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Agilent 7820A Chromatograph Operating Guide PDF
Summary of Content for Agilent 7820A Chromatograph Operating Guide PDF
Agilent 7820A Gas Chromatograph
Operating Guide
Agilent Technologies
Notices Agilent Technologies, Inc. 2016
No part of this manual may be reproduced
in any form or by any means (including
electronic storage and retrieval or transla-
tion into a foreign language) without prior
agreement and written consent from
Agilent Technologies, Inc. as governed by
United States and international copyright
laws.
Manual Part Number
G4350-90012
Edition
Fifth edition, August 2016
Fourth edition, June 2015
Third edition, June 2011
Second edition, October 2009
First edition, March 2009
Printed in China
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Acknowledgements
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Safety Notices
CAUTION
A CAUTION notice denotes a hazard. It
calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
WARNING
A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.
Contents
1 Introduction
Operation Manual
Where to Find Information 10
Online User Documentation 10
Agilent Customer Portal 11
Chromatography Using a GC 12
The Front View of the Agilent 7820A GC 13
The Back View of the Agilent 7820A GC 14
The Inlets 15
The GC Column and Oven 17
Detectors 18
The Operating Panel 19
The display 19
Indicator Lights 20
Alert Tones 20
The keypad 21
2 Operating Basics
Overview 24
Instrument Control 25
To Start Up the GC 26
To Shut Down the GC for Less Than a Week 27
To Shut Down the GC for More Than a Week 28
Correcting Problems 29
3 Software Keypad Operation
To Install the Software Keypad 32
The Software Keypad 33
To connect to a GC 33
To disconnect from a GC 34
Other program settings 34
To minimize or expand the software keypad 35
To troubleshoot a connection 35
To get help 35
The Run Keys 36
The GC Component Keys 37
3
4
The Status Key 38
The Info Key 39
The General Data Entry Keys 40
The Supporting Keys 41
Method Storage and Automation Keys 42
Keypad Functionality When the GC Is Controlled by an Agilent Data
System 43
The Service Mode Key 44
About GC Status in the Software Keypad 45
Indicators 45
Error conditions 45
Blinking setpoint 45
About Logs 47
4 Running a Method or a Sequence from the Software Keypad
Loading, Storing, and Running Methods from the Software Keypad 50
To manually inject a sample with a syringe and start a run 50
To run a method to process a single ALS sample 50
To abort a method 50
Loading, Storing, and Running Sequences from the Software Keypad 51
To start running a sequence 51
To pause a running sequence 51
To resume a paused sequence 52
To stop a running sequence 52
To resume a stopped sequence 52
Aborting a sequence 52
To resume an aborted sequence 52
5 Methods and Sequences
What Is a Method? 54
What Is Saved in a Method? 54
What Happens When You Load a Method? 55
Creating Methods 56
To load a method 57
To store a method 57
What Is a Sequence? 59
Creating Sequences 59
Automating Data Analysis, Method Development, and Sequence
Development 63
Operation Manual
Operation Manual
Recoverable Errors 64
6 Chromatographic Checkout
About Chromatographic Checkout 66
To Prepare for Chromatographic Checkout 67
To Check FID Performance 69
To check FID performance with a packed column inlet (PCI) 69
To check FID performance with a purged packed, split splitless or cool-on
column inlet 73
To Check TCD Performance 77
To check TCD performance with a packed column inlet (PCI) 77
To check TCD performance with a purged packed, split splitless or
cool-on column inlet 81
To Check NPD Performance 85
To Check uECD Performance 89
To Check FPD+ Performance (Sample 5188-5953) 93
Preparation 93
Phosphorus performance 94
Sulfur performance 97
To Check FPD+ Performance (Sample 5188-5245, Japan) 99
Preparation 99
Phosphorus performance 100
Sulfur performance 103
To Check FPD Performance (Sample 5188-5953) 105
Preparation 105
Phosphorus performance 106
Sulfur performance 109
To Check FPD Performance (Sample 5188-5245, Japan) 111
Preparation 111
Phosphorus performance 112
Sulfur performance 115
7 Configuration
About Configuration 118
Assigning GC resources to a device 118
Setting configuration properties 119
General Topics 120
To Unlock the GC Configuration 120
Ignore Ready = 120
Information displays 121
5
6
Unconfigured: 121
Oven 122
Front Inlet/Back Inlet 123
To configure the Gas type 123
Column # 124
To view a summary of column connections 126
About Heaters 127
Front Detector/Back Detector 128
To configure the makeup/reference gas 128
Lit offset 128
To configure the FPD or FPD+ heaters 128
To ignore the FID, FPD, or FPD+ ignitor 129
Analog Out 130
Fast peaks 130
Valve Box 131
To assign a GC power source to a valve box heater 131
Thermal Aux 132
PCM A/PCM B 134
Status 135
Time 136
Valve # 137
Front injector/Back injector 138
Instrument 139
8 Options
About Options 142
Calibration 142
To zero a specific flow or pressure sensor 144
Column calibration 144
Communication 149
Configuring the IP address for the GC 149
Keyboard and Display 150
9 Configuration Tasks
About the GC IP Address 154
To set the IP address at the GC 155
To Use DHCP to Provide the GC IP Address 156
Operation Manual
Operation Manual
To restore the default GC IP address 157
To Reconfigure an EPC Module for Another Detector 158
7
8
Agilent 7820A Gas Chromatograph Operating Guide
1 Introduction
Where to Find Information 10
Chromatography Using a GC 12
The Front View of the Agilent 7820A GC 13
The Back View of the Agilent 7820A GC 14
The Inlets 15
The GC Column and Oven 17
Detectors 18
The Operating Panel 19
This document provides an overview of the individual components that make up the Agilent 7820A Gas Chromatograph (GC).
9Agilent Technologies
1 Introduction
Where to Find Information
10
In addition to this document, Agilent provides several learning products that document how to install, operate, maintain, and troubleshoot the Agilent 7820A GC.
Before operating your GC, be sure to read the safety and regulatory information included on the Agilent GC and GC/MS User Manuals & Tools DVD. The most common safety hazards when working on the GC are:
Burns caused by touching heated areas on or in the GC
Release of pressurized gas containing hazardous chemical compounds caused by opening inlets
Glass cuts or puncture wounds caused by sharp capillary column ends
Use of hydrogen as a GC carrier gas
Online User Documentation
Now your Agilent instrument documentation is in one place, at your fingertips.
The Agilent GC and GC/MS User Manuals & Tools DVD that ships with your instrument provides an extensive collection of online help, videos, and books for current Agilent gas chromatographs, mass selective detectors, and GC samplers. Included are localized versions of the information you need most, such as:
Getting Familiar documentation
Safety and Regulatory guide
Site Preparation information
Installation information
Operating Guide
Introduction 1
Operating Guide
Operating guides
Maintenance information
Troubleshooting details
Agilent Customer Portal
Agilent also provides customized information for the products you own through a customer portal. This web service provides many customizable services as well as information related directly to your Agilent products and orders. Log onto the portal at http://www.agilent.com/chem.
11
1 Introduction
Chromatography Using a GC
12
Chromatography is the separation of a mixture of compounds into individual components.
There are three major steps involved with separating and identifying components of a mixture using a GC. They are:
1 Injecting a sample into the GC. (This takes place at the inlet.)
2 Separating the sample into individual components. (This takes place inside the column in the oven.)
3 Detecting what compounds were in the sample. (This is done in the detector.)
During this process, status messages from the Agilent 7820A GC are shown on the display. User changes to parameter settings can be made through the software keypad.
Each part of this process is described in brief on the following pages of this document. Refer to the Advanced Operating Manual and the Getting Started manual for more details.
Inlet
Detector
Oven
Operating panel
Operating Guide
Introduction 1
The Front View of the Agilent 7820A GC
Operating Guide
Detector cover
Detectors
Inlets
Valves (not shown)
Display
Keypad
Power switch
Oven latch
13
1 Introduction
The Back View of the Agilent 7820A GC
14
Inlet vent
Gas supply connections
Electronic cable connections
Oven cooling intake and exhaust vent
Power connection
Operating Guide
Introduction 1
The Inlets
Operating Guide
Inlets are where samples are injected into the GC. The Agilent 7820A GC can have a maximum of two inlets, identified as Front Inlet and Back Inlet.
The following inlet types are available:
Split/splitless inlet
Purged packed inlet
Packed column inlet
Cool on column inlet
The type of inlet chosen is based on the type of analysis being done, the type of sample being analyzed, and the column being used.
Samples can be injected into the inlets by hand using a syringe, or an automatic sampling device (such as an Agilent Automatic Liquid Sampler or Agilent Headspace Sampler).
15
16
1 Introduction
Automatic injectors
The Agilent 7820A GC can accommodate up to two autoinjectors, identified as Front Injector and Back Injector.
Automatic gas sampling valves
The optional sampling valves are simple mechanical devices that introduce a sample of fixed size into the carrier gas stream. Valves are most frequently used to sample gases in constantly flowing streams.
The Agilent 7820A GC can accommodate up to two gas sampling valves, identified as Valve # 1 and Valve #2.
The valves are located inside the gas sampling valve box.
Autoinjector
Turret
Operating Guide
Introduction 1
The GC Column and Oven
Operating Guide
GC columns are located inside a temperature-controlled oven. Generally, one end of the column is attached to the inlet, while the other end is attached to the detector.
Columns vary in length, diameter, and internal coating. Each column is designed for use with different compounds.
The purpose of the column and the oven is to separate the injected sample into individual compounds as it travels through the column. To aid this process, the GC oven can be programmed to speed the sample flow through the column.
17
1 Introduction
Detectors
18
Detectors identify the presence of compounds as they exit the column.
As each compound enters the detector, an electrical signal proportional to the amount of compound detected is generated. This signal is generally sent to a data analysis systemsuch as Agilent OpenLAB CDS ChemStation editionwhere it shows up as a peak on a chromatogram.
The Agilent 7820A GC can accommodate up to two detectors, identified as Front Det and Back Det.
A complete selection of detectors (FID, TCD, NPD, FPD, FPD+, ECD, and MSD) is available. The type of detector chosen is based on the type of analysis required.
Operating Guide
Introduction 1
The Operating Panel
Operating Guide
The operating panel consists of the display, status lights, and keypad. See Software Keypad Operation and the Advanced Operation Manual, along with the complete suite of documentation included on the Agilent GC and GC/MS User Manuals & Tools DVDs that are included with your GC shipment for more detailed information.
Actual Setpoint
Stop Prep Run Start
STATUS READY Last run 0.15 Next run time 3.00 Oven temperature 35 35
RunNot Ready
Display
Indicator lights
Keys
The display
The display shows details of what is currently happening in the Agilent 7820A GC.
The cursor, <, shows the current active line. The display shows current temperatures, flows, pressures, and information about GC readiness. Use the scroll keys to select a different line in the display and to view additional lines in the display.
19
1 Introduction
Indicator Lights
20
The GC has two status indicators below the display, Not Ready and Run.
When the GC is ready to begin a run, the display screen shows STATUS Ready for Injection. Alternatively, when a component of the GC is not ready to begin a run, the Not Ready indicator lights. Scroll to see a message explaining why the GC is not ready.
Not Ready Lights when the GC is not yet ready to process a
sample and blinks when a fault occurs. Scroll to see
which parameters are not ready or what faults have
occurred.
Run Lights when the instrument is executing a
chromatographic run. Blinks green when in pre-run
state, for example when a split/splitless inlet is
purging.
Alert Tones
A series of warning beeps sounds before a shutdown occurs. After a short time the component with the problem shuts down, the GC emits one beep, and a brief, numbered message is displayed. For example, a series of beeps sounds if the front inlet gas flow cannot reach setpoint. The message Front inlet flow shutdown is briefly displayed. The flow shuts down after 2 minutes. See Correcting Problems.
A continuous tone sounds if a hydrogen flow is shut down or a thermal shutdown occurs.
WARNING Before resuming GC operations, investigate and resolve the cause of the hydrogen shutdown. See Hydrogen Shutdown in the Troubleshooting manual for details.
One beep sounds when a problem exists, but the problem will not prevent the GC from executing the run. The GC will emit one beep and display a message. The GC can start the run and the warning will disappear when the run starts.
Other messages indicate hardware problems that require user intervention. Depending on the type of error, the GC emits no beep or a single beep.
Operating Guide
Introduction 1
The keypad
Operating Guide
The GC has three operating keys.
[Stop] Immediately terminates the run. If the GC is in the middle of a run, the data from that run may be lost. Refer to the Advanced Operation Manual for information on how to restart the GC after pressing [Stop].
[Prep Run] Activates processes required to bring the GC to the starting condition dictated by the method (such as turning off the inlet purge flow for a splitless injection or restoring normal flow from gas saver mode).
[Start] Starts a run after manually injecting a sample. (When you are using an automatic liquid sampler or gas sampling valve, the run is automatically activated at the appropriate time.)
Scrolls up and down through the display one line at a time. Use to view:
Remaining run time
Next run time
Current status messages (what the GC is doing)
Current temperatures, pressures, and flows
Valve state
GC firmware revision
GC IP address
System date and time
21
22
1 Introduction
Operating Guide
Agilent 7820A Gas Chromatograph Operating Guide
2 Operating Basics
Overview 24
Instrument Control 25
To Start Up the GC 26
To Shut Down the GC for Less Than a Week 27
To Shut Down the GC for More Than a Week 28
Correcting Problems 29
This section describes a few basic tasks that an operator performs when using the Agilent 7820A GC.
23Agilent Technologies
2 Operating Basics
Overview
24
Operating the GC involves the following tasks:
Installing the software keypad.
Setting up the GC hardware for an analytical method.
Starting up the GC. See To Start Up the GC.
Preparing the automatic liquid sampler. Install the method-defined syringe; configure solvent and waste bottle usage and syringe size; and prepare and load solvent, waste, and sample vials.
For the 7693A ALS, see its Installation, Operation, and Maintenance manual.
Loading the analytical method or sequence into the GC control system.
See the Agilent data system documentation.
For standalone GC operation see To load a method and To load a stored sequence.
Running the method or sequence.
See the Agilent data system documentation.
For standalone GC operation, see To manually inject a sample with a syringe and start a run, To run a method to process a single ALS sample, and To start running a sequence.
Monitoring sample runs from the GC control panel or the Agilent data system program. See About GC Status in the Software Keypad or the Agilent data system documentation.
Shutting down the GC. See To Shut Down the GC for Less Than a Week or To Shut Down the GC for More Than a Week.
Operation requires an available PC with the software keypad installed. See Software Keypad Operation for details.
Operating Guide
Operating Basics 2
Instrument Control
Operating Guide
The Agilent 7820A GC is typically controlled by an attached data system such as Agilent OpenLAB CDS EZChrom Compact. Alternately, the GC can be controlled entirely from a software keypad, with output data being sent to an attached integrator for report generation.
Agilent data system users Please refer to the online help included in the Agilent data system for details on how to load, run, or create methods and sequences using the data system.
