Agilent 6890 Series Gas Chromatograph

Agilent 6890 Series Gas Chromatograph
Operating Manual
Volume 1. General Information
Agilent 6890 Series Gas
Chromatograph
Agilent Technologies 2000
All 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.G153090440 Operating Manual
Volume 1
Printed in USA
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 AC 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.
Agilent Technologies
assumes no liability for the
customer’s failure to
comply with these
requirements.
WARNING
A warning calls attention to
a condition or possible
situation that could cause
injury to the user.
CAUTION
A caution calls attention to
a condition or possible
situation that could damage
or destroy the product or
the user’s work.
See accompanying
instructions for
more information.
Indicates a hot
surface.
Indicates
hazardous
voltages.
Indicates earth
(ground) terminal.
Indicates radioactive hazard.
Indicates
explosion hazard.
Electromagnetic
compatibility
Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610
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, Agilent
Technologies, or an
experienced technician
for assistance.
7. Changes or modifications
not expressly approved
by Agilent Technologies
could void the user’s
authority to operate the
equipment.
HP® is a registered
trademark of HewlettPackard Co.
Microsoft®, Windows®,
and Windows NT® are
registered trademarks of
Microsoft Corporation.
Sound Emission
Certification for
Federal Republic of
Germany
Sound pressure Lp
< 65 dB(A)
During normal operation
At the operator position
According to ISO 7779
(Type Test)
When operating the 6890
with cryo valve option, the
sound pressure 74.6 dB(A)
during cryo valve operation
for short burst pulses.
Schallemission
Schalldruckpegel LP < 65
dB(A)
Am Arbeitsplatz
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(A) auf.
Contents
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
Automation ........................................................................................................................... 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 Keyboard and 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
i
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 and 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
Additional notes on column configuration..................................................................... 50
Configure the carrier gas......................................................................................................... 51
Procedure: Configuring the carrier gas......................................................................... 51
Select a column mode.............................................................................................................. 52
ii
Contents
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
Auxiliary 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
Adapters for measuring flow rates .................................................................................. 77
Procedure: Measuring gas flows with a bubble meter ................................................ 78
Interpreting flow meter measurements ................................................................................. 79
Part 4. Flow and pressure problems .................................................................. 80
A gas does not reach the setpoint pressure or flow............................................................. 80
A 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
iii
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 and 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. Packed metal columns .......................................................................... 122
Overview: installing packed metal columns ....................................................................... 122
Fittings ..................................................................................................................................... 123
iv
Contents
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. Packed 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. Conditioning columns ........................................................................... 136
Procedure: Preliminary column conditioning steps ......................................................... 137
Procedure: Conditioning a capillary column .................................................................... 138
Procedure: Conditioning packed columns ........................................................................ 139
Part 5. Conditioning 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 Handling
Using the signal control tables.............................................................................................. 150
Signal type......................................................................................................................... 150
Value .................................................................................................................................. 150
Analog output settings—zero, range, and attenuation ...................................................... 154
Analog zero ....................................................................................................................... 154
Procedure: Zeroing signal output................................................................................. 154
Range—for analog outputs only .................................................................................... 155
Attenuation—for analog outputs only........................................................................... 156
Data rates .......................................................................................................................... 157
Procedure: Selecting fast peaks ................................................................................... 157
Digital data handling .............................................................................................................. 157
Digital zero........................................................................................................................ 157
v
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: Adding 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: Adding events to the clock table ............................................................. 177
Procedure: Editing clock time events ......................................................................... 177
Procedure: Deleting clock time events ....................................................................... 178
Chapter 8. Analytical Methods
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
vi
Contents
Method listings........................................................................................................................ 187
Chapter 9. Valve Control
The valve box .......................................................................................................................... 190
Heating the valves ............................................................................................................ 190
Valve temperature programming ................................................................................... 191
Configuring an Aux 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 Liquid 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
vii
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
Aborting 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 Ready messages ............................................................................. 237
Temperature zone not ready................................................................................................. 240
Pressure and/or flow not ready ............................................................................................ 241
viii
Contents
Detector not ready..................................................................................................................241
Valve not ready ....................................................................................................................... 243
Other not ready messages ..................................................................................................... 244
Part 2. Shutdown messages .............................................................................. 246
Part 3. Warning messages ................................................................................. 252
Part 4. Fault messages ...................................................................................... 256
ix
Contents
x
1
The 6890 Series
Gas Chromatograph
What’s unique to this instrument.
Maintenance. Strategy.
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.
2
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
Visible setpoints in the display
Not-currently-visible setpoints
•
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.
Installed 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.
3
The 6890 Series Gas Chromatograph
Using control tables
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. Analyze 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]
Oven
Front
Inlet
Col 1
Front
Det
Signal 1
Col
Comp 1
Aux #
Back
Inlet
Col 2
Back
Det
Signal 2
Col
Comp 2
Temp
Pres
Flow
Det
Control
Ramp #
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.
4
The 6890 Series Gas Chromatograph
Using control tables
Cool on-column
Purged packed
Split/Splitless
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.
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.
5
The 6890 Series Gas Chromatograph
Some specifics
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 should be set up before the inlet!
Inlets and detectors
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.
Methods and 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.
A 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.
6
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.
7
The 6890 Series Gas Chromatograph
Strategy
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:
8
•
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. Always 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.
The 6890 Series Gas Chromatograph
Maintenance information
Maintenance information
Fuses and batteries
The GC requires fuses and batteries for proper operation. These should only be
accessed by Agilent service personnel.
Table 1
Mainboard Fuses and Batteries
Fuse designation
Fuse rating and type
F1, F2, F3, F4
8A, 250 Vac, IEC 127 type f (non-time delay), glass body
Battery designation
Battery rating and type
BT1
3-volt lithium battery, Panasonic BR3032
Table 2
AC Board Fuses
Fuse designation
Line voltage
Fuse rating and type
F1, F2
120 V
20 A, 250 Vac, IEC 127 type f (non-time delay), ceramic body
F1, F2
200 V - 240 V
15 A, 250 Vac, IEC type f (non-time delay), ceramic body
F3, F4
All
8 A, 250 Vac, IEC type f (non-time delay), glass body
9
The 6890 Series Gas Chromatograph
Maintenance information
Maintenance schedule
The frequency of maintenance depends upon:
•
•
•
•
•
The level of usage of the GC
The type of samples injected
Whether injections are manual or automatic
Whether the instrument is used for multiple applications or dedicated to one
Other environmental factors, such as dirt, ambient temperature, etc.
Table 3
10
Maintenance Schedule
Maintenance frequency
Items
Daily
Change septa, run a calibration sample, check the tightness of liner and
column nuts1
Weekly
Change glass liners and O-rings, if applicable
Monthly
Clean the split/splitless inlet vent line trap
Perform a leak check for hydrogen. Check all the connections from the initial
supply. At the GC, leak check the inlet and the column connections to the
inlet and detector.
Quarterly
Renew gas cylinders2
Semiannually
Clean detectors, perform wipe test on ECD
Annually
Recondition or replace internal and external traps and chemical filters
1
Very important for temperature programming using Vespel or Vespel/graphite ferrules
2
With typical usage, A-size cylinders will supply two dual-channel chromatographs for about
three months. Replace the cylinder when its pressure drops below 500 psig.
The 6890 Series Gas Chromatograph
General warnings
General warnings
Many internal parts of the GC carry dangerous voltages
If the GC is connected to power sources, even if the power switch is off,
potentially dangerous voltages exist on:
• The wiring between the detector power cord and power switch
• The wiring between the GC power cord and the AC power supply, the AC
power supply itself, and the wiring from the AC power supply to the power
switch.
With the power switches on, potentially dangerous voltages also exist on:
• All electronics boards in the instrument
• The internal wires and cables connected to these boards.
WARNING
All these parts are shielded by covers. With the covers in place, it should be
difficult to accidentally make contact with dangerous voltages. Unless
specifically instructed to, never remove a cover unless the detector, inlet, or
oven are turned off.
If the power cord insulation is frayed or worn, the cord must be replaced. Contact
your Agilent service representative.
Electrostatic discharge is a threat to GC electronics
The printed circuit (PC) boards in the GC can be damaged by electrostatic
discharge. Do not touch any of the boards unless it is absolutely necessary. If
you must handle them, wear a grounded wrist strap and take other antistatic
precautions. Wear a grounded wrist strap any time you must remove the
electronics side panel.
11
The 6890 Series Gas Chromatograph
General warnings
Many parts are dangerously hot
Many parts of the GC operate at temperatures high enough to cause serious
burns. These parts include but are not limited to:
• The inlets
• The oven
• The detectors
• The column nuts attaching the column to an injection port or detector
You should always cool these areas of the GC to room temperature before
working on them. They will cool faster if you first set the temperature of the
heated zone to room temperature. Turn the zone off after it has reached the
setpoint. If you must perform maintenance on hot parts, use a wrench and wear
gloves. Whenever possible, cool the part of the instrument that you will be
maintaining before you begin working on it.
WARNING
Be careful when working behind the instrument. During cooldown cycles, the
GC emits hot exhaust which can cause burns.
The insulation around the inlets, detectors, valve box, and the insulation cups
is made of refractory ceramic fibers. To avoid inhaling fiber particles, we
recommend the following safety procedures: ventilate your work area; wear
long sleeves, gloves, safety glasses, and a disposable dust/mist respirator;
dispose of insulation in a sealed plastic bag; wash your hands with mild soap
and cold water after handling the insulation.
12
The 6890 Series Gas Chromatograph
Shutting down the GC
Shutting down the GC
For less than one week
In general you can always leave the GC power on when not in use. If you will
not use the GC for up to approximately one week, conserve gases and energy
as follows:
WARNING
•
Reduce detector, inlet, and column temperatures to 150–200°C to save
energy.
•
Turn off corrosive or potentially hazardous gas flows, such as oxygen and
hydrogen.
•
Reduce flows of carrier and makeup gases.
•
Turn off coolant supplies at their sources.
Never leave flammable gas flows on if the GC will be unmonitored for long
periods of time. If a leak develops, the gas could create a fire or explosion hazard.
Maintaining the instrument with a lowered temperature and reduced carrier and
makeup gas flows keeps impurities from building in your column, inlet, and
detector.
For more than one week
1. Set all heated zones to ambient temperature and turn off the detector support
gas flows. Leave the carrier gas flow on.
2. When the GC is cool, turn it off.
3. Turn off all gas and coolant supplies at their sources.
4. Remove the column and cap its ends to prevent contamination. Store the
column in a cool, dry place.
5. To prevent contamination, cap the inlet and detector column fittings.
6. If gas connections are removed from the GC, cap the intake fittings on the
back panel of the GC and on the inlet manifold.
7. If desired, replace the split vent trap filter cartridge (if present).
13
The 6890 Series Gas Chromatograph
Shutting down the GC
14
2
The Keyboard and
Display
Keyboard, control tables, and the display.
The Keyboard and Display
Display
The title and three lines of a
control table are visible at
one time.
Status board
Flashing or solid display LEDs
show information about the
current state of the instrument.
Keyboard
Press a key to view a
control table or to enter
setpoints.
Figure 2
16
The GC controls
The Keyboard and Display
The display
The display
Think of this as a window through which you view the control tables. The top
line is a title—the other lines show the table content. If the table is more than
three lines long, use the scroll keys to see the additional lines.
Scroll keys (▲,▼)
Move the control table up or down in the display window.
The cursor (<)
Points to the line that is in editing position. Changes that you make using the
keyboard apply to the “cursored” line.
Asterisk (*)
A blinking asterisk prompts you to press [Enter] to store a setpoint or [Clear] to abort the
entry. You cannot perform any other task until this is done.
If this asterisk blinks, you cannot perform
any other function until you press [Enter]
or [Clear].
The asterisk on the left of a Mode/Type table indicates the current selection.
Press [Mode/Type] twice.
17
The Keyboard and Display
The display
Beeping instrument
If a gas flow cannot reach setpoint, you hear a series of beeps. The flow shuts
down after 1 or 2 minutes.
If a hydrogen flow is shut down or a thermal shutdown occurs, a continuous
beep sounds. Cancel the beep by pressing [Clear].
Any other type of fault, warning, or shutdown is accompanied by one beep.
Blinking setpoint
If a gas flow, multiposition valve, or the oven is shut down by the system, Off
will blink at the appropriate line of the control table. This helps you identify
where the problem occurred.
The detector On/Off line blinks if there is a pneumatics shutdown or a failure in
another part of the detector, such as a TCD filament.
Actual and setpoint values
When there are two values in one line of a control table, the left value is always
actual and the right value is always a setpoint. When there is only one value, it
is either an actual or setpoint, depending on the table. On some control tables—
such as those controlling columns—the far right number is both actual and
setpoint.
Actual values
Setpoint values
Actual value
Actual value
Setpoint value
Setpoint and actual values
18
The Keyboard and Display
The display
Messages
Cautions are reminders that your instrument may be configured incorrectly.
You see this message when:
•
[Column 1] and [Column 2] are configured to one inlet or one detector.
•
An auxiliary flow channel is used as an inlet, and the auxiliary carrier gas
type is configured as air. You cannot use air as a carrier gas.
Caution message:
Press [Clear] to remove the message. You can
then reconfigure the instrument, if desired,
or continue with your current configuration.
Errors mean that:
•
The setpoint you’ve entered is out of the allowable range.
•
You do not have the hardware on your instrument to support the operation
you have requested.
Error message:
Press [Clear] to remove the message.
You must enter a new setpoint, change
that hardware, or reconfigure the
instrument before continuing.
Popups appear when a Shutdown, Fault, or Warning occurs. They contain the
type and number of the error and a brief description. See chapter 12, in this
volume, for more information.
Popup message:
Press [Clear] to remove the message.
19
The Keyboard and Display
The status board
The status board
Oven Ramp
Final
Temp
Post
Run
Rate
Pre
Run
Figure 3
Table 4
20
Not
Ready
Run
Remote
Clock
Table
Gas Saver
Front
Initial
Temp
Run
Log
Back
The status board
The Display LEDs
LED
Description
Pre Run
Lit when the GC is in the Pre Run state (after [Prep Run] is pressed). See the Inlets volume
for more information.
Oven Ramp LEDs
Show the progress of the oven temperature program. The Rate LED blinks if the
oven is unable to follow the program.
Post Run
Lit when the instrument is executing a post run.
Not Ready
Lit when the GC is not yet ready to make a run. Blinks when the instrument has
one or more fault conditions. Press the [Status] key to see which parameters are
not ready or what faults have occurred.
Run
Lit when the instrument is executing a chromatographic run.
Remote
Indicates that communication with a remote device has been established.
Clock Table
Indicates that the clock table has entries.
Gas Saver
Indicates that the front or back gas saver is on.
Run Log
Indicates that the run log has entries. This information can be used for Good
Laboratory Practice (GLP) standards.
The Keyboard and Display
The keyboard
The keyboard
Stop
Prep
Run
Start
Instant action
keys
Oven
Front
Inlet
Col 1
Front
Det
Signal 1
Col
Comp 1
Aux #
Back
Inlet
Col 2
Back
Det
Signal 2
Col
Comp 2
Function keys
Temp
Pres
Flow
Det
Control
Ramp #
Short-cut keys
Information keys
Status
Mode
Type
Info
Time
On
Enter
Post
Run
Off
7
Run
Log
Front
4
5
6
Options
Back
1
2
3
Config
Delete
0
••
Clear
8
9
Numeric and
modifier keys
——
Miscellaneous keys
Method Storage and Automation
Load
Method
Run
Table
Front
Injector
Valve #
Store
Seq
Clock
Table
Back
Injector
Sample
Tray
Figure 4
Seq
Control
Method storage
and automation
The keyboard
21
The Keyboard and Display
Instant action keys [Start], [Stop], and [Prep Run]
Instant action keys [Start], [Stop], and [Prep Run]
These keys cause the instrument to do something now.
[Start] and [Stop]
Start and stop any type of run. [Stop] cancels a Pre Run, Post Run, or power fail
recovery and aborts an INET or local sequence.
[Prep Run]
If you are using one or more of the following functions, you must press [Prep
Run] to prepare for a run:
•
Gas saver—cancels gas saver flow and brings inlet flow to its setpoint value.
•
Splitless injection—closes the purge valve.
•
Pulsed split or splitless injection—increases inlet pressure to the pulse
setpoint.
•
Solvent vent injection—changes inlet pressure to the vent pressure setpoint
and split vent flow to the vent flow setpoint.
Pressing [Prep Run] turns on the Pre Run LED. When the LED is blinking, the
instrument is preparing for a run and waiting for instrument setpoints (other than the
ones associated with Prep Run) to be reached. Once these setpoints are ready, the LED
remains on and the Prep Run events occur. After a 6-second equilibration time, the
instrument is ready for a run and the Not Ready light goes out.
