

In a series of runs, retention times suddenly decrease: This could be due to increased carrier flow or increased column temperature. Check the pressure and temperature setpoints.

Retention time wander (reproducibility) 1. Retention time reproducibility is erratic for successive runs of similar composition: 2. Temperature or pressure variations may cause this and may indicate possible detector or control failure. Radical differences in molecular concentrations can also alter retention time. When the earliest peaks elute very rapidly, they may not have had time to achieve chromatographic equilibrium with the stationary phase. They act like solvent peaks and are blown straight through the column. A useful rule is that the peaks of interest should require at least four times as long to elute as an unretained solvent or air peak. If this problem is suspected, try lowering the column temperature. A 30C drop approximately doubles the retention time.

Reproducibility is good later in the run but not for the first few peaks:

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3.

Retention time changes with amount of sample: When there is more sample than the column can handle, peaks are deformed and the peaks are shifted to shorter retention times. Try diluting the sample or injecting less of it.

Peak symptoms
No peaks This is usually due to operator error. Possibilities include incorrect signal assignment, low sensitivity setting (peaks are there but you cant see them) and detector failure. There are many others. Try to reproduce the symptom. Inverted peaks This is most likely an inappropriate signal definition or an incorrect polarity setting with the thermal conductivity detector. Extra peaks These are divided into two classes: additional peaks appear in addition to those expected from the sample. Ghost peaks appear even when no sample is injected (and also found among the genuine peaks during a sample run). 1. Peaks appear during a blank run: Ghost peaks are often observed when a column has been at its starting temperature for some time. For example, the first few runs in the morning (especially Monday morning) often show ghost peaks. Ghost peaks can arise from carrier gas impurities and plumbing contamination by oils, greases and other materials. Less commonly, they may be caused by reaction of stationary phase with trace levels of oxygen, water and other materials in the carrier gas. A contaminated inlet can cause ghost peaks. Residues in the inlet are volatilized or pyrolyzed and swept onto the head of the column. Try reducing inlet temperature. If this eliminates or reduces ghosts, clean the inlet. These might be ghost peaks as described above. Make a blank run (carrier gas only); if the peaks persist, they are not sample-related. Another cause, assuming the sample is pure, is thermal degradation of one or more components by an overheated inlet. Test this by reducing inlet temperature.

2.

Additional peaks appear when pure sample is injected:

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Deformed peaks
The ideal peak, seldom seen in real chromatography, is a pure Gaussian shape. In practice, some asymmetry is always present, particularly near the baseline. 1. The peak rises normally, then drops sharply to baseline:

The most likely cause is column overloading. Try diluting the sample by a factor 10 or, if you have a variable volume injector, reduce the sample volume by 10 . This could also be two (or more) closely merged (unresolved) peaks. Lower the run temperature 30C and repeat the analysis. If the peaks separate more, you have merged peaks.

2.

The peak rises sharply and then falls normally to baseline:

Column overload with a gas sample often shows this effect. Try injecting less. This may be a merged peak situation. Running at lower temperature increases resolution, perhaps enough to reveal merged peaks. Too low an inlet temperature can also do this.

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3.

Top (apex) of the peak is deformed:

Cigar shaped top

Detector overload is the probable cause. In severe cases, doubling the amount injected may cause little or no increase in peak size. Inject less sample. Since the detector is at the upper limit of its response, a substantial reduction is needed to get into normal operating range.

4.

Top (apex) of the peak is split:

Verify that this is not a merged peak pair by running at a lower temperature. Decrease volume of sample injected by a factor of at least 10 and repeat the run. If the split disappears, detector overload was the problem. This usually improves linearity as well. Hydrogen peaks, analyzed with a thermal conductivity detector and helium carrier, often show a split top. Reduce sample size until the split vanishes.

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Method problems
This section shows you how to troubleshoot a method and solve problems that arise from incorrect instrument parameter settings, wrong peak identification windows, and inappropriate peak detection parameters. All of these situations translate into an erroneous calculation of the mole percent composition of your samples. You will need to troubleshoot your method if you observe the following signs in your reports and chromatograms when running a calibration standard: Zeroes in the mole % reports for components known to be present. Peaks are not being integrated or are integrated incorrectly. Unusually high or low mole % composition. Samples with unnormalized totals outside the 95 to 105% range when the calibration is close in concentration to the sample.

In many cases you will only need to make a few adjustments and/or perform minor instrument maintenance to correct instrument performance. Begin by cleaning the system through the instrument bakeout procedure.

Column and detector bakeout

This procedure cleans your column and detector of residue (i.e., high molecular weight components) from previous samples that may interfere in subsequent analyses. Over time, small amounts of contaminants accumulate especially in the column, and can cause peak tailing and retention time shifts. Agilent recommends creating a bakeout method for your instrument. Run this method: After first installation After installing a replacement GC module After the micro GC has been turned off or stored Periodically as needed to refresh column performance

To perform the bakeout procedure: 1. In Cerity Chemical, create a method called Bakeout for <instrument or GC module>. Use the values in Table 22 to set the flow rates, run times, and temperatures for each GC module. If the GC contains columns with different durations, create a bakeout method for each set of GC modules that use the same bakeout time.

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The table below summarizes the bakeout conditions and time for each type of 3000 GC column, as well as a general recommendation for bakeout frequency.

Table 22.
Column type Alumina PLOT

Bakeout Conditions and Frequency

Column temperature, C 180 180 180 180 160 160 180 Duration, hours 812 812 2 2 812 812 2 Recommended frequency for general use Weekly Weekly Weekly Weekly Weekly Weekly Weekly

MolSieve 5A PLOT OV-1 OV-1701 PLOT Q PLOT U Stabilwax-DB

2. 3. 4. 5. 6. 7. 8. 9.