Standalone GC users If you are running your GC without an attached data system, see the following for details on loading methods and sequences from the software keypad:
To Install the Software Keypad
To load a method
To load a stored sequence
For details on running methods and sequences from the software keypad see:
To manually inject a sample with a syringe and start a run
To run a method to process a single ALS sample
To start running a sequence
Refer to the Advanced User Guide for details on how to create methods and sequences using the software keypad.
25
2 Operating Basics
To Start Up the GC
26
Successful operation begins with a properly installed and maintained GC. The utility requirements for gases, power supply, venting of hazardous chemicals, and required operational clearances around the GC are detailed in the Agilent GC, GC/MS, and ALS Site Preparation Guide Site Preparation Guide.
1 Check gas source pressures. For required pressures, see the Site Preparation Guide.
2 Turn on the carrier and detector gases at their sources and open the local shutoff valves.
3 Turn on the GC power. Wait for Power on successful to display.
4 Install the column.
5 Check that the column fittings are leak free. See the Troubleshooting manual.
6 Load the analytical method. See To load a method.
7 Wait for the detector(s) to stabilize before acquiring data. The time required for the detector to reach a stable condition depends on whether the detector was turned off or its temperature was reduced while the detector remained powered.
Table 1 Detector stabilization times
Detector type Stabilization time starting from a reduced temperature (hours)
Stabilization time starting from detector off (hours)
FID 2 4
TCD 2 4
uECD 4 18 to 24
FPD 2 12
FPD+ 2 12
NPD 4 18 to 24
Operating Guide
Operating Basics 2
To Shut Down the GC for Less Than a Week
Operating Guide
1 Wait for the current run to finish.
2 If the active method has been modified, save the changes.
Never leave flammable gas flows on if the GC will be unmonitored.
3 Turn off all gases, except the carrier gas, at their sources. (Leave the carrier gas on to protect the column from atmospheric contamination.)
4 Reduce detector, inlet, and column temperatures to between 150 and 200 C. If desired, the detector can be turned off. See the following table to determine if it is advantageous to shut down the detector for a short time period. The time required to return the detector to a stable condition is a factor. See Table 1.
27
2 Operating Basics
To Shut Down the GC for More Than a Week
28
See for procedures for installing columns, consumables, and so on.
1 Load a GC maintenance method and wait for the GC to become ready. For more information about creating maintenance methods, see the Maintaining Your GC manual. (If a maintenance method is not available, set all heated zones to 40 C.)
2 Turn off the main power switch.
3 Shut off all gas valves at the gas source.
Be careful! The oven, inlet, and/or detector may be hot enough to
4 When the GC is cool, remove the column from the oven and cap both ends to keep out contaminants.
5 Cap the inlet and detector column fittings and all GC external fittings.
Operating Guide
Operating Basics 2
Correcting Problems
Operating Guide
If the GC stops operation because of a fault, check the display for any messages. Press [Status] and scroll to view any additional messages.
1 Use the software keyboard or data system to stop the alert tone. Click [Clear] on the software keyboard or turn off the offending component in the data system. (For details on the software keyboard, see Software Keypad Operation.)
2 Resolve the problem, for example, by changing gas cylinders or fixing the leak. See the Troubleshooting Guide for details.
3 Once the problem is fixed, you may need to either power cycle the instrument, or use the software keyboard or data system to turn the problem component off, then on again. For shutdown errors, you will need to do both.
29
30
2 Operating Basics
Operating Guide
Agilent 7820A Gas Chromatograph Operating Guide
3 Software Keypad Operation
To Install the Software Keypad 32
The Software Keypad 33
The Run Keys 36
The GC Component Keys 37
The Status Key 38
The Info Key 39
The General Data Entry Keys 40
The Supporting Keys 41
Method Storage and Automation Keys 42
Keypad Functionality When the GC Is Controlled by an Agilent Data
System 43
The Service Mode Key 44
About GC Status in the Software Keypad 45
About Logs 47
This section describes the basic operation of the Agilent 7820A GC Remote Controller (software keypad). This software provides a keypad interface that allows you to connect to and control a 7820A GC. For additional information on keypad functionality, see the Advanced Operation Manual.
31Agilent Technologies
3 Software Keypad Operation
To Install the Software Keypad
32
Agilent provides 7820A GC Remote Controller software on the Agilent GC and GC/MS User Manuals & Tools DVD. To install the software, insert the DVD into your PCs DVD drive, then follow the online instructions for installing the 7820A GC documentation. After installation, you can open the software keypad from a desktop icon or from the Start menu.
The software keypad requires a LAN connection to the GC.
Operating Guide
Software Keypad Operation 3
The Software Keypad
Operating Guide
Use the software keypad to:
Operate the GC without an Agilent data system
View instrument error conditions
Prepare the GC for maintenance
Clear fault conditions
The software keypad can control only one 7820A Series GC at a time. It can connect to any 7820A GC on the PCs network.
Use only one software keypad at a time to connect to a given GC.
To connect to a GC
1 Go to Connection > Connect.
2 Select IP to enter/select an IP address, or Name to select a GC using a previously assigned name.
3 From the Target list, either enter or select the GC IP address or name.
4 Click Connect.
33
34
3 Software Keypad Operation
The software keyboard window title displays the name or IP address of the connected GC. This information also appears at the bottom of the window.
If desired, you can enable AutoConnect to always connect to the selected GC when launching the software keypad.
To disconnect from a GC
Select Connection > Disconnect.
Other program settings
Settings > Option > Connection
The Connection tab provides options for displaying user-friendly names for GCs and for enabling automatic connection to a GC when the software loads.
Enable AutoConnect to connect to the default GC when starting the software keypad. You can also set this feature from Connection > Connect.
Use Connection History to assign the default GC that appears in the Connect list. The connection history lists each GC to which you have connected.
To assign a name that will appear in the Connect list, select the GC, then click Change Name. Enter the name in the Name field, then click Save Name.
To make a GC appear as the first entry in the Connect list, select it in the history then click Set as Default.
To permanently delete all saved names and all connection history, click Clear History.
Settings > Option > ShortCuts
The ShortCuts tab allows you to enable, disable, and customize keyboard shortcuts usable with the software.
To enable keyboard shortcuts, select Enable shortcut on main panel.
Once shortcuts are enabled, you can use the default shortcuts, or select and modify them as desired. To change a shortcut, select it then click Change. Press the keystrokes for the new shortcut, then click Store to save it and OK to close the Option dialog. Shortcuts must be unique. Click Default to restore the factory shortcut values.
Operating Guide
Software Keypad Operation 3
Operating Guide
Settings > Option > Log
Select the Log tab to display the log entries compiled by the software keypad. The software logs connection events, communication errors, and similar events.
Settings > Language
Use Settings > Language to select the language for the software keypad user interface. After a brief pause, the UI reloads in the new language. This setting changes only the software keypad language, not the language of the GC.
You can also turn off language selection during program startup by deselecting Settings > Select Language Before Startup.
To minimize or expand the software keypad
Click or in the bottom right corner of the window to toggle keypad display.
To troubleshoot a connection
If the software keypad cannot connect to the GC, check the following:
Verify GC is turned on.
Verify LAN cabling is connected properly.
Verify entered IP address is correct for GC. On the GC front panel, press or to scroll to the IP entry. This the GCs current IP address.
Verify basic communications to the GC by using the ping command. See the Troubleshooting manual.
Verify that no one else is currently controlling the GC.
Make sure your PC is able to communicate with the GC. The PC IP address must be set for a similar network and subnet. For example, if the GC IP address reads 192.168.0.26 (the default value), then your PC IP address must be 192.168.0.xx, where xx is any number from 0 to 25 or 27 to 255. If the PC is set for a different LAN than the GC, you must change the PC IP address. Refer to Windows help for details. This operation may require administrative privileges on the PC.
To get help
To open the keypad software help, go to Help > Contents.
35
3 Software Keypad Operation
The Run Keys
36
These keys are used to start, stop, and prepare the GC to run a sample.
[Prep Run] Activates processes required to bring the GC to
the starting condition dictated by the method (such as turning off the inlet purge flow for a splitless injection or restoring normal flow from gas saver mode). See the Advanced Operation Manual for details.
[Start] Starts a run after manually injecting a sample. (When you are using an automatic liquid sampler or gas sampling valve, the run is automatically activated at the appropriate time.)
[Stop] Immediately terminates the run. If the GC is in the middle of a run, the data from that run may be lost. Also see To resume an aborted sequence on page 52.
Operating Guide
Software Keypad Operation 3
The GC Component Keys
Operating Guide
These keys are used to set the temperature, pressure, flow, velocity, and other method operating parameters.
To display the current settings, press any one of these keys. More than three lines of information may be available. Use the scroll keys to view additional lines, if necessary.
To change settings, scroll to the line of interest, enter the change, and press [Enter].
For context-sensitive help, press [Info]. For example, if you press [Info] on a setpoint entry, the help provided would be similar to: Enter a value between 0 and 350.
[Oven] Sets oven temperatures, both isothermal and temperature programmed.
[Front Inlet] [Back Inlet]
Controls inlet operating parameters.
[Col #] Controls column pressure, flow, or velocity. Can set pressure or flow ramps.
[PCM #] Controls column pressure, flow, or velocity for accessory pneumatic control module(s). Can set pressure or flow ramps.
[Front Det] [Back Det]
Controls detector operating parameters.
[Lite EPC #] Provides pneumatics to an inlet, detector, or other device. Use to configure the detector EPC for use. Can be used for pressure programming.
[Injector] Edits injector control parameters such as injection volumes and sample and solvent washes.
[Valve #] Allows control of a sampling valve and/or switching valves (on or off).
[Analog Out] Assigns a signal to the analog output. The analog output is located on the back of the GC.
37
3 Software Keypad Operation
The Status Key
38
[Status] Displays ready, not ready, and fault
information.
When the Not Ready status light is blinking, a fault has occurred. Press [Status] to see which parameters are not ready and what fault has occurred.
The order in which items appearin the scrolling display window for [Status] can be modified. You may, for example, want to display the things you most frequently check in the top three lines so that you do not need to scroll to see them. To change the order of the Status display:
1 Press [Config] [Status].
2 Scroll to the setpoint you want to appear first and press [Enter]. This setpoint will now appear at the top of the list.
3 Scroll to the setpoint you want to appear second and press [Enter]. This setpoint will now be the second item on the list.
4 Continue as above until the list is in the order you require.
Operating Guide
Software Keypad Operation 3
The Info Key
Operating Guide
[Info] Provides help for the currently shown
parameter. For example, if Oven Temp is the active line in the display (has a < next to it), [Info] will display the valid range of oven temperatures. In other cases, [Info] will display definitions or actions that need to be performed.
39
3 Software Keypad Operation
The General Data Entry Keys
40
[Mode/Type] Accesses a list of possible parameters associated
with a components non-numeric settings. For example, if the GC is configured with a split/splitless inlet with EPC and the [Mode/Type] key is pressed, the options listed will be split, splitless, pulsed split, or pulsed splitless.
[Clear] Removes a misentered setpoint before pressing [Enter]. It can also be used to return to the top line of a multiline display, return to a previous display, cancel a function during a sequence or method, or cancel loading or storing sequences and methods.
[Enter] Accepts changes you enter or selects an alternate mode.
Scrolls up and down through the display one line at a time. The < in the display indicates the active line.
Numeric Keys Are used to enter settings for the method parameters. (Press [Enter] when you are finished to accept the changes.)
For EPR (electronic pneumatics regulation) equipped GCs, the 2/+ and 8/- keys are used to adjust parameters settings up and down, respectively.
[On/Yes] [Off/No]
Are used when you are setting up parameters, such as the warning beep, method modification beep, and key click or for turning on or off a device like a detector.
[Front] [Back] Are mostly used during configuration operations. For example, when configuring a column, use these keys to identify the inlet and detector to which the column is attached.
[Delete] Removes methods, sequences, run table entries, and clock table entries. [Delete] also aborts the adjust offset process for nitrogen-phosphorus detectors (NPD) without interrupting other detector parameters. See the Advanced Operation Manual for more details.
Operating Guide
Software Keypad Operation 3
The Supporting Keys
Operating Guide
[Time] Displays the current date and time on the first line.
The two middle lines show the time between runs, the elapsed time and time remaining during a run, and the last run time and post-time during a post-run. The last line always displays a stopwatch. While on the stopwatch line, press [Clear] to set the clock to zero and [Enter] to start or stop the stopwatch.
[Post Run] Is used to program the GC to do something after a run, such as bakeout or backflush a column. See the Advanced Operation Manual for details.
[Logs] Toggles between two logs: the Run Log and the System Event Log. The information in these logs can be used to support Good Laboratory Practices (GLP) standards.
[Options] Accesses the instrument parameters setup option, such as keypad and display. Scroll to the desired line and press [Enter] to access the associated entries. See Options on page 141.
[Config] Is used to set up components that are not automatically detectable by the GC but are essential to running a method, such as column dimensions, carrier and detector gas types, makeup gas configurations, and column plumbing to inlets and detectors. These settings are part of, and are stored with, the method. To view the current configuration for a component (such as the inlet or detector), press [Config], then the component key of interest. For example, [Config][Front Det] opens front detector configuration parameters.
41
3 Software Keypad Operation
Method Storage and Automation Keys
42
These keys are for loading and storing methods and sequences locally on your GC. They cannot be used to access methods and sequences stored by your Agilent data system.
[Load] [Method] [Store] [Seq]
Are used together to load and store methods and sequences on your GC.
For example, to load a method, press [Load] [Method] and select one from the list of methods stored in the GC. See To load a method on page 57.
[Run Table] Is used to program special events you require during a run. A special event could be switching a valve, for example. See the Advanced Operation Manual for details.
[Clock Table] Is used to program events to occur at a time of day, as opposed to during a run, and to access the Instrument Schedule. The clock table events could, for example, be used to start a shutdown run at 5:00 p.m. every day. page 106See the Advanced Operation Manual for details.
[Seq Control] Starts, stops, pauses, or resumes a sequence, or views the status of a sequence. See Loading, Storing, and Running Sequences from the Software Keypad on page 51.
Operating Guide
Software Keypad Operation 3
Keypad Functionality When the GC Is Controlled by an Agilent Data System
Operating Guide
When an Agilent data system controls the GC, the data system defines the setpoints and runs the samples. The Remote indicator on the software keypad lights when a data system is controlling the GC.
CAUTION Using the software keypad to change setpoints when a data system
controls the GC can cause erroneous data. When using the software
keypad, the GC does not automatically communicate setpoint
changes to the connected data system.
When an Agilent data system controls the GC, the software keypad should be used:
To view run status by selecting [Status]
To view the method settings by selecting the GC component key
To display the last and next run times, the run time remaining, and the post-run time remaining by repeatedly selecting [Time]
To abort a run by selecting [Stop]
To find which computer is controlling the GC by pressing [Options] > Communication, then scrolling. The name of the computer controlling the GC is listed after the Enable DHCP setting, along with the number of hosts connected to the GC.