If you press [Prep Run] while the Pre Run LED is blinking, the LED stops blinking
before all setpoints are ready. At this point, the gas saver and purge valve portions of
your split/splitless inlet are ready for a run.
With most automatic injection systems, you do not need to use the [Prep Run]
key. If your sampler or automation controller (for example, an integrator or
workstation) does not support the Prep Run function, you must set the
instrument to Auto Prep Run. See the example on page 35.
22
The Keyboard and Display
Function keys
Function keys
Table 5 lists the function keys, a brief description of their use, and where to find
detailed information.
Table 5
The Function Keys
Key
Use to:
For more information:
[Oven]
Set oven temperatures, both isothermal and
temperature programmed.
Chapter 4, The Column Oven
[Aux #] [1] and
[Aux #] [2]
Control extra temperature zones such as a
heated valve box, a mass selective detector,
an atomic emission detector transfer line, or
an “unknown” device. Can do temperature
programming.
Chapter 9, Valve Control
[Aux #] [3],
[Aux #] [4], and
[Aux #] [5]
Provide auxiliary pneumatics to an inlet,
detector, or other device. Can do pressure
programming.
Chapter 3, Flow and Pressure
Control, and Chapter 11, Valve
Control
[Front Inlet] and
[Back Inlet]
Control inlet operating parameters.
Inlets volume
[Col 1] and [Col 2]
Control column pressure, flow, or velocity.
Can set pressure or flow ramps.
Chapter 3, Flow and Pressure
Control
Inlets and Detectors volumes
[Front Det] and
[Back Det]
Control detector operating parameters.
Detectors volume
[Signal 1] and
[Signal 2]
Assign a signal, usually to the front or back
detector.
Chapter 6, Signal Handling
[Col Comp 1] and
[Col Comp 2]
Create a column compensation profile.
Chapter 6, Signal Handling
23
The Keyboard and Display
Short-cut keys [Temp], [Pres], [Flow], [Det Control], [Ramp #]
Short-cut keys [Temp], [Pres], [Flow], [Det Control], [Ramp #]
Quickly access a setpoint from within a table.
[Temp], [Pres], and [Flow]
If no control table is open, pressing these keys gives you:
[Temp] Oven temperature
[Pres] Front inlet pressure (back or auxiliary pressure channel if front inlet is not
installed)
[Flow] Column 1 or 2 flow if EPC inlet. If not EPC, front detector or back detector
flow.
If the parameter is in the open control table, the cursor jumps to that line:
[Front Det] table open, cursor on
Mkup (He)
Cursor moves to Temp
Press
[Temp]
If the parameter is not in the open table, the key opens an appropriate table. For
example, if the oven control table is open and you push [Pres], the front inlet
control table opens with the cursor on the Pressure line.
[Oven] table open
[Front inlet] table opens
Press
[Pres]
24
The Keyboard and Display
Short-cut keys [Temp], [Pres], [Flow], [Det Control], [Ramp #]
[Det Control]
When viewing a detector control table, [Det Control] moves the cursor to the
on/off control for that detector.
[Front Det] table open, cursor on
Temp line
Press [Det Control]
Cursor on Filament, the
On/Off line for the thermal
conductivity detector
With a nondetector control table, [Det Control] opens the front detector control
table (or back, if a front detector is not installed). The cursor is at the on/off
control for that detector.
[Front Inlet]
[Det Control]
Cursor on Flame, the on/off
control for the flame ionization
detector
25
The Keyboard and Display
Short-cut keys [Temp], [Pres], [Flow], [Det Control], [Ramp #]
[Ramp #]
With a control table open that has no temperature, flow, or pressure ramps,
[Ramp #] plus a number opens the Oven control table. If no ramps are specified,
the cursor is on the Rate 1 (off) line.
Press [Ramp # [2]
Oven control table opens. Because no
temperature ramps are set on this table,
cursor is on the Rate 1 (off) line.
With a control table that contains temperature, flow, or pressure ramps,
[Ramp #] (1-6) moves the cursor to the first line of the ramp number specified.
If the ramp number does not exist, the cursor goes to the highest ramp number
in the control table.
[Col 1] table open, cursor on Pressure
line.
Press [Ramp #] [2]
Cursor moves to Rate 2 line.
26
The Keyboard and Display
[Info]
[Info]
This is a context-sensitive help that provides information about an active
parameter (line with the cursor).
These info messages may be in several different forms,
•
Definitions
•
Setpoint ranges
•
Actions to perform
The following examples are possible, depending upon the control table you are
in. Press [Info].
Definition:
Setpoint ranges:
Perform an action:
27
The Keyboard and Display
[Status]
[Status]
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. See chapter 12 for detailed information about the not ready, fault, and
warning status displays. The method mismatch displays are discussed in chapter 8,
“Methods”.
Ready for injection display
Ready display—check for warnings.
Not ready display
Not ready—items that are not ready.
If you have a not ready display, check
for faults or warnings.
Fault—a hardware problem requiring
user intervention.
Warning—problems that user should
be aware of but that will not prevent
instrument from executing a run.
Method mismatch—message appears
if hardware or user-entered
configuration has changed after
loading a method or power on.
28
The Keyboard and Display
[Status]
The setpoint status table
This table lists setpoints compiled from the active control tables on the
instrument. This is a quick way to view active setpoints during a run without
having to open multiple control tables.
Procedure: Configuring 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.
Press [Config][Status]
a. Scroll to Signal 1 and press [Enter].
b. Signal 1 is now the first item on the list.
29
The Keyboard and Display
Miscellaneous keys
Miscellaneous keys
[Time]
The time control table does not have a title. The first line always displays the
current date and time, and the last line always displays a stopwatch. The two
middle lines vary as shown.
Time display between runs
Actual time and date
Static display of last and next runtime in
minutes
Stopwatch
Time display during a run
Counts time elapsed during run
Counts down time remaining in run
Time display during Post Run
Static display of last runtime
Counts down time remaining in Post Run
Procedure: Setting time and date
Press [Config][Time]
Enter new time.
Enter new date.
30
The Keyboard and Display
Miscellaneous keys
Procedure: Using the stopwatch
In the stopwatch mode, both the time (to 0.1 second) and reciprocal time
(to 0.01 min-1) are displayed. The stopwatch is useful when measuring flows with a
bubble flowmeter.
1. Scroll to the stopwatch line of the Time Control Table.
2. Press [Enter] to start the stopwatch.
3. Press [Enter] again to stop.
4. Press [Clear] to set to zero.
You can access other functions while the stopwatch is running. Press [Time]
again to view the stopwatch display.
Procedure: Setting up [Post Run]
Use this key to program the instrument to clean out a column after a run. To set
up a Post Run:
1. Press [Post Run]
When Time is set at 0.00, other
lines of the control table are not
available.
2. Enter the post-run (column cleanout) Time, in minutes.
Once a setpoint for Time is entered,
other lines of control table become
available.
31
The Keyboard and Display
Miscellaneous keys
3. Enter Oven temp and Column pres.
The instrument is now programmed to
maintain the oven temperature at 250°C
for 10 minutes following a run, with
column 2 head pressure at 15.0 psi.
The Post Run LED on the status board is lit during a Post Run.
If you press [Time] while in a Post Run, you can view the amount of time
remaining.
[Run Log]
Deviations from the planned method (including keyboard intervention) during
the most recent run are listed in the run log table. Up to 50 run log entries can
be stored. The run log information can be used for Good Laboratory Practice
(GLP) standards. The run log can be uploaded to a workstation or printed out
on an integrator.
Press [Run Log]
The Run Log LED is lit if there are any entries in the run log for the run in progress.
The run log is cleared at the start of a new run.
32
The Keyboard and Display
Miscellaneous keys
If no run deviations have been logged, the display is:
[Options]
The option key accesses instrument parameter setup options.
Press [Options]
Scroll to the appropriate line and press [Enter] to access the associated control
table.
Calibration
Lists the parameters that can be calibrated. The calibration displays are
discussed in the Agilent 6890 Service Manual.
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, and turn Auto flow zero on.
Communication
Allows access to the communications setpoint parameters. The communication
displays are discussed in the Agilent 6890 Site Preparation and Installation
Manual.
33
The Keyboard and Display
Miscellaneous keys
Diagnostics
The diagnostic parameters are for use by your Service Representative.
Diagnostics are discussed in the Agilent 6890 Service Manual.
Keyboard and display
User interface setpoints are accessed in the keyboard and display control table.
The following parameters are turned on and off by pressing the [On] or [Off]
keys.
•
Keyboard lock—the following 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.
•
Key click—click sound when keys are pressed, can be turned on or off.
•
Warning beep—allows you to hear warning beeps.
•
Method mod 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
psi—pounds per square inch, lb/in2
bar—absolute cgs unit of pressure, dyne/cm2
kPa—mks unit of pressure, 103 N/m2
•
Radix type—determines the numeric separator type—1.00 or 1,00
Press [Mode/Type]
34
The Keyboard and Display
Miscellaneous keys
[Config]
The [Config] key sets up configurations for instrument control. The column
mode and dimensions, inlet, and makeup gas type configurations are critical to
proper operation of EPC.
Use [Config] with other keys for infrequently changed parameters.
Press [Config] [Oven]
Press the [Config] key to obtain a listing of configurable parameters:
Scroll to the Instrument
parameter. Press [Enter] to access the
Config Instrument control
table. Types shown depend on the
installed equipment
35
The Keyboard and Display
Modifier keys
Modifier keys
Modifier keys extend the functions of some setpoint control keys.
[Mode/Type]
Use this key to access a list of possible modes or types associated with
nonnumeric setpoints. To change mode or type, scroll to the desired line and
press [Enter]. An asterisk (*) marks the present mode or type.
The following are several examples of Mode/Type functions.
Mode:
Press
[Mode/Type]
Type:
Press
[Mode/Type]
Examples of instances when the words “Mode” or “Type” do not appear.
When in doubt, press [Info] to find out if [Mode/Type] is to be used.
Press
[Mode/Type]
36
The Keyboard and Display
Modifier keys
[Clear]
The [Clear] key is used to:
•
Clear mis-entered setpoints in a control table before pressing [Enter] (when
the * is still flashing).
•
Back out of Mode/Type select before pressing [Enter].
•
Return to upper level in nested control tables (config, option).
•
Clear the stopwatch to zero.
•
Clear info message and return to previous display.
•
Clear error messages (popup messages, errors on setpoint entries, etc.).
•
Cancel a function during a sequence, method, clock table, or run table and
loading or storing sequences and methods.
Press [Clear] to cancel
[Delete]
Deletes methods and sequences or run table and clock table entries.
Press [Delete]
[Delete] aborts the adjust offset process for the nitrogen-phosphorus (NPD) and
electron capture (ECD) detectors, without interrupting other detector
parameters.
37
The Keyboard and Display
Modifier keys
[.]
The radix is a decimal place holder. This parameter can be changed from the
decimal point to the comma in the Keyboard options control table, which is
nested under the Options control table.
Press [Options]
Press [Mode/Type]
[–]
The dash key is used to denote ranges of numbers (inclusive).
Sample range: 1 to 3, press [1] [–] [3]
Bottle # range: 1 to 10, press [1] [–] [1] [0]
This key is also used as a minus sign for negative values.
For –5, press [–] [5]
38
The Keyboard and Display
Storage and automation
Storage and automation
Table 6 lists the storage and automation keys, a brief description of their use,
and a place to find detailed information.
Table 6
Method and Sequence Storage and Automation Keys
Key
Use to:
For more information:
[Load]
Load up to five stored methods and five stored
sequences.
Chapter 8, Analytical Methods
Chapter 11, Analytical Sequences
[Store]
Store up to five methods and five sequences.
Stored methods and sequences are labeled
and dated.
Chapter 8, Analytical Methods
Chapter 11, Analytical Sequences
[Method]
Review a table of stored methods. You can
load, store, delete, or set default method.
Chapter 8, Analytical Methods
[Seq]
Review a table of stored sequences. The [Seq]
key toggles between the stored sequences
control table and sequence definition control
table.
Chapter 11,
Analytical Sequences
[Run Table]
View a table of events and the run time at
which they occur.
Chapter 7,
Instrument Automation
[Clock Table]
Display the clock time table of events in the
order that they occur based on a 24-hour
clock. You load, store, or delete.
Chapter 7,
Instrument Automation
[Front Injector]
or
[Back Injector]
Edit injector control parameters such as
injection volumes, sample and solvent washes,
etc.
Chapter 10,
Automatic Liquid Sampler
[Valve#]
Turn GSV and selection valves 1 to 8 on or off.
Sets multiposition valve position.
Chapter 9, Valve Control
[Sample Tray]
Display the tray status.
Chapter 10,
Automatic Liquid Sampler
[Seq Control]
Start, stop, pause or resume a sequence, and
view sequence status.
Chapter 11,
Analytical Sequences
39
The Keyboard and Display
Default parameters
Default parameters
The GC software supplies default values for most parameters if you do not
specify them. These values are reasonable operating parameters for inlets and
detectors. Once you change a parameter, the default value for that parameter is
erased.
At some time, you may find it desirable to reload the default parameters. Doing
this erases all current parameters except any methods you have stored and
replaces them with the default set.
Procedure: Loading the default parameters
1. Press [Method]
2. Scroll to the Set default method line and press [Enter].
3. This message will appear:
4. Press [Enter] to load the default parameters.
40
3
Flow and Pressure Control
Control types. Shutdown conditions.
Electronic Pneumatic Control (EPC)
inlets and detectors. NonEPC inlets
and detectors. Measuring flows.
Flow and Pressure Control
The 6890 Series Gas Chromatograph (the GC) has two types of gas control. Both
types can be present on the same instrument.
•
EPC—Electronic Pneumatic Control. Flows and pressures (inlets, detectors, and up to three auxiliary gas streams) are set at the keyboard.
•
NonEPC —Conventional flow/pressure control. Inlets use flow controllers
and pressure regulators in a pneumatics module on the left side of the GC.
Detector controls are on top of the GC behind the detectors. Flows are
measured with a bubble meter or other device.
Table 7
Detector and Inlet Controls
Module type
Control type
Control location
Inlet
EPC
Internal, via keyboard
Inlet
nonEPC
Module on left side
Detector
EPC
Internal, via keyboard
Detector
nonEPC
Top cover, behind detectors
Auxiliary
EPC
Internal, via keyboard
NonEPC detector controls
NonEPC inlet controls
Figure 5
Control location
The pneumatics module (dashed lines) is present if a nonEPC inlet is installed.
42
Flow and Pressure Control
Hydrogen shutdown
Hydrogen shutdown
Hydrogen gas may be used as a carrier or as fuel for some detectors. When mixed
with air, hydrogen can form explosive mixtures.
The GC monitors inlet and auxiliary gas streams. If a stream shuts down because
it is unable to reach its flow or pressure setpoint and if that stream is configured
to use hydrogen, the GC assumes that a leak has occurred and declares a
hydrogen safety shutdown. The effects are:
•
The carrier supply valve to the inlet closes and both pressure and flow
controls are turned off.
•
The split valves in the split/splitless and PTV inlets open.
•
The oven heater and fan turn off. The flaps at the rear open fully.
•
The small heated zones are turned off.
To recover from this state, fix the cause of the shutdown (tank valve closed,
serious leak, others). Turn the instrument off, then back on.
WARNING
The GC cannot detect leaks in the detector gas streams. For this reason, it is
vital that the column fittings of the FID, NPD, and any other detectors that use
hydrogen always be connected to a column or have a cap or plug installed and
that hydrogen streams be configured so that the GC is aware of them.
Column shutdown
If the carrier gas source shuts down, the oven heater turns off to avoid column
damage from heat without carrier gas. The flaps at the rear open halfway.
To recover from this state, fix the cause of the shutdown (tank valve closed,
serious leak, others). Turn the oven and the offending inlet or auxiliary channel
back on.
43
Flow and Pressure Control
Turning gas flows on and off
Turning gas flows on and off
All gas flows can be turned on or off from the keyboard without disturbing the
flow or pressure settings. However, the effect of an Off command depends on
whether the gas stream is EPC-controlled or not.
EPC-controlled streams
The valves in an EPC gas control module are designed for gas metering rather
than On/Off operation. When this type of valve is driven to the Off state, there
may still be a small flow, as much as 0.2 mL/min, through it. The display will
show this flow even though Off also appears. Note that this is an internal leak,
not a leak to the outside.
NonEPC-controlled streams
The valves in a nonEPC gas control module are designed only for On/Off action.
They are gas-tight when Off.
