Agilent Technologies 6890 Series User manual

Operating Manual
Volume 1. General Information
Agilent 6890 Series Gas
Chromatograph

gilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610
gilent Technologies 2000
ll Rights Reserved.
Reproduction, adaptation,
or translation without
permission is prohibited,
except as allowed under the
copyright laws.
Part No. G1530-90447
First edition, Jan 2000
Replaces Part No.G1530-
90440 Operating Manual
Volume 1
Printed in US
Safety Information
The 6890 Gas
Chromatograph meets the
following IEC
(International
Electrotechnical
Commission)
classifications: Safety Class
1, Transient Overvoltage
Category II, and Pollution
Degree 2.
This unit has been designed
and tested in accordance
with recognized safety
standards and designed for
use indoors. If the
instrument is used in a
manner not specified by the
manufacturer, the
protection provided by the
instrument may be
impaired. Whenever the
safety protection of the
6890 has been
compromised, disconnect
the unit from all power
sources and secure the unit
against unintended
operation.
Refer servicing to qualified
service personnel.
Substituting parts or
performing any
unauthorized modification
to the instrument may
result in a safety hazard.
Disconnect the C power
cord before removing
covers. The customer
should not attempt to
replace the battery or fuses
in this instrument. The
battery contained in this
instrument is recyclable.
Safety Symbols
Warnings in the manual or
on the instrument must be
observed during all phases
of operation, service, and
repair of this instrument.
Failure to comply with
these precautions violates
safety standards of design
and the intended use of the
instrument.
gilent Technologies
assumes no liability for the
customer’s failure to
comply with these
requirements.
WARNING
warning calls attention to
a condition or possible
situation that could cause
injury to the user.
CAUTION
caution calls attention to
a condition or possible
situation that could damage
or destroy the product or
the user’s work.
See accompanying
instructions for
more information.
Indicates a hot
surface.
Indicates
hazardous
voltages.
Indicates earth
(ground) terminal.
Indicates radio-
active hazard.
Indicates
explosion hazard.
Electromagnetic
compatibility
This device complies with
the requirements of
CISPRII. Operation is
subject to the following two
conditions:
1. This device may not
cause harmful
interference.
2. This device must accept
any interference
received, including
interference that may
cause undesired
operation.
If this equipment does
cause harmful interference
to radio or television
reception, which can be
determined by turning the
equipment off and on, the
user is encouraged to try
one or more of the
following measures:
1. Relocate the radio or
television antenna.
2. Move the device away
from the radio or
television.
3. Plug the device into a
different electrical outlet,
so that the device and the
radio or television are on
separate electrical
circuits.
4. Make sure that all
peripheral devices are
also certified.
5. Make sure that
appropriate cables are
used to connect the
device to peripheral
equipment.
6. Consult your equipment
dealer, gilent
Technologies, or an
experienced technician
for assistance.
7. Changes or modifications
not expressly approved
by gilent Technologies
could void the user’s
authority to operate the
equipment.
HP® is a registered
trademark of Hewlett-
Packard Co.
Microsoft®, Windows®,
and Windows NT® are
registered trademarks of
Microsoft Corporation.
Soun Emission
Certification for
Fe eral Republic of
Germany
Sound pressure Lp
< 65 dB( )
During normal operation
t the operator position
ccording to ISO 7779
(Type Test)
When operating the 6890
with cryo valve option, the
sound pressure 74.6 dB( )
during cryo valve operation
for short burst pulses.
Schallemission
Schalldruckpegel LP < 65
dB( )
m rbeitsplatz
Normaler Betrieb
Nach DIN 45635 T. 19
(Typprüfung)
Bei Betrieb des 6890 mit
Cryo Ventil Option treten
beim Oeffnen des Ventils
impulsfoermig
Schalldrucke Lp bis ca. 74.6
dB( ) auf.