In the method, turn detector filaments on. Save the method. Make sure carrier gas flow is ON (this protects the column and detector). From Cerity Chemicals instrument view, download the method to the instrument. Allow the method to run for the duration listed in Table 22. After bakeout is complete, load your analytical method and run a set of calibration samples. Check the report. Adjust the calibration settings, retention times, and response factors as needed. If the problem persists, replace the 10-micron sample inlet filter and re-run your calibration sample.

Correcting instrument parameter settings

Adjusting column head pressure Column head pressure controls flow through the column, affects the retention time of all peaks in the run, and changes peak windows. 1. 2. Determine the retention time for the start of the unretained peak (first peak) for all channels in your calibration standard. Adjust column head pressure so that all peaks elute within specifications.

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3.

Any new method will be saved automatically by Cerity Chemical under a different name. This way you keep original method values intact. Once a new method is saved, it becomes the active method.

Before continuing, you should have completed the bakeout procedure and made the pressure and temperature adjustments. Recalibrating The changes in pressure and temperature may have shifted peak retention times significantly, such that new RT and peak windows are required. You will now need to recalibrate.

Checking the vacuum system

1. 2. 3. 4. Remove external inlet filter assembly or any sample conditioner from the GC inlet. Connect vacuum pressure gauge to the front inlet. From Cerity Chemical, set the sample time to 30 sec. Start a blank run and monitor the vacuum level. You should hear the vacuum pump turn on, then off. While the pump is on, pressure for a new GC should be approximately as shown in Table 23 below.

Table 23.

Expected Vacuum Levels

kPa (psi)* 2 (0.3) 2 (0.3) 2 (0.3)

Injector type Backflush Fixed volume Variable/timed

* Measured over a 10 second interval

If the vacuum level is low, or if the pump will not turn on, call Agilent Technologies. 5. If vacuum system is satisfactory, reassemble normal inlet filters or conditioners.

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Replacement and Service Procedures

Prepare the GC and control software for servicing
Before beginning work on an instrument, use the Agilent Cerity Chemical software to prepare the instrument for service. When the instrument is not in a sample run: 1. 2. 3. 4. Set the heated zones where you will be working to < 40C or OFF Turn OFF all gas flows that will be disconnected Turn OFF any other feature that could be hazardous or waste resources When the heated zones reach < 40C, open the ConnectAdmin utility.

Caution

The instrument must be disconnected from Cerity Chemical before replacing hardware. 5. Select the instrument to be serviced in the Instruments Enabled list, and press Disconnect.

It is now safe to proceed with GC service.

Tools required for any replacement procedure

Pozidriv screwdriver 5/16-inch wrench Needle nose pliers (helpful for disconnecting cables) T-20 Torx screwdriver T-10 Torx screwdriver Flat blade screwdriver

Remove the covers

Caution
During this process, you will expose the internal components of the unit. To avoid damaging the unit, turn the power switch off and disconnect all external power to the unit.

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With a Pozidriv screwdriver, remove the two screws on each side of the cover you need to take off. Lift and remove the cover.
Top cover screws

Bottom cover screws

Figure 42. Cover screws (2-channel unit shown)

Remove and replace a GC module

The photos and screen images used in this procedure illustrate how to remove and replace the left, or Channel A, GC module in a 2-channel instrument. The process is similar for any channel and instrument chassis. You can replace only one GC module at a time.

Update the instrument firmware

Each new GC module comes from the factory with the latest firmware installed. To keep your instrument up-to-date with the new GC module, Agilent provides the latest instrument firmware as part of the GC module replacement kit. Before installing the new GC module, you must update the instrument firmware. To update the instrument firmware: 1. 2. 3. Insert the CD-ROM labeled Firmware Update provided in the kit into your PC. Browse the CD, and open the file called readme.htm. Follow the instructions in the file.

Caution

During firmware update, do NOT turn off instrument power until prompted to do so by the update program. Turning off power during the update can render the instrument unusable.

Types of replacement modules

In general, you can replace any type of GC module with one of a different type. For example, you could replace a 4 m OV-1 unit with fixed injector (part no. G2801-60507) with a 6 m PLOT U unit with fixed injector (part no.
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G2801-60514) or a 4 m OV-1 unit with variable injector. However, the new module must use the same carrier gas as the unit it replaces. At this time, installing a GC module in a previously unused channel is not supported.

Decommission the old GC module

Caution
Decommission only one GC module at a time. The 3000 Micro GC internally communicates to each installed GC module using a unique address. For a 2-channel system, the addresses used are 1 and 2. For a 4-channel system, these addresses are 1 through 4. See Figure 43.

Address:

Front 2-channel GC

Front 4-channel GC

Communications address 1 2 3 4

Corresponding Cerity Chemical channel A B C D

Figure 43. Default GC module serial communications addresses

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Before replacing a GC module, you must first disable the GC modules internal address by decommissioning it. The procedure below describes this process for replacing GC module 1 (channel A) in a 2-channel instrument. The process is similar for other configurations. 1. 2. Open Internet Explorer and enter the GCs IP address, for example, http:\\10.1.1.101. The instruments internal utilities will appear. Select the Status tab, and review the status information for the defective GC module. If no status information appears for it, skip the rest of this section and proceed with Remove the old GC module on page 121. Select the Utilities tab. Select Change Module Config.

3. 4.

5.

Two caution messages appear. Select OK on each to continue.

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6.

Select Remove.

Caution

Once a GC module is decommissioned, it can no longer be used until it is recommissioned. 7. Select Remove next to the GC module to decommission. A caution appears. Select OK to decommission the GC module.

Select appropriate button

8.

A confirmation message appears. Select Shutdown. The instrument software will start to shut down.