44
Part 1. Electronic Pneumatic Control (EPC)
Part 1.
Flow and Pressure Control
Interpreting flow and pressure readings
Electronic Pneumatic Control (EPC)
The GC can electronically control all the gas flows and pressures in the
instrument. It provides:
•
Flow and/or pressure control for all inlets, including flow and pressure
programming for the carrier gas through the column
•
Flow control via pressure regulation across fixed restrictors for all detector
gases
•
Pressure control for three auxiliary channels
•
A gas saver mode to reduce carrier gas consumption with the split/splitless
inlet, PTV inlet, and volatiles interface.
•
Direct entry of split ratios, provided the column is configured
The controlling hardware is mounted internally at the top rear of the instrument.
Setpoints are entered in the inlet, detector, or auxiliary control tables.
Interpreting flow and pressure readings
The EPC control board uses sensors for atmospheric pressure and the
temperature of the flow pneumatics modules to eliminate local conditions as
causes of retention time variability.
All flow and pressure displays are corrected to a defined set of conditions. These
conditions, which we call Normal Temperature and Pressure (NTP), are 25°C
and 1 atmosphere pressure. Similarly, setpoints are adjusted for the local
conditions.
Thus a flow displayed on the instrument and the flow measured with a bubble
meter may not agree, because the bubble meter readings represent local
conditions rather than NTP conditions. However, retention times become
independent of the local environment.
45
Flow and Pressure Control
Configuration
Part 1. Electronic Pneumatic Control (EPC)
VERY IMPORTANT
The 6890 with EPC measures flows and pressures continuously. This has a
strong effect on how the user sets up the instrument, and the rules for doing
so are different from the conventional approach to gas chromatography. The
differences are described in the next few pages.
Configuration
The GC identifies EPC inlets and detectors and most other devices by running
presence checks during power-up. Some information must be entered manually.
This is called configuration. A few things that must be configured are:
•
A description of the column (optional, but extremely desirable for capillary
columns)
•
NonEPC inlets and detectors (configured at the factory, if installed there)
•
The carrier gas in use
•
Some detector gases (if there is a choice)
Configuration information is stored in a battery-powered section of memory
independent of line power.
46
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Columns and inlets
Columns and inlets
The GC, with an EPC inlet, allows you to specify gas flow through capillary
columns directly. To use this feature:
1. Configure the column (supply length, inside diameter, and film thickness).
2. Configure the carrier gas. (What gas are you using?)
3. Select a column mode (constant flow or pressure, ramped flow or pressure).
4. Enter the initial flow or pressure or average linear velocity.
5. Enter a flow or pressure program (optional).
6. Enter the rest of the inlet parameters.
47
Flow and Pressure Control
Configure the column
Part 1. Electronic Pneumatic Control (EPC)
The rest of this chapter assumes that you have a split/splitless capillary column
inlet. If you have a different inlet, the discussion still applies but some details
differ. The procedures used as illustrations in the rest of this chapter are
somewhat simplified, because they show the most common ways to do things
but not all the alternatives. For the full details, see the Inlets and Detectors
volumes.
Configure the column
You define (configure) a capillary column by entering its length, diameter, and
film thickness. 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:
48
•
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.
•
Perform splitless injections with no need to measure gas flows.
•
Choose any of the four flow modes (discussed soon). If the column is not
defined, your choices are limited and vary depending on the inlet.
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Configure the column
Procedure: Configuring a capillary column
1. Press [Config] [Col 1] or [Config] [Col 2]. The column configuration screen
appears.
2. If necessary, use the ▲ and ▼ keys to move (scroll) the cursor to the Length
line.
Enter column dimensions
Identify the inlet
Identify the detector
3. Type the column length, in meters, followed by [Enter].
4. Scroll to Diameter, type the column inside diameter in microns, followed
by [Enter].
5. 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 dimensions—they are usually supplied with the
column—or if you do not wish to use the GC calculating features, enter 0 for
either length or diameter. The column will be not defined.
6. Scroll to Inlet and press [Front] or [Back] to identify the inlet that the
column is connected to.
7. Scroll to Detector and press [Front] or [Back] to identify the detector
that the column is connected to.
This completes configuration for a capillary column. See the Inlets and Detectors
volumes for more detail.
49
Flow and Pressure Control
Configure the column
Part 1. Electronic Pneumatic Control (EPC)
Additional notes on column configuration
•
Vacuum correct—If the detector exhausts into the atmosphere, this
parameter should be Off. If a column is connected directly to a mass selective
detector, the parameter should be On. This allows the GC to compensate for
either the local atmospheric pressure (Off) or for the reduced pressure in a
mass selective detector (On).
•
Pres correct—Some detectors, such as an atomic emission detector,
operate at pressures that are neither atmospheric or vacuum. This parameter
lets the user enter an appropriate pressure value.
•
Packed columns should be entered as column not defined. To do this, enter
0 for either column length or column diameter.
•
You should check configurations for both columns to verify that they specify
separate inlets. If you are only using one column, it is still important that the
second column be indicated for a different inlet, even if it is undefined.
Failure to do this will lead to some very unusual flow calculations.
It is possible, and sometimes appropriate, to configure both installed
columns to the same inlet.
•
50
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.
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Configure the carrier gas
Configure the carrier gas
The GC needs to know what carrier gas is being used.
Procedure: Configuring the carrier gas
1. Press [Config] [Front Inlet] or [Config] [Back Inlet].
2. Press [Mode/Type] to see the carrier gas menu.
Carrier gas type.
Press [Mode/Type] to get menu.
3. Scroll to the gas you will use. Press [Enter].
This completes carrier gas configuration. See the Inlets volume for more detail.
51
Flow and Pressure Control
Select a column mode
Part 1. Electronic Pneumatic Control (EPC)
Select a column mode
The flow modes
Flow rates are corrected to NTP (normal temperature and pressure, 25°C and
1 atmosphere. For more detail, see pages 45 and 79.
•
Constant flow—Maintains a constant mass flow rate of carrier gas in the
column throughout the run. If the column resistance changes due to a
temperature program, the column head pressure is adjusted to keep the flow
rate constant. This can shorten runs significantly.
•
Ramped flow—Increases the mass flow rate in the column during the run
according to a program you enter. A column flow profile can have up to three
ramps, each consisting of a programmed increase followed by a hold period.
The pressure modes
Pressures are gauge pressures—the difference between the absolute pressure
and the local atmospheric pressure. Because most detectors present little
resistance to the column flow, the gauge pressure at the column head is usually
the same as the pressure difference between column inlet and exit. The mass
selective detector and the atomic emission detector are the exceptions.
52
•
Constant pressure—Maintains a constant gauge pressure at the head of
the column throughout the run. If the column resistance changes, the gauge
pressure does not change but the mass flow rate does.
•
Ramped pressure—Increases the column head gauge pressure during the
run according to a program you enter. A column pressure profile can have
up to three ramps, each consisting of a programmed increase followed by a
hold period.
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Select a column mode
Procedure: Selecting a column mode
1. Press [Col 1] or [Col 2].
2. Scroll to the Mode line.
3. Press [Mode/Type] to see the column mode menu.
Here is your carrier gas choice.
These are the column length and
inside diameter that you entered.
Press [Mode/Type] to see
the Column Mode menu.
4. Scroll to the column mode you want. Press [Enter].
This completes column mode selection. Next you must specify the inlet
conditions either during the entire run (if you selected either of the constant
modes) or at the beginning of the run (if you selected either of the ramped
modes).
53
Flow and Pressure Control
Enter the initial flow or pressure or average linear velocity
Part 1. Electronic Pneumatic Control (EPC)
Enter the initial flow or pressure or average linear
velocity
If the column is defined, you can enter any one of these quantities—the GC will
calculate and display the other two.
For example, you may have selected Constant pressure as the column
mode. You decide to specify, as a starting condition, the column flow. The GC
will compute the pressure necessary to achieve this flow (as well as the average
linear velocity) and hold this pressure constant during the run.
If you select Constant flow as the mode and specify column flow as the
initial condition, the GC will still calculate the pressure necessary to achieve
this flow, but it will adjust the pressure as necessary to maintain constant flow.
If the column is not defined, you can enter only pressure. Constant flow can still
be specified, but the GC cannot know what the flow is.
See the following table for recommended flows for various column diameters.
These are close to optimum for a wide variety of components.
54
Part 1. Electronic Pneumatic Control (EPC)
Table 8
Flow and Pressure Control
Enter the initial flow or pressure or average linear velocity
Column Size and Carrier Gas Flow Rate
Carrier gas flow rate
Column type
Column size
Packed
1/8-inch
30
1/4-inch
60
Capillary
Hydrogen
Helium
50 µm id
0.5
0.4
100 µm id
1.0
0.8
200 µm id
2.0
1.6
250 µm id
2.5
2.0
320 µm id
3.2
2.6
530 µm id
5.3
4.2
These flow rates, in mL/min at normal temperature and pressure (25°C and 1 atm)
are recommended for all column temperatures.
For capillary columns, flow rates are proportional to column diameter and are 20%
lower for helium than for hydrogen.
55
Flow and Pressure Control
Enter the initial flow or pressure or average linear velocity
Part 1. Electronic Pneumatic Control (EPC)
Procedure: Setting initial flow or pressure or average linear velocity
1. Press [Col 1] or [Col 2].
The column length and inside diameter.
You set one of these. The GC
calculates the other two.
The column mode; see below.
The control table will have one of these, depending on the column mode selected:
2. Scroll to the Pressure or Flow or Velocity line.
3. Type the desired initial value, followed by [Enter]. The GC will compute and
display the other two values. Adjust them, if you choose to, by repeating
steps 2 and 3 but note that changing any one changes all three.
This completes setting the initial carrier gas condition.
56
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Enter a flow or pressure program (optional)
Enter a flow or pressure program (optional)
If you selected either the ramped pressure or ramped flow column mode, the
column control table contains entries for setting up a ramp program.
You begin with an initial value, either Init Pres or Init Flow, and an
Init time. At the end of that time, Rate 1 begins and runs until it reaches
Final pres (or Final flow). It remains at that value for
Final time 1. You can then add a second and third ramp, each consisting of
a Rate, a Final value (pressure or flow), and a Final time.
The program ends when it reaches a Rate that is set to 0 (off).
When a flow or pressure program is running, the Pressure, Flow, and
Velocity lines that you used to set constant conditions show the progress of
the program.
The oven program determines the length of the run. If a flow or pressure program
ends before the analytical run does, the flow (or pressure) remains at the last
final value.
Procedure: Programming column pressure or flow
1. Press [Col 1] or [Col 2].
Pressure (in this example) is the
controlled setpoint; the others
are reported values.
Because Mode is Ramped
pres, the ramp is given in
pressure units.
57
Flow and Pressure Control
Enter a flow or pressure program (optional)
Part 1. Electronic Pneumatic Control (EPC)
2. Scroll to Init Pres (or Init flow). Type the desired value and press
[Enter].
3. Similarly, enter a value for Init time. This completes the initial (constant
pressure) part of the program.
4. To begin a ramp, enter a positive value for Rate 1. It does not matter
whether you are programming up or down—the rate is always positive.
5. If Rate 1 is zero, the program ends here. If you enter any other value, the
Final value lines for the first ramp appear and the cursor moves to the line.
6. Enter values for Final pres 1 (or Final flow 1) and Final
time 1. This completes the first ramp.
7. To enter a second (or third) ramp, scroll to the appropriate Rate line and
repeat steps 5 and 6.
58
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Enter the rest of the inlet parameters
SUMMARY
Note that, except when setting the carrier gas type, we have been
concerned only with the Column tables. This is fundamental to successful
operation of the 6890 with EPC inlets.
FIRST:
THEN:
Set up the column
Set up the rest of the instrument
Enter the rest of the inlet parameters
The split/splitless inlet has four operating modes:
•
Split—The sample is divided between the column and a vent flow.
•
Splitless—The sample is not divided. Most of it enters the column. A small
amount is purged from the inlet to avoid excessive peak broadening and
solvent tailing.
•
Pulsed split—Similar to split, except that the inlet pressure is raised before
and during injection and returned to normal at a user-specified time. Total
flow is increased as well so that the split ratio does not change. This special
kind of “programming” is independent of the three-ramp flow or pressure
programming.
•
Pulsed splitless—Like pulsed split, but splitless.
The split/splitless inlet has a gas saver feature. This reduces the flow of carrier
into the inlet and out the split vent after the injection is complete. It does not
alter the flow through the column.
The septum purge flow is set automatically on all EPC inlets.
And, of course, the inlet temperature can be controlled.
59
Flow and Pressure Control
Enter the rest of the inlet parameters
Part 1. Electronic Pneumatic Control (EPC)
Procedure: Setting the rest of the inlet parameters
1. Press [Front Inlet] or [Back Inlet].
2. Scroll to the Mode line.
3. Press [Mode/Type] to see the inlet mode menu.
Press [Mode/Type] to see
the Inlet Mode menu.
4. Move the cursor to the inlet mode you want. Press [Enter]. The inlet table
may change, depending on your choice. The possibilities for the definedcolumn case are shown on the next page.
5. Scroll to Temp. Type the temperature you want. Press [Enter].
6. If you selected Split, and if the column is defined, you may enter the split
ratio directly.
For details on the inlet parameters, see the Inlets volume.
60
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Enter the rest of the inlet parameters
Split mode
Inlet temperature
Split parameters
Gas saver parameters
Splitless mode
Splitless parameters
The pulsed modes
Pulse
parameters
Figure 6
Control tables for the Split/Splitless inlet
61
Flow and Pressure Control
Detectors
Part 1. Electronic Pneumatic Control (EPC)
Detectors
Although EPC detectors have built-in pressure regulation, you still need external
regulators so that the electronic control has a stable gas supply to work with.
You may want to use traps to remove contaminants from the gas supply. If so,
they should be as close to the back of the GC as possible.
EXTERNAL
pressure
regulators
6890 GC
Proportional
valves
Pressure
sensors
Air in
Control
Restrictions
FID
or
NPD
H2 in
Makeup in
Figure 7
Internal/external plumbing: FID and NPD with EPC
For more detail, see the Detectors volume.
62
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Detectors
6890 GC
EXTERNAL
pressure
regulator
TCD
Proportional
valves
Pressure
sensors
Restrictors
Reference
switching
valve
Reference and
makeup in
Control
Makeup flow
Figure 8
Internal/external plumbing: TCD with EPC
For more detail, see the Detectors volume.
63
Flow and Pressure Control
Detectors
Part 1. Electronic Pneumatic Control (EPC)
6890 GC
External
pressure
regulator
Proportional
valves
Pressure
sensors
Restrictors
Anode purge
and makeup in
Control
Anode purge
Makeup flow
Figure 9
Internal/external plumbing: ECD with EPC
For more detail, see the Detectors volume.
64
ECD
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Detectors
Vent
Filter Proportional Pressure
valves
sensors
frits
Restrictors
Emission zone
Air
Shield
H2
Window
Wavelength
filter
Makeup
Figure 10 Internal/external plumbing: FPD with EPC
For more details, see the Detectors volume.
Gas configuration
The GC assumes that hydrogen is plumbed to the FID, FPD and NPD H2 locations
and that air is plumbed to the air locations (see the labels on the EPC gas
modules).
Some locations allow a choice of gases. In these cases (mostly makeup gases),
you must identify the gas using the [Config] process.
Makeup gas
You can select either constant makeup flow or constant (makeup + column)
flow. See the Detectors volume for details, since they vary with the detector type.
65
Flow and Pressure Control
Auxiliary channels
Part 1. Electronic Pneumatic Control (EPC)
Auxiliary channels
Three additional auxiliary pressure control channels are available as an option.
They are controlled by the Aux 3, Aux 4, and Aux 5 tables (Aux 1 and 2 are heater
controls).
If an auxiliary channel is specified as the Inlet during column configuration,
the channel allows run time programming as well as three-ramp programming.
The most common case of this is when a gas sampling valve is used.
The auxiliary channels are controlled by a pressure setpoint. To work properly,
there must be adequate flow resistance downstream of the pressure sensor. The
auxiliary channel pneumatics manifold provides a frit-type restrictor for each
channel. Four frits are available:
Frit marking
Flow resistance
Part no.
Blue Dot
High
19234-60660
Red Dot
Medium
19231-60770
Brown Dot
Low
19231-60610
None (brass tube)
Zero
G1570-20540
The Red Dot frit is in all three channels when the instrument is shipped.
The figures on the next two pages show approximate pressure/flow
relationships for the three Dot frits, assuming there is no significant additional
resistance downstream of the frits.
If the Zero resistance frit is installed, the user must provide flow resistance
downstream and generate the pressure/flow relationships.