Contents
i
Chapter 1. The 6890 Series Gas Chromatograph
Manuals........................................................................................................................................2
Control tables..............................................................................................................................3
Using control tables ...................................................................................................................4
Some specifics ............................................................................................................................6
Gas control............................................................................................................................6
Columns ................................................................................................................................6
Inlets and detectors .............................................................................................................6
Signals ...................................................................................................................................6
utomation ...........................................................................................................................6
Methods and sequences ......................................................................................................6
Valves.....................................................................................................................................7
Strategy........................................................................................................................................8
Maintenance information ..........................................................................................................9
Fuses and batteries..............................................................................................................9
Maintenance schedule.......................................................................................................10
General warnings......................................................................................................................11
Many internal parts of the GC carry dangerous voltages .............................................11
Electrostatic discharge is a threat to GC electronics....................................................11
Many parts are dangerously hot.......................................................................................12
Shutting down the GC..............................................................................................................13
For less than one week .....................................................................................................13
For more than one week...................................................................................................13
Chapter 2. The Keyboar an Display
The display ................................................................................................................................17
The status board .......................................................................................................................20
The keyboard ............................................................................................................................21
Instant action keys [Start], [Stop], and [Prep Run] ..............................................................22
Function keys............................................................................................................................23
Short-cut keys [Temp], [Pres], [Flow], [Det Control], [Ramp #] ....................................24
[Temp], [Pres], and [Flow]................................................................................................24
[Det Control].......................................................................................................................25
[Ramp #]..............................................................................................................................26
[Info]...........................................................................................................................................27

ii
Contents
[Status]....................................................................................................................................... 28
The Ready/Not Ready status table................................................................................... 28
The setpoint status table................................................................................................... 29
Procedure: Configuring the setpoint status table........................................................ 29
Miscellaneous keys .................................................................................................................. 30
[Time] .................................................................................................................................. 30
Procedure: Setting time and date .................................................................................. 30
Procedure: Using the stopwatch.................................................................................... 31
Procedure: Setting up [Post Run] .................................................................................. 31
[Run Log] ............................................................................................................................ 32
[Options] ............................................................................................................................. 33
[Config] ............................................................................................................................... 35
Modifier keys ............................................................................................................................ 36
[Mode/Type] ....................................................................................................................... 36
[Clear].................................................................................................................................. 37
[Delete]................................................................................................................................ 37
[.].......................................................................................................................................... 38
[–]......................................................................................................................................... 38
Storage and automation ..........................................................................................................39
Default parameters................................................................................................................... 40
Procedure: Loading the default parameters................................................................. 40
Chapter 3. Flow an Pressure Control
Hydrogen shutdown................................................................................................................. 43
Column shutdown .................................................................................................................... 43
Turning gas flows on and off .................................................................................................. 44
EPC-controlled streams.................................................................................................... 44
NonEPC-controlled streams............................................................................................. 44
Part 1. Electronic Pneumatic Control (EPC) ................................................... 45
Interpreting flow and pressure readings ............................................................................... 45
Configuration............................................................................................................................ 46
Columns and inlets................................................................................................................... 47
Configure the column .............................................................................................................. 48
Procedure: Configuring a capillary column.................................................................. 49
dditional notes on column configuration..................................................................... 50
Configure the carrier gas......................................................................................................... 51
Procedure: Configuring the carrier gas......................................................................... 51
Select a column mode.............................................................................................................. 52