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Caution

Do not turn off the power immediately. The GC must write to its configuration files. If you turn the power off too soon, you can corrupt the files and make the instrument unusable. You must wait 3 full minutes before turning the instrument off. 9. Wait at least 3 full minutes.

10. Turn off the instrument.

Remove the old GC module

The photos illustrate how to replace the left, or Channel A, GC module in a 2-channel GC. The process is similar for any channel.

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Caution

During this process, you will expose the internal components of the unit. To avoid damaging the unit, turn the power switch off and disconnect all external power to the unit. Electrostatic Discharge can damage electronic components. Wear a grounded wrist strap to avoid damaging the instrument. A disposable wrist strap is provided. 1. 2. Remove the top cover. See Remove the covers on page 116 for details. Loosen the thumbscrews in the manifold cover plate and remove it. In the two screw design, slide the manifold cover plate towards the GC module to disengage the hook in the cover plate from the tab in the chassis.

Loosen thumbscrews

Manifold cover plate

Three screw design

Loosen thumbscrews

Manifold cover plate

Two screw design

Figure 44. Loosen thumbscrews and remove manifold cover plate

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3.

Carefully remove the manifold insulation. Save it for re-use.

Remove insulation

2-channel instrument shown. Others are similar.

Figure 45. Remove inlet manifold insulation

4. In the Micro GC Portable, the DC-DC converter assembly blocks access to the GC modules. Remove the screws that secure the DC-DC converter to the side of the GC. Without disconnecting any wires, slide the assembly off of the standoffs and gently lift it away from the GC modules.

DC-DC converter assembly

Remove screws

Figure 46. DC-DC converter assembly (Micro GC Portable only)

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5.

Loosen the screw in the manifold fitting at the back of the GC module.
Back of micro GC

Manifold fitting screw

Loosen screw

2-channel instrument shown. Others are similar.

Figure 47.

Disconnect GC module gang block

6. Disconnect the inlet manifold fitting from the GC module input fitting.
Channel A Channel B

GC module

Inlet manifold

Disconnect inlet fitting

2-channel instrument shown. Others are similar.

Figure 48. Disconnect inlet fitting

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7.

For a 2-channel unit: Disconnect the cables leading from both GC modules, if present, to the communications board connectors for both GC modules. For a 4-channel unit: Disconnect any communications cable leading to the GC module. If needed, also disconnect the power cables leading to the fan.

Back of GC module

Communications board

Remove cable

Remove cable

Back view of GC modules

Figure 49.

Disconnect communication cable

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8.

Tilt the back of the GC module up until the mounting flange clears the alignment pins. See Figure 50. Slide the GC module towards the back of the instrument until it clears the inlet manifold frame and can be lifted and removed from the front.

Caution

Be sure to lift and remove the GC module from the front end of the GC to avoid damage to the sampling pumps in the rear. Also, be careful to avoid damaging any nearby wires or cables.

Tilt GC module

Mounting flange

Mounting flange Tilt until mounting flange is free from alignment pins

2-channel instrument shown. Others are similar.

Figure 50. Remove the GC module

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9.

Inspect the gang block fitting on the bottom of the chassis to make sure the mating surface is clean.

Gang block, lower half

Alignment pins

Figure 51. Inspect the gang block fitting

Install the new GC module

1. Remove the small metal plate covering the O-rings on the upper gang block. See Figure 52.

Retaining screw Metal plate covering O-rings and upper gang block

Figure 52. Protective plate on upper gang block

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2.

Inspect the GC module mounting flange fitting to verify all new O-rings on the replacement GC module are undamaged and seated flat.

Mounting flange Verify O-ring placement

Gang block, upper half

Figure 53. Inspect the new O-rings

3. 4. Remove the protective cap over the GC module inlet fitting. Lower the back of the GC module into position until the front can fit into place under the lip of the inlet manifold frame and the module input fitting mates with the Swagelok fitting in the inlet manifold (see Figure 54). Slide the GC module forward until it fits into place.

5.

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Install GC module below frame

Mate module and manifold fittings

View from back of GC

Figure 54. Install the new module

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6.

Connect the communications cables. See Figure 55 for typical cabling examples. Connect no more than 2 GC modules in series per communications board connection. The GC modules and communications board use parallel communications; both connectors on each item function equivalently.
Channel C Channel B Channel A Communications Board

Channel D

If fan installed

If fan installed

Figure 55.

Examples of GC module cabling

7. Connect the inlet manifold to the GC module input fitting. Using a wrench, tighten 1/4-turn past finger tight.

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8. 9.

Tighten the screw in the mounting flange. Carefully replace the inlet manifold insulation.

10. Install the manifold cover plate and the top cover.

Commission the new module

After, installing the new GC module, you must configure it for use by commissioning it. 1. 2. 3. Turn on the GC and wait about 2 minutes. In you web browser, select the Top tab. When the GC responds, it has completed its reboot process. Select the Utilities tab, then select Set to give the new GC module an address.

4.

Use the drop down menu on the lower left portion of the screen to select the correct address for the new GC module. Only the available addressees are listed See Figure 43 for default values

Message text will vary. A 2-channel system is shown. Select the new GC module address. In this example, we select 1.

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5.

After selecting the address, select Restart to incorporate the changes.

Caution

Do not turn off the power. The GC must write to its configuration files. If you turn the power off, you can corrupt the files and make the instrument unusable. 6. After restart, wait at least 3 full minutes.

7.

Select the Top tab, or use one of the links provided on the GC web page. When the GC responds, installation is complete. Verify the new GC module status.

Enable the instrument in Cerity Chemical

After installing the replacement GC module and updating the GC firmware, configure Cerity to use the updated GC. 1. 2. 3. Open the ConnectAdmin Utility in Cerity. In the Instruments Available list, select the instrument containing the new GC module. Press Connect.