Pressing [Stop] during a GC run immediately ends the run. The data system may retain the data already collected, but no further data is collected for that sample. Agilent data systems may allow the next run to begin, depending on the data system and its settings for handling errors.
43
3 Software Keypad Operation
The Service Mode Key
44
[Service Mode] Is used to access maintenance functions and
settings, service counters, and diagnostics for the GC. See the Advanced Operation Manual for details.
Operating Guide
Software Keypad Operation 3
About GC Status in the Software Keypad
Operating Guide
When the GC is ready to begin a run, the display screen shows STATUS Ready for Injection. Alternately, when a component of the GC is not ready to begin a run, the Not Ready indicator on the software keypad is lit. Press [Status] to see a message explaining why the GC is not ready.
Indicators
A lit indicator means:
The current progress of a run (Pre Run or Run).
Items which may require attention (Not Ready, Service Due, and Run Log).
The GC is controlled by an Agilent data system (Remote).
The GC is in gas saver mode (Gas Saver).
Error conditions
If a problem occurs, a status message appears. If the message indicates broken hardware, more information may be available. Press the applicable component key (for example, Front Det, Oven, or Front Inlet).
Blinking setpoint
If the system shuts down a gas flow or the oven, Off will blink on the appropriate line of the components parameter listing.
45
46
3 Software Keypad Operation
If there is a detector pneumatics shutdown or failure in another part of the detector, the detector On/Off line of the detectors parameter list blinks.
For any flow or pressure parameter, and for oven temperature, go to the blinking parameter, then press [Off/No] to clear the fault. Resolve the problem if possible, then press [On/Yes] on the parameter to use it again. If the problem is not fixed, the fault will recur.
If the shutdown includes safety concerns, for example a shutdown for hydrogen carrier gas flow, you must power cycle the GC. See the Troubleshooting manual for more information.
Operating Guide
Software Keypad Operation 3
About Logs
Operating Guide
Two logs are accessible from the keypad: the run log and the system event log. To access the logs, press [Logs] then scroll to the desired log and press [Enter]. The display will indicate the number of entries the log contains. Scroll through the list.
Run log
The run log is cleared at the start of each new run. During the run, any deviations from the planned method (including keypad intervention) are listed in the run log table. When the run log contains entries, the Run Log indicator lights.
System event log
The system event log records significant events during the GCs operation. Some of the events also appear in the run log if they are in effect during a run.
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3 Software Keypad Operation
Operating Guide
Agilent 7820A Gas Chromatograph Operating Guide
4 Running a Method or a Sequence from the Software Keypad
Loading, Storing, and Running Methods from the Software Keypad 50
Loading, Storing, and Running Sequences from the Software Keypad 51
This section explains how to load, store, and run a method or sequence using the software keypad, without the use of an Agilent data system. The keypad can be used to select and run a method or automated sequence stored in the GC and run it. In this case, the data generated from the run is normally sent to an integrator for the data analysis report.
For information on creating a method or sequence using keypad entry, see Chapter 5, Methods and Sequences."
49Agilent Technologies
4 Running a Method or a Sequence from the Software Keypad
Loading, Storing, and Running Methods from the Software Keypad
To manually inject a sample with a syringe and start a run
50
1 Prepare the sample syringe for injection.
2 Load the desired method. (See "To load a method".)
3 Press [Prep Run].
4 Wait for STATUS Ready for Injection to be displayed.
5 Insert the syringe needle through the septum and all the way into the inlet.
6 Simultaneously depress the syringe plunger to inject the sample and press [Start].
To run a method to process a single ALS sample
1 Prepare the sample for injection.
2 Load the sample vial into the assigned location in the ALS turret.
3 Load the desired method. (See "To load a method".)
4 Press [Start] on the GC keypad to initiate the ALS syringe cleaning, sample loading, and sample injection method. After the sample is loaded into the syringe, the sample is automatically injected when the GC reaches the ready state.
To abort a method
1 Press [Stop].
2 When you are ready to resume running analyses, load the appropriate sequence or method. (See "To load a method" or "To load a stored sequence".)
Operating Guide
Running a Method or a Sequence from the Software Keypad 4
Loading, Storing, and Running Sequences from the Software Keypad
Operating Guide
A sequence can specify up to five subsequences to be run, as well as post-run sequences, if defined. Each sequence is stored as a number (from 1 to 9).
To start running a sequence
1 Load the sequence. (See "To load a stored sequence".)
2 Press [Seq Control].
3 Verify the status of the sequence:
Runningthe sequence is running
Ready/waitthe instrument is not ready (due to oven temperature, equilibration times, and so forth.)
Pausedthe sequence is paused
Stoppedproceed to step 4
Abortedthe sequence stopped without waiting for the run to finish (See "Aborting a sequence".)
No sequencethe sequence is off or not defined
4 Scroll to the Start sequence line and press [Enter] to change the status to Running.
The Run indicator will light and stay lit until the sequence is completed. The sequence continues to run until all subsequences are executed or until the sequence is aborted.
Ready wait
If a sequence is started but the instrument is not ready (due to oven temperature, equilibration times, and so forth), the sequence will not start until all instrument setpoints are ready.
To pause a running sequence
1 Press [Seq Control].
2 Scroll to Pause sequence and press [Enter].
The sequence stops when the current sample run is complete. The sequence status changes to paused, and you are given the option to resume or stop the paused sequence.
51
4 Running a Method or a Sequence from the Software Keypad
To resume a paused sequence
52
1 Press [Seq Control].
2 Scroll to Resume sequence and press [Enter].
The sequence resumes with the next sample.
To stop a running sequence
1 Press [Seq Control].
2 Scroll to Stop sequence and press [Enter].
The sequence stops at the end of the currently running subsequence unless [Seq] > Repeat sequence is On.A stopped sequence can only be restarted from the beginning.
To resume a stopped sequence
1 Press [Seq Control].
2 Scroll to Resume sequence and press [Enter].
The sequence restarts from the beginning of the sequence.
Aborting a sequence
When a sequence is aborted, it stops immediately without waiting for the current run to finish.
The following will cause a sequence to abort:
The [Stop] key is pressed.
A sampler error occurs, producing an error message.
The GC detects a configuration mismatch during a method load.
A running sequence tries to load a method that doesnt exist.
The sampler is turned off. You can correct the problem and then resume the sequence. The aborted sample run will be repeated.
To resume an aborted sequence
1 Correct the problem. (See "Aborting a sequence".)
2 Press [Seq Control].
3 Scroll to Resume sequence and press [Enter].
The aborted sample run will be repeated.
Operating Guide
Agilent 7820A Gas Chromatograph Operating Guide
5 Methods and Sequences
What Is a Method? 54
What Is Saved in a Method? 54
What Happens When You Load a Method? 55
Creating Methods 56
To program a method 56
To load a method 57
To store a method 57
Method mismatch 57
What Is a Sequence? 59
Creating Sequences 59
About the priority sequence 60
To program a sequence 60
To program a priority sequence 61
To program an ALS subsequence 61
To program a valve subsequence 62
To program post sequence events 62
To store a sequence 62
To load a stored sequence 63
To determine sequence status 63
Automating Data Analysis, Method Development, and Sequence
Development 63
Recoverable Errors 64
53Agilent Technologies
5 Methods and Sequences
What Is a Method?
54
A method is the group of settings required to analyze a specific sample.
Since every type of sample reacts differently in the GCsome samples require a higher oven temperature, others require a lower gas pressure or a different detectora unique method must be created for each specific type of analysis.
What Is Saved in a Method?
Some of the settings saved in a method define how the sample will be processed when the method is used. Examples of method settings include:
For GCs equipped with EPR (electronic pneumatics regulation), detector,
The oven temperature program
The type of carrier gas and flows
The type of detector and flows
The type of inlet and flows
The type of column
The length of time to process a sample
Data analysis and reporting parameters are also stored in a method when it is created on an Agilent data system, for example Agilent OpenLAB CDS EZChrom Compact. These parameters describe how to interpret the chromatogram generated by the sample and what type of report to print.
See the Advanced Operation Manual for more details on what can be included in a method.
Operating Guide
Methods and Sequences 5
What Happens When You Load a Method?
Operating Guide
There are two kinds of methods:
The active methodThis is sometimes referred to as the current method. The settings defined in this method are the settings the GC is currently maintaining.
Stored methodsUp to 9 user-created methods can be stored in the GC, along with a default method.
For EPC (electronic pneumatics control) equipped GCs, when a method is loaded from the GC or Agilent data system, the setpoints of the active method are immediately replaced with the setpoints of the method loaded.
For EPR (electronic pneumatics regulation) equipped GCs, when a method is loaded from the GC or Agilent data system, the manually set parameters are not replaced with the setpoints of the method loaded.
The method loaded becomes the active (current) method.
The Not Ready light will stay lit until the GC reaches all of the settings specified by the method that was just loaded.
Refer to Running a Method or a Sequence from the Software Keypad for details on using the keypad to load, modify, and save methods.
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5 Methods and Sequences
Creating Methods
56
A method is the group of setpoints needed to run a single sample on the GC, such as oven temperature programs, pressure programs, inlet temperatures, sampler parameters, and so forth. A method is created by saving a group of setpoints as a numbered method using the [Store] key.
Components for which setpoint parameters can be stored are shown in Table 2.
The GC also saves ALS setpoints.
See the 7693A Installation, Operation, and Maintenance manual for details on its setpoints.
See 7650 Installation, Operation, and Maintenance manual for details on its setpoints.
Current setpoint parameters are saved when the GC is turned off, and loaded when you turn the instrument back on.
Table 2 Setpoint parameter components
Component Component
Oven Analog Out
Valve 12 Front and back injector (see the ALS
operating manual)
Front and back inlet Aux temp
Columns 1 to 4 Post run
Front and back detector Run table
To program a method
1 Individually select each component for which setpoint parameters are appropriate for your method. (See Table 2.)
2 Examine the current setpoints and modify as desired. Repeat for each component as appropriate.
3 Examine the current setpoints for the ALS, if appropriate, and modify as desired.
4 Save the setpoints as a stored method. (See To store a method on page 57.)
Operating Guide
Methods and Sequences 5
To load a method
Operating Guide
1 Press [Load].
2 Press [Method].
3 Enter the number of the method to be loaded (1 through 9).
4 Press [On/Yes] to load the method and replace the active method. Alternatively, press [Off/No] to return to the stored methods list without loading the method.
To store a method
1 Ensure that the proper parameters are set.
2 Press [Method].
3 Scroll to the method to store, then press [Enter].
4 Press [On/Yes] to store the method and replace the active method. Alternatively, press [Off/No] to return to the stored methods list without storing the method.
Method mismatch
This section applies only to a standalone (not connected to a data system) GC. When a data system, such as OpenLAB CDS or MassHunter, controls the GC, methods are stored in the data system and can be edited there. See your data system documentation for more information.
Suppose your standalone GC is equipped with a single FID. You have created and saved methods that use this detector. Now you remove the FID and install a TCD in its place. When you try to load one of your stored methods, you observe an error message saying that the method and the hardware do not match.
The problem is that the actual hardware is no longer the same as the hardware configuration saved in the method. The method cannot run because it does not know how to operate the recently-added TCD.
On inspecting the method, you find that the detector-related parameters have all been reset to the default values.
Method mismatch occurs only for electronic devices in the GC, such as inlets, detectors, and EPC modules. The GC does generate a mismatch for consumables such as columns, liners, and syringes.
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5 Methods and Sequences
Correcting a method mismatch on a standalone GC
This problem can be avoided if you follow this procedure for any hardware change, even including the simple replacement of a defective detector board.
1 Before changing any hardware, press [Config][hardware module], where [hardware module] is the device you intend to replace, for example, [Config][Front Detector].
2 Press [Mode/Type]. Select Remove module and press [Enter]. The module is now Unconfigured.
3 Turn the GC off.
4 Make the hardware change that you intended (in this example, remove the FID and its flow module and replace them with the TCD and its module).
5 Turn the GC on. Press [Config][hardware module], for example, [Config][Front Detector]
6 Press [Mode/Type]. Select Install module and press [Enter]. The GC will install the new hardware module, which corrects the active method (but not the stored one!).
7 Save the corrected method using the same number (which overwrites the stored method) or a new number (which leave the original method unchanged).
Operating Guide
Methods and Sequences 5
What Is a Sequence?
Operating Guide
A sequence is a list of samples to be analyzed along with the method to be used for each analysis.
Refer to Running a Method or a Sequence from the Software Keypad and Creating Sequences for details on how to create, load, modify, and save sequences using the keypad.
Creating Sequences
A sequence specifies the samples to be run and the stored method to be used for each. The sequence is divided into a priority sequence (ALS only), subsequences (each of which uses a single method), and post-sequence events
Priority sequence allows you to interrupt a running ALS or valve sequence to analyze urgent samples. (See About the priority sequence on page 60.)
Subsequences contain the stored method number and information that defines a set of vials (or valve positions) to be analyzed using a particular method. Sampler and/or valve subsequences can be used in the same sequence.
Post sequence names a method to be loaded and run after the last run in the last subsequence. Specifies whether the sequence is to be repeated indefinitely or halted after the last subsequence.
Samples in each subsequence are specified as either ALS locations or sampling valve positions (gas sampling valves).
Nine sequences with up to two subsequences each can be stored.
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5 Methods and Sequences
About the priority sequence
60
The priority sequence consists of a single sampler or valve subsequence and a special Use priority parameter, which can be activated at any time, even when a sequence is running. This feature allows you to interrupt a running sequence without having to edit it.
If Use priority is On, then:
1 The GC and ALS complete the current run, then the sequence pauses.
2 The GC runs the priority sequence.
3 The GC resets the Use priority parameter to Off.
4 The main sequence resumes where it paused.
To program a sequence
1 Press [Seq]. (Press again, if necessary, to display subsequence information.)
2 Create a priority sequence, if desired. (See To program a priority sequence on page 61.) If you might want to use a priority sequence, you must program it now. (Once the sequence starts, you cannot edit it without stopping it.)
3 Scroll to the Method # line of Subseq 1 and enter a method number. Use 1 to 9 for the stored methods, 0 for the currently active method, or [Off/No] to end the sequence.
4 Press [Mode/Type] to select a valve or injector type. (See To program a valve subsequence on page 62 or To program an ALS subsequence on page 61.)
5 Create the next subsequence or scroll to Post Sequence. (See To program post sequence events on page 62.)
6 Save the completed sequence. (See To store a sequence on page 62.)
Operating Guide
Methods and Sequences 5
To program a priority sequence
Operating Guide
1 Press [Seq]. (Press again, if necessary, to display subsequence information.)
2 Scroll to Priority Method # and enter a method number. Use 1 to 9 for the stored methods, 0 for the currently active method, or [Off/No] to end the sequence. Press [Enter].