Contents
iii
The flow modes..................................................................................................................52
The pressure modes...........................................................................................................52
Procedure: Selecting a column mode............................................................................ 53
Enter the initial flow or pressure or average linear velocity ..............................................54
Procedure: Setting initial flow or pressure or average linear velocity...................... 56
Enter a flow or pressure program (optional)........................................................................57
Procedure: Programming column pressure or flow .................................................... 57
Enter the rest of the inlet parameters....................................................................................59
Procedure: Setting the rest of the inlet parameters..................................................... 60
Detectors ...................................................................................................................................62
Gas configuration...............................................................................................................65
Makeup gas .........................................................................................................................65
uxiliary channels....................................................................................................................66
Procedure: Changing an auxiliary channel frit............................................................. 69
Maintaining EPC calibration ...................................................................................................70
Flow sensors.......................................................................................................................70
Pressure sensors ................................................................................................................70
Zero conditions ..................................................................................................................70
Procedure: Zeroing flow and pressure sensors............................................................ 71
Part 2. NonEPC control ...................................................................................... 72
Inlets...........................................................................................................................................72
Septum purge......................................................................................................................72
Detectors ...................................................................................................................................73
Internal/external plumbing: FID and NPD without EPC ...........................................73
Internal/external plumbing: TCD without EPC...........................................................74
Internal/external plumbing: ECD without EPC...........................................................74
Part 3. Measuring flow rates .............................................................................. 76
Measuring flow rates with a bubble meter............................................................................76
Where to measure flows ..........................................................................................................77
dapters for measuring flow rates ..................................................................................77
Procedure: Measuring gas flows with a bubble meter ................................................ 78
Interpreting flow meter measurements.................................................................................79
Part 4. Flow an pressure problems .................................................................. 80
gas does not reach the setpoint pressure or flow.............................................................80
gas exceeds the setpoint pressure or flow ........................................................................81
The inlet pressure or flow fluctuates.....................................................................................81
The measured flow is not equal to the displayed flow ........................................................82

iv
Contents
Chapter 4. The Column Oven
Oven capabilities ...................................................................................................................... 84
Oven safety................................................................................................................................ 85
Configuring the oven................................................................................................................ 86
Procedure: Setting up an isothermal run ............................................................................ 87
Making a temperature-programmed run ............................................................................... 88
Oven temperature programming setpoints .................................................................... 89
Oven ramp rates.................................................................................................................90
Procedure: Setting up a single-ramp program .................................................................... 91
Procedure: Setting up a multiple-ramp program ................................................................ 92
Fast chromatography............................................................................................................... 93
Fast-heating oven...............................................................................................................93
Configuring the oven......................................................................................................... 93
Using the oven insert for fast chromatography.................................................................... 94
To install the oven insert .................................................................................................. 94
Removing the insert...........................................................................................................96
Cryogenic operation................................................................................................................. 97
Cryogenic control setpoints ............................................................................................. 97
Chapter 5. Columns an Traps
Part 1. Capillary columns ................................................................................. 100
Column hanger ....................................................................................................................... 100
Procedure: Preparing capillary columns ........................................................................... 101
Procedure: Installing capillary columns in the split/splitless inlet ................................ 103
Procedure: Installing capillary columns in the cool on-column inlet ............................ 105
Procedure: Installing capillary columns in the purged packed inlet ............................. 106
Procedure: Installing capillary columns in the PTV inlet and Volatiles Interface ....... 109
Procedure: Installing capillary columns in NPD and FID detectors .............................. 109
Procedure: Installing capillary columns in the TCD ........................................................ 113
Procedure: Installing capillary columns in the ECD and µ-ECD .................................... 114
Procedure: Installing capillary columns in the FPD ........................................................ 118
Ferrules for capillary columns ............................................................................................. 121
Graphite and graphitized-Vespel ferrules..................................................................... 121
Vespel ferrules.................................................................................................................. 121
Part 2. Packe metal columns .......................................................................... 122
Overview: installing packed metal columns ....................................................................... 122
Fittings..................................................................................................................................... 123