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Replacement and Service Procedures To set the carrier gas type

Confirm or update Cerity Chemical methods

Changes that require Cerity method updates If updating GC firmware from revision 1.x, or if replacing a GC module with one of a different type (for example, the new GC module uses a different column than the original), Cerity will treat the 3000 Micro GC as a new instrument. Your old methods will be saved but must be updated before use. (This behavior prevents the accidental use of an outdated or inappropriate method.) Refer to the file readme.htm on the firmware update CD-ROM for the latest details about method compatibility issues. To update existing methods Update each desired method as follows: 1. 2. In Cerity, go to the Method View and select Create. In the dialog box that appears, select Copy an existing method. Enter the required information, and select the old 3000 GC method to copy. Select OK. Cerity will create a new method, compatible with the updated instrument, containing all applicable settings from the old method. If you installed a different GC module type, input any new parameters.

3.

See the Cerity on-line help for details about using the software.

To set the carrier gas type

1. Using your web browser, establish communication between the GC and your computer. See To change the instruments IP address on page 136 for details. Select tab Gas Type. You will get a screen similar to that shown in Figure 56. The current gas configuration for installed modules is shown. (Note that in the Used By column, m1 and m2 represent channels A and B respectively. Entries m3 and m4 represent channels C and D, if installed.)

2.

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Figure 56. Representative screen for current gas configuration

3. 4. To change the gas configuration, press Make Changes... When prompted for a user name and password, enter gasconfig for both. You will see a screen similar to the one shown below.

Figure 57. Representative screen for changing gas configuration

5. 6. Select the carrier gas connection corresponding to the appropriate GC module(s). Select Submit. Select the new carrier gas type from the drop-down list.

Select new gas type

Figure 58. Selecting a new carrier gas type

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7.

Select Submit. This turns the column heaters off (to cool the columns and avoid thermal shock) and displays the Check Status view.

Figure 59. Check status view

8. Select Check Status to display a window which shows the current column temperature(s). When the column temperatures are below 60C, close the Check Status window. You can cancel changes up to this point by closing the browser or by using the browser Back feature.

Periodically refresh display

Actual column temperatures

Figure 60. Representative check status window

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9.

Now, select Continue from the 3000 Micro GC Status view to implement the configuration change.

Figure 61. Restart screen for gas configuration

10. Change the gas supply connections at the GC back panel, and check for leaks.

Caution

After selecting Restart, do not turn off power to the instrument! Wait at least 2 minutes for the instrument software to restart, then select the Status tab from the browser. When the GC responds, it is available for use. 11. Select Restart. The Restart command resets the GC electronics, and takes approximately 3 minutes. To use the reconfigured GC, open Agilent Cerity Chemical. You must create a new method for the instrument. Note that changing the gas type turns off the detector filaments. Turn the filament(s) on before use. To verify the change, select the Utilities tab from the Agilent 3000 web page and select Full Config.

To change the instruments IP address

To use the system on a local LAN, first obtain the IP address, Subnet mask, and default Gateway for the GC from your local LAN administrator to avoid conflicts with other devices on the network (including printers).

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Replacement and Service Procedures To change the instruments IP address

The LAN administrator may also add DNS (Domain Name System) and WINS (Windows Internet System) addresses, if desired. They are used to access the web or to browse a network that uses DHCP (Dynamic Host Control Protocol). If using DHCP, the GCs must be assigned fixed IP addresses. If you will use the instrument with a crossover cable connected directly to the PC, make sure that the following parts of the IP address are identical between the GC and the PC: 1. The first three parts of the IP address, e.g. 10.1.1 The subnet mask Start a web browser, and enter the current GC IP address into the address line. Your browser will connect to the GC. For example, if the IP address is 10.1.1.101, enter: http://10.1.1.101. See Figure 62.

Figure 62. Agilent 3000 web page

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Replacement and Service Procedures To change the instruments IP address

2.

Select the IP Config tab. The screen displays the current IP communication settings for the GC.

Figure 63. Representative screen displaying current IP settings

3. Select Make changes... When prompted, enter ipconfig as the user name, and ipconfig as the password. You will get a screen similar to Figure 64.

Figure 64. Representative screen for changing IP settings

4. Enter the new Host Name, Domain Name, IP address, Subnet Mask, Gateway Address, and DNS server information. Print this screen using the web browser to make a record of this information. Keep the printout in a safe, convenient place.

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Replacement and Service Procedures To change the instruments IP address

5.

Select Submit. An information screen appears.

Figure 65. Preparing for shutdown Caution

Do not turn off the GC yet. The changes can be lost. After selecting the Shutdown or Restart button, it takes 3 minutes for the GC to complete the changes. 6. Select Shutdown. The GC will respond that it is shutting down. Wait 3 full minutes. (Note: new links are shown on screen will not work until you complete the next steps.)

Figure 66. Example shutdown screen

7. 8. Turn off the GC. If needed, reconfigure your PCs IP address for local LAN use.

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Replacement and Service Procedures To restore a lost or unknown IP address

9.

If needed, disconnect the crossover cable, and connect the GC and the PC to the local LAN using standard LAN cables (part no. G1530-61485).

LAN hub (customer provided)

LAN cables G1530-61485 Simple LAN installation

Figure 67. A typical LAN cabling setup

10. If needed, reboot the PC. 11. Turn on the GC. 12. After approximately 3 minutes, the GC will beep. Reconnect to the GC using the new IP address. If available, the link(s) shown on the GC web page should connect to it. (See Figure 66.) Alternately, open the Command Prompt [C:\>], and use the ping command to verify the connection. For example, if your new GC IP address is 10.1.1.102, enter ping 10.1.1.102. You should see a reply similar to that shown in Figure 68. If the GC does not reply, see Verify communications on page 101.