WARNING
66
When hydrogen is used, dangerously high flows are possible if insufficient flow
resistance is provided downstream of the supply tube. Always use either the
High (Blue Dot) or Medium (Red Dot) frit with hydrogen.
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Auxiliary channels
Pressure requirements for AUX EPC flow restrictors
with air, nitrogen, or helium
(ambient conditions: 25°C, 14.7 psia)
80
70
19234-60660
(blue dot)
60
50
19231-60770
(red dot)
Minimum
source
pressure
(psig)
40
30
19231-60610
(brown dot)
20
10
0
0.1
1.0
10.0
Gas flow in mL/min
100.0
1000.0
67
Flow and Pressure Control
Auxiliary channels
Part 1. Electronic Pneumatic Control (EPC)
Pressure requirements for AUX EPC flow restrictors
with hydogen
(ambient conditions: 25°C, 14.7 psia)
80
70
19234-60660
(blue dot)
60
Minimum
source
pressure
(psig)
50
19231-60770
(red dot)
40
30
20
19231-60610
(brown dot)
10
0
0.1
68
1.0
10.0
Gas flow in mL/min
100.0
1000.0
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Auxiliary channels
Procedure: Changing an auxiliary channel frit
1. Locate the block that connects the three gas outlet tubes for the auxiliary
channels to the pneumatics module.
2. Remove the screw that holds the block to the pneumatics module. Pull the
block free of the module and rotate it so that the frits are on top.
Changeable
gas restrictions
Aux 4
Aux 5
Aux 3
Aux 3
Aux 4
Aux 5
Gas outlets
3. Pull the frit to be changed out of the block. Also remove the O-ring that seals
it.
4. Place an O-ring on the new frit. Place the O-ring/frit combination in the block.
5. Reconnect the block to the pneumatics module. Tighten the screw firmly.
69
Flow and Pressure Control
Maintaining EPC calibration
Part 1. Electronic Pneumatic Control (EPC)
Maintaining EPC calibration
The EPC 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 and purged packed inlet modules use flow sensors. If the
Auto flow zero feature (see page 33) is on, they are zeroed automatically
after each run. This is the recommended way. They can also be zeroed
manually—see the next page.
Pressure sensors
All EPC control modules use pressure sensors. They can be zeroed as a group
or individually. There is no automatic zero for pressure sensors.
Zero conditions
IMPORTANT
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.
Table 9
70
Flow and Pressure Sensor Zero Intervals
Sensor type
Module type
Zero interval
Flow
All
Use Auto flow zero
Pressure
Inlets
Packed columns
Every 12 months
Small capillary columns
(id 320 µm or less)
Every 12 months
Large capillary columns
(id > 320 µm)
At 3 months, at 6 months, then every
12 months
Auxiliary channels
Every 12 months
Detector gases
Every 12 months
Part 1. Electronic Pneumatic Control (EPC)
Flow and Pressure Control
Maintaining EPC calibration
Procedure: Zeroing flow and pressure sensors
To zero a flow or pressure sensor in a specific module
1. Press [Options], scroll to Calibration, and press [Enter]
2. Scroll to the module to be zeroed and press [Enter]
Note: After zeroing or flow calibration,
the Factory Calibration
line is replaced by the time and date of the
recalibration.
To restore the Factory Calibration, select
the time and date line and press [Delete].
This destroys the user calibration.
3. Scroll to a zero line and press [Info]
or
4. To cancel, press [Clear]
5. To zero flow, verify that the carrier gas
is connected and is turned on.
6. Press [On] to zero or [Clear] to cancel.
4. To cancel, press [Clear]
5. To zero pressure, verify that the
supply gas line is not connected.
6. Press [On] to zero or [Clear] to cancel.
To zero all pressure sensors in all modules
1. Press [Options], scroll to Diagnostics, and press [Enter]
2. Scroll to Electronics and press [Enter]
3. Scroll to Pneumatics Board and press [Enter]
4. Scroll to Zero all p sensors and press [Info]
5. To cancel, press [Clear]
6. To zero, verify that the supply gas lines are disconnected from all modules.
7. Press [On] to zero or [Clear] to cancel.
71
Flow and Pressure Control
Inlets
Part 2.
Part 2. NonEPC control
NonEPC control
Control tables for nonEPC inlet and detector gases provide on/off control but
do not control flow rates or pressures. These must be set manually and verified
using a bubble meter or other flow meter. See page 76 for bubble meter
operation.
Inlets
Pressure regulators, flow controllers, and other controls for nonEPC sample
inlets are mounted in a module on the left side of the GC. See the Inlets volume
for operating information.
PURGED
PACKED
COLUMN
HEAD PRESSURE
CARRIER FLOW
INCR
SPLIT
Purged packed
inlet gas controls
Split/splitless
inlet gas controls
SEPTUM PURGE
INCR
COLUMN
HEAD PRESSURE
TOTAL FLOW
INCR
SEPTUM PURGE
INCR
SPLIT/SPLITLESS SEPTUM PURGE
INLET VENT
VENT
VENT
Figure 11 NonEPC inlet gas controls
Septum purge
Septum purge flow is set automatically on the nonEPC purged packed inlet; it
can be measured at a vent on the front panel. Septum purge is a user adjustment
on the nonEPC split/splitless inlet.
72
Part 2. NonEPC control
Flow and Pressure Control
Detectors
Detectors
NonEPC detectors have internal single-stage pressure regulators for some gas
streams. You should still use external two-stage regulators.
You may also want to use traps to remove contaminants from the gas supply. If
so, they should be as close to the back of the GC as possible.
Internal/external plumbing:
FID and NPD without EPC
Hydrogen and air flows for these detectors are controlled by external pressure
regulators and internal flow restrictors. Makeup gas is controlled by an internal
pressure regulator located behind the detector positions. See the Detectors
volume for flow rate details.
EXTERNAL
pressure
regulators
6890 GC
Keyboard-controlled
On/off solenoid
valves
Restrictors
Air in
FID
or
NPD
H2 in
Makeup in
Internal
pressure
regulator
Figure 12 FID and NPD without EPC
73
Flow and Pressure Control
Detectors
Part 2. NonEPC control
Internal/external plumbing: TCD without EPC
This detector has two internal pressure regulators, one for reference gas and
one for makeup gas, that are supplied from a single fitting. The pressure
regulators are located behind the detector positions.
6890 GC
EXTERNAL
pressure
regulators
INTERNAL
pressure
regulators
TCD
Keyboard-controlled
On/off solenoid
valves Restrictors
Reference
switching
valve
Reference and
make up in
Makeup flow
Figure 13 TCD without EPC
See the Detectors volume for flow rate details.
Internal/external plumbing: ECD without EPC
This detector has an internal pressure regulator that supplies both the anode
purge gas and the makeup gas. The pressure regulator is located behind the
detector positions.
74
Part 2. NonEPC control
Flow and Pressure Control
Detectors
6890 GC
EXTERNAL
pressure
regulator
Anode purge
and makeup in
INTERNAL
pressure
regulator
Keyboard-controlled
On/off solenoid
valves Restrictors
Anode purge
ECD
Makeup flow
Figure 14 ECD without EPC
See the Detectors volume for flow rate details.
75
Flow and Pressure Control
Measuring flow rates with a bubble meter
Part 3.
Part 3. Measuring flow rates
Measuring flow rates
This section describes how to measure flow rates in the GC and how to convert
the measurements to the conditions used by the GC. If your GC uses EPC, please
note that the flow and pressure sensors in the GC are often more accurate than
off the shelf, inexpensive flow meters. If you can establish a calibrated flow or
pressure in the GC, a measurement that agrees with the GC within a few percent
(after conversion to NTP; see page 79) should verify the GC’s manifolds are
operating properly and do not need replacement
Measuring flow rates with a bubble meter
A bubble flow meter is a very basic, reliable tool for measuring gas flow. It
creates a bubble meniscus across a tube through which the gas is flowing. The
meniscus acts as a barrier, and its motion reflects the speed of the gas through
the tube. Most bubble flow meters have sections of different diameters so they
can measure a wide range of flows conveniently.
A bubble flow meter with rate ranges of 1, 10, and 100 mL/min is suitable for
measuring both low flow rates (such as carrier gases) and higher flow rates
(such as air for an FID).
Start
1 mL
10 mL
Figure 15 A three-volume bubble meter
76
100 mL
Part 3. Measuring flow rates
Flow and Pressure Control
Where to measure flows
Where to measure flows
EPC inlets—Septum purge and split vent flows exit through the pneumatic
module at the top rear of the GC.
Split vent
Septum purge
Split/splitless and PTV
pneumatic module
Septum purge
Purged packed and cool
on-column pneumatic module
EPC and nonEPC detectors—Measure all flows, including carrier, at the exit of
the detector. Use the control tables to select one gas at a time.
NonEPC inlets—The flow vents are on the front panel. See page 72.
Adapters for measuring flow rates
A rubber adapter tube attaches directly to an NPD, ECD, or TCD exhaust vent.
A separate adapter is supplied for the FID and similar detectors. Insert the
adapter into the detector exhaust vent as far as possible. You will feel resistance
as the adapter O-ring is forced into the detector exhaust vent. Twist and push
the adapter during insertion to ensure a good seal.
77
Flow and Pressure Control
Where to measure flows
Part 3. Measuring flow rates
Procedure: Measuring gas flows with a bubble meter
Tools:
WARNING
•
Bubble meter graduated at 1, 10, and 100 mL. Bulb half-filled with soapy
water.
•
Adapter for detector or vent
•
GC internal stopwatch
Do not measure hydrogen together with air or oxygen. This can create explosive
mixtures that may be ignited by the automatic ignitor.
To avoid this hazard:
Turn the automatic ignitor off before you begin.
Always measure gases separately.
1. Attach the inlet line of the bubble meter to the fitting where you will measure
flow. Use the appropriate adapter, if needed.
2. Hold the bubble flow meter vertically—squeeze and release the bulb to
create a meniscus in the bubble meter. Do this several times to wet the sides
before taking measurements.
3. Press [Time] to see the stopwatch screen. Squeeze the bulb.
4. Press [Enter] to start the stopwatch when the meniscus passes the START
(lowest) line in the bubble flow meter.
5. Press [Enter] again to stop the stopwatch when the meniscus passes the
1 mL, 10 mL, or 100 mL line.
6. Calculate the flow rate in mL/min from the 1/t value:
•
If you used the 1 mL line, the flow rate in mL/min = 1/t.
•
If you used the 10 mL line, the flow rate in mL/min = 10 × 1/t.
•
If you used the 100 mL line, the flow rate in mL/min = 100 × 1/t.
7. Press [Clear] to reset the stopwatch. Repeat the measurement at least once
to verify the flow.
78
Part 3. Measuring flow rates
Flow and Pressure Control
Interpreting flow meter measurements
Interpreting flow meter measurements
Bubble meter measurements yield flow rates at the local temperature and local
atmospheric pressure. Electronic flow meters may be calibrated for
temperatures other than 25°C or for pressures other than 1 atm. However, the
GC display shows values corrected to Normal Temperature and Pressure (NTP)
conditions. If you do not correct your meter’s flow rate to NTP, the readings will
not agree with the GC.
To convert meter flow rate measurements to NTP (25°C and
1 atmosphere), you must know:
•
The local atmospheric pressure or the electronic meter calibrated pressure
•
The bubble meter temperature at the time of measurement or the electronic
meter’s calibration temperature.
The conversion is:
Flow rate at NTP =
Flow ratelocal x 298 x Pressurelocal
Temperaturelocal
where:
Flow rate at NTP
is the flow rate in mL/min corrected to Normal
Temperature (25°) and Pressure (1 atmosphere)
Flow ratelocal
is the flow rate in mL/min measured by the bubble
meter
Temperaturelocal
is the temperature of the bubble meter at the time
of measurement or the meter’s calibration
temperature. This number is in Kelvins
(Kelvin = Centigrade + 273).
Pressurelocal
is the local atmospheric pressure at the time of
measurement or the meter’s calibration
temperature. This number is in atmospheres
(1 atm = 1.01325 bars = 760 Torr = 760 mm Hg (at
0°C) = 101.325 kPa = 14.7 psi).
79
Flow and Pressure Control
A gas does not reach the setpoint pressure or flow
Part 4.
Part 4. Flow and pressure problems
Flow and pressure problems
A gas does not reach the setpoint pressure or flow
The gas cannot reach the pressure entered at the keyboard. If an EPC inlet does
not reach its pressure setpoint it will shut down in an amount of time determined
by the type of inlet:
Type of inlet
Time before shutdown
Purged packed, cool on-column
2 minutes
Split/splitless, PTV, volatiles inteface
5.5 minutes
Auxiliary
4 minutes
•
The gas supply pressure is too low to reach the setpoint. The pressure at the
supply should be at least 10 psi greater than the desired setpoint.
•
A large leak is present somewhere in the system. Use an electronic leak
detector to find leaks; correct them. Don’t forget to check the column—a
broken column is a very large leak.
•
If you are using gas saver, be sure that the gas saver flow rate is high enough
to maintain the highest column-head pressure used during a run.
•
The flow is too low for the column in use.
•
The column is plugged or misinstalled.
•
The inlet or detector pressure sensor is not operating correctly. Contact your
Agilent service representative.
If you are using a split/splitless, PTV inlet, or volatiles interface:
•
The split ratio is too low. Increase the amount of split flow.
•
The inlet proportional control valve is stuck because of contamination or
other fault. Contact your Agilent service representative.
If you are using a purged packed or cool on-column inlet:
•
80
The inlet control valve is stuck closed because of contamination or other
fault. Contact your Agilent service representative.
Part 4. Flow and pressure problems
Flow and Pressure Control
A gas exceeds the setpoint pressure or flow
A gas exceeds the setpoint pressure or flow
•
The pressure sensor for that device is not operating properly. Contact your
Agilent service representative.
If you are using a split/splitless inlet, PTV inlet, or volatiles interface:
•
The split ratio is too high. Decrease the split ratio.
•
The proportional control valve is stuck closed. Contact your
Agilent service representative.
•
The trap on the split vent line is contaminated. Contact your
Agilent service representative.
If you are using a purged packed or cool on-column inlet:
•
The inlet proportional control valve is stuck open. Contact your
Agilent service representative.
The inlet pressure or flow fluctuates
A fluctuation in inlet pressure will cause variations in the flow rate and retention
times during a run.
•
A small leak is present in the flow system. Use an electronic leak detector
to find leaks; correct them. You should also check for leaks in the gas supply
plumbing.
•
Large restrictions, such as a blockage in a liner or the split vent trap, are
present in the split/splitless or PTV inlets. Make sure that you are using the
correct liner. Replace liners with large pressure drops caused by design or
tight packaging. If the liner does not appear to be causing the problem, the
split vent trap may be blocked. Contact your Agilent service representative.
•
Extreme changes in room temperature during runs. Correct laboratory
temperature problem or move the instrument to a more suitable location.
81
Flow and Pressure Control
The measured flow is not equal to the displayed flow
•
Part 4. Flow and pressure problems
Large volumes have been added to the system (this may occur if you are
using a sampling valve). Decrease the sample volume. Use EPC inlets which
correct for variations in temperature and pressure.
The measured flow is not equal to the displayed flow
You checked the flow at an inlet with a bubble flow meter, corrected the
measurement to NTP conditions, and discovered that it does not match the
calculated flow displayed on the GC.
82
•
The column length, internal diameter, or gas type is configured incorrectly.
Enter the correct information. Press [Config] [Column 1] or [Config]
[Column 2] to enter the column specifications. Press [Config] [Front Inlet]
or [Config] [Back Inlet] to enter the gas type. If a considerable amount has
been cut off a capillary column, its actual length may no longer match its
original. Configure the column with a new length.
•
A new pressure setpoint was not entered after constant flow mode was
selected. Enter a new pressure setpoint each time constant flow is turned
on or off.
•
A short (<15 m) 0.58 to 0.75 mm id WCOT column is being used with a split/
splitless capillary inlet. The total flow controller is set for a high flow rate,
which creates some pressure in the inlet and causes column flow even with
a setpoint pressure of zero. (In these situations, an actual pressure may be
shown on the display, even with a zero setpoint.) With short, 530 to 750 mm
columns, keep the total flow rate as low as possible (for example,
20 to 30 mL/min). Install a longer column with higher resistance (for
example, 15 to 30 m).
•
The split vent line may be partly plugged, creating an actual inlet pressure
higher than the setpoint pressure. Replace the split vent line.
•
A Mass Selective Detector is in use and vacuum compensation is not
selected.
4
The Column Oven
Controlling the oven. Making isothermal
and programmed runs. Cryogenic operation.