Contents
v
Preparing packed metal columns.........................................................................................124
Procedure: Making a spacer from Teflon tubing ..............................................................125
Procedure: Installing ferrules on a metal column ............................................................127
Procedure: Installing an adapter in a detector fitting ......................................................128
Procedure: Installing packed metal columns ....................................................................129
Ferrules for packed metal columns .....................................................................................130
Part 3. Packe glass columns ............................................................................ 131
Overview: Installing glass packed columns ........................................................................131
Procedure: Installing glass packed columns .....................................................................133
Ferrules and O-rings for glass packed columns .................................................................135
Part 4. Con itioning columns ........................................................................... 136
Procedure: Preliminary column conditioning steps .........................................................137
Procedure: Conditioning a capillary column ....................................................................138
Procedure: Conditioning packed columns ........................................................................139
Part 5. Con itioning chemical traps ................................................................ 140
Part 6. Calibrating your capillary column (optional) ..................................... 141
Calibration modes ..................................................................................................................141
Column calibration procedures............................................................................................142
Procedure: Estimate the actual column length or diameter from
an elution time................................................................................................................ 142
Procedure: Estimate the actual column length or diameter from
the measured flow rate................................................................................................... 144
Procedure: Estimate the actual column length and diameter................................... 146
Chapter 6. Signal Han ling
Using the signal control tables..............................................................................................150
Signal type.........................................................................................................................150
Value ..................................................................................................................................150
nalog output settings—zero, range, and attenuation ......................................................154
nalog zero .......................................................................................................................154
Procedure: Zeroing signal output................................................................................. 154
Range—for analog outputs only ....................................................................................155
ttenuation—for analog outputs only...........................................................................156
Data rates..........................................................................................................................157
Procedure: Selecting fast peaks................................................................................... 157
Digital data handling ..............................................................................................................157
Digital zero........................................................................................................................157

vi
Contents
Baseline level shifts......................................................................................................... 157
ChemStation.....................................................................................................................159
INET .................................................................................................................................. 160
Column compensation........................................................................................................... 160
Procedure: Creating a column compensation profile ............................................... 162
Procedure: Making a run using column compensation ............................................ 162
Procedure: Plotting a stored column compensation profile .................................... 164
Test plot................................................................................................................................... 164
Chapter 7. Instrument Automation
Executing events during the run .......................................................................................... 168
Run time programming.......................................................................................................... 168
Using run time events ............................................................................................................ 169
Procedure: Programming run time events.................................................................. 170
The run table........................................................................................................................... 171
Procedure: dding events to the run table................................................................. 171
Procedure: Editing events in the run table................................................................. 172
Procedure: Deleting run time events........................................................................... 172
Clock time programming....................................................................................................... 173
Using clock time events.........................................................................................................174
Procedure: Programming clock time events.............................................................. 174
Procedure: dding events to the clock table ............................................................. 177
Procedure: Editing clock time events......................................................................... 177
Procedure: Deleting clock time events....................................................................... 178
Chapter 8. Analytical Metho s
What is a method?.................................................................................................................. 180
What can you do with it?....................................................................................................... 180
Creating a method.................................................................................................................. 181
Procedure: Storing a method ....................................................................................... 182
Procedure: Loading a previously stored method....................................................... 183
Procedure: Loading the default method ..................................................................... 184
Method mismatch................................................................................................................... 185
User-entered configuration changes ............................................................................. 185
Hardware configuration changes................................................................................... 185
Procedure: Modifying a previously stored method .......................................................... 186
Procedure: Deleting a stored method ................................................................................ 187

Contents
vii
Method listings........................................................................................................................187
Chapter 9. Valve Control
The valve box..........................................................................................................................190
Heating the valves............................................................................................................190
Valve temperature programming ...................................................................................191
Configuring an ux thermal zone ..................................................................................191
Valve control ...........................................................................................................................192
The valve drivers..............................................................................................................192
The internal valve drivers......................................................................................................192
The external valve drivers.....................................................................................................193
Valve configurations...............................................................................................................194
Procedure: Configuring a valve.................................................................................... 195
Valve control ...........................................................................................................................196
Procedure: Controlling valves from the keyboard..................................................... 196
From the run or clock time tables .................................................................................196
Valve control examples..........................................................................................................197
Simple valve—column selection....................................................................................197
Gas sampling valve ..........................................................................................................197
Multiposition stream selection valve and sampling valve ..........................................199
Chapter 10. The Automatic Liqui Sampler
Part 1. The 7673 ALS ......................................................................................... 202
Injector control table .............................................................................................................204
Procedure: Editing injector setpoints ......................................................................... 205
Configuring the injector.........................................................................................................205
Procedure: Configuring the injector............................................................................ 206
Sample tray setpoints.............................................................................................................206
Procedure: Editing the sample tray setpoints............................................................ 206
Procedure: Configuring the bar code reader.............................................................. 207
Storing injector setpoints ......................................................................................................208
Part 2. The 7683 ALS ........................................................................................209
Injector control table .............................................................................................................211
Procedure: Editing injector setpoints ......................................................................... 212
Configuring the injector.........................................................................................................213
Procedure: Configuring the injector............................................................................ 214
Sample tray setpoints.............................................................................................................214