The active method, 0, will change during the sequence if the subsequences use stored methods. Therefore, method 0 should be chosen for the priority sequence only if all subsequences use method 0.
3 Press [Mode/Type] and select the injector type.
4 Program the ALS subsequence. (See To program an ALS subsequence on page 61.)
5 Store the completed sequence. (See To store a sequence on page 62.)
Once a priority subsequence exists in a sequence, you can activate it when the urgent samples are ready to be processed by:
1 Press [Seq]. (Press again, if necessary, to display subsequence information.)
2 Scroll to Use Priority and press [On/Yes].
When the priority samples are completed, the normal sequence resumes.
To program an ALS subsequence
1 See step 1 through step 3 of To program a sequence on page 60.
2 Press [Mode/Type] and select the injector type.
3 Enter injector sequence parameters:
Number of Injections/vialthe number of repeat runs from each vial. Enter 0 if no samples are to be injected. For example, you could enter 0 to perform a blank (no injection) run to clean the system after running a dirty sample.
Samplesthe range (firstlast) of sample vials to be analyzed.
4 Proceed with step 5 of To program a sequence on page 60.
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5 Methods and Sequences
To program a valve subsequence
62
1 See step 1 through step 3 of To program a sequence on page 60.
2 Press [Mode/Type] and select Valve.
3 Enter the valve sequence parameters :
#inj/positionnumber of injections at each position (099)
Position rngfirstlast valve positions to sample (132)
Times thru rangenumber of times to repeat the range (199)
# injectionsnumber of injections for each sample
4 Proceed with step 5 of To program a sequence on page 60.
To program post sequence events
1 See step 1 through step 4 of To program a sequence on page 60.
2 Scroll to the Method # line of Post Sequence and enter a method number. Use 1 to 9 for the stored methods, or 0 if there is no method to be loaded (keep the active method loaded).
3 Press [On/Yes] at Repeat sequence to keep repeating the sequence (useful for valve sequences). Otherwise, press [Off/No] to halt the sequence when all subsequences are finished.
To store a sequence
1 Press [Store][Seq].
2 Enter an identifying number for the sequence (19).
3 Press [On/Yes] to store the sequence. Alternatively, press [Off/No] to cancel.
A message is displayed if a sequence with the number you selected already exists.
Press [On/Yes] to replace the existing sequence or [Off/No] to cancel.
Sequences can also be stored from within the stored sequence list ([Seq]) by scrolling to the appropriate sequence number and pressing the [Store] key.
Operating Guide
Methods and Sequences 5
To load a stored sequence
Operating Guide
1 Press [Load][Seq].
2 Enter the number of the sequence to be loaded (19).
3 Press [On/Yes] to load the sequence or [Off/No] to cancel the load.
An error message is displayed if the specified sequence number has not been stored.
To determine sequence status
Press [Seq Control] to display the current status of the active sequence. There are six possible sequence status modes:
Start/running
Ready wait
Paused/resume
Stopped
Aborted
No sequence
Automating Data Analysis, Method Development, and Sequence Development
The output of the detectors is digitized and can be sent to an automated data analysis system (such as Agilent OpenLAB CDS), where it is analyzed and the results summarized in reports.
The Agilent data system also can be used to create and store methods and sequences that are sent to the GC through a network.
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5 Methods and Sequences
Recoverable Errors
64
Some types of errors, such as an ALS missing vial error or a headspace sampler vial size mismatch, may not always justify stopping an entire sequence. These errors are called recoverable errors, since you may be able to recover from them and continue running a sequence, if desired. Agilent data systems now provide features to allow you to control how the system will react to these types of errors. When using an Agilent data system, the data system will now control whether or not the sequence pauses, aborts completely, continues with the next sample, and so on, for each type of recoverable error.
Note that the data system only controls what happens to the next run in the sequence, not the current run, except when set to immediately abort. (In that case, the data system typically aborts the current run and the sequence.)
For example, pressing [Stop] on the GC always halts the current run. However, the data systems can allow you to choose whether to continue with the next run or to pause or to abort the whole sequence.
For details on how this feature works in your data system, refer to its help and documentation.
Operating Guide
Agilent 7820A Gas Chromatograph Operation Manual
6 Chromatographic Checkout
About Chromatographic Checkout 66
To Prepare for Chromatographic Checkout 67
To Check FID Performance 69
To Check TCD Performance 77
To Check NPD Performance 85
To Check uECD Performance 89
To Check FPD+ Performance (Sample 5188-5953) 93
To Check FPD+ Performance (Sample 5188-5245, Japan) 99
To Check FPD Performance (Sample 5188-5953) 105
To Check FPD Performance (Sample 5188-5245, Japan) 111
This section described the general procedure for verifying performance against the original factory standards. The checkout procedures described here assume a GC that has been in use for some period of time. Therefore the procedures ask that you perform bakeouts, replace consumable hardware, install the checkout column, and so forth. For a new GC installation, refer to Installation and First Startup manual for the steps you can skip in this case.
65Agilent Technologies
6 Chromatographic Checkout
About Chromatographic Checkout
66
The tests described in this section provide basic confirmation that the GC and detector can perform comparably to factory condition. However, as detectors and the other parts of the GC age, detector performance can change. The results presented here represent typical outputs for typical operating conditions and are not specifications.
The tests assume the following:
Use of an automatic liquid sampler. If not available, use a suitable manual syringe instead of the syringe listed.
Use of a 10-L syringe in most cases. However, a 5-L syringe is an acceptable substitute.
Use of the septa and other hardware (liners, jets, adapters, and so forth) described. If you substitute other hardware, performance can vary.
Operation Manual
Chromatographic Checkout 6
To Prepare for Chromatographic Checkout
Operation Manual
Because of the differences in chromatographic performance associated with different consumables, Agilent strongly recommends using the parts listed here for all checkout tests. Agilent also recommends installing new consumable parts whenever the quality of the installed ones is not known. For example, installing a new liner and septum ensures that they will not contribute any contamination to the results.
When the GC is delivered from the factory, these consumable parts are new and do not need replacement.
For a new GC, check the installed inlet liner. The liner shipped in the inlet
1 Check the indicators/dates on any gas supply traps. Replace/recondition expended traps.
2 Install new consumable parts for the inlet and prepare the correct injector syringe (and needle, as needed).
Table 3 Recommended parts for checkout by inlet type
Recommended part for checkout Part number
Split splitless inlet
Syringe, 10-L 5181-1267
O-ring 5188-5365
Septum 5183-4757
Liner 5062-3587 or
5181-3316
Purged packed column inlet
Syringe, 10-L 5181-1267
O-ring 5080-8898
Septum 5183-4757
Packed column inlet
Syringe, 10-L 5181-1267
O-ring 5080-8898
Septum 5183-4757
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6 Chromatographic Checkout
Cool on-column inlet
Septum 5183-4758
Septum nut 19245-80521
Syringe, 5-L on-column 5182-0836
0.32-mm needle for 5-L syringe 5182-0831
7693A ALS: Needle support insert, COC G4513-40529
Insert, fused silica, 0.32-mm id 19245-20525
Table 3 Recommended parts for checkout by inlet type (continued)
Recommended part for checkout Part number
Operation Manual
Chromatographic Checkout 6
To Check FID Performance
Operation Manual
FID performance is checked differently depending on the inlet being used. For GCs equipped with a packed column inlet (PCI), use To check FID performance with a packed column inlet (PCI). For all other inlet types, use To check FID performance with a purged packed, split splitless or cool-on column inlet on page 73.
To check FID performance with a packed column inlet (PCI)
1 Gather the following:
Evaluation column, 10% OV-101, 5 ft, OD 1/8, ID 2 mm (G3591-81093)
FID MDL sample (5188-5953)
Chromatographic-grade isooctane
4-mL solvent and waste bottles or equivalent for autoinjector
2-mL sample vials or equivalent for sample
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Packed column jet installed. If not, select and install a packed column jet.
Packed column adapter installed (adaptable FID only). If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL solvent vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Install the evaluation column. (See the procedure for the PCI in the Maintenance manual.)
Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the PCI in the Maintenance manual.)
Be sure to configure the column.
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6 Chromatographic Checkout
5 Check the FID baseline output. The output should be between 5 pA and 20 pA and relatively stable. (If using a gas generator or ultra pure gas, the signal may stabilize below 5 pA.) If the output is outside this range or unstable, resolve this problem before continuing.
6 If the output is too low:
Check that the electrometer is on.
Check that the flame is lit.
Check that the signal is set to the correct detector.
7 Create or load a method with the parameter values listed in Table 4.
Table 4 FID Checkout Conditions - Packed Column Inlet
Column and sample
Type 10% OV-101, 5 ft, OD 1/8, ID 2 mm
(G3591-81093)
Sample FID MDL sample (5188-5953)
Column flow 20 mL/min
Column mode Flow mode
Packed column inlet
Temperature 250 C
Detector
Temperature 300 C
H2 flow 30 mL/min
Air flow 400 mL/min
Makeup flow (N2) OFF
Mode Constant makeup flow OFF
Flame On
Lit offset Typically 2 pA
Oven
Constant temperature 180 C
Time 15 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Operation Manual
Chromatographic Checkout 6
Operation Manual
8 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
If not using a data system, create a one sample sequence using the GC keypad.
9 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed and nitrogen makeup gas.
Sample wash volume 8 L
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8 L
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
Plunger speed (7683) fast
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 4 FID Checkout Conditions (continued)- Packed Column Inlet
71
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6 Chromatographic Checkout
Operation Manual
Chromatographic Checkout 6
To check FID performance with a purged packed, split splitless or cool-on column inlet
Operation Manual
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
FID performance evaluation (checkout) sample (5188-5372)
Chromatographic-grade isooctane
4-mL solvent and waste bottles or equivalent for autoinjector
2-mL sample vials or equivalent for sample
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column jet installed. If not, select and install a capillary column jet.
Capillary column adapter installed (adaptable FID only). If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL solvent vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Be sure to configure the column.
5 Check the FID baseline output. The output should be between 5 pA and 20 pA and relatively stable. (If using a gas generator or ultra pure gas, the signal may stabilize below 5 pA.) If the output is outside this range or unstable, resolve this problem before continuing.
6 If the output is too low:
Check that the electrometer is on.
73
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6 Chromatographic Checkout
Check that the flame is lit.
Check that the signal is set to the correct detector.
7 Create or load a method with the parameter values listed in Table 5.
Table 5 FID Checkout Conditions
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413)
Sample FID checkout 5188-5372
Column flow 6.5 mL/min
Column mode Constant flow for EPC equipped GCs.
Constant pressure mode (30 psi) for
EPR equipped GCs.
Split/splitless inlet
Temperature 250 C
Mode Splitless
Purge flow 40 mL/min
Purge time 0.5 min
Gas saver Off
Purged packed column inlet
Temperature 250 C
Cool on-column inlet
Temperature Oven Track
Septum purge 15 mL/min
Detector
Temperature 300 C
H2 flow 30 mL/min
Air flow 400 mL/min
Makeup flow (N2) 25 mL/min
Lit offset Typically 2 pA
Oven
Initial temp 75 C
Initial time 0.5 min
Operation Manual
Chromatographic Checkout 6
Operation Manual
8 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
If not using a data system, create a one sample sequence using the GC keypad.
9 Start the run.
Rate 1 20 C/min
Final temp 190 C
Final time 0 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 5 FID Checkout Conditions (continued)
75
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6 Chromatographic Checkout
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed and nitrogen makeup gas.
mi0 1 2 3 4 5
pA
0
50
100
150
200
250
300
350
400
FID1 A, (C:\FID.D)
C13 C14
C15 C16
Operation Manual
Chromatographic Checkout 6
To Check TCD Performance
Operation Manual
TCD performance is checked differently depending on the inlet being used. For GCs equipped with a packed column inlet (PCI), use To check TCD performance with a packed column inlet (PCI). For all other inlet types, use To check TCD performance with a purged packed, split splitless or cool-on column inlet on page 81.
To check TCD performance with a packed column inlet (PCI)
1 Gather the following:
Evaluation column, 10% OV-101, 5 ft, OD 1/8, ID 2 mm (G3591-81093)
FID/TCD performance evaluation (checkout) sample (18710-60170)
4-mL solvent and waste bottles or equivalent for autoinjector
Chromatographic-grade hexane
2-mL sample vials or equivalent for sample
Chromatographic-grade helium as carrier, makeup, and reference gas
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Chromatographic-grade gases plumbed and configured: helium as carrier gas and reference gas.
Empty waste vials loaded in sample turret.
4-mL solvent vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Install the evaluation column. (See the procedure for the PCI in the Maintenance manual.)
Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the PCI in the Maintenance manual.)
Configure the column
5 Create or load a method with the parameter values listed in Table 6.
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6 Chromatographic Checkout
Table 6 TCD Checkout Conditions - Packed Column Inlet
Column and sample
Type 10% OV-101, 5 ft, OD 1/8, ID 2 mm
(G3591-81093)
Sample FID/TCD checkout 18710-60170
Column flow 20 mL/min
Column mode Flow mode
Packed column inlet
Temperature 250 C
Detector
Temperature 300 C
Reference flow (He) 20 mL/min
Makeup flow (He) OFF
Baseline output < 30 display counts on Agilent
OpenLAB CDS ChemStation Edition
(< 750 V)
Oven
Constant temp 180 C
Time 15 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 L
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8 L
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
Plunder speed (7683) fast
Operation Manual
Chromatographic Checkout 6
Operation Manual
6 Display the signal output. A stable output at any value between 12.5 and 750 V (inclusive) is acceptable.
If the baseline output is < 0.5 display units (< 12.5 V), verify that the detector filament is on. If the offset is still < 0.5 display units (< 12.5 V), your detector requires service.
If baseline output is > 30 display units (> 750 V), there may be chemical contamination contributing to the signal. Bakeout the TCD. If repeated cleanings do not give an acceptable signal, check gas purity. Use higher purity gases and/or install traps.
7 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
8 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed.
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 2 L
Data system
Data rate 5 Hz
Table 6 TCD Checkout Conditions (continued)- Packed Column Inlet
79
80
6 Chromatographic Checkout
Operation Manual
Chromatographic Checkout 6
To check TCD performance with a purged packed, split splitless or cool-on column inlet
Operation Manual
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
FID/TCD performance evaluation (checkout) sample (18710-60170)
4-mL solvent and waste bottles or equivalent for autoinjector
Chromatographic-grade hexane
2-mL sample vials or equivalent for sample
Chromatographic-grade helium as carrier, makeup, and reference gas
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Chromatographic-grade gases plumbed and configured: helium as carrier gas and reference gas.
Empty waste vials loaded in sample turret.
4-mL solvent vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Configure the column
5 Create or load a method with the parameter values listed in Table 7.
Table 7 TCD Checkout Conditions
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413)
Sample FID/TCD checkout 18710-60170
81
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6 Chromatographic Checkout
Column flow 6.5 mL/min
Column mode Constant flow for EPC equipped GCs.