The Column Oven
Oven capabilities
Capability
Range
Temperature range
–80°C (liquid N2) or –60°C (CO2) to the configured limit
Maximum temperature
450°C
Temperature programming
Up to six ramps
Maximum run time
999.99 minutes
Temperature ramp rates
0 to 120°C/min, depending on instrument configuration
The oven holds two inlets and two detectors, up to four valves in a heated box
on top of the oven and two valves inside the oven, and either capillary or packed
columns.
On/Off
switch
Oven door
latch
Figure 16 Column oven
84
The Column Oven
Oven safety
Oven safety
For safety, opening the oven door turns off power to the oven heater, fan, and
cryogenic valve (if installed) but maintains the setpoints in memory.
Closing the oven door returns the oven to normal operation.
If the oven cannot attain or maintain an entered setpoint temperature during
normal above-ambient operation, a problem is assumed and the oven is switched
off.
Possible problems include:
•
The oven vent flaps not working
•
The oven fan, heater, or temperature sensor not working properly
•
An electronic problem
When a shutdown occurs, the Off line in the oven control table blinks and the
oven remains off until switched on again via [Oven] [On] or by editing the Temp
setpoint in the oven control table.
When the oven shuts itself off, the following display appears:
See chapter 12 in this volume for more information on shutdowns.
85
The Column Oven
Configuring the oven
Configuring the oven
Oven configuration sets maximum temperature, equilibration time, and the
cryogenic setpoints, if cryo is installed.
Press [Config] [Oven]
Maximum temp setpoint range: 70 to 450°C
Maximum temp Maximum allowable oven temperature setpoint. Some
accessories, such as the valve box, valves and columns have specific
temperature limits. When configuring Maximum temp, these limits should be
considered so that the accessories are not damaged. Oven setpoints are verified
as they are entered; a message is displayed when an entered setpoint is
inconsistent with a previously defined maximum.
Equib time The time required for the oven temperature to equilibrate after
temperature is modified. Equilibration time begins when the actual oven
temperature comes within 1°C of the oven temperature setting. The Equib
time setpoint can be 0 to 999.99 minutes.
86
The Column Oven
Procedure: Setting up an isothermal run
Procedure: Setting up an isothermal run
An isothermal run is one in which the oven is maintained at a constant
temperature. To create an isothermal run, set Rate 1 to zero.
1. Press [Oven] to access the oven control table.
2. Enter the oven temperature for the isothermal run. Note that your actual
and setpoint values will probably differ from the example.
3. Enter the number of minutes (Init time) that you want the oven to stay
at this temperature. This time is the duration of the run.
4. If Rate 1 is not 0, enter zero for an isothermal run.
87
The Column Oven
Making a temperature-programmed run
Making a temperature-programmed run
You can program the oven temperature from an initial temperature to a final
temperature using up to six ramps during a run.
A single ramp temperature program raises the initial oven temperature to a
specified final temperature at a specified rate and holds at the final temperature
for a specified period of time.
Final temp
Final time
Rate
Temp
(Init temp)
Init time
Figure 17 Single ramp
The multiple-ramp temperature program is similar. You can program the oven
from an initial temperature to a final temperature, but with various rates, times,
and temperatures in between. Multiple ramps can also be programmed for
temperature decreases as well as increases.
Final temp 2
Final time 2
Rate 2
Final temp 1
Final time 1
Rate 1
Temp
Init time
Figure 18 Multiple ramp
88
The Column Oven
Making a temperature-programmed run
Oven temperature programming setpoints
Temp Starting temperature of a temperature programmed run. When the
program begins, this value is copied into a temporary setpoint called Init
temp. At the end of the run, Temp is reset to the value in Init temp and
the oven returns to its starting temperature.
Init temp Equal to Temp except during a programmed run (Init temp
remains constant; Temp changes as directed by the program). Changing Init
temp changes the starting temperature for the next run. Changing Temp causes
an immediate change but the value is not saved to the next run.
Init time Time in minutes that the oven will stay at the starting temperature
after a programmed run has begun.
Rate
The rate in °C/min at which the oven will be heated or cooled.
Final temp
Temperature of the oven at the end of a heating or cooling rate.
Final time Time in minutes that the oven will be held at the final
temperature of a temperature-programmed rate.
Total length of a run is determined by its oven temperature program. The
maximum allowable time for a run is 999.99 minutes. If the program is still
running at that time, the run terminates.
89
The Column Oven
Making a temperature-programmed run
Oven ramp rates
To use the fast oven ramp rates (a 240 V power option is required), your electric
service must be able to supply ≥ 200V at ≥ 15 Amp.
The highest rate that you can achieve depends on many factors, including the
room temperature, temperatures of the inlets and detectors, the amount of
material inside the oven (columns, valves, etc.), and whether or not this is the
first run of the day. The optional oven insert for fast chromatography (see
page 94), increases oven ramp rates for the back column. Table 10 lists typical
oven ramp rates.
Table 10 Oven Ramp Rates
90
100/120 V oven
ramp rate (°C/minute)
200/220/230/240 V oven
ramp rate (°C/minute)
Temperature
range (°C)
Without
insert
With optional
insert
Without
insert
With optional
insert
50 to 70
75
120
120
120
70 to 115
45
95
95
120
115 to 175
40
65
65
110
175 to 300
30
45
45
80
300 to 450
20
35
35
65
The Column Oven
Procedure: Setting up a single-ramp program
Procedure: Setting up a single-ramp program
This example increases the oven temperature from 50°C to 150°C at a rate of
10°C/minute.
1. Press [Oven] to access the oven control table.
2. Enter a starting temperature (Temp).
3. Enter the time (Init time) that you want the oven to stay at Temp.
4. Enter the rate (Rate 1) at which the oven temperature is to increase.
5. Enter the final temperature (Final temp 1).
6. Enter the time (Final time 1) the oven is to hold Final temp 1.
7. To end the oven ramp program after Ramp 1, set Rate 2 to zero.
91
The Column Oven
Procedure: Setting up a multiple-ramp program
Procedure: Setting up a multiple-ramp program
Set up the first oven ramp as described on the preceding page.
In a multiple-ramp temperature program, the Final time for one ramp is
also the Init time for the next ramp. Thus, there is only one Init time
(before Ramp 1).
1. Enter the rate (Rate 2) at which you want the oven temperature to increase
for the second oven ramp.
2. Enter the final temperature (Final temp 2).
3. Enter the number of minutes (Final time 2) that you want the oven to
hold the final temperature.
4. To end the temperature program after Ramp 2, set Rate 3 to zero.
To add additional oven ramps, repeat the steps described above.
92
The Column Oven
Fast chromatography
Fast chromatography
The 6890 GC has several options for increasing throughput and cycle time. These
are the fast heating oven (optional in some countries), the oven insert for fast
chromatography (see page 94), and cryogenic cooling (see page 97).
Fast-heating oven
The fast-heating oven requires the following:
•
A GC equipped with a fast-heating oven. A fast heating oven is standard with
most 200–240 V power option GCs. A GC ordered for the United States, Canada, Switzerland, China, and Australia must be ordered with the fast heating
oven option, or must be converted (contact Agilent service).
•
The electric service must be capable of providing ≥ 200 V at ≥ 15 amperes.
•
In the United States, the electric service must be 240 V.
Configuring the oven
GCs ordered with the fast-heating oven will be properly configured from the
factory. If you convert a regular oven to a fast-heating oven, and have the correct
electric service installed, you will need to configure the GC to use the new oven
heater properly.
WARNING
Do not perform this procedure unless your GC meets all of the criteria listed
under “Fast-heating oven” above. Conversion from a regular to fast-heating oven
(and the reverse) requires replacement of the oven heater, internal fuses, and
power circuitry by qualified Agilent personnel. Changing the oven configuration
at the keypad without making the proper hardware changes can damage your
instrument and may present a fire hazard.
1. Press [Config], scroll to [Instrument], and press [Enter].
2. To change the oven type, press [.][.], then [Mode/Type].
3. Select the correct oven type (fast or regular), then press [Enter].
93
The Column Oven
Using the oven insert for fast chromatography
Using the oven insert for fast chromatography
The 6890 Oven Insert for Fast Chromatography reduces the oven volume so that
the column and sample heat more quickly, yielding faster separation and faster
chromatography. Furthermore, the smaller volume oven cools faster than a fullsized oven, reducing the overall analytical cycle time.
Carrying strap
Warning!
Metal surfaces
may become hot
Front
Back
Figure 19 Oven insert
The oven insert is used with any inlet, column, and detector mounted in the back
position. It is not compatible with any accessory which obstructs access to the
back of the oven or which requires the use of either the front inlet or the front
part of the oven.
To install the oven insert
1. Turn off your GC oven and allow it to cool.
Caution
94
The cutouts in the interior oven walls may have sharp edges that can damage
the oven insert fabric.
The Column Oven
Using the oven insert for fast chromatography
2. Orient the oven insert as shown in Figure 20 below. Tilt the upper edge away
from you and insert it between the column fittings for the front inlet/detector
and the back column hanger.
Align behind front
inlet, if installed
Align insert to rest
against front edge
of back column
hanger
Carrying strap
is vertical
Figure 20 Installing the insert in front of the back column hanger
3. Push the bottom of the insert into place as shown in Figure 21. Keep the
insert upright as shown.
4. If a TCD, ECD, µ-ECD, or NPD is installed in the front detector position, cap
off the make-up adapter and establish a purge flow.
95
The Column Oven
Using the oven insert for fast chromatography
Top of oven
Keep insert vertical
Figure 21 Oven insert installed in the oven
Removing the insert
1. To remove the insert, turn off the GC oven, inlet, and detector heated zones
and allow them to cool.
WARNING
The metal fasteners on the oven insert may remain hot even after the oven has
cooled. Always handle the insert only by its carrying strap, or wear heat-resistant
gloves.
2. Use the carry strap to remove the oven insert, pulling out the bottom edge
first.
96
The Column Oven
Cryogenic operation
Cryogenic operation
The cryogenic valve lets you operate the oven below ambient temperature.
Minimum attainable oven temperature depends on the type of valve installed.
The GC senses the presence and type of cryogenic valve and disallows setpoints
if no valve is installed. When cryogenic cooling is not needed or cryogenic
coolant is not available, the cryogenic operation should be turned off. If this is
not done, proper oven temperature control may not be possible, particularly at
temperatures near ambient.
For information on installation and coolants see “Cryogenic Cooling
Requirements” in the Agilent 6890 Site Preparation and Installation Manual.
Cryogenic control setpoints
All cryogenic setpoints are in the [Config] [Oven] control table.
If your instrument is not equipped
with the cryogenic option, part of
the display will look like this
Cryo setpoints
Cryo
[ON] enables cryogenic cooling, [OFF] disables it.
Quick cryo cool This feature is separate from Cryo. Quick cryo cool
makes the oven cool faster after a run than it would without assistance. This
feature is useful when maximum sample throughput is necessary, however it
does use more coolant. Quick cryo cool turns off soon after the oven reaches
its setpoint and Cryo takes over, if needed.
Ambient temp The temperature in the laboratory. This setpoint determines
the temperature at which cryogenic cooling is enabled:
97
The Column Oven
Cryogenic operation
•
Ambient temp + 25°C, for regular cryo operation
•
Ambient temp + 45°C, for Quick Cryo Cool.
Cryo timeout Cryo timeout occurs, and the oven shuts off, when a run does
not start within a specified time (10 to 120 minutes) after the oven equilibrates.
Turning cryo timeout off disables this feature. We recommend that it be turned
on because cryo timeout conserves coolant at the end of a sequence or if
automation fails.
Cryo fault Shuts the oven down if it does not reach setpoint temperature
after 16 minutes of continuous cryo operation. Note that this is the time to reach
the setpoint, not the time to stabilize and become ready at the setpoint. For
example, with a cool on-column inlet and cryo control in the oven track mode,
it may take the oven 20 to 30 minutes to achieve readiness.
If the temperature goes below the minimum allowed temperature (–90°C for
liquid nitrogen,–70°C for liquid CO2), the oven will shut down with the following
display:
98
5
Columns and Traps
Preparing and installing capillary columns,
metal columns, and glass columns.
Columns and Traps
Part 1.
Capillary columns
This section contains information on preparing and installing capillary columns
in inlets and detectors. See page 122 for packed metal columns and page 131 for
packed glass columns.
Column hanger
Agilent capillary columns are wound on wire frames that mount on a hanger
connected to the top of the oven interior.
You can connect the column hanger in two positions. Use the position that best
centers the column in the oven. Column ends should make smooth curves to the
inlet and detector fittings. Do not let any section of the column come in contact
with the oven surfaces.
Column hanger,
Part no. 1460-1914
Capillary column
100
Part 1. Capillary columns
Columns and Traps
Procedure: Preparing capillary columns
Procedure: Preparing capillary columns
You must prepare your capillary column before installation. Proper preparation
assures that the column end has no burrs or jagged edges and is not
contaminated with graphite or other material.
WARNING
Wear safety glasses to protect your eyes from flying particles while handling,
cutting, or installing glass or fused silica capillary columns. Use care in handling
these columns to prevent puncture wounds.
Materials required
Column nut and ferrule
Capillary column
Column cutter
Magnifying loop
Isopropanol
Tissue
1. Place a capillary column nut and ferrule on the column.
Ferrule
Column nut
Column
101
Columns and Traps
Procedure: Preparing capillary columns
Part 1. Capillary columns
2. Score the column using a glass scribing tool. The score must be square to
ensure a clean break.
Glass scribing
tool
3. Break off the column end by supporting it against the column cutter opposite
the scribe. Inspect the end with a magnifying glass to make certain there are
no burrs or jagged edges.
4. Wipe the column walls with a tissue dampened with isopropanol to remove
fingerprints and dust.
102
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the split/splitless inlet
Procedure: Installing capillary columns in the split/splitless inlet
Before installing the column, be sure you have the correct glass liner installed.
Instructions on choosing and installing liners are in the Inlets volume.
Materials required
Column nut and ferrule
Column cutter
Typewriter correction fluid
1/4-inch wrench
Metric ruler
1. Prepare the column. See page 101 for instructions.
2. Position the column so it extends 4 to 6 mm above the end of the ferrule.
Mark the column with typewriter correction fluid at a point even with the
column nut.
FP
4 to 6 mm
Mark column here
3. Insert the column in the inlet and slide the nut and ferrule up the column to
the inlet base. Finger tighten the column nut until it starts to grab the column.
Insulation
cover
103
Columns and Traps
Procedure: Installing capillary columns in the split/splitless inlet
Part 1. Capillary columns
4. Adjust the column position so that the correction fluid mark on the column
is even with the bottom of the column nut.
Correction fluid mark
5. Tighten the column nut an additional 1/4 to 1/2 turn so that the column cannot
be pulled from the fitting with gentle pressure.
1/4 turn
6. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperature. Allow them to cool, and then retighten the fittings.
104
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the cool on-column inlet
Procedure: Installing capillary columns in the cool on-column inlet
Before installing the column, be certain you have the correct hardware installed
for the column and type of injection you are doing. See the Inlets volume for
detailed information.
Materials required
Column nut and ferrule
Column cutter
1/4-inch wrench
1. Prepare the column. See page 101 for instructions.
2. Gently insert the column into the inlet until it bottoms. Insert the column
nut into the inlet fitting and tighten the nut finger tight.
3. Tighten an additional 1/4-turn with a wrench or until the column does not
move.
4. If you are using an automatic injection system with 250 µm or 320 µm
columns, verify the installation by pushing the syringe manually into the
inlet.
5. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperatures. Allow them to cool, and then retighten the fittings.
105
Columns and Traps
Procedure: Installing capillary columns in the purged packed inlet
Part 1. Capillary columns
Procedure: Installing capillary columns in the purged packed inlet
Before installing a column in this inlet, be sure you have a capillary liner and
glass insert installed. Instructions on choosing and installing this hardware are
in the Inlets volume. If your insulation cup is not installed, begin with Step 1.
Otherwise, begin with Step 4.
Materials required
Column nut and ferrule
Column cutter
Typewriter correction fluid
1/4-inch wrench
Metric ruler
Insulation cup
No-hole ferrule to use as a plug when installing the insulation cup
1. Install a plug in the inlet fitting.
Inlet fitting
Capillary liner
Column nut with
no-hole ferrule
Insulation cup
106
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the purged packed inlet
2. Install the insulation cup, if needed. Push the cup spring to the right. Slide
the cup over the inlet fitting so that the insulation at the top of the cup is
flush against the oven roof.
3. Place the spring into the groove in the inlet liner. Remove the column nut
and put the no-hole ferrule aside.