To restore a lost or unknown IP address

In addition to the default IP address listed in Table 2 on page 20, a second, fixed address is available. GC Emergency address:
IP Address Subnet mask 192.168.1.99 255.255.255.0

Restore communications as described below: 1. Connect the computer directly to the instrument using a crossover cable (part 5183-4649).

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Replacement and Service Procedures To restore a lost or unknown IP address

2.

Set the computers IP address to the following:

Computer IP Address Subnet mask Gateway* DNS server* 192.168.1.100 255.255.255.0

* The gateway and DNS server entries are not used for direct connection.

See Set IP address on page 19 for details. 3. Open the MS DOS Command Prompt [C:\>], and enter: ping 192.168.1.99 The instrument should respond as shown below.

Figure 68. Ping reply from 192.168.1.99

If communication cannot be established, contact your Agilent service representative. 4. Change the instruments IP address as needed. For details, see To change the instruments IP address on page 136.

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Replacement and Service Procedures Replacing the Micro GC Portable battery

Replacing the Micro GC Portable battery

To replace the battery, do the following: 1. 2. 3. 4. Turn the carrier gas off, turn off the power and disconnect the power cord. Remove the top cover (see Remove the covers on page 116). Turn the unit over and remove the bottom cover. Facing the front panel of the unit, you will see the battery compartment on the left side. See Figure 69. The panel covering the compartment is held by two Torx screws on the outer edge of the panel. Remove these screws and remove the panel.

Battery compartment cover

Battery

Figure 69. Micro GC Portable battery compartment

5. Lift the dual battery pack to expose the wiring connections. a. Disconnect the positive (+) wires from the batterys male spade lugs.

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Replacement and Service Procedures Replacing the Micro GC Portable battery cable fuse

b.

Disconnect the batterys negative () jumper wires from the GC power harness. The new battery comes with negative jumper wires installed. See Figure 70.

Connect negative () harness leads from GC to female spade lugs on battery jumper wires

Connect positive (+) harness leads from GC to male spade lugs on battery

NOTE: Figure shown is not to scale Battery lifting strap is not shown

Figure 70.

Battery and connections

6. 7. Connect the wires to the new battery as shown in Figure 70. As you lower the new battery into place, guide the wires through the chassis holes and pull any remaining slack through the other side of the chassis to avoid crimping or pinching the wires. The positive battery terminals should be nearest the GC back panel when the battery is properly installed. 8. 9. Replace the battery compartment and bottom cover. Replace the top cover.

Send the lead-acid battery back to Agilent for recycling (see Recycling the Product on page 2) or dispose of the battery in accordance with your local laws.

Replacing the Micro GC Portable battery cable fuse

The battery cable fuse is located as shown in Figure 71.

WARNING

Be sure to turn the GC power off and unplug the instrument before replacing the fuse. Momentary flashing of some LEDs inside the GC is normal when replacing the battery cable fuse.

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Replacement and Service Procedures Accessory replacement procedures

Fuse, 3AG Slow-Blow, 10 A 32 V Type T

Figure 71. Battery cable fuse location

Accessory replacement procedures

Replacing the external 10-micron particle filter
To GC Part B Part A Ferrule Filter disk

Figure 72. Replacing the standard filter disk

1. 2. 3. 4. 5. 6. Shut off any sample flow to the GC. Let the GC inlet cool. Disconnect any sample line or conditioner to the filter body. Using a 5/16-inch wrench remove Part B in Figure 72 above. Replace used filter with a new one. (part 5183-4652, 5/pk). Reassemble filter body. Turn part B clockwise until finger-tight, then turn it 1/4 turn passed finger-tight using the wrench.

Caution

Do not overtighten the external filter onto the GC. Use a wrench to secure the external filter when installing the sample line. 7. 8. Attach sample line or conditioner to filter body. Resume sample flow as needed.

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Replacement and Service Procedures Accessory replacement procedures

Replacing the 2-micron filter in the G2819A heated vaporizer

WARNING
Disconnect power before servicing. Refer servicing to Agilent Technologies personnel. The filter trap disconnect assembly uses a replaceable cartridge filter, part number 5181-1294 (4/pk). If the sample vessel is installed on the sample line, remove it as follows: 1. 2. Close the ball valve stopcock on the sample vessel, if attached to the sample line. Open the relief valve (turn to Vent) on the heated vaporizer and release all residual pressure remaining in the sample line. Close the relief valve (turn to Sample). Disconnect the sample vessel from the sample line at the quick disconnect. See Figure 28. Disassemble the trap halves and replace the filter unit.

3. 4.

Replacing the 7-micron filter in the G2818A heated regulator

The filter trap disconnect assembly uses a replaceable cartridge filter, part number 5180-4108. 1. 2. 3. Turn off the sample flow to the instrument and vent any backpressure. Unplug the heated sample conditioner power cord and allow the unit to cool. Loosen the screws that secure the cover in place and remove the cover.

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Replacement and Service Procedures Accessory replacement procedures

4.

Remove the 1/16-inch line at the bottom of the filter assembly, then remove the nut at the bottom of the filter.

Remove from heater block

7-m filter

Remove nut. Remove 1/16-inch line

Figure 73. Replacing the 7-m filter

5. 6. Disconnect the filter from the heater block. Disassemble the trap halves and replace the filter unit.

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Replacement Parts
This section lists the replacement part numbers for the 3000 Micro GC. Before attempting to perform an on-site replacement, contact your Agilent service representative to discuss possible solutions.

Power cables and converters

Each 3000 Micro GC requires one converter and one power cable.