viii
Contents
Procedure: Editing the sample tray setpoints............................................................ 214
Procedure: Configuring the bar code reader.............................................................. 215
Storing injector setpoints......................................................................................................215
Chapter 11. Analytical Sequences
What is a sequence? ............................................................................................................... 218
What can you do with it?....................................................................................................... 218
Defining a sequence ............................................................................................................... 220
Priority sequence ............................................................................................................. 221
Subsequences................................................................................................................... 221
Post Sequence ..................................................................................................................222
Procedure: Creating a sequence ......................................................................................... 222
Procedure: Creating a sampler subsequence ............................................................. 222
Procedure: Creating a valve subsequence.................................................................. 223
Procedure: Setting the Post Sequence events............................................................ 224
Procedure: Storing a sequence ........................................................................................... 225
Procedure: Loading a previously stored sequence .......................................................... 226
Procedure: Modifying a previously stored sequence ....................................................... 227
Procedure: Deleting a sequence ......................................................................................... 228
Sequence control.................................................................................................................... 228
Sequence status................................................................................................................229
Procedure: Starting/running a sequence..................................................................... 229
Procedure: Pausing and resuming a sequence........................................................... 230
Procedure: Stopping a sequence.................................................................................. 230
borting a sequence ........................................................................................................ 231
Special considerations when using an integrator .............................................................. 232
Chapter 12. Messages
Not Ready ......................................................................................................................... 234
Method Mismatches ........................................................................................................ 234
Warning............................................................................................................................. 235
Shutdown.......................................................................................................................... 235
Faults................................................................................................................................. 235
Bad mainboard and Fatal error messages.................................................................... 235
Part 1. Not Rea y messages ............................................................................. 237
Temperature zone not ready................................................................................................. 240
Pressure and/or flow not ready ............................................................................................ 241

Contents
ix
Detector not ready..................................................................................................................241
Valve not ready .......................................................................................................................243
Other not ready messages .....................................................................................................244
Part 2. Shut own messages .............................................................................. 246
Part 3. Warning messages ................................................................................. 252
Part 4. Fault messages ...................................................................................... 256

x
Contents

1
The 6890 Series
Gas Chromatograph
What’s unique to this instrument.
Maintenance. Strategy.

2
The 6890 Series
Gas Chromatograph
The 6890 Series Gas Chromatograph is referred to as “the GC” throughout this
manual.
Manuals
The Operating Manual is in three volumes:
•The General Information volume (this one) contains everything except
information on Inlets and Detectors.
•The Inlets volume is devoted to inlet systems, including maintenance and
troubleshooting procedures.
•The Detectors volume discusses detector systems, including maintenance
and troubleshooting procedures.
Each volume has its own index.

3
The 6890 Series Gas Chromatograph
Control tables
Control tables
This GC is controlled by a lengthy list of setpoints (temperatures, times, choice
of signal, and so on) that are organized into control tables. This is a typical oven
control table:
• Control table title—This line identifies the table. It does not move when the
rest of the table moves up or down.
• Visible setpoints in the display—The display has four lines. The title uses
one line leaving three to show setpoints and, in the Temp line, the current
actual value.
• Not-currently-visible setpoints—This table contains six setpoint lines. The
lower three can be moved into the viewing window when needed.
Installe equipment
Your instrument only displays control tables for items that are physically
present. There is no way to see a control table for an inlet, detector, or other
device that is not installed.
Control tables that list many instrument functions, such as [Status] or [Config],
only show items that are installed. Therefore, the sample displays in this manual
may be somewhat different than those on your instrument.
Control table title
Visible setpoints in the display
Not currently visible setpoints