Groove
4. Prepare the column. See page 101 for instructions.
5. Position the column so it extends above the end of the column nut by 1 to
2 mm. Mark the column with typewriter correction fluid at a point even with
the column nut.
FP
1 to 2 mm
Mark column here
107
Columns and Traps
Procedure: Installing capillary columns in the purged packed inlet
Part 1. Capillary columns
6. Push the column up 1 cm and guide it into the inlet liner. Slide the nut and
ferrule up the column to the inlet liner. Adjust the column position so that
the correction fluid mark on the column is even with the bottom of the
column nut. Finger tighten the column nut until it starts to grab the column.
Correction fluid mark
7. Tighten the column nut an additional 1/4 to 1/2 turn so that the column cannot
be pulled from the fitting when gentle pressure is applied.
1/4 turn
8. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperatures. Allow these to cool, and then retighten the fittings.
108
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the PTV inlet and Volatiles Interface
Procedure: Installing capillary columns in the PTV inlet and Volatiles Interface
The column installation procedures for these two inlets are unique to them.
Details are in the PTV and Volatiles Interface chapters of the Inlets volume.
Procedure: Installing capillary columns in NPD and FID detectors
Be sure you have the correct jet installed in your detector before installing a
column. Details about choosing and installing detector jets are later in this
chapter.
There are two types of NPD/FID detector fittings:
•
Adaptable– for use with both packed and capillary columns
•
Capillary optimized– for use with capillary columns only. If your adaptable
fitting does not have a capillary adapter installed, begin with step 1. If you
have a capillary optimized fitting or if the capillary adapter is already
installed in your adaptable fitting, begin with step 5.
Materials required
Both fitting types:
Column nut and ferrule
Column cutter
1/4-inch wrench
Metric ruler
Typewriter correction fluid
For adaptable fitting only:
1/4-inch nut and ferrule
Capillary column adapter
9/16-inch wrench
109
Columns and Traps
Procedure: Installing capillary columns in NPD and FID detectors
Part 1. Capillary columns
1. Assemble a brass nut and graphite/Vespel ferrule onto the adapter.
1/4-inch ferrule
1/4-inch nut
Capillary column
adapter
2. Insert the adapter straight into the detector base as far as possible. Hold the
adapter in this position and tighten the nut finger tight. Use a wrench to
tighten the nut an additional 1/4 turn.
Detector fitting
Capillary column adapter
3. Prepare the column (see page 101 for instructions). If the column id is greater
than 100 µm, follow steps 7 to 9. If the column id is less than 100 µm, follow
steps 4 to 6, then follow steps 8 and 9.
110
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in NPD and FID detectors
4. If your column inside diameter is less than 100 µm:
Position the column so it extends above the ferrule by 48 mm (capillary
optimized fitting) or 68 mm (adaptable fitting). Mark the column with typewriter
correction fluid even with the column nut.
Capillary optimized fitting
Adaptable fitting
P
P
P
P
4848mm
mm
mm
mm
6868mm
68
68 mm
mm
Markcolumn
columnhere
here
Mark
Mark column here
Mark column here
5. Insert the column in the detector. Slide the nut and ferrule up the column to
the detector base. Finger tighten the column nut until it starts to grab the
column.
111
Columns and Traps
Procedure: Installing capillary columns in NPD and FID detectors
Part 1. Capillary columns
6. Adjust the column position so that the correction fluid mark on the column
is even with the bottom of the column nut. Proceed to step 8.
Correction fluid mark
7. Gently insert the column into the detector until it bottoms; do not attempt
to force it further.
8. Tighten the column nut finger tight, then withdraw the column about 1 mm.
Use a wrench to tighten the nut an additional 1/4 turn.
9. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperatures. Allow them to cool and then retighten the fittings.
112
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the TCD
Procedure: Installing capillary columns in the TCD
Materials required
Capillary column adapter
Column nut and ferrule set
Column cutter
Wrenches
1. Assemble the ferrules and a 1/8-inch brass nut on the column as shown.
Detector fitting
Front ferrule
Back ferrule
Column nut 1/8-inch brass
Part no. 5180-4103 (10/pk)
Column
See Table 11 for the proper ferrules. Trim off a short piece of column to
remove any ferrule fragments inside the column.
2. Insert the column into the detector until it bottoms. Do not attempt to force
it.
3. Slide the column nut and ferrule up the column to the detector and tighten
the nut finger tight.
4. Pull the column out 1 mm. Use a wrench to tighten the nut an additional
1/4 turn. The column should not move.
113
Columns and Traps
Procedure: Installing capillary columns in the ECD and µ-ECD
Part 1. Capillary columns
Table 11 Ferrules for the TCD detector
Column outside diameter
Back ferrule
Front ferrule
0.8 mm
G1530-80400
G1530-80410
0.53 mm
G1530-80400
G1530-80420
0.45 mm
G1530-80400
G1530-80430
No-hole ferrule
G1530-80400
G1530-80440
Procedure: Installing capillary columns in the ECD and µ-ECD
Both detectors are shipped with a capillary column adapter installed. If it has
been removed, you must replace it before installing a capillary column.
There are two kinds of adapter liner. The straight liner is a simple tube and is a
light brown color. The indented liner is necked down near one end and is clear.
The µ-ECD requires the indented liner.
Materials required
Capillary column adapter
Fused silica liner, straight or indented (required for µ-ECD)
1/4-inch nut and 1/4-inch graphitized Vespel ferrule
Column nut and ferrule
Column cutter
1/4-inch and 9/16-inch wrenches
1. Remove the adapter cap and check the liner. Replace it if it is broken and
reinstall the cap. If you use an indented liner, the indentation must be at the
cap end of the adapter.
Cap
Fused silica liner
Capillary column adapter
114
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the ECD and µ-ECD
2. Install a 1/4-inch nut and graphitized-Vespel ferrule on the
adapter.
1/4-inch graphitized Vespel ferrule
1/4-inch nut
3. Prepare the column. See page 101 for instructions.
4. If you are using an indented liner (required for µ-ECD):
If the column id is 200 µm or more, push the column into the adapter until
it stops at the indentation. Pull it back 1 to 2 mm and tighten the column
nut firmly.
If the id is less than 200 µm, mark the column 70±1 mm from the end. Insert
column and nut into the adapter with the mark at the rear of the column
nut, and tighten the column nut firmly.
Mark
70 + 1 mm
115
Columns and Traps
Procedure: Installing capillary columns in the ECD and µ-ECD
Part 1. Capillary columns
5. If you are using a straight liner:
Insert the column in the ECD adapter so that 1 mm extends above the cap
extension. Tighten the capillary column nut firmly.
P
P
1 mm
Capillary column nut
Capillary column
6. Slowly install the adapter straight into the detector fitting. Make sure that
the adapter is seated all the way into the detector fitting—jiggle it if necessary. Be careful not to break the column end.
Detector fitting
116
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the ECD and µ-ECD
If the adapter is properly installed, the distance between the
1/4-inch nut and the bottom of the adapter will be 19 ± 1 mm. If it is
22–23 mm, reinstall the adapter into the detector fitting.
19 ± 1 mm
7. Slide the nut and ferrule up to the detector fitting and tighten the nut finger
tight. Use a 9/16-inch wrench to tighten the nut an additional 1/4 turn.
8. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperatures. Allow them to cool, and then retighten the fittings.
117
Columns and Traps
Procedure: Installing capillary columns in the FPD
Part 1. Capillary columns
Procedure: Installing capillary columns in the FPD
The FPD uses an adaptable fitting that can use both packed and capillary
columns. If your adaptable fitting does not have a capillary adapter installed,
begin with step 1. If the capillary adapter is already installed in your adaptable
fitting, begin with step 5.
The FPD uses a special adapter for capillary columns. The FPD Capillary
Adapter, part number 19256-80570, allows fused silica columns as large as
530 mm ID to be run right to the base of the FPD flame, minimizing sample tailing
or loss of chemically active sites.
19256-80590
FPD 1/8-inch adapter
19256-80570
FPD Capillary Adapter
Materials required
Column nut and ferrule
FPD Capillary column adapter
1/4-inch nut and ferrule
Column cutter
1/4-inch wrench
9/16-inch wrench
Metric ruler
Typewriter correction fluid
118
Part 1. Capillary columns
Columns and Traps
Procedure: Installing capillary columns in the FPD
1. Assemble a brass nut and graphite/Vespel ferrule onto the
adapter.
1/4-inch ferrule
1/4-inch nut
Capillary column adapter
2. Insert the adapter straight into the detector base as far as possible. Hold the
adapter in this position and tighten the nut finger tight. Use a wrench to
tighten the nut an additional 1/4 turn.
Detector fitting
Capillary column adapter
3. Install a column nut (part no. 18740-20870) and graphite ferrule (1.0 mm ID,
part no. 5080-8773 or 0.5 mm ID, part no. 5080-8853) on the column.
4. After installing the nut and ferrule, prepare a fresh column end by cutting
off a short piece of the column. See page 101 for instructions.
5. Position the ferrule about 153 mm from the end of the column.
Optimum height depends on sample type and gas flow rates. If it is too high,
the column end will be exposed to the flame. If too low, the sample may be
exposed to hot stainless steel, causing slight tailing.
119
Columns and Traps
Procedure: Installing capillary columns in the FPD
Part 1. Capillary columns
Mark the column at a point even with the bottom of the nut. Typewriter
correction fluid works well.
153 mm
Mark column here
6. Insert the column in the detector. Slide the nut and ferrule up the column to
the detector base. Finger tighten the column nut until it starts to grab the
column.
7. Adjust the column position so that the correction fluid mark on the column
is even with the bottom of the column nut. Proceed to step 8.
Correction fluid mark
8. Tighten the column nut finger tight, then withdraw the column about 1 mm.
Use a wrench to tighten the nut an additional 1/4 turn.
9. After the column is installed at both inlet and detector, establish a flow of
carrier gas through the inlet. Heat the oven, inlet, and detector to operating
temperatures. Allow them to cool and then retighten the fittings.
120
Part 1. Capillary columns
Columns and Traps
Ferrules for capillary columns
Ferrules for capillary columns
Table 12 lists some of the ferrules used with capillary columns and inlet and
detector liners/adapters. See the Agilent catalog for consumables and supplies
for a more complete listing.
Graphite and graphitized-Vespel ferrules
Place some ferrules in a petri dish in the GC oven at 250 to 300°C for 30 minutes
to remove compounds absorbed by the graphite. Leave a dish of assorted
ferrules in the oven to ensure a clean supply.
The ferrule should slide onto the column but not fall off from its own weight. If
it fits properly, 1/4 turn from finger tight will make a good seal. If it is loose, the
column nut must compress the ferrule around the column. This is not a problem
with soft graphite ferrules, but hard ferrules may require so much force that the
inlet fitting may, the nut, or the ferrule may be damaged. With hard ferrules, it
is best to start with an undersize hole and drill it to fit the column.
Vespel ferrules
These ferrules can be more leak-tight than graphite but have a lower temperature
limit. Retighten after a few oven temperature cycles.
Table 12 Hardware Used with Capillary Columns
Item*
Typical use
Part no.
1/4-inch graphitized Vespel ferrule, pkg of 10
Inlet/detector liner/adapters
5080-8774
1.0-mm graphite ferrule, pkg of 10
Capillary columns
5080-8773
0.5-mm graphite ferrule, pkg of 10
Capillary columns
5080-8853
Column nut
Connect column to inlet or detector
5181-8831
Column cutter
Cutting capillary columns
5181-8836
* Ferrule and O-ring ids
121
Columns and Traps
Overview: installing packed metal columns
Part 2.
Part 2. Packed metal columns
Packed metal columns
Overview: installing packed metal columns
There are two sizes of packed metal columns, 1/4-inch and 1/8-inch, in common
use. This general procedure applies to both sizes of columns, as well as PTFE
columns used with the FPD.
1. Prepare your packed column (page 124).
2. See Table 13 or Table 14 for fittings required.
3. Install the adapter, if needed (page 128).
4. Install the column (page 129).
5. Establish a flow of carrier gas through the inlet. Heat the oven, inlet, and
detector to operating temperatures. Allow them to cool, and then retighten
the fittings.
122
Part 2. Packed metal columns
Columns and Traps
Fittings
Fittings
Table 13
Fittings for 1/4-inch and 1/8-inch Packed Metal Columns
Inlet or
detector
1/4-inch packed metal column
1/8-inch packed metal column
Where to install
Comments
Where to install
Comments
Purged-packed
inlet
1/4-inch liner
See Inlets volume for instructions
on installing liner.
1/8-inch liner
See Inlets volume for
instructions on installing liner.
Adaptable
NPD*, FID or
FPD
1/4-inch adapter
(Part no. 1923180530)
Remove or install adapter, as
desired.
See page 128 for instructions on
installing an adapter.
1/8-inch adapter
(Part no. 1923180520)
See page 128 for instructions
on installing an adapter.
ECD
Detector fitting
Remove adapter, if necessary.
1/8-inch adapter.
(Part no. 1930180530)
See page 128 for instructions
on installing an adapter.
TCD
1/4-inch adapter
(Part no. G153220710)
See page 128 for instructions on
installing an adapter.
Detector fitting
Remove adapter, if necessary.
* Do not remove the plugs from your NPD until you are ready to connect the column and operate the detector. Failure to observe
this simple procedure may reduce the collector’s effectiveness or slow down the bead’s stabilization period the first time the
detector is used.
The FPD 1/8-inch OD Adapter, part number 19256-80590, allows installation of
PTFE columns concentrically around the FPD fused silica liner, eliminating
exposed hot stainless steel.
Table 14 Fittings for FPD with a PTFE Column
1/4-in PTFE column
1/8-in PTFE column
Where to install
Comments
Where to install
Comments
1/4-inch adapter
(Part no. 19231-80530)
Remove or install
adapter, as desired.
See page 128 for
instructions on
installing an adapter.
1/8-inch adapter
(Part no. 19256-80590)
See page 128 for
instructions on
installing an adapter.
123
Columns and Traps
Preparing packed metal columns
Part 2. Packed metal columns
Preparing packed metal columns
Before installing these columns, a ferrule should be locked on the column end
so that it is flush with the end of the column. This prevents problems caused by
dead volume in the fitting.
Recommended
Minimum exposed column
Not Recommended
Too much column extends past the ferrule;
may cause problems due to dead volume.
Use the following instructions to install new SWAGELOK nuts and ferrules onto
1/8-inch or 1/4-inch metal columns. If your column already has ferrules installed,
proceed to the instructions on installing adapters (page 128) or installing packed
metal columns (page 129).
124
Part 2. Packed metal columns
Columns and Traps
Procedure: Making a spacer from Teflon tubing
Procedure: Making a spacer from Teflon tubing
Materials required
1/4-inch or 1/8-inch Teflon tubing
1/4-inch or 1/8-inch nut and ferrule set
Bench vise
Male SWAGELOK fitting
9/16-inch or 7/16-inch wrench
Razor or sharp knife
1. Secure a new male SWAGELOK fitting in a bench vise.
Male SWAGELOK fitting
2. Slide a SWAGELOK nut, back ferrule, and front ferrule onto a piece of Teflon
tubing. If the end of the tubing is not cut straight, use a razor or sharp knife
to make a flat, smooth end.
Front ferrule
Back ferrule
SWAGELOK nut
Teflon tubing
125
Columns and Traps
Procedure: Making a spacer from Teflon tubing
Part 2. Packed metal columns
3. Insert the Teflon tubing, ferrules, and nut into the vise-held SWAGELOK
fitting. Tighten the nut 3/4 turn past finger tight to set the ferrules on the
tubing.
Tubing, nut, and ferrule assembly
Male SWAGELOK fitting (vise not shown)
4. Loosen the nut and remove the assembly from the male SWAGELOK fitting.
5. Cut off the end of the tubing extending beyond the ferrule with a razor or
sharp knife. This piece of tubing is the spacer.
=
+
6. Insert the spacer into the vise-held SWAGELOK fitting.
The male SWAGELOK fitting and spacer should be kept on hand to be used
whenever new ferrules are being installed on a column.
126
Part 2. Packed metal columns
Columns and Traps
Procedure: Installing ferrules on a metal column
Procedure: Installing ferrules on a metal column
Materials required
Male SWAGELOK fitting with Teflon tubing spacer
SWAGELOK nut and ferrule set
Wrenches
1. Install new SWAGELOK nut and ferrules on the column.
Front ferrule
Back ferrule
SWAGELOK nut
Column
2. Install the Teflon tubing spacer in the male fitting. Fully insert the column
with its nut and ferrules into the vise-held fitting. Tighten the nut finger tight.
Use a wrench to tighten the nut an additional 1-1/4 turn for 1/4-inch columns
or 3/4 turn for 1/8-inch columns.