2 2-Conductor, 70 VA power cable and converter for G2801A/G2803A shown. Description 1. Power Cord, 2-conductor, for G2801-60569 converter - United States - South Africa/India - Europe/Switzerland/Israel - Australia/New Zealand - UK/Hong Kong/Singapore/ Malaysia - China - Chile - Argentina - Japan - Korea 2. Converter, 70 VA, for 12-channel standard Micro GCs (G2801A/G2803A) 3. Power Cord, 3-conductor, for G2801-60639/60634 converters - United States 8120-1378 8120-6313 8120-8421 8120-8340 8120-8337 8120-8719 8120-8689 8120-8452 8120-8451 8120-8336 8120-8420 G2801-60569 Agilent part no.

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Replacement Parts GC modules

Description - South Africa/India - Europe - Switzerland - Israel - Australia/New Zealand - UK/Hong Kong/Singapore/Malaysia - China - Chile - Argentina - Japan - Denmark 4. 24 VDC AC Adapter for 3 and 4-channel Micro GCs 5. 15 VDC AC Adapter for the Micro GC Portable 6. Automobile power charger for the Micro GC Portable 7. Replacement Dual Battery Pack for the Micro GC Portable

Agilent part no. 8120-4211 8120-1689 8120-2104 8120-5182 8120-1369 8120-8705 8120-8376 8120-6978 8120-6869 8120-4753 8120-3997 G2801-60639 G2801-60634 G2751-60530 G2801-61066

GC modules
Label

Remove cap over inlet fitting

Figure 74. The Agilent 3000 GC module

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Replacement Parts GC modules

The GC module assembly contains the injector, column, column heater, detector and connecting tubing. To order a replacement GC module with either a fixed or variable injector, order the Agilent part number specified in Table 24.

Table 24.

Original GC Module and Replacement Kit Part Numbers

Injector type Fixed Fixed Fixed Fixed Fixed Fixed Fixed Fixed Fixed Fixed Fixed Fixed Variable Variable Variable Variable Variable Variable Variable Variable Variable Variable Variable Variable Fixed 1 Fixed 1 Part no. on top of original GC module G2801-60507 G2801-60508 G2801-60509 G2801-60850 G2801-60860 G2801-60510 G2801-60511 G2801-60512 G2801-60513 G2801-60514 G2801-60506 G2801-60516 G2801-60537 G2801-60538 G2801-60539 G2801-60535 G2801-60545 G2801-60540 G2801-60541 G2801-60542 G2801-60543 G2801-60544 G2801-60536 G2801-60546 G2801-61107 G2801-61114 Order replacement kit part no. Replacement G2801-61002 G2801-61003 G2801-61004 G2801-61000 G2801-61010 G2801-61005 G2801-61006 G2801-61007 G2801-61008 G2801-61009 G2801-61001 G2801-61011 G2801-61014 G2801-61015 G2801-61016 G2801-61012 G2801-61022 G2801-61017 G2801-61018 G2801-61019 G2801-61020 G2801-61021 G2801-61013 G2801-61023 G2801-61042 G2801-61061 Exchange G2801-69002 G2801-69003 G2801-69004 G2801-69000 G2801-69010 G2801-69005 G2801-69006 G2801-69007 G2801-69008 G2801-69009 G2801-69001 G2801-69011 G2801-69014 G2801-69015 G2801-69016 G2801-69012 G2801-69022 G2801-69017 G2801-69018 G2801-69019 G2801-69020 G2801-69021 G2801-69013 G2801-69023 G2801-69042 G2801-69061

Column option OV-1, 4 m 0.15 mm 1.2 m OV-1, 8 m 0.15 mm 1.2 m OV-1, 6 m 0.15 mm 2.0 m OV-1, 8 m 0.15 mm 2.0 m OV-1701, 8 m 0.1 mm 0.5 m MolSieve 5A PLOT, 10 m 0.32 mm Alumina PLOT, 10 m 0.32 mm PLOT Q, 8 m 0.32 mm PLOT U, 4 m 0.32 mm PLOT U, 6 m 0.32 mm PLOT U, 8 m 0.32 mm Stabilwax DB, 10 m 0.5 m OV-1, 4 m 0.15 mm 1.2 m OV-1, 8 m 0.15 mm 1.2 m OV-1, 6 m 0.15 mm 2.0 m OV-1, 8 m 0.15 mm 2.0 m OV-1701, 8 m 0.1 mm 0.5 m MolSieve 5A PLOT, 10 m 0.32 mm Alumina PLOT, 10 m 0.32 mm PLOT Q, 8 m 0.32 mm PLOT U, 4 m 0.32 mm PLOT U, 6 m 0.32 mm PLOT U, 8 m 0.32 mm Stabilwax DB, 10 m 0.5 m OV-1, 10 m 0.15 mm 2.0 m 1 OV-1, 14 m 0.15 mm 2.0 m 1

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Replacement Parts GC modules

Table 24.

Original GC Module and Replacement Kit Part Numbers (Continued)

Injector type Variable 1.0 L Backflush 0.4 L Backflush 0.4 L Backflush 1.0 L Backflush 1.0 L Backflush 0.4 L Backflush Part no. on top of original GC module G2801-61115 G2801-61108 G2801-61109 G2801-61110 G2801-60501 G2801-60502 G2801-60503 Order replacement kit part no. Replacement G2801-61062 G2801-61043 G2801-61044 G2801-61045 G2801-61046 G2801-61047 G2801-61048 Exchange G2801-69062 G2801-69043 G2801-69044 G2801-69045 G2801-69046 G2801-69047 G2801-69048