Constant pressure mode (30 psi) for
EPR equipped GCs.
Split/splitless inlet
Temperature 250 C
Mode Splitless
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 250 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 300 C
Reference flow (He) 20 mL/min
Makeup flow (He) 2 mL/min
Baseline output < 30 display counts on Agilent
OpenLAB CDS ChemStation Edition
(< 750 V)
Oven
Initial temp 40 C
Initial time 0 min
Rate 1 20 C/min
Final temp 90 C
Final time 0 min
Rate 2 15 C/min
Final temp 170 C
Final time 0 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Table 7 TCD Checkout Conditions (continued)
Operation Manual
Chromatographic Checkout 6
Operation Manual
6 Display the signal output. A stable output at any value between 12.5 and 750 V (inclusive) is acceptable.
If the baseline output is < 0.5 display units (< 12.5 V), verify that the detector filament is on. If the offset is still < 0.5 display units (< 12.5 V), your detector requires service.
If baseline output is > 30 display units (> 750 V), there may be chemical contamination contributing to the signal. Bakeout the TCD. If repeated cleanings do not give an acceptable signal, check gas purity. Use higher purity gases and/or install traps.
7 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
8 Start the run.
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 7 TCD Checkout Conditions (continued)
83
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6 Chromatographic Checkout
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed.
2 4 6 8 20
30
40
50
60
70
Time (min.)
25 uV
C14 C15 C16
Operation Manual
Chromatographic Checkout 6
To Check NPD Performance
Operation Manual
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
NPD performance evaluation (checkout) sample (18789-60060)
4-mL solvent and waste bottles or equivalent for autoinjector.
Chromatographic-grade isooctane
2-mL sample vials or equivalent for sample.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column jet installed. If not, select and install a capillary column jet.
Capillary column adapter installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 If present, remove any protective caps from the inlet manifold vents.
5 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Bake out the evaluation column for at least 30 min at 180 C. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Be sure to configure the column
6 Create or load a method with the parameter values listed in Table 8.
85
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6 Chromatographic Checkout
Table 8 NPD Checkout Conditions
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413)
Sample NPD checkout 18789-60060
Column mode Constant flow
Column flow 6.5 mL/min (helium)
Split/splitless inlet
Temperature 200 C
Mode Splitless
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 200 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 300 C
H2 flow 3 mL/min
Air flow 60 mL/min
Makeup flow (N2) Makeup + column = 10 mL/min
Output 30 display units (30 pA)
Oven
Initial temp 60 C
Initial time 0 min
Rate 1 20 C/min
Final temp 200 C
Final time 3 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Operation Manual
Chromatographic Checkout 6
Operation Manual
7 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
8 Start the run.
If performing an injection using an autosampler, start the run using the data system, or creating a one sample sequence and pressing [Start] on the GC.
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 8 NPD Checkout Conditions (continued)
87
88
6 Chromatographic Checkout
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed.
min1 2 3 4 5 6 7 8 9
pA
10
20
30
40
50
60
70
NPD1 B, (C:\NPD.D)
Azobenzene
Malathion
Octadecane
Operation Manual
Chromatographic Checkout 6
To Check uECD Performance
Operation Manual
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
uECD performance evaluation (checkout) sample (1871360040, Japan: 5183-0379)
4-mL solvent and waste bottles or equivalent for autoinjector.
Chromatographic-grade isooctane
2-mL sample vials or equivalent for sample.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Clean fused silica indented mixing liner installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium for carrier gas, nitrogen for makeup.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with hexane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Bake out the evaluation column for at least 30 minutes at 180 C. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Be sure to configure the column.
5 Display the signal output to determine baseline output. A stable baseline output at any value between 0.5 and 1000 Hz (OpenLAB CDS ChemStation Edition display units) (inclusive) is acceptable.
If the baseline output is < 0.5 Hz, verify that the electrometer is on. If the offset is still < 0.5 Hz, your detector requires service.
89
90
6 Chromatographic Checkout
If the baseline output is > 1000 Hz, there may be chemical contamination contributing to the signal. Bakeout the uECD. If repeated cleanings do not give an acceptable signal, check gas purity. Use higher purity gases and/or install traps.
6 Create or load a method with the parameter values listed in Table 9.
Table 9 uECD Checkout Conditions
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413
Sample ECD checkout (18713-60040 or
Japan: 5183-0379)
Column mode Constant flow
Column flow 6.5 mL/min (helium)
Split/splitless inlet
Temperature 200 C
Mode Splitless
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 200 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 300 C
Makeup flow (N2) 30 mL/min (constant + makeup)
Baseline output Should be < 1000 display counts. In
Agilent OpenLAB CDS ChemStation
Edition (< 1000 Hz)
Oven
Initial temp 80 C
Initial time 0 min
Rate 1 15 C/min
Operation Manual
Chromatographic Checkout 6
Operation Manual
7 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
8 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
Final temp 180 C
Final time 10 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 9 uECD Checkout Conditions (continued)
91
92
6 Chromatographic Checkout
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
9 The following chromatogram shows typical results for a new detector with new consumable parts installed. The Aldrin peak will be missing when using the Japanese sample 5183-0379.
min2 4 6 8 10 12
Hz
0
2000
4000
6000
8000
10000
12000
ECD1 B, (C:\ECD.D)
Lindane (18713-60040 5183-0379)
Aldrin (18713-60040)
Operation Manual
Chromatographic Checkout 6
To Check FPD+ Performance (Sample 5188-5953)
Operation Manual
To check FPD+ performance, first check the phosphorus performance, then the sulfur performance.
Preparation
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
FPD performance evaluation (checkout) sample (5188-5953), 2.5 mg/L ( 0.5%) methylparathion in isooctane
Phosphorus filter
Sulfur filter and filter spacer
4-mL solvent and waste bottles or equivalent for autoinjector.
2-mL sample vials or equivalent for sample.
Chromatographic-grade isooctane for syringe wash solvent.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column adapter installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Verify that the Lit Offset is set appropriately. Typically, it should be about 2.0 pA for the checkout method.
5 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, or COC in the Maintenance manual.) Be sure to configure the column.
93
6 Chromatographic Checkout
Phosphorus performance
94
1 If it is not already installed, install the phosphorus filter.
2 Create or load a method with the parameter values listed in Table 10.
Table 10 FPD+ Checkout Conditions (P)
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413)
Sample FPD checkout (5188-5953)
Column mode Constant pressure
Column pressure 25 psi
Split/splitless inlet
Temperature 200 C Split/splitless
Mode Splitless
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 200 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 200 C (On)
Hydrogen flow 60 mL/min (On)
Air (Oxidizer) flow 60 mL/min (On)
Mode Constant makeup flow OFF
Makeup flow 60 mL/min (On)
Makeup gas type Nitrogen
Flame On
Lit offset Typically 2 pA
PMT voltage On
Emission Block 125 C
Operation Manual
Chromatographic Checkout 6
Operation Manual
Oven
Initial temp 70 C
Initial time 0 min
Rate 1 25 C/min
Final temp 1 150 C
Final time 1 0 min
Rate 2 5 C/min
Final temp 2 190 C
Final time 2 4 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 10 FPD+ Checkout Conditions (continued)(P)
95
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6 Chromatographic Checkout
3 Ignite the FPD flame, if not lit.
4 Display the signal output and monitor. This output typically runs between 40 and 55 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationary phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter.
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed.
Operation Manual
Chromatographic Checkout 6
Operation Manual
Sulfur performance
Methylparathion
Isooctane
1 Install the sulfur filter and filter spacer.
2 Ignite the FPD flame if not lit.
3 Display the signal output and monitor. This output typically runs between 50 and 60 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter.
If the baseline output is zero, verify the electrometer is on and the flame is lit.
4 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
5 Start the run.
97
98
6 Chromatographic Checkout
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
6 The following chromatogram shows typical results for a new detector with new consumable parts installed.
Methylparathion
Isooctane
Operation Manual
Chromatographic Checkout 6
To Check FPD+ Performance (Sample 5188-5245, Japan)
Operation Manual
To verify FPD+ performance, first check the phosphorus performance, then the sulfur performance.
Preparation
1 Gather the following:
Evaluation column, DB5 15 m 0.32 mm 1.0 m (123-5513)
FPD performance evaluation (checkout) sample (5188-5245, Japan), composition: n-Dodecane 7499 mg/L ( 5%), Dodecanethiol 2.0 mg/L ( 5%), Tributyl Phosphate 2.0 mg/L ( 5%), tert-Butyldisulfide 1.0 mg/L ( 5%), in isooctane as solvent
Phosphorus filter
Sulfur filter and filter spacer
4-mL solvent and waste bottles or equivalent for autoinjector.
2-mL sample vials or equivalent for sample.
Chromatographic-grade isooctane for syringe wash solvent.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column adapter installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Verify the lit offset is set appropriately. Typically, it should be about 2.0 pA for the checkout method.
5 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
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6 Chromatographic Checkout
Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Configure the column.
Phosphorus performance
1 If it is not already installed, install the phosphorus filter.
2 Create or load a method with the parameter values listed in Table 11.
Table 11 FPD+ Phosphorus Checkout Conditions
Column and sample
Type DB-5MS, 15 m 0.32 mm 1.0 m
(123-5513)
Sample FPD checkout (5188-5245)
Column mode Constant flow
Column flow 7.5 mL/min
Split/splitless inlet
Temperature 250 C
Mode Splitless
Total purge flow 69.5 mL/min
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 250 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 200 C (On)
Hydrogen flow 60.0 mL/min (On)
Air (oxidizer) flow 60.0 mL/min (On)
Mode Constant makeup flow Off
Makeup flow 60.0 mL/min (On)
Operation Manual
Chromatographic Checkout 6
Operation Manual
Makeup gas type Nitrogen
Flame On
Lit offset Typically 2 pA
PMT voltage On
Emission Block 125 C
Oven
Initial temp 70 C
Initial time 0 min
Rate 1 10 C/min
Final temp 105 C
Final time 0 min
Rate 2 20 C/min
Final temp 2 190 C
Final time 2 7.25 min for sulfur
12.25 min for phosphorus
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
Table 11 FPD+ Phosphorus Checkout Conditions (continued)
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6 Chromatographic Checkout
3 Ignite the FPD flame, if not lit.
4 Display the signal output and monitor. This output typically runs between 40 and 55 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data System
Data rate 5 Hz
Table 11 FPD+ Phosphorus Checkout Conditions (continued)
Operation Manual
Chromatographic Checkout 6
Operation Manual
7 The following chromatogram shows typical results for a new detector with new consumable parts installed.
Sulfur performance
Tributylphosphate
Isooctane t-Butyldisulfide
1 Install the sulfur filter.
2 Ignite the FPD flame, if not lit.
3 Display the signal output and monitor. This output typically runs between 50 and 60 but can be as high as 70. Wait for the output to stabilize. This takes approximately 2 hours.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter
If the baseline output is zero, verify the electrometer is on and the flame is lit.
4 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure the data system will output a chromatogram.
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6 Chromatographic Checkout
5 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
6 The following chromatogram shows typical results for a new detector with new consumable parts installed.
t-Butyldisulfide
1-Dodecanethiol
Isooctane
Operation Manual
Chromatographic Checkout 6
To Check FPD Performance (Sample 5188-5953)
Operation Manual
To check FPD performance, first check the phosphorus performance, then the sulfur performance.
Preparation
1 Gather the following:
Evaluation column, HP-5 30 m 0.32 mm 0.25 m (19091J-413)
FPD performance evaluation (checkout) sample (5188-5953), 2.5 mg/L ( 0.5%) methylparathion in isooctane
Phosphorus filter
Sulfur filter and filter spacer
4-mL solvent and waste bottles or equivalent for autoinjector.
2-mL sample vials or equivalent for sample.
Chromatographic-grade isooctane for syringe wash solvent.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column adapter installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Verify that the Lit Offset is set appropriately. Typically, it should be about 2.0 pA for the checkout method.
5 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Be sure to configure the column.
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6 Chromatographic Checkout
Phosphorus performance
106
1 If it is not already installed, install the phosphorus filter.
2 Create or load a method with the parameter values listed in Table 12.
Table 12 FPD Checkout Conditions (P)
Column and sample
Type HP-5, 30 m 0.32 mm 0.25 m
(19091J-413)
Sample FPD checkout (5188-5953)
Column mode Constant pressure
Column pressure 25 psi
Split/splitless inlet
Temperature 200 C Split/splitless
Mode Splitless
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 200 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 200 C (On)
Hydrogen flow 75 mL/min (On)
Air (Oxidizer) flow 100 mL/min (On)
Mode Constant makeup flow OFF
Makeup flow 60 mL/min (On)
Makeup gas type Nitrogen
Flame On
Lit offset Typically 2 pA
PMT voltage On
Oven
Operation Manual
Chromatographic Checkout 6
Operation Manual
3 Ignite the FPD flame, if not lit.
Initial temp 70 C
Initial time 0 min
Rate 1 25 C/min
Final temp 1 150 C
Final time 1 0 min
Rate 2 5 C/min
Final temp 2 190 C
Final time 2 4 min
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data system
Data rate 5 Hz
Table 12 FPD Checkout Conditions (continued)(P)
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6 Chromatographic Checkout
4 Display the signal output and monitor. This output typically runs between 40 and 55 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter.
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
c The following chromatogram shows typical results for a new detector with new consumable parts installed.
Operation Manual
Chromatographic Checkout 6
Operation Manual
Sulfur performance
Methylparathion
Isooctane
1 Install the sulfur filter and filter spacer.
2 Make the following method parameter changes.
3 Ignite the FPD flame if not lit.
4 Display the signal output and monitor. This output typically runs between 50 and 60 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Table 13 Sulfur method parameters (S)
Parameter Value ( mL/min)
H2 flow 50
Air flow 60
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6 Chromatographic Checkout
Wrong flows set for installed filter.
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
7 The following chromatogram shows typical results for a new detector with new consumable parts installed.
Methylparathion
Isooctane
Operation Manual
Chromatographic Checkout 6
To Check FPD Performance (Sample 5188-5245, Japan)
Operation Manual
To verify FPD performance, first check the phosphorus performance, then the sulfur performance.
Preparation
1 Gather the following:
Evaluation column, DB5 15 m 0.32 mm 1.0 m (123-5513)
FPD performance evaluation (checkout) sample (5188-5245, Japan), composition: n-Dodecane 7499 mg/L ( 5%), Dodecanethiol 2.0 mg/L ( 5%), Tributyl Phosphate 2.0 mg/L ( 5%), tert-Butyldisulfide 1.0 mg/L ( 5%), in isooctane as solvent
Phosphorus filter
Sulfur filter and filter spacer
4-mL solvent and waste bottles or equivalent for autoinjector.
2-mL sample vials or equivalent for sample.
Chromatographic-grade isooctane for syringe wash solvent.
Inlet and injector hardware (See To Prepare for Chromatographic Checkout.)
2 Verify the following:
Capillary column adapter installed. If not, install it.