3. Unscrew the column nut from the vise-held fitting and remove the column.
Ferrules should now be set in place on the column with the column correctly
positioned.
127
Columns and Traps
Procedure: Installing an adapter in a detector fitting
Part 2. Packed metal columns
Procedure: Installing an adapter in a detector fitting
This is a general procedure for installing many types of adapters onto detector
fittings. See Table 13 for adapter part numbers.
Materials required
7/16-inch or 9/16-inch wrench
Graphitized Vespel ferrule
Nut
Adapter
1. Assemble a brass nut and a graphitized Vespel ferrule onto the adapter.
Graphitized Vespel ferrule
Nut
Adapter
2. Insert the adapter straight into the detector base as far as possible. Hold the
adapter in this position and tighten the nut finger tight.
Detector fitting
Adapter
1/4-inch column, tighten an additional 3/4 turn with a 9/16-inch wrench.
1/8-inch column, tighten an additional 1/4 turn with a 7/16-inch wrench.
3. Proceed to “Installing Packed Metal Columns” on page 129.
128
Part 2. Packed metal columns
Columns and Traps
Procedure: Installing packed metal columns
Procedure: Installing packed metal columns
Before following this procedure, make sure an adapter or liner is installed
(page 128), if needed, and that your column is prepared (page 124.)
Materials required
Prepared metal column
Column adapter, if needed
Wrench
1. Insert the column into the adapter, detector, or inlet liner until it bottoms.
Tighten the nut finger tight.
Adapter
Prepared column
2. If you are installing a column directly into the detector fitting:
1/4-inch column, tighten an additional 3/4 turn with a 9/16-inch wrench.
1/8-inch column, tighten an additional 1/4 turn with a 7/16-inch wrench.
3. If you are installing a column onto an adapter:
Tighten the column nut using two wrenches in opposition, one on the column
nut and the other on the liner or adapter body. This prevents the liner or
adapter from rotating while you tighten the column nut.
1/4-inch column, tighten an additional 3/4 turn with a 9/16-inch wrench.
1/8-inch column, tighten an additional 1/4 turn with a 7/16-inch wrench.
4. Establish a flow of carrier gas through the inlet. Heat the oven, inlet, and
detector to operating temperatures. Allow them to cool, and then retighten
the fittings.
129
Columns and Traps
Ferrules for packed metal columns
Part 2. Packed metal columns
Ferrules for packed metal columns
Table 15 lists some of the nuts and ferrules used with packed metal columns.
Consult the Agilent catalog for consumables and supplies for a more complete
listing.
Ferrules that are prepared improperly cause leaks and contamination. Here are
some hints to avoid problems.
Graphite and graphitized-Vespel ferrules. Place these ferrules in a petri dish
and bake in the GC oven at 250 to 300°C for 30 minutes before use to remove
organic compounds absorbed by the graphite. Leave a petri dish of assorted
ferrules in the GC oven to ensure a clean supply.
Vespel ferrules. These ferrules can be more leaktight than graphite, but have
a lower temperature limit. They should be retightened after a few oven
temperature cycles to ensure a good seal. Be sure to use the correct ferrule for
the size column you are using.
Table 15 Nuts and Ferrules Used with Packed Metal Columns
Item*
Typical use
Part no.
1/4-inch swage stainless steel, pkg of 20
(nut, front ferrule, back ferrule)
1/4-inch
5080-8753
1/8-inch swage stainless steel, pkg of 20
(nut, front ferrule, back ferrule)
1/8-inch
5080-8751
1/4-inch swage brass, pkg of 20 each
(nut, front ferrule, back ferrule)
1/4-inch
5080-8752
1/8-inch swage brass, pkg of 20 each
(nut, front ferrule, back ferrule)
1/8-inch
5080-8750
1/4-inch graphitized Vespel ferrule,
pkg of 10
inlet/detector liner/adapters
1/4-inch columns
5080-8774
1/8-inch graphitized Vespel ferrule,
pkg of 10
1/8-inch columns
0100-1107
* O-ring and ferrule ids
130
Part 3. Packed glass columns
Part 3.
Columns and Traps
Overview: Installing glass packed columns
Packed glass columns
Glass packed columns must be installed simultaneously at the inlet and the
detector and must be installed parallel to the oven door:
Front to front
Back to back
You can install glass packed columns directly in the purged-packed inlet, ECD,
and adaptable NPD, FID, and FPD fittings. The TCD requires an adapter.
There are three types of glass packed columns available. You must make certain
that your column is compatible with the inlet fitting and detector used. Table 16
summarizes the inlet and detector fittings required and the appropriate column
configuration.
Overview: Installing glass packed columns
1. See Table 16 for information on fittings and column configuration required.
2. Remove or install an adapter, if necessary (see page 128).
3. Follow the general procedure for installing glass columns on page 133.
131
Columns and Traps
Overview: Installing glass packed columns
Part 3. Packed glass columns
Table 16 Installing Glass Packed Columns
Inlet or
detector
Where to
install
Column
configuration
Purged-packed
inlet
Inlet fitting (no
liner installed)
or 1/4-inch liner*
A or B, depending on
the detector
C (works with all
detectors)
Allow at least 50 mm of empty column
to prevent an inserted syringe needle
from contacting either the glass wool
plug or column packing.
Adaptable
NPD, FID, or FPD
Cannot use with
capillary optimized
detector
Detector fitting
A
Remove adapter, if installed.
There must be at least 40 mm of empty
column to prevent the bottom end of the
jet from touching either column packing
or the glass wool plug.
ECD
Detector fitting
A
Remove capillary column adapter, if
installed.
TCD
1/4-inch adapter
(Part no.
G1532-20710)
B
Instructions for installing adapters are
on page 128.
* See the Inlets volume for instructions on installing liners
132
Comments
Part 3. Packed glass columns
Columns and Traps
Procedure: Installing glass packed columns
Procedure: Installing glass packed columns
Materials required
Recommended:
Two 1/4-inch graphitized Vespel ferrules
Two 1/4-inch nuts
9/16-inch wrench
Alternative:
Four O-rings
Two back ferrules
Two 1/4-inch nuts
9/16-inch wrench
1. Assemble a brass nut and graphitized Vespel ferrule on each end of the
column. Alternative method: Install a 1/4-inch nut, back ferrule, and two
O-rings on each end of the column. An extra O-ring below the nut keeps the
nut from dropping into the coiled portion of the column.
Alternative installation method
Recommended
O-rings
Graphitized vespel ferrule
1/4-inch nut
Back ferrule (note orientation)
1/4-inch nut
1/4-inch od glass column
133
Columns and Traps
Procedure: Installing glass packed columns
Part 3. Packed glass columns
2. Insert the column into the inlet until it bottoms. Insert the column into the
detector fitting but do not force it. It may be necessary to start the long end of the
column in the inlet at an angle to clear the oven floor.
3. Withdraw the column 1 to 2 mm from both the inlet and detector. Tighten
both column nuts finger tight.
4. Tighten both column nuts 1/4 turn with a wrench. If you use graphitized
Vespel ferrules, proceed to step 5. If you use O-rings, proceed to step 6.
Caution
Overtightening the column nut or forcing it to bottom in both the inlet and detector may shatter the column.
5. Set flow through the column and raise the inlet, detector, and oven to operating temperature. Then set the oven to ambient and allow it to cool.
6. Use the wrench to tighten the nut an additional 1/2 turn. Tighten further, as
necessary, to prevent leakage.
134
Part 3. Packed glass columns
Columns and Traps
Ferrules and O-rings for glass packed columns
Ferrules and O-rings for glass packed columns
Table 17 lists ferrules and O-rings used with glass packed columns. Consult the
Agilent Catalog for consumables and supplies for a more complete listing.
Ferrules that are prepared improperly cause leaks and contamination. To avoid
problems, place graphitized Vespel ferrules in a petri dish and bake in the GC
oven at 250 to 300°C for 30 minutes before use to remove organic compounds
absorbed by the graphite. Leave a petri dish of assorted ferrules in the GC oven
to ensure a clean supply.
Table 17 Glass Packed Columns Consumables
Item*
Typical use
Part no.
1/4-inch graphitized Vespel ferrule,
pkg of 10
Inlet/detector liners,
1/4-inch glass packed
columns
5080-8774
Silicone O-ring, 6.0-mm
1/4-inch glass packed
columns
0905-0322
* O-ring and ferrules ids
135
Columns and Traps
Part 4.
Part 4. Conditioning columns
Conditioning columns
Conditioning involves establishing a flow of carrier gas through a column and
then heating it for one-half hour for capillary columns and overnight for packed
columns. This drives off contaminants and makes the column fit for analytical
use.
New packed columns should be conditioned, since they often contain volatile
contaminants from the coating process. It may also be necessary to condition a
used column that has been stored for some time without end caps or plugs.
Conditioning is not as important with capillary columns since they contain a
minimal amount of stationary phase.
The following procedures include preliminary steps and the actual conditioning
procedure, which differs for packed and capillary columns.
136
Part 4. Conditioning columns
Columns and Traps
Procedure: Preliminary column conditioning steps
Procedure: Preliminary column conditioning steps
Materials required
Two 7/16-inch wrenches
No-hole ferrule and capillary nut for detector connection
1. Turn off the detectors. Shut off the detector support gases. It is especially
important to shut off hydrogen!
2. If the column to be conditioned is not already installed, connect one end to
an available inlet. If you are not sure how to install a column, see the instructions earlier in this chapter. DO NOT connect the remaining end to a detector!
3. If you plan to condition a capillary column in a split/splitless inlet, install the
proper liner and attach the column in the normal manner, making sure about
5 to 7 mm of column extends above (in front of) the column ferrule.
4. Cap the detector(s) fittings with the no-hole ferrule and column nut.
Plugged detector connection
Capillary column detached
from detector
137
Columns and Traps
Procedure: Conditioning a capillary column
Part 4. Conditioning columns
Procedure: Conditioning a capillary column
WARNING
Do not use hydrogen as the carrier for conditioning! It could vent into the oven
and present an explosion hazard.
1. Select an appropriate column pressure—given as psi (kPa)—from this table.
Inside diameter
Length, m
0.10 mm
0.20 mm
0.25 mm
0.32 mm
0.53 mm
10
25 (170)
6 (40)
3.7 (26)
2.3 (16)
0.9 (6.4)
15
39 (270)
9 (61)
5.6 (39)
3.4 (24)
1.4 (9.7)
25
68 (470)
15 (104)
9.5 (65)
5.7 (40)
2.3 (16)
30
83 (570)
18 (126)
12 (80)
7 (48)
2.8 (19)
50
32 (220)
20 (135)
12 (81)
4.7 (32)
60
39 (267)
24 (164)
14 (98)
5.6 (39)
2. Enter the selected pressure. Let gas flow through the column at room
temperature for 15 to 30 minutes to remove air.
3. Program the oven temperature from room temperature to the maximum
temperature for the column. Increase the temperature at a rate of
10 to 15°C/min and hold at the maximum temperature for 30 minutes.
4. If you will not be using the conditioned column immediately, remove it from
the oven. Cap both ends to prevent air, moisture, and other contaminants
from entering the column.
138
Part 4. Conditioning columns
Columns and Traps
Procedure: Conditioning packed columns
Procedure: Conditioning packed columns
WARNING
Do not use hydrogen as the carrier for conditioning! It could vent into the oven
and present an explosion hazard.
1. Press [Col 1] or [Col 2] to open the column control table.
2. Enter an appropriate column flow:
•
20 to 30 mL/min for 2 mm ID glass or 1/8 inch OD metal columns.
• 50 to 60 mL/min for 4 mm ID glass or 1/4 inch OD metal columns.
3. The conditioning temperature is never greater than the maximum temperature limit for the column; 30°C less than the maximum is usually sufficient.
Slowly raise oven temperature to the conditioning temperature for the
column.
4. Continue conditioning overnight at the final temperature. If you will not be
using the conditioned column immediately, remove it from the oven. After
removing the column, cap both ends to prevent air, moisture, or other
contaminants from entering the column.
139
Columns and Traps
Part 5.
Part 5. Conditioning chemical traps
Conditioning chemical traps
If your traps are preconditioned, you will not need to perform a conditioning
procedure before using them. However, all traps need regeneration periodically,
for example after using one to four cylinders of gas, or if gases of the highest
purity were not used. You can recondition Agilent moisture and activated
charcoal traps. Agilent oxygen traps cannot be reconditioned; you must replace
them if they become contaminated. Follow the manufacturer’s instructions for
reconditioning traps.
The molecular sieve and activated charcoal traps can also be repacked.
Instructions for repacking traps are shipped with each trap.
Table 18 Ordering Information for Agilent Traps
140
Item
Part no.
Moisture trap (packed with Molecular Sieve 5A, 45/60 mesh)
5060-9077
Conditioned moisture trap (packed with preconditioned
Molecular Sieve 5A, 45/60 mesh)
5060-9084
Activated charcoal trap
5060-9096
Molecular Sieve 5A (100 grams, 45/60 mesh)
5080-6759
Activated charcoal (100 grams, 30/60 mesh)
5080-6751
Cap for ends of traps, 1/8-inch, 6 per package
5180-4124
Reducer trap fittings
5062-3502
Part 6. Calibrating your capillary column (optional)
Part 6.
Columns and Traps
Calibration modes
Calibrating your capillary column (optional)
Preparation
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 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:
•
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 µm.
Calibration modes
There are three ways to calibrate the column length and/or diameter:
Caution
•
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
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. See
"Interpreting bubble meter flow measurements" on page 79 for details.
141
Columns and Traps
Column calibration procedures
Part 6. Calibrating your capillary column (optional)
Column calibration procedures
These procedures are described below using Column 1 as an example.
Procedure: 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. For more
information, see "Setting up an isothermal run" on page 87 or "Configure the
column" on page 48.
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 Column 1 or Column 2 and press [Enter].
Select the column to calibrate
5. The GC displays the current calibration mode for the column. In this example, the column is uncalibrated.
142
Part 6. Calibrating your capillary column (optional)
Columns and Traps
Column calibration procedures
6. To recalibrate or to change calibration mode, press [Mode/Type] to see the
column calibration mode menu.
Available calibration modes
The * indicates the current mode
7. Scroll to Length or Diameter and press [Enter]. The following menu
appears:
Dimension to be calibrated
Actual column flow rate, mL/min (input)
Elution time, min (input)
Calc length/Calc diameter:
current estimated column length or
ID based in input
8. Scroll to Unretain pk and enter the actual elution time from the run
performed above.
9. 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.
143
Columns and Traps
Column calibration procedures
Part 6. Calibrating your capillary column (optional)
Procedure: 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. For more
information, see "Setting up an isothermal run" on page 87 or "Configure the
column" on page 48.
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. See chapter 5 for details.
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. See
"Interpreting bubble meter flow measurements" on page 79 for details.
4. Measure the actual flow rate through the column using a bubble meter.
Record the value. Reinstall the column.
5. Press [Options]. Scroll to Calibration and press [Enter].
6. From the calibration list, select Column 1 or Column 2 and press [Enter].
Select the column to calibrate
7. The GC displays the current calibration mode for the column. In this example, the column is uncalibrated.
144
Part 6. Calibrating your capillary column (optional)
Columns and Traps
Column calibration procedures
8. To recalibrate or change calibration mode, press [Mode/Type] to see the
column calibration mode menu.
Available calibration modes
The * indicates the current mode
9. Scroll to Length or Diameter and press [Enter]. The following menu
appears:
Actual column flow rate, mL/min (input)
Elution time, min (input)
Calc length: current estimated column
length based on input
Calc diameter: current estimated column
ID based in input
10. Scroll to Measured flow and enter the corrected column flow rate (in
mL⁄min) from the run performed above.
11. 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.
145
Columns and Traps
Column calibration procedures
Part 6. Calibrating your capillary column (optional)
Procedure: Estimate the actual column length and diameter
1. Set oven ramp 1 to 0.00, then verify that the column is defined. For more
information, see "Setting up an isothermal run" on page 87 or "Configure the
column" on page 48.
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. See chapter 5 for details.
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. See
"Interpreting bubble meter flow measurements" on page 79 for details.
5. Measure the actual flow rate through the column using a bubble meter.
Record the value. Reinstall the column.
6. Press [Options]. Scroll to Calibration and press [Enter].
7. From the calibration list, select Column 1 or Column 2 and press [Enter].
Select the column to calibrate
146
Part 6. Calibrating your capillary column (optional)
Columns and Traps
Column calibration procedures
8. The GC displays the current calibration mode for the column. In this example, the column is uncalibrated.
9. To recalibrate or change calibration mode, press [Mode/Type] to see the
column calibration mode menu.