Column option OV-1, 14 m 0.15 mm 2.0 m OV-1, 10 m 0.15 mm 2.0 m Stabilwax DB 1.2 m 0.25 mm 0.5 m Alumina PLOT, 14 m, 0.25 mm Alumina PLOT, 1 m 0.25 mm Alumina PLOT, 14 m 0.32 mm Alumina PLOT, 1 m 0.32 mm MolSieve 5A PLOT, 10 m 0.32 mm PLOT U, 3 m 0.32 mm PLOT U, 8 m 0.32 mm PLOT Q, 1 m 0.32 mm Alumina PLOT, 10 m 0.32 mm Alumina PLOT, 1 m 0.32 mm
1

For RGA analyzer

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Replacement Parts Accessories and filters

Accessories and filters

Description
Gas-liquid separator Pressure reducer Gas-liquid separator and pressure reducer Heated regulator for gas sampling for G2801A/G2803A for G2802A/G2804A for G2805A Gas sampling tubing, 1/16-inch, stainless steel with fittings 7-micron particle filter for G2818A/G2845A Heated vaporizer for LPG sampling for G2801A/G2803A for G2802A/G2804A for G2805A 2-micron particle filter element for G2819A/G2846A (4/pk) External 10-micron particle filter body External 10-micron particle filter (5/pk) Dual-end sample filter ferrule Carrier gas filter Digital I/O module Cylinder Recharging Kit (for Micro GC Portable)

Part no. G2817A G2815A G2816A

G2818A G2845A G2857A 5185-5817 3150-0786

G2819A G2846A G2858A 0100-2034 G2801-60900 5183-4652 FRL-1269 3150-0602 G2847A PNU-2058

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Replacement Parts Cables

Cables
Description
Cable, LAN 10/100 BaseT, RJ-45, 25 feet Cable, cross-over, ethertwist, 10 feet General purpose remote cable (for digital I/O module)

Part no. G1530-61485 5183-4649 G2801-60618

Plumbing supplies
Description MPC plumbing kit 1/8-inch Swagelok brass T fitting 1/8-inch Swagelok brass nut and ferrule sets 1/8-inch ball valves Copper tubing, 1/8-inch 1 2 2 12 feet (3.7 m) Qty. Part no. G1290-60515

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Replacement Parts Calibration samples

Calibration samples
Description Regulator for calibration mix cylinders Carry case for calibration mix cylinders Universal calibration mix cylinder NGA calibration mix cylinder RGA calibration mix cylinder Universal calibration kit contains: - Universal calibration mix cylinders - Regulators for calibration mix cylinders - Sample gas tubing - Carry case for calibration mix cylinders NGA calibration kit contains: - Universal calibration mix cylinder - NGA calibration mix cylinder - Regulators for calibration mix cylinders - Sample gas tubing - Carry case for calibration mix cylinders Refill cylinders for NGA calibration kit RGA calibration kit contains: - Universal calibration mix cylinder - RGA calibration mix cylinder - Regulators for calibration mix cylinders - Sample gas tubing - Carry case for calibration mix cylinders Refill cylinders for RGA calibration kit 1 1 2 2 1 1 set 5184-3545 1 1 2 2 1 1 set 5184-3544 5184-3548 2 2 2 1 5184-3547 Shipping qty. 1 1 2 2 2 Part no. 5184-3539 5184-3540 5184-3541 5184-3542 5184-3543 5184-3546

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Site Preparation
Tools and items needed for installation
Hardware
1/8-inch (or 1/4-inch) preconditioned copper tubing 1/8-inch (or 1/4-inch, if used) Swagelok nuts, and front and back ferrules Two 7/16-inch wrenches 5/16-inch wrench 9/16-inch wrench 1/4-inch wrench

Other items
IP address settings for GC and computer (for LAN use) Personal computer compatible with the Agilent Cerity Chemical software LAN cables (for LAN use) Electronic leak detector (optional) Flowmeter (optional; digital flowmeter preferred)

Ventilation requirements
For optimum instrument performance and lifetime, allow unrestricted airflow around the instrument to allow heat generated by the instrument to dissipate. Safely vent carrier and sample streams, potentially toxic, noxious, or flammable gases outside the instrument away from the operating area. If needed, vent toxic gases or components to a chemical trap or reaction medium. Avoid venting your instrument into an area with wind pressure variations, such as in front of a heating/cooling vent.

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Site Preparation Carrier gases

Carrier gases
A continuous, controlled flow of carrier gas before and during analysis is necessary. Agilent recommends instrument or chromatographic purity grades of gases specifically intended for chromatographic use. Generally, all gas supplies should be in the 99.995% to 99.9995% purity range, with only very low levels (< 0.5 ppm) of oxygen and total hydrocarbons present. Helium is the preferred carrier gas for natural gas applications, but the instrument is also compatible with hydrogen and argon. Use 1/8-inch Swagelok fittings for connections.

Gas plumbing
Compressed gas cylinder safety
1. Securely fasten all compressed gas cylinders to an immovable structure or permanent wall. Store and handle compressed gases in accordance with relevant safety codes. Do not store gas cylinders in the path of heated oven exhausts or other sources of heat. To avoid possible eye injury, wear eye protection when using compressed gas.

2. 3.

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Site Preparation Gas plumbing

Installation
1. Follow the general plumbing diagram when preparing gas supply plumbing. Use traps to protect the columns. Place traps in the order shown.
Main supply on/off valve Two stage regulator (high quality stainless-steel packless diaphragm type) On/off valve with packless diaphragms Moisture trap Hydrocarbon trap To GC Carrier gas filter 3180-0602 Shut-off valve Main gas supply Seal connections with instrument-grade Teflon tape (0460-1266) Oxygen trap

Figure 75.

General plumbing diagram

Agilent also recommends installing shut-off valves near the GC.