Chromatographic-grade gases plumbed and configured: helium as carrier gas, nitrogen, hydrogen, and air.
Empty waste vials loaded in sample turret.
4-mL vial with diffusion cap filled with isooctane and inserted in Solvent A injector position.
3 Replace consumable parts (liner, septum, traps, syringe, and so forth) as needed for the checkout. See To Prepare for Chromatographic Checkout.
4 Verify the lit offset is set appropriately. Typically, it should be about 2.0 pA for the checkout method.
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6 Chromatographic Checkout
5 Install the evaluation column. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Set the oven, inlet, and detector to 250 C and bake out for at least 15 minutes. (See the procedure for the SS, PP, or COC in the Maintenance manual.)
Configure the column.
Phosphorus performance
1 If it is not already installed, install the phosphorus filter.
2 Create or load a method with the parameter values listed in Table 14.
Table 14 FPD Phosphorus Checkout Conditions
Column and sample
Type DB-5MS, 15 m 0.32 mm 1.0 m
(123-5513)
Sample FPD checkout (5188-5245)
Column mode Constant flow
Column flow 7.5 mL/min
Split/splitless inlet
Temperature 250 C
Mode Splitless
Total purge flow 69.5 mL/min
Purge flow 60 mL/min
Purge time 0.75 min
Purged packed column inlet
Temperature 250 C
Cool on-column inlet
Temperature Oven track
Septum purge 15 mL/min
Detector
Temperature 200 C (On)
Hydrogen flow 75.0 mL/min (On)
Air (oxidizer) flow 100.0 mL/min (On)
Mode Constant makeup flow Off
Operation Manual
Chromatographic Checkout 6
Operation Manual
Makeup flow 60.0 mL/min (On)
Makeup gas type Nitrogen
Flame On
Lit offset Typically 2 pA
PMT voltage On
Emission Block 125 C
Oven
Initial temp 70 C
Initial time 0 min
Rate 1 10 C/min
Final temp 105 C
Final time 0 min
Rate 2 20 C/min
Final temp 2 190 C
Final time 2 7.25 min for sulfur
12.25 min for phosphorus
ALS settings (if installed)
Sample washes 2
Sample pumps 6
Sample wash volume 8 (maximum)
Injection volume 1 L
Syringe size 10 L
Solvent A pre washes 2
Solvent A post washes 2
Solvent A wash volume 8
Solvent B pre washes 0
Solvent B post washes 0
Solvent B wash volume 0
Injection mode (7693A) Normal
Airgap Volume (7693A) 0.20
Viscosity delay 0
Inject Dispense Speed (7693A) 6000
Table 14 FPD Phosphorus Checkout Conditions (continued)
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6 Chromatographic Checkout
3 Ignite the FPD flame, if not lit.
4 Display the signal output and monitor. This output typically runs between 40 and 55 but can be as high as 70. Wait for the output to stabilize. This takes approximately 1 hour.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Wrong flows set for installed filter
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure that the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
PreInjection dwell 0
PostInjection dwell 0
Manual injection
Injection volume 1 L
Data System
Data rate 5 Hz
Table 14 FPD Phosphorus Checkout Conditions (continued)
Operation Manual
Chromatographic Checkout 6
Operation Manual
7 The following chromatogram shows typical results for a new detector with new consumable parts installed.
Sulfur performance
Tributylphosphate
Isooctane t-Butyldisulfide
1 Install the sulfur filter.
2 Make the following method parameter changes.
3 Ignite the FPD flame, if not lit.
4 Display the signal output and monitor. This output typically runs between 50 and 60 but can be as high as 70. Wait for the output to stabilize. This takes approximately 2 hours.
If the baseline output is too high:
Check column installation. If installed too high, the stationery phase burns in the flame and increases measured output.
Check for leaks.
Bake out the detector and column at 250 C.
Table 15 Sulfur method parameters
Parameter Value ( mL/min)
H2 flow 50
Air flow 60
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6 Chromatographic Checkout
Wrong flows set for installed filter
If the baseline output is zero, verify the electrometer is on and the flame is lit.
5 If using a data system, prepare the data system to perform one run using the loaded checkout method. Make sure the data system will output a chromatogram.
6 Start the run.
If performing an injection using an autosampler, start the run using the data system or press [Start] on the GC.
If performing a manual injection (with or without a data system):
a Press [Prep Run] to prepare the inlet for splitless injection.
b When the GC becomes ready, inject 1 L of the checkout sample and press [Start] on the GC.
7 The following chromatogram shows typical results for a new detector with new consumable parts installed.
t-Butyldisulfide
1-Dodecanethiol
Isooctane
Operation Manual
Agilent 7820A Gas Chromatograph Operating Guide
7 Configuration About Configuration 118
Assigning GC resources to a device 118
General Topics 120
To Unlock the GC Configuration 120
Ignore Ready = 120
Information displays 121
Unconfigured: 121
Oven 122
Front Inlet/Back Inlet 123
Column # 124
To configure a single column 124
Front Detector/Back Detector 128
Analog Out 130
Fast peaks 130
Valve Box 131
Thermal Aux 132
To assign a GC power source to an Aux thermal zone 132
To configure a MSD transfer line heater 133
To configure a nickel catalyst heater 133
PCM A/PCM B 134
Status 135
Time 136
Valve # 137
Front injector/Back injector 138
Instrument 139
117Agilent Technologies
7 Configuration
About Configuration
118
Configuration is a two-part process for most GC accessory devices that require power and/or communication resources from the GC. In the first part of the configuration process, a power and/or communication resource is assigned to the device. The second part of the configuration process allows setting of any configuration properties associated with the device.
Assigning GC resources to a device
A hardware device requiring but not assigned GC resources is given a mode of Unconfigured by the GC. Once you assign GC resources to a device, the GC gives the device a mode of Configured, allowing you to access other property settings (if any) for the device.
To assign GC resources to a device with an Unconfigured mode:
1 Unlock the GC configuration. Press [Options], select Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No].
2 Press [Config] on the GC keypad and select a device from the list, then press [Enter].
The [Config] key opens a menu similar to this:
Oven Front inlet Back Inlet Column # Front detector Back detector Analog out Valve Box Thermal Aux 1 PCM A PCM B Status Time Valve # Injector Instrument
In many cases you can move directly to the item of interest by pressing [Config][device].
Operating Guide
Configuration 7
Operating Guide
3 When the Configure Device Display opens, the cursor should be on the Unconfigured field. Press [Mode/Type] and follow the GC prompts to assign resources to the device.
4 After assigning resources, the GC prompts for you to power cycle the GC. Turn the GC power switch off and then on.
When the GC starts, select the device just assigned the GC resources for further configuration if needed. When accessed, its mode should indicate Configured and the other configuration properties are displayed.
Setting configuration properties
A devices configuration properties are constant for an instrument hardware setup unlike method settings which can change from sample run to sample run. Two example configuration settings are the gas type flowing through a pneumatic device and the operation temperate limit of a device.
To change the setting configuration properties for a Configured device:
1 Press [Config] on the GC keypad and select a device from the list, then press [Enter].
In many cases you can move directly to the item of interest by pressing [Config][device].
2 Scroll to the device setting and change the property. This can involve making a selection from a list using [Mode/Type], using [On/Yes] or [Off/No], or entering a numeric value. Press [Info] for help on changing numeric settings, or see the section of this document describing the specific configuration of the device.
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7 Configuration
General Topics
To Unlock the GC Configuration
120
Accessory devices including inlets, detectors, pressure controllers (PCM), and temperature control loops (Thermal AUX) have electrical connections to a power source and/or the communication bus in the GC. These devices must be assigned GC resources before they can be used. Before assigning resources to a device, you must first unlock the GC configuration. If you try to configure an Unconfigured device without unlocking the GC configuration, the GC displays the message CONFIGURATION IS LOCKED Go to Keyboard options to unlock.
It is also necessary to unlock the GC configuration if you are removing the GC resources from a Configured device. This action returns the device state to Unconfigured.
To unlock the GC configuration:
1 Press [Options], select Keyboard & Display and press [Enter].
2 Scroll down to Hard Configuration Lock and press [Off/No].
The GC configuration remains unlocked until the GC is power cycled off and on.
Ignore Ready =
The states of the various hardware elements are among the factors that determine whether the GC is Ready for analysis.
Under some circumstances, you may not wish to have a specific element readiness considered in the GC readiness determination. This parameter lets you make that choice. The following elements allow readiness to be ignored: inlets, detectors, the oven, PCM, and auxiliary EPC modules.
For example, suppose an inlet heater is defective but you dont plan to use that inlet today. By setting Ignore Ready = TRUE for that inlet, you can use the rest of the GC. After the heater is repaired, set Ignore Ready = FALSE or the run could start before that inlets conditions are ready.
To ignore an element's readiness, press [Config], then select the element. Scroll to Ignore Ready and press [On/Yes] to set it to True.
Operating Guide
Configuration 7
Operating Guide
To consider an element's readiness, press [Config], then select the element. Scroll to Ignore Ready and press [Off/No] to set it to False.
Information displays
Below are some examples of configuration displays:
[ EPC1 ] = (INLET) (SS) EPC #1 is used for an inlet of type split/splitless. It is not available for other uses.
[ EPC3 ] = (DET-EPC) (FID) EPC #3 is controlling detector gases to an FID.
FINLET (OK) 68 watts 21.7 This heater is connected to the front inlet. Status = OK, meaning that it is ready for use. At the time that the GC was turned on, the heater was drawing 68 watts and the inlet temperature was 21.7 C.
[ F-DET ] = (SIGNAL) (FID) The signal board for the front detector is type FID.
Unconfigured:
Accessory devices requiring GC power or communication must be assigned these GC resources before they can be used. To make this hardware element usable, first To Unlock the GC Configuration on page 120 then go to the Unconfigured parameter and press [Mode/Type] to install it. If the hardware element you are configuring requires selection of additional parameters, the GC asks for that selection. If no parameters are required, press [Enter] at the GC prompt to install that element. You are required to power the GC off and then power the GC on to complete this configuration.
After restarting the GC, a message reminding you of this change and its effect on the default method is displayed. If needed, change your methods to accommodate the new hardware.
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7 Configuration
Oven
122
See Unconfigured: on page 121 and Ignore Ready = on page 120.
Maximum temperature Sets an upper limit to the oven temperature. Used to prevent accidental damage to columns. The range is 70 to 425 C. See the column manufacturers recommendations.
Equilibration time The time after the oven approaches its setpoint before the oven is declared Ready. The range is 0 to 999.99 minutes. Used to ensure that the oven contents have stabilized before starting another run.
Limit ballistic power Reduce oven power when heating at maximum rate to limit the current drawn from the power line.
To configure the oven
1 Press [Config][Oven].
2 Scroll to Maximum temperature. Enter a value and press [Enter].
3 Scroll to Equilibration time. Enter a value and press [Enter].
Operating Guide
Configuration 7
Front Inlet/Back Inlet
Operating Guide
See Unconfigured: on page 121 and Ignore Ready = on page 120.
To configure the Gas type
The GC needs to know what carrier gas is being used.
1 Press [Config][Front Inlet] or [Config][Back Inlet].
2 Scroll to Gas type and press [Mode/Type].
3 Scroll to the gas you will use. Press [Enter].
This completes carrier gas configuration.
123
7 Configuration
Column #
124
Length The length, in meters, of a capillary column. Enter 0 for a packed column or if the length is not known.
Diameter The inside diameter, in millimeters, of a capillary column. Enter 0 for a packed column.
Film thickness The thickness, in microns, of the stationary phase for capillary columns.
Inlet Identifies the source of gas for the column.
Outlet Identifies the device into which the column effluent flows.
Thermal zone Identifies the device that controls the temperature of the column.
To configure a single column
You define a capillary column by entering its length, diameter, and film thickness. You then enter the device controlling the pressure at the Inlet (end of the column), the device controlling the pressure at the column Outlet, and the Thermal zone that controls its temperature.
With this information, the instrument can calculate the flow through the column. This has great advantages when using capillary columns because it becomes possible to:
Enter split ratios directly and have the instrument calculate and set the appropriate flow rates.
Enter flow rate or head pressure or average linear velocity. The instrument calculates the pressure needed to achieve the flow rate or velocity, sets that, and reports all three values. (Split/splitless inlet only.)
Perform splitless injections with no need to measure gas flows.
Choose any column mode. If the column is not defined, your choices are limited.
Except for the simplest configurations, such as a column connected to a specific inlet and detector, we recommend that you begin by making a sketch of how the column will be connected.
Operating Guide
Configuration 7
Operating Guide
To configure a column:
1 Press [Config][Col #] then enter the number of the column to be configured.
2 Scroll to the Length line, type the column length, in meters, followed by [Enter].
3 Scroll to Diameter, type the column inside diameter in microns, followed by [Enter].
4 Scroll to Film thickness, type the film thickness in microns, followed by [Enter]. The column is now defined.
If you do not know the column dimensionsthey are usually supplied with the columnor if you do not wish to use the GC calculating features, enter 0 for either Length or Diameter. The column will be not defined.
5 Scroll to Inlet. Press [Mode/Type] to select a gas pressure control device for this end of the column. Selections include the installed GC inlets and installed PCM channels.
Select the appropriate gas pressure control device and press [Enter].
6 Scroll to Outlet. Press [Mode/Type] to select a gas pressure control device for this end of the column.
Select the appropriate gas pressure control device and press [Enter].
When a detector is selected, the outlet end of the column is controlled at 0 psig for the FID, TCD, FPD, FPD+, NPD, and uECD or vacuum for the MSD.
Selecting Other enables the Outlet pressure setpoint. If the column exhausts into a nonstandard detector or environment (neither ambient pressure nor complete vacuum), select Other and enter the outlet pressure.
7 Scroll to Thermal zone. Press [Mode/Type] to see the available choices. In most cases this will be GC oven, but you may have an MSD transfer line heated by an auxiliary zone, valves in a separately-heated valve box or other configurations.
Select the appropriate Thermal zone and press [Enter].
8 Scroll to Column ID lock. If using an optional barcode scanner, this will be set to On by the data system. Normally, set to Off when not using a barcode scanner.
This completes configuration for a single capillary column.
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126
7 Configuration
Additional notes on column configuration
Packed columns should be configured as column not defined. To do this, enter 0 for either column length or column diameter.
You should check configurations for all columns to verify that they specify the correct pressure control device at each end. The GC uses this information to determine the flow path of the carrier gas. Only configure columns that are in current use in your GCs carrier gas flow path. Unused columns configured with the same pressure control device as a column in the current flow path cause incorrect flow results.
It is possible, and sometimes appropriate, to configure both installed columns to the same inlet.
Some pneumatic setpoints change with oven temperature because of changes in column resistance and in gas viscosity. This may confuse users who observe pneumatics setpoints changing when their oven temperature changes. However, the flow condition in the column remains as specified by the column mode (constant flow or pressure, ramped flow or pressure) and the initial setpoint values.