Available calibration modes
The * indicates the current mode
10. Scroll to Length or Diameter and press [Enter]. The following menu
appears:
Actual column flow rate, mL/min (input)
Elution time, min (input)
Calc length: current estimated column
length based on input
Calc diameter: current estimated column
ID based in input
11. Scroll to Measured flow and enter the corrected column flow rate (in
mL⁄min) from the run performed above.
12. Scroll to Unretain pk and enter the actual elution time from the run
performed above.
13. 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.
147
Columns and Traps
Column calibration procedures
148
Part 6. Calibrating your capillary column (optional)
6
Signal Handling
Specifying and controlling output
signals, analog signals, digital signals,
Chem Station and INET considerations
Signal Handling
Signal is the GC output to a data handling device, analog or digital. It can be a
detector output or the output from temperature, flow, or pressure sensors. Two
signal output channels are provided.
Signal output can be either analog or digital, depending on your data handling
device. Analog output is available at either of two speeds, suitable to peaks with
minimum widths of 0.004 minutes (fast data rate) or 0.01 minutes (normal rate).
Analog output ranges are 0 to 1 V, 0 to 10 V, and 0 to 1 mV.
Digital output to the ChemStation is available at 11 speeds ranging from 0.1 Hz
to 200 Hz, capable of handling peaks from 0.001 to 2 minutes wide. Set this rate
from your ChemStation.
Data for INET integrators is at 20 Hz, capable of handling peaks of at least
0.01 minute width.
Using the signal control tables
Signal type
When assigning detector signals, use the [Mode/Type] key and choose from the
Signal Type control table, or press a key or combination of keys. [Front], [Back],
[–], [Col Comp 1], and [Col Comp 2] will work — alone or in combination. For
example, press [Back] for back detector or [Back] [–][Front] for back detector
minus front detector.
The nondetector signals are test plot, thermal, pneumatic, and diagnostic.
Access them by pressing [Mode/Type]. Diagnostic signals are for use by your
service representative and are not described in detail here.
Signal type can be programmed as a run time event. See chapter 7 for details.
Value
Value on the signal control table is the same as Output on the detector control
table if your signal type is Front or Back. If you are subtracting one signal
from another (as in Front - Back), the signal Value will be the difference.
You cannot enter a setpoint for Value.
150
Signal Handling
Using the signal control tables
A conversion factor may be involved when interpreting Value—for example,
one FID unit is one picoamp; one ECD unit is 5 Hz (1 Hz for the µ-ECD). The
units for detector and other signals are listed below.
Table 19 Signal Conversions
Signal type
1 display unit is equivalent to:
Detector:
FID, NPD
1.0 pA (1.0 × 10-12 A)
FPD
150pA (150 ×10-12 A)
TCD
25 mV (2.5 × 10-5 V)
ECD
5 Hz
µ-ECD
1 Hz
Analog input board
(use to connect GC to non-Agilent detector)
15 µV
Nondetector:
Thermal
1°C
Pneumatic:
Flow
Pressure
Diagnostic
1 mL/min
1 pressure display unit (psi, bar, or kPa)
Mixed, some unscaled
151
Signal Handling
Using the signal control tables
Press [Signal 1] or [Signal 2]
Many choices, see change signal type below
Actual output value
For analog output signals only
To change signal type, press [Mode/Type]:
Detector signals.
Scroll to the approriate signal
type and press [Enter].
Test Pilot
Nondetector signals. Scroll to one of these
lines and press [Enter] to get the expanded
list of signals- see next page.
Figure 22 Signal control table
152
Signal Handling
Using the signal control tables
Thermal signals:
Diagnostic signals:
Pneumatic signals:
Only installed items are listed in submenus.
Column flows and pressures are only listed when
you have electronic pneumatics control (EPC).
153
Signal Handling
Analog output settings—zero, range, and attenuation
Analog output settings—zero, range, and attenuation
If you use an analog recorder, you may need to adjust the signal to make it more
usable. Zero, Range, and Attn in the Signal control table do this.
Press [Signal 1] or [Signal 2].
Subtrracts value entered from baseline
(press [On] to set to current Value
or [Off] to cancel)
Scales data coming from the detector
(Valid setpoints are 0 to 13, depending
on detector type)
Scales presentation of output to
strip chart recorders
(Valid setpoints are 0 to 10)
Analog zero
This is used to correct baseline elevation or offsets. A common application is to
correct a baseline shift that occurs as the result of a valve operation. After
zeroing, the analog output signal is equal to the Value line of the control table
minus the Zero setpoint.
Zero can be programmed as a run time event. For details, see chapter 7.
Procedure: Zeroing signal output
1. Verify that the detector is on and in a ready state.
2. Press [Signal 1] or [Signal 2] to access the signal control table.
Press [On] to set the
current signal (15 in
this case) or enter a number.
3. Scroll to Zero.
154
Signal Handling
Analog output settings—zero, range, and attenuation
4. Press [On] to set Zero at the current signal value,
or
Enter a number between -500000 and +500000. A value smaller than the
current Zero shifts baseline up.
Range—for analog outputs only
Range is also referred to as gain, scaling, or sizing. It sizes the data coming
from the detector to the analog signal circuits to avoid overloading the circuits
(clamping). Range scales all analog signals (1 mV, 1 V, etc.)
If a chromatogram looks like A or B in Figure 23, the data needs to be scaled (as
in C) so that all peaks are visible on the paper.
Valid setpoints are from 0 to 13 and represent 20 (1) to 213 (8192). Changing a
setpoint by 1 changes the width of the chromatogram by a factor of 2. The
chromatograms in Figure 23 illustrate this. Use the smallest possible value to
minimize integration error.
See Table 20 for output scaling with different analog output devices.
Table 20 Output Scaling
Analog
One display unit =
Digital
One display count =
0 to 1 mV
1mV/2Range*2Attn
ChemStation
1 height count
0 to 1 V
1 mV/2Range
INET
(3396B and
3396C)
10,000 height counts
2SIGRANGE
(set from 3396)
0 to 10 V
1 mV/2Range
INET area counts (on INET SIGRANGE 0) are
approximately 10,000 * ChemStation area counts
155
Signal Handling
Analog output settings—zero, range, and attenuation
g6-5
A: Range = 0
B: Range = 3
C: Range = 1
Figure 23 Range settings
There are limits to usable range settings for some detectors. The table below
lists the valid range setpoints by detector.
Detector
Usable range
settings (2x)
FID
0 to 13
NPD
0 to 13
FPD
0 to 13
TCD
0 to 6
ECD
0 to 6
Analog input
0 to 7
Range may be run time programmed. See chapter 7 for details.
Attenuation—for analog outputs only
Attenuation(Attn) scales the presentation of output on 0- to 1-mV strip chart
recorders. Valid setpoints are from 0 to 10 and represent 20 to 210. As with range,
each higher setpoint value reduces the size of the chromatogram by one half,
while each higher setpoint doubles the size.
Attenuation is in addition to range. Thus, the total scaling factor is:
2Range × 2Attenuation
156
Signal Handling
Digital data handling
Attenuation may be run time programmed. See chapter 7 for details.
Data rates
Your integrator or recorder must be fast enough to process data coming from
the GC. If it cannot keep up with the GC, the data may be damaged. This usually
shows up as broadened peaks and loss of resolution.
Speed is measured in terms of bandwidth. Your recorder or integrator should
have a bandwidth twice that of the signal you are measuring.
The GC allows you to operate at two speeds. The faster speed—to be used only
with the FID, FPD, and NPD—allows minimum peak widths of 0.004 minutes
(8 Hz bandwidth), while the standard speed—which can be used with all
detectors— allows minimum peak widths of 0.01 minutes (1.6 Hz bandwidth).
If you use the fast peaks feature, your integrator should operate at around 15 Hz.
Procedure: Selecting fast peaks
1. Press [Config][Signal 1] or [Config][Signal2].
2. Press [ON] (FID only).
Digital data handling
Digital zero
Digital signal outputs respond to the Zero command by subtracting the signal
level at the time of the command from all future values.
Baseline level shifts
Some run time operations, such as changing signal assignment or switching a
valve, can produce large changes in the signal baseline position. This can
complicate signal processing by external devices. The GC provides two run table
commands minimize such problems—see chapter 7 for information on using the
run table.
157
Signal Handling
Digital data handling
Store signal value
command.
Saves the value of the signal at the time of the
Sig zero - value Creates a new zero by subtracting the stored value from
the current value of the signal and applies this zero to all future values.
When these commands surround a baseline-shifting command, the effect is to
bring the new baseline to the previous level, as shown in Figure 24.
The Store event must occur before the event that shifts the baseline, and the
zero - value event must occur after the baseline has stabilized at the shifted
level.
No correction
Signal
Baseline level change
Baseline-shifting event occurs
Time
3. Sig zero – val event occurs
Run time correction
Signal
2. Baseline-shifting event occurs
1. Store signal value event occurs
Time
Figure 24 Correcting baseline level shifts in digital signals
158
Signal Handling
Digital data handling
ChemStation
The GC can process data at 11 different data rates, each corresponding to a
minimum peak width. The table shows the effect of data rate selection.
Table 21 ChemStation Signal Processing
Data
rate
Minimum peak width
(Hz)
(minutes)
Relative noise
200
0.001
3.1
100
0.002
2.2
50
0.004
1.6
20
0.01
1
10
0.02
0.7
5
0.04
0.5
2
0.1
0.3
1
0.2
0.22
0.5
0.4
0.16
0.2
1.0
0.10
0.1
2.0
0.07
Detector
Column type
Narrow-bore (50 µm)
FID/FPD/NPD
only
capillary
to
All types
Slow packed
You cannot change the data rate during a run.
You will see higher relative noise at the faster sampling rates. Doubling the data
rate can double peak height while the relative noise increases by 40%. Although
noise increases, the signal-to-noise ratio is better at the faster rates.
This benefit only occurs if the original rate was too low, leading to peak
broadening and reduced resolution. We suggest that rates be chosen so that the
product of data rate and peak width in seconds is about 10 to 20.
Figure 25 shows the relationship between relative noise and data rates. Noise
decreases as the data rate decreases until you get to data rates of around 5 Hz.
159
Signal Handling
Column compensation
Relative noise magnitude
As the sampling rate slows, other factors such as thermal noise increase noise
levels.
Excess noise (due to flow,
oven temperature, detector
block temperatures,etc.)
Faster data rates
Slower data rates
Figure 25 Relationship of noise to data rates
INET
This applies only to 3395A/B or 3396B/C integrators with an INET board
installed.
INET transmits data digitally at a rate of 20 Hz and can handle peaks of at least
0.01 minute width. INET can select which of the two GC signals to use—you
define what those signals are with the control table.
Column compensation
Peaks are integrated more accurately and repeatably on a flat baseline than on
a rising baseline. Column compensation corrects for baseline rise during
temperature programming. This is done by making a blank run—one with no
160
Signal Handling
Column compensation
sample injected. This run is stored and subtracted from the real run to produce
a flat baseline. Figure 26 illustrates the concept.
All conditions must be identical in the column compensation run and the real
run. The same detector and column must be used, operating under the same
temperature and gas flow conditions. Two baseline profiles may be stored (as
[Col Comp 1] and [Col Comp 2]).
Chromatogram
with a rising
baseline
Chromatogram
with column
compensation
Blank column
compensation run
Figure 26 Column compensation
161
Signal Handling
Column compensation
Procedure: Creating a column compensation profile
1. Set up the instrument for a run.
2. Make a blank run to verify that the baseline is clean. This is particularly
important for new conditions or if the GC has been idle for several hours.
3. Press [Col Comp 1] or [Col Comp 2] to open the control table.
4. Press [Front] or [Back] depending on the detector you are using.
Message indicates status.
After a successful run, it
says Data ok.
Press [Front] or [Back] key
to change the detector.
Press [Enter] to start run.
Press [Enter] to create two
profiles-Col Comp 1 and
Col Comp 2
5. Select Start comp run or Start comp 1&2 run. Press [Enter].
a. Start comp run creates one profile.
b. Start comp 1&2 run creates two profiles (using different detectors
and columns but the same oven temperature program).
6. If the run is successful, the first line of the control table will say
Data ok, and a time and date will appear at the bottom.
Procedure: Making a run using column compensation
1. Set the up chromatographic conditions. They must be identical to those in
the stored column compensation run except that Final time in the last
ramp of the oven program can be longer or shorter.
2. Press [Signal 1] or [Signal 2] to access the signal control table.
162
Signal Handling
Column compensation
3. Scroll to Type: and press [Mode/Type].
Press [Signal 1] or [Signal 2]
Press [Mode/Type]
4. Choose Front - col comp 1 or one of the other three column compensation options on the list.
5. Enter setpoints for Zero, Range, and Attn, if applicable.
6. Start your run.
163
Signal Handling
Test plot
Procedure: Plotting a stored column compensation profile
1. Press [Signal 1] or [Signal 2] to open the signal control table.
2. Scroll to Type: and press [Mode/Type].
3. Choose Col comp 1 or Col comp 2.
4. Press [Start].
Press [Mode/Type].
Test plot
Test plot is an internally generated “chromatogram” that can be assigned to
a signal output channel. It consists of three baseline-resolved, repeating peaks.
164
Signal Handling
Test plot
The area of the largest is approximately 1 Volt-sec, the middle one is 0.1 times
the largest, and the smallest is 0.01 times the largest.
Test plot can be used to verify the operation of external data processing
devices without having to perform repeated chromatographic runs. It may also
be used as a stable signal to compare the results from different data processing
devices.
165
Signal Handling
Test plot
166
7
Instrument Automation
Creating and using timed events.
Executing events during a run. Using
the clock table.
Instrument Automation
Executing events during the run
Instrument automation allows you to program events using run time programming via
the run table or clock time programming via the clock table. Up to 25 timed events can
be executed in each of these tables.
Run time programming
Run time programming allows certain setpoints to change automatically during a run
as a function of the chromatographic run time. Thus an event that is programmed to
occur at 2 minutes will occur 2 minutes after every injection.
Its uses include:
•
Controlling column switching or other valves
•
Changing signal definition, zero, range, or attenuation
•
Controlling an auxiliary pressure channel
•
Changing polarity of a thermal conductivity detector (TCD)
•
Turning the hydrogen flow to a nitrogen-phosphorus detector (NPD) on or
off
•
Pausing (freezing) and resuming a signal value
The changes are entered into a run table that specifies the setpoint to be changed, the
time for the change, and the new value. At the end of the chromatographic run, most
setpoints changed by a run time table are returned to their original values.
Valves can be run time programmed but are not restored to their starting position at
the end of the run. You must program the reset operation in the run table if this action
is desired. See chapter 9 for more information.
168
Instrument Automation
Using run time events
Using run time events
The [Run Table] key is used to program timed events.
You can control the following events during a run.
•
Valves (1-8)
•
Multiposition valve
•
Signal type (see page 150)
•
Analog signal zero, attenuation, and range
•
Digital signal zero and baseline level shifts (see page 157)
•
Auxiliary pressures (3, 4, 5)
•
TCD negative polarity (on/off)
•
NPD H2 flow (on/off)
•
Pausing (freezing) and resuming a signal value
169
Instrument Automation
Using run time events
Procedure: Programming run time events
1. Press [Run Table] to open the run time control table. The
following message will be displayed if no programmed
entries presently exist.
2. Press [Mode/Type] to see the run time event types.
Note: Only those types that are
possible with your configuration
will appear.
3. Scroll to the event type to be programmed.
Run time for event to occur
Event type for entry #1
Setpoint parameter:
varies with event type
4. Enter values for the Time: and Setpoint: parameters.
170
Instrument Automation
The run table
The run table
The programmed events are arranged in order of execution time in the
Run Table. The following is a brief example:
Event 1 rotates a valve, which
might be a column switching
valve.
Event 2 adjusts the signal attenuation. It will be reset to its original
value at the end of the run.
Event 3 resets Valve #2 to its
original position in preparation
for another run. Valves do not
reset automatically
Figure 27 A run table example
Procedure: Adding events to the run table
1. To add new events to the run table, press [Mode/Type] while
on the Time: or Type: line of any entry.
2. Select the event type.
3. Set appropriate Time: and Setpoint: parameters.
Repeat until all entries are added. Events are automatically placed in
order by execution time.
171
Instrument Automation
The run table
Procedure: Editing events in the run table
1. Press [Run Table].
2. Move the cursor to the event you want to change.
3. To edit the time for an event, move the cursor to the line
labeled Time. Type the desired time and press [Enter].
4. To edit a setpoint value, scroll to the setpoint item and press
the [On] or [Off] key or enter a numeric value for the setpoint.
Press [Enter].