Table 25.
Description

Recommended Traps
Agilent part no. 5060-9084

Preconditioned moisture trap: metal casing, s-shaped trap for carrier gas cleanup. Contains Molecular Sieve 5A, 45/60 mesh, and 1/8-inch fittings. Hydrocarbon trap: metal casing, s-shaped trap filled with 40/60 mesh activated charcoal, and 1/8-inch fittings. Oxygen trap (for carrier gas): glass casing, indicating, with 1/8-inch fittings. Oxygen trap cannot be reconditioned. Carrier gas filter

5060-9096 IOT-2-HP 3150-0602

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Site Preparation Gas plumbing

Regulators Set your input pressure between 538 and 566 kPa (78 and 82 psi). The Agilent 3000 pressure-controlling devices require at least 10 psi (138 kPa) pressure differential across them to operate properly. Be sure that source pressures and capacities are high enough to provide this. Locate auxiliary pressure regulators close to the instrument rather than at the source; pressure at the source may be different if the gas supply tubing is long or narrow. Tubing Do not use ordinary copper tubing which contains oils and contaminants. Do not use plastic tubing for supplying inlet gases to the GC. It is permeable to oxygen and other contaminants that can damage columns and detectors and can melt if near hot exhaust or components. The necessary tubing diameter depends upon the distance between the supply gas and the GC and the total flow rate for the particular gas. Oneeighth-inch tubing is adequate when the supply line is less than 15 feet (4.6 m) long. Use larger diameter tubing (1/4-inch) for distances greater than 15 feet (4.6 m) or when multiple instruments are connected to the same source. Be generous when cutting tubing for local supply lines. A coil of flexible tubing between the supply and the instrument lets you move the GC without moving the gas supply. Do not use pipe dope to seal the threads; it contains volatile materials that will contaminate the tubing.

Ensuring gas purity

After installing or replacing traps, check the gas supply lines for leaks.

Connections to the GC
The GC uses 1/8-inch Swagelok fittings for the sample and carrier gases. One 1/8-inch Swagelok nut and ferrule set is required to connect to each fitting. The GC uses 1/8-inch Luer-locking fittings for low pressure gases (column and sample vents). Refer to the Agilent consumables and supplies catalog for ordering information, or visit the Agilent web site at: www.agilent.com/chem.

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Site Preparation Swagelok connections

Swagelok connections
The gas supply tubing is attached with Swagelok fittings. If you are not familiar with making Swagelok connections, review the following procedure. The procedure explains how to connect tubing to a fitting, such as inlet and detector manifolds or the gas supply tank.

Materials needed:
1/8-inch (or 1/4-inch, if used) preconditioned copper tubing 1/8-inch (or 1/4-inch, if used) Swagelok nuts, and front and back ferrules Two 7/16-inch wrenches

1.

Attach a 1/8-inch Swagelok nut, back ferrule, and front ferrule to the tubing. Use brass hardware.
Front ferrule (1/4- or 1/8-inch) Back ferrule (1/4- or 1/8-inch) Swagelok nut (1/4- or 1/8-inch)

Tubing (1/4- or 1/8-inch)

Caution

Use a separate stainless steel fitting in a vise for initial tightening of the nut. Do not use the GC fitting. Strong forces are required to properly set the ferrules, and damage to the GC fitting is very costly to repair. 2. 3. 4. Clamp a stainless steel female fitting in a bench vise. Push the tubing into the stainless steel female fitting. Make sure that the front ferrule is touching the fitting, and then slide the Swagelok nut over the ferrule and tighten it finger-tight.
Tubing, nut and ferrule assembly

Fitting in vise

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Site Preparation Swagelok connections

5.

Push the tube fully into the female fitting, then withdraw it approximately 12 mm.
Nut

Back ferrule Front ferrule

Insert tubing fully

Withdraw 12 mm

Tighten nut

6.

Mark the Swagelok fitting with a pencil line.

7.

If you are using 1/8-inch Swagelok fittings, while holding the fitting steady with the other 7/16-inch wrench, tighten the fitting 3/4 of a turn. If you are using 1/4-inch fittings, tighten them 1 1/4 turn.

8.

Unscrew the nut. Connect the tubing with the swaged ferrules to its intended location. Tighten the nut 1/4-turn past finger-tight.

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Specifications
Technical specifications
G2801A, G2803A Micro GC Main voltage Power Frequency Height Width Depth Weight 100240 VAC 100 VA 5060 Hz 15 cm (6 inches) 25 cm (10 inches) 41 cm (16.5 inches) 8.2 kg (18 lb.) G2802A, G2804A Micro GC 100240 VAC 130 VA 5060 Hz 15.5 cm (6.1 inches) 48 cm (18.5 inches) 42 cm (16.5 inches) 11.2 kg (24.8 lb.) G2805A Micro GC Portable 100240 VAC 130 VA 5060 Hz 15.5 cm (6.1 inches) 36.4 cm (14.3 inches) 41.3 cm (16.3 inches) 16.6 kg (36.5 lb.) G2819A, G2846A Heated vaporizer 115/230 VAC 1.2/0.6 A 5060 Hz 15 cm (6 inches) 12.5 cm (5 inches) 9 cm (3.5 inches) 1.4 kg (3.1 lb.)* G2818A, G2845A Heated regulator 115/230 VAC 1.2/0.6 A 5060 Hz 15 cm (6 inches) 12.5 cm (5 inches) 9 cm (3.5 inches) 1.65 kg (3.64 lb.)*

* Does not include mounting bracket.

Environmental conditions
Micro GC Operating temperature range Relative humidity Altitude Usage 0 to 50C 5 to 95% (non-condensing) to 15,000 ft. (4,572 m) Indoor or enclosed Heated vaporizer or heated regulator 0 to 50C 5 to 95% (non-condensing) to 15,000 ft. (4,572 m) Indoor or enclosed

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