To view a summary of column connections
To view a summary of column connections, press [Config][Col #], then press [Enter]. The GC lists the column connections, for example:
Actual Setpoint
COLUMN CONFIGURATION SUMMARY
Front Inlet -> Column 1
Column 1 -> Front detector
Operating Guide
Configuration 7
About Heaters
Operating Guide
Inlets, detectors, valve boxes, and so on are heated. When configuring a device, it is sometimes necessary to know the connector used for that devices heater. Use the information in this section as needed when configuring a device.
The GC provides five heater connectors on the GC mainframe:
FI
BI
FD
BD
A1
Front of GC
Near front inlet
Near back inlet
Near top right corner of front detector board
Near top right corner of back detector board
End of valve bracket
All heater connectors are square, 4-conductor receptacles mounted on brackets. Note that access to the detector and valve connectors generally requires removing GC covers, and should be performed only by Agilent-trained service personnel.
The Table 16 describes the heater locations that are available for each module.
A front FPD or FPD+ uses heater connectors FD and A1. A back FPD or FPD+ uses heater connectors BD and A1.
Table 16 Possible heater connections by module
Module Possible heater connections
Front inlet FI or None
Back inlet BI or None
Front detector FD
Back detector BD
Valve box A1
Aux heater 1 A1
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7 Configuration
Front Detector/Back Detector
128
See Ignore Ready = and Unconfigured: on page 121.
To configure the makeup/reference gas
The makeup gas line of your detector parameter list changes depending on your instrument configuration.
1 If you have an inlet with the column not defined, the makeup flow is constant. If you are operating with column defined, you have a choice of two makeup gas modes. Press [Config][device], where [device] is one of the following:
[Front Det]
[Back Det]
2 Scroll to Makeup gas type (or Makeup/reference gas type) and press [Mode/Type].
3 Scroll to the correct gas and press [Enter].
Lit offset
The GC monitors the difference between the detector output with the flame lit and the output when the flame is not lit. If this difference falls below the setpoint, the GC assumes that the flame has gone out and tries to reignite it. See the Advanced Operation manual for details on how to set the Lit Offset:
FID
FPD
FPD+
If set too high, the lit detector baseline output can be below the Lit Offset setpoint, causing the GC to erroneously try to reignite the flame.
To configure the FPD or FPD+ heaters
The flame photometric detector (FPD and FPD+) uses two heaters, one in the transfer line near the base of the detector and one near the combustion chamber. When configuring the FPD or FPD+ heaters, select Install Detector 2 htr rather than the default Install Detector (FPD or FPD+). This two heater configuration controls the detector body using the detector heated zone, and the transfer line using Thermal Aux 1 for a front detector or Thermal Aux 2 for a back detector.
Operating Guide
Configuration 7
To ignore the FID, FPD, or FPD+ ignitor
Operating Guide
In general, do not ignore the ignitor for normal operation. Ignoring
Use this feature only if the ignitor is defective, and only until the ignitor is repaired.
If using an FID, FPD, or FPD+, you can ignite the flame manually by setting the GC to ignore the ignitor.
1 Press [Config][Front Det] or [Config][Back Det].
2 Scroll to Ignore Ignitor.
3 Press [On/Yes] to ignore the ignitor (or [Off/No] to enable the ignitor.
When Ignore Ignitor is set to True, the GC does not try to light the flame using the ignitor. The GC also completely ignores the Lit Offset setpoint and does not attempt autoignition. This means that the GC cannot determine if the flame is lit, and will not shut down the fuel gas.
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7 Configuration
Analog Out
Fast peaks
130
The GC allows you to output analog data at two speeds. The faster speedto be used only with the FID, FPD, FPD+, and NPDallows minimum peak widths of 0.004 minutes (8 Hz bandwidth), while the standard speedwhich can be used with all detectors allows minimum peak widths of 0.01 minutes (3.0 Hz bandwidth).
To use fast peaks:
1 Press [Config][Analog Out].
2 Scroll to Fast peaks and press [On/Yes].
The fast peaks feature does not apply to digital output.
If you are using the fast peaks feature, your integrator must be fast enough to process data coming from the GC. Integrator bandwidth should be at least 15 Hz.
Operating Guide
Configuration 7
Valve Box
Operating Guide
See Unconfigured: on page 121 and Ignore Ready = on page 120.
The valve box mounts on top of the column oven. It may contain up to two valves mounted on heated blocks. The block can accommodate two valves.
Valve positions on the blocks are numbered. We suggest that valves be installed in the blocks in numeric order.
All heated valves in a valve box are controlled by the same temperature setpoint.
To assign a GC power source to a valve box heater
1 Unlock the GC configuration, press [Options], select Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No].
2 Press [Config], scroll to Valve Box and press [Enter].
3 With Unconfigured selected, press [Mode/type], select one of the following and press [Enter].
Install heater A1 - for a valve box containing a single heater plugged into the connector labeled A1 on the valve box bracket.
Install heater A2 - for a valve box containing a single heater plugged into the connector labeled A2 on the valve box bracket.
The valve box bracket is located inside the GC right side electrical compartment in the upper right location.
4 When prompted by the GC, turn the power off then on again.
This completes the configuration of the valve box. To set the valve box temperature for your method press the [Valve #] key, and scroll to Valve Box.
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7 Configuration
Thermal Aux
132
See Unconfigured: on page 121 and Ignore Ready = on page 120.
The GC provides one additional channel of temperature control, Thermal Aux 1.
To assign a GC power source to an Aux thermal zone
Devices such as valve boxes and transfer lines have heaters which can be plugged into one of several connectors on the GC. Before use, you must configure these devices so that the GC knows the type of device plugged into the connector (inlet heater, detector heater, transfer line heater, and so on) and how to control it.
This procedure assigns the heater power source from heater plug A1 to the Thermal Aux 1 temperature control zone.
1 Unlock the GC configuration. Press [Options], select Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No].
2 Press [Config] and scroll to Thermal Aux 1.
3 With Unconfigured selected, press [Mode/Type], and select:
Install Heater A1 to configure a valve box heater plugged into the valve box bracket plug labeled A1.
4 Press [Enter] after making the selection.
5 For devices such as a valve box, inlet, or detector, configuration is complete. When prompted by the GC, turn the power off then on again. Skip the rest of the steps in this procedure.
For other devices, next configure the specific device type: Press [Clear] to skip the reboot for now.
6 Press [Config] and scroll to Thermal Aux 1 or Back inlet depending on where the MSD heater was assigned, and press [Enter].
7 Scroll to Auxiliary type, press [Mode/Type], scroll to and select the desired device type, and press [Enter]. Types may include:
Nickel catalyst
MSD transfer line
Operating Guide
Configuration 7
Operating Guide
8 When prompted, reboot the GC to implement the changes.
To configure a MSD transfer line heater
1 Check that a power source for the MSD heater was assigned. See To assign a GC power source to an Aux thermal zone on page 132.
2 Press [Config] and scroll to Thermal Aux 1 or Back inlet depending on where the MSD heater was assigned, and press [Enter].
For a single channel GC, select Back inlet.
For a dual channel GC, select Thermal Aux 1.
3 Scroll to Auxiliary type, press [Mode/Type], scroll to and select the MSD transfer line, and press [Enter].
To configure a nickel catalyst heater
1 Check that a power source for the Nickel Catalyst heater was assigned. See To assign a GC power source to an Aux thermal zone on page 132.
2 Press [Config] and scroll to Back inlet, and press [Enter].
3 Scroll to Auxiliary type, press [Mode/Type], scroll to and select Nickel catalyst, and press [Enter].
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7 Configuration
PCM A/PCM B
134
See Unconfigured: on page 121 and Ignore Ready = on page 120.
A pressure control module (PCM) provides one channel of gas control.
This channel is a simple forward-pressure regulator that maintains a constant pressure at its output. With a fixed downstream restrictor, it provides constant flow.
To assign a GC communication source to a PCM
1 Unlock the GC configuration, press [Options], select Keyboard & Display and press [Enter]. Scroll down to Hard Configuration Lock and press [Off/No].
2 Press [Config], scroll to a PCMx and press [Enter].
3 With Unconfigured selected, press [Mode/Type], select Install EPCx and press [Enter].
4 When prompted by the GC, turn the power off then on again.
To configure the other parameters on this PCM, see To configure a PCM.
To configure a PCM
1 Press [Config], scroll to the PCMx and press [Enter].
2 Scroll to Gas type, press [Mode/Type], make a selection and press [Enter].
The pressure control mode is set by pressing [PCM #]. Select Mode:, press [Mode/Type], select the mode and press [Enter].
Operating Guide
Configuration 7
Status
Operating Guide
The [Status] key has two tables associated with it. You switch between them by pressing the key.
The Ready/Not Ready status table
This table lists parameters that are Not Ready or gives you a Ready for Injection display. If there are any faults, warnings, or method mismatches present, they are displayed here.
The setpoint status table
This table lists setpoints compiled from the active parameter lists on the instrument. This is a quick way to view active setpoints during a run without having to open multiple lists.
To configure the setpoint status table
You can change the order of the list. You might want the three most important setpoints to appear in the window when you open the table.
1 Press [Config][Status].
2 Scroll to the setpoint that should appear first and press [Enter]. This setpoint will now appear at the top of the list.
3 Scroll to the setpoint that should appear second and press [Enter]. This setpoint will now be the second item on the list.
4 And so on, until the list is in the order you wish.
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7 Configuration
Time
136
Press [Time] to open this function. The first line always displays the current date and time, and the last line always displays a stopwatch. The two middle lines vary:
Between runs Show last and next (calculated) run times.
During a run Show time elapsed and time remaining in the run.
During Post Run Show last run time and remaining Post Run time.
To set time and date
1 Press [Config][Time].
2 Select Time zone (hhmm) and enter the local time offset from GMT using a 24 hour format.
3 Select Time (hhmm) and enter the local time.
4 Select Date (ddmmyy) and enter the date.
To use the stopwatch
1 Press [Time].
2 Scroll to the time= line.
3 To begin the timed period press [Enter].
4 To stop the timed period press [Enter].
5 Press [Clear] to reset the stopwatch.
Operating Guide
Configuration 7
Valve #
Operating Guide
Up to 2 valves can be mounted in a temperature-controlled valve box.
To configure a valve
1 Press [Config][Valve #] and enter the number of the valve you are configuring. The current valve type is displayed.
2 To change the valve type, press [Mode/Type], select the new valve type, and press [Enter].
Valve types
Sampling Two-position (load and inject) valve. In load position, an external sample stream flows through an attached (gas sampling) or internal (liquid sampling) loop and out to waste. In inject position, the filled sampling loop is inserted into the carrier gas stream. When the valve switches from Load to Inject, a run starts if one is not already in progress. See the Advanced Operation manual for details.
Not installed Self-explanatory.
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7 Configuration
Front injector/Back injector
138
The injectors are normally plugged into the Front ALS Port on the GC when used for injections into the front inlet, and the Back ALS Port on the GC when used for injections into the back inlet. However, the GC will detect an injectors location (front or back inlet) automatically, so both connectors work for an injector on either inlet.
To configure the 7693A sampler system, see the 7693A Installation, Operation, and Maintenance manual. To configure the 7650A sampler system, see the 7650A Installation, Operation, and Maintenance manual.
Operating Guide
Configuration 7
Instrument
Operating Guide
1 Press [Config]. Scroll to Instrument and press [Enter].
2 Scroll to Serial #. Enter a serial number and press [Enter]. This function can only be done by Agilent service personnel.
3 Scroll to Auto prep run. Press [On/Yes] to enable Auto prep run, [Off/No] to disable it. See the Advanced Operation manual for details.
4 Scroll to Zero Init Data Files.
Press [On/Yes] to enable it. When it is On, the GC immediately begins to subtract the current detector output from all future values. This applies only to digital output, and is useful when a non-Agilent data system has problems with baseline data that is non-zero.
Press [Off/No] to disable it. This is appropriate for all Agilent data systems.
5 Scroll to Require Host Connection. Set On to consider whether or not the remote host reports Ready as part of GC readiness.
6 Press [Clear] to return to the Config menu or any other function to end.
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140
7 Configuration
Operating Guide
Agilent 7820A Gas Chromatograph Operating Guide
8 Options
About Options 142
Calibration 142
Maintaining EPC and EPR calibrationinlets, detectors, and
PCM 142
Auto flow zero 143
Zero conditions 143
Zero intervals 144
To zero a specific flow or pressure sensor 144
Column calibration 144
Communication 149
Configuring the IP address for the GC 149
Keyboard and Display 150
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8 Options
About Options
142
The [Options] key is used for a group of functions that are usually set on installation and seldom changed afterward. It accesses this menu:
Calibration
Communication
Keyboard and Display
Calibration
Press [Calibration] to list the parameters that can be calibrated. These include:
Inlets
Detectors
ALS
Columns
Oven
Atmospheric pressure
In general, you will only need to calibrate the EPC or EPR modules and capillary columns. ALS, oven, and atmospheric pressure calibration should only be performed be trained service personnel.
The calibration displays are discussed in the Agilent 7820A Service Manual.
Maintaining EPC and EPR calibrationinlets, detectors, and PCM
The EPC and EPR gas control modules contain flow and/or pressure sensors that are calibrated at the factory. Sensitivity (slope of the curve) is quite stable, but zero offset requires periodic updating.
Flow sensors
The split/splitless, packed column and purged packed inlet modules use flow sensors. If the Auto flow zero feature (see page 143) is on, they are zeroed automatically after each run. This is the recommended way. They can also be zeroed manuallysee To zero a specific flow or pressure sensor.
Operating Guide
Options 8
Operating Guide
Pressure sensors
All EPC and EPR control modules (with the exception of the packed column inlet with EPR) use pressure sensors. They must be zeroed individually. There is no automatic zero for pressure sensors.
Auto flow zero
A useful calibration option is Auto flow zero. When it is On, after the end of a run the GC shuts down the flow of gases to an inlet, waits for the flow to drop to zero, measures and stores the flow sensor output, and turns the gas back on. This takes about two seconds. The zero offset is used to correct future flow measurements.
To activate this, select Calibration on the Options menu, then choose either Front inlet or Back inlet, press [Enter], and turn Auto flow zero on.
Zero conditions
Flow sensors are zeroed with the carrier gas connected and flowing.
Pressure sensors are zeroed with the supply gas line disconnected from the gas control module.
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144
8 Options
Zero intervals
Table 17 Flow and Pressure Sensor Zero Intervals
Sensor type Module type Zero interval
Flow All Use Auto flow zero and/or
Auto zero septum purge
Pressure Inlets
Packed columns Every 12 months
Small capillary columns
(id 0.32 mm or less)
Every 12 months
Large capillary columns
(id > 0.32 mm)
At 3 months, at 6 months,
then every 12 months
Auxiliary channels Every 12 months
Detector gases Every 12 months
To zero a specific flow or pressure sensor
1 Press [Options], scroll to Calibration, and press [Enter].
2 Scroll to the module to be zeroed and press [Enter].
3 Set the flow or pressure:
Flow sensors. Verify that the gas is connected and flowing (turned on).