The 6890 Series Gas Chromatograph
Using control tables
4
Using control tables
The general procedure for setting up the instrument is:
1. Press a key to call up a control table. It appears in the display. The first line
is a title that identifies the table.
2. Inspect the setpoints in the table (you may have to scroll up or down if it is
a long table).
3. Edit selected setpoints in the table.
4. Repeat this process with other tables until you have what you want.
5. nalyze the sample.
The advantage of a table is that it contains groups of related setpoints. You can
inspect them and alter them easily and quickly without having to execute key
sequences for each.
For example, to set up the front inlet, press [Front Inlet]
The control table for the type of inlet in the front position appears in the display.
Control tables for three inlet types, all with Electronic Pneumatic Control (EPC),
are on the next page.
Oven Front
Inlet
Back
Inlet
Col 1
Col 2
Front
Det
Back
Det
Signal 1
Signal 2
Col
Comp 1
Col
Comp 2
Ramp #
Det
Control
FlowPres
Aux #
Temp

5
The 6890 Series Gas Chromatograph
Using control tables
Figure 1 Some inlet control tables
Use the cursor keys (▲ and ▼) to move the cursor (<) to the line you wish to
change, type the new value, and press [Enter]. Repeat until the table is as you
want it.
Tables change depending on the modes you select and the instrument
configuration. Your tables are probably somewhat different from these.
Cool on-column
Split/Splitless
Purged packed
The top of the table. Use the scroll keys
(page to move it into the display).
The title line does not move.
You can view three lines of
the table in the display
The bottom of the table. Use the scroll
keys to move it into the display.

The 6890 Series Gas Chromatograph
Some specifics
6
Some specifics
Gas control
The GC can control all gas streams—inlets, detectors, and three auxiliary
flows—from the keyboard using Electronic Pneumatic Control (EPC). EPC
allows flow and pressure setting plus a variety of program modes.
Some nonEPC inlets and detectors are also available. They function in the
conventional manner using flow controllers, pressure regulators and a separate
flow meter. Only on/off control is available from the keyboard.
Columns
You can control the behavior of the carrier gas in the column, specifying constant
or ramped flow or constant or ramped pressure. EPC inlet systems maintain this
behavior for the entire run, even with temperature programming.
The column shoul be set up before the inlet!
Inlets an etectors
These are covered in the separate Inlets and Detectors volumes.
Signals
Signals are the data streams that exit the GC for processing by some other device.
There is a wide selection, both analog and digital.
Automation
The run time table executes commands at specified times after injection. The
clock time table executes commands at specified times of day.
Metho s an sequences
The active method is the set of control tables and values that is presently
controlling the GC. Up to five methods can be stored in memory.
sequence is a list of sample locations and the stored methods to be used to
run them. Up to five sequences can be stored. Samples may come from either
an automatic liquid sampler or a sampling valve with a stream selector valve.
Sequences can be interrupted to run urgent samples.

7
The 6890 Series Gas Chromatograph
Some specifics
Valves
Switching valves can be used for various column operations. Gas sampling
valves can be used either manually or with a multiposition stream selection
valve. If the multiposition valve is used, it can be combined with a sequence to
control the sample selection and analysis.

The 6890 Series Gas Chromatograph
Strategy
8
Strategy
The GC is organized around a set of control tables, each containing a group of
related setpoints. It is controlled by viewing and editing the tables to meet your
analytical needs. Some suggestions for doing this are:
• The content of many tables depends on what equipment is present. While
the GC can sense many of its components, some information (such as what
carrier gas is in use) must be entered by you. lways configure (define)
instrument elements before trying to use them.
• When setting up for analysis, configure the carrier gas first, then the column
mode, and finally the inlet. Detectors can be set up at any time.
• Use the [Config] key routinely to verify that the configuration is what you
believe it to be.
• Use the [Info] key for help with setpoint ranges, next action to perform, and
other advice.
• Many setpoints require that you select from a list of choices. The [Mode/
Type] key opens these lists. If a setpoint seems to call for an entry other than
a number or [On] or [Off], try [Mode/Type] to see if there is an underlying
menu.