Pressure sensors. Disconnect the gas supply line at the back of the GC. Turning it off is not adequate; the valve may leak.
4 Scroll to the desired zero line.
5 Press [On/Yes] to zero or [Clear] to cancel.
6 Reconnect any gas line disconnected in step 3 and restore operating flows
Column calibration
As you use a capillary column, you may occasionally trim off portions, changing the column length. If measuring the actual length is impractical, and if you are using EPC or EPR with a defined column, you can use an internal calibration routine to estimate the actual column length. Similarly, if you do not know the column internal diameter or believe it is inaccurate, you can estimate the diameter from related measurements.
Before you can calibrate the column, make sure that:
Operating Guide
Options 8
Operating Guide
You are using a capillary column
The column is defined
There are no oven ramps
The column gas source (usually the inlet) is On and non-zero
Also note that column calibration fails if the calculated column length correction is > 5 m, or if the calculated diameter correction is > 20 m.
Calibration modes
There are three ways to calibrate the column length and/or diameter:
Calibrate using an actual measured column flow rate
Calibrate using an unretained peak time (elution time)
Calibrate both length and diameter using flow rate and elution time
CAUTION When you measure the column flow rate, be sure to convert the
measurement to normal temperature and pressure if your
measurement device does not report data at NTP. If you enter
uncorrected data, the calibration will be wrong.
To estimate the actual column length or diameter from an elution time
1 Set oven ramp 1 to 0.00, then verify that the column is defined.
2 Perform a run using an unretained compound and record the elution time.
3 Press [Options], scroll to Calibration and press [Enter].
4 From the calibration list, select the column and press [Enter]. The GC displays the current calibration mode for the column.
5 To recalibrate or to change calibration mode, press [Mode/Type] to see the column calibration mode menu.
6 Scroll to Length or Diameter and press [Enter]. The following choices appear:
Mode
Measured flow
Unretained peak
Calculated length or Calculated diameter
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146
8 Options
Not calibrated
7 Scroll to Unretained peak and enter the actual elution time from the run performed above.
8 When you press [Enter], the GC will estimate the column length or diameter based on the elution time input and will now use that data for all calculations.
To estimate the actual column length or diameter from the measured flow rate
1 Set oven ramp 1 to 0.00, then verify that the column is defined.
2 Set the oven, inlet, and detectors temperatures to 35 C and allow them to cool to room temperature.
3 Remove the column from the detector.
CAUTION When you measure the column flow rate, be sure to convert the
measurement to normal temperature and pressure if your
measurement device does not report data at NTP. If you enter
uncorrected data, the calibration will be wrong.
4 Measure the actual flow rate through the column using a calibrated flow meter. Record the value. Reinstall the column.
5 Press [Options], scroll to Calibration and press [Enter].
6 From the calibration list, select the column and press [Enter]. The GC displays the current calibration mode for the column.
7 To recalibrate or to change calibration mode, press [Mode/Type] to see the column calibration mode menu.
8 Scroll to Length or Diameter and press [Enter]. The following choices appear:
Mode
Measured flow
Unretained peak
Calculated length or Calculated diameter
Not calibrated
9 Scroll to Measured flow and enter the corrected column flow rate (in mL/min) from the run performed above.
Operating Guide
Options 8
Operating Guide
10 When you press [Enter], the GC will estimate the column length or diameter based on the elution time input and will now use that data for all calculations.
To estimate the actual column length and diameter
1 Set oven ramp 1 to 0.00, then verify that the column is defined.
2 Perform a run using an unretained compound and record the elution time.
3 Set the oven, inlet, and detectors temperatures to 35 C and allow them to cool to room temperature.
4 Remove the column from the detector.
CAUTION When you measure the column flow rate, be sure to convert the
measurement to normal temperature and pressure if your
measurement device does not report data at NTP. If you enter
uncorrected data, the calibration will be wrong.
5 Measure the actual flow rate through the column using a calibrated flow meter. Record the value. Reinstall the column.
6 Press [Options], scroll to Calibration and press [Enter].
7 From the calibration list, select the column and press [Enter]. The GC displays the current calibration mode for the column.
8 To recalibrate or to change calibration mode, press [Mode/Type] to see the column calibration mode menu.
9 Scroll to Length & diameter and press [Enter]. The following choices appear:
Mode
Measured flow
Unretained peak
Calculated length
Calculated diameter
Not calibrated
10 Scroll to Measured flow and enter the corrected column flow rate (in mL/min) from the run performed above.
11 Scroll to Unretained peak and enter the actual elution time from the run performed above.
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8 Options
12 When you press [Enter], the GC will estimate the column length or diameter based on the elution time input and will now use that data for all calculations.
Operating Guide
Options 8
Communication
Configuring the IP address for the GC
Operating Guide
For network (LAN) operation, the GC needs an IP address. It can get this from a DHCP server, or it can be entered directly from the keyboard. In either case, see your LAN administrator.
To use a DHCP server
1 Press [Options]. Scroll to Communications and press [Enter].
2 Scroll to Enable DHCP and press [On/Yes]. When prompted, turn the GC off and then on again.
To set the LAN address at the keyboard
1 Press [Options]. Scroll to Communications and press [Enter].
2 Scroll to Enable DHCP and, if necessary, press [Off/No]. Scroll to Reboot GC. Press [On/Yes] and [On/Yes].
3 Press [Options]. Scroll to Communications and press [Enter].
4 Scroll to IP. Enter the numbers of the GC IP address, separated by dots, and press [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
5 Scroll to GW. Enter the Gateway number and press [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
6 Scroll to SM and press [Mode/Type]. Scroll to the appropriate subnet mask from the list given and press [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Press [Clear].
7 Scroll to Reboot GC. Press [On/Yes] and [On/Yes] to power cycle the instrument and apply the LAN setpoints.
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8 Options
Keyboard and Display
150
Press [Options] and scroll to Keyboard and Display. Press [Mode/Type].
The following parameters are turned on and off by pressing the [On/Yes] or [Off/No] keys.
Keyboard lock These keys and functions are operational when the keyboard lock is On:
[Start], [Stop], and [Prep Run]
[Load][Method] and [Load][Seq]
[Seq]to edit existing sequences
[Seq Control]to start or stop sequences.
When Keyboard lock is On, other keys and functions are not operational. Note that an Agilent data system can independently lock the GC keyboard. To edit GC setpoints using the GC keyboard, turn off both the GC keyboard lock and the data system keyboard lock.
Hard configuration lock On prevents keyboard configuration changes; Off removes lock.
Key click Click sound when keys are pressed.
Warning beep Allows you to hear warning beeps.
Warning beep mode There are 9 different warning sounds that may be selected. This allows you to give multiple GCs individual voices. We suggest you experiment.
Method modified beep Turn on for high pitched beep when method setpoint is modified.
Press [Mode/Type] to change the pressure units and radix type.
Pressure units psipounds per square inch, lb/in2
barabsolute cgs unit of pressure, dyne/cm2
kPamks unit of pressure, 103 N/m2
Language Select English or Chinese or Japanese.
Operating Guide
Options 8
Operating Guide
Radix type Determines the numeric separator type1.00 or 1,00
Display saver If On, dims the display after a period of inactivity. If Off, disabled.
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Agilent Technologies
Agilent 7820A Gas Chromatograph Operating Guide
9 Configuration Tasks
About the GC IP Address 154
To set the IP address at the GC 155
To Use DHCP to Provide the GC IP Address 156
To restore the default GC IP address 157
To Reconfigure an EPC Module for Another Detector 158
This section describes a several configuration tasks that may be required as part of normal operation.
153Agilent Technologies
9 Configuration Tasks
About the GC IP Address
154
From the factory, the GC is set to:
The installation procedures assume that you will connect to the GC using this address. However, after installation you may need to change the GC IP address or set it to use DHCP.
IP address 192.168.0.26 Subnet Mask 255.255.255.0 Gateway 192.168.0.1
Operating Guide
Configuration Tasks 9
To set the IP address at the GC
Operating Guide
1 Start the software keyboard. From the Windows Start program menu, Agilent > All Programs > Agilent Technologies > 7820A GC Remote Controller.
2 Connect to the GC. Go to Connection > Connect. In the Target field, enter the current GC IP address.
If the connection fails, see To troubleshoot a connection.
3 Click [Options]. Scroll to Communications and click [Enter].
4 Verify DHCP is Off. Scroll to Enable DHCP. If Enable DHCP is Off, skip to the next step.
If Enable DHCP is On, turn it off by clicking [Off/No]. Scroll to Reboot GC. Click [On/Yes] and [On/Yes]. After reboot, click [Options]. Scroll to Communications and click [Enter].
5 Scroll to IP. Use the numeric keypad to enter the numbers of the GC IP address, separated by dots, and click [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Click [Clear].
6 Scroll to GW. Enter the Gateway number and click [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Click [Clear].
7 Scroll to SM and click [Mode/Type]. Scroll to the appropriate subnet mask from the list given and click [Enter]. A message tells you to power cycle the instrument. Do not power cycle yet. Click [Clear].
8 Scroll to Reboot GC. Click [On/Yes] and [On/Yes] to power cycle the instrument and apply the LAN setpoints.
9 Ping the GC using the IP address entered above. See the Troubleshooting manual for details or if the GC does not respond.
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9 Configuration Tasks
To Use DHCP to Provide the GC IP Address
156
To set the GC to use DHCP:
1 Turn off the GC.
2 While pressing and holding [Prep Run] and [Stop] on the GC keypad, turn on the GC. This will set the GC to use DHCP to obtain an IP address.
3 Ping the GC using the static IP address or hostname assigned to the GC by your network administrator. See the Troubleshooting manual for details or if the GC does not respond.
You can also set the GC to use DHCP using the software keypad.
1 Click [Options]. Scroll to Communications and click [Enter].
2 Set Enable DHCP to On (press [On/Yes]).
3 Reboot the GC.
Operating Guide
Configuration Tasks 9
To restore the default GC IP address
Operating Guide
During installation and sometimes during operation, you may need to reset the GC IP address or change its IP addressing mode.
To restore the default IP address, press and hold the [Prep Run] key while power cycling the GC. After reboot, the GC IP address will return to:
IP address 192.168.0.26 Subnet Mask 255.255.255.0 Gateway 192.168.0.1
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9 Configuration Tasks
To Reconfigure an EPC Module for Another Detector
158
Your GC may include EPC (electronic pneumatics control) flow modules, EPR (electronic pneumatics regulation) flow modules, or a mix of both. Additionally, Agilent previously manufactured universal electronic pneumatics control (UEPC) modules. UEPC modules are configurable flow module that supply gas flows to the detectors installed in the GC.
The 7820A GC is a single channel instrument. If your GC only includes a single flow module, it can supply gases to only one detector at a time.
If you have one detector flow module and two detectors, and wish to switch the detector used, you can reconfigure the flow module as described below.
If you have two detectors and two flow modules, you do not need to perform this procedure.
To reconfigure the GC to use a detector flow module with another detector:
1 Determine the gas types needed for the new detector. The new detector may require changes to the gas supply plumbing.
2 Prepare the tubing and gas supplies before beginning. See the Installation Guide for gas plumbing details and the Site Preparation Guide supply requirements.
3 Connect to the GC with the software keypad.
4 Cool down the detector in use. The detector must be cool in order to prevent damage during the changeover.
5 If changing the carrier gas, or if you will need to disconnect or shut off the carrier gas supply in order to change detector gases, cool down the inlet and oven.
6 Turn off the detector flows. If changing detector gas types, also shut off detector gas supplies.
7 Close any online data system session for this GC.
8 Remove the detector cover.
9 Remove the pneumatics cover to expose the detector flow modules. See Figure 1 and Figure 2.
Operating Guide
Configuration Tasks 9
Operating Guide
Figure 1 Example back detector UEPC flow module with FID tubing attached
Flow module
Detector tubing (in use)
Detector tubing (not in use)
Gas line routing slot for detector in use with back flow module (Epc 2)
Gas line routing slot for detector in use with front flow module (Epc 1)
10 Click [Config][Lite EPC#].
11 Scroll to the EPC module to reconfigure.
12 Click [Mode/Type].
Figure 2 Example EPC flow module with FID tubing attached
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9 Configuration Tasks
13 Scroll to the desired detector to use, then click [Enter]. The choices are:
Front detector
Back detector
Not installed (do not use the flow module for a detector)
14 Follow the prompts in the software keypad display. Click [Enter] to continue when prompted. As a minimum, you will be prompted to close any online data session, then to reboot the GC.
After the GC reboots, the software keypad will temporarily loose communication with the GC. When the GC completes reboot, click Reconnect, or simply wait a few moments.
15 Turn off the new detector and its gas flows. Turning off the detector and its flows protects the detector and prevents shutdown errors while you connect any new gas supplies.
When handling the detector flow tubing, avoid bending the tubing at
16 For GCs equipped with the UEPC module, do the following:
a Loosen the thumbscrews that secure the old detector tubing to the flow module.
b Lift the old detector tubing from the flow module. See Figure 1.
Be careful not to cross-thread the knurled nuts onto the supply
c Locate the new detectors tubing.
d Place the new tubing over the flow manifold fittings, then fully tighten the thumbscrews.
e Make sure the gas type label is shown clearly.
17 For GCs equipped with EPC or EPR modules, do the following:
a Remove the Torx screws securing the detector tubing weldments to the flow module.
b Lift the old detector tubing from the flow module. See Figure 2.
Operating Guide
Configuration Tasks 9
Operating Guide
c Locate the new detectors tubing.
d Place the new tubing weldments over the flow manifold fittings, positioning them so they align with the corresponding guide pins on the flow module.
e Install the Torx screws and secure by tightening finger tight.
18 Carefully arrange the new detector tubing so that it fits through the correct routing slot. See Figure 1.
19 Route the tubing for the unused detector tubing through the other routing slot, and gently push its fittings into the open manifold space. See Figure 1.
20 If the detector gas types differ between the new detector and the old detector, connect the new gas supplies to the detector flow module.
Refer to the label on the detector tubing for the expected gas type for each flow module fitting.
Turn on the supply gases and check for supply gas leaks at the fittings.
Set source gas pressures. [Typically, set helium, hydrogen, and nitrogen supplies to 400 kPa (60 psi), and detector air to 550 kPa (80 psi).]
21 Click [Lite EPC#]. The new detector should be listed as the owner of the flow module.
22 Use the software keypad to configure any new gases (carrier or detector). For example, click [Config][Back Det], then scroll to Makeup gas type.
23 Turn on the detector gas flows using the software keypad.
24 Reinstall the covers.
After reconfiguring the flow module, you will need to update any configuration settings in your Agilent data system. You will also need to resolve your method to use the new detector and column configuration, or create a new method.
If using Agilent EZChrom Elite Compact, you may wish to create a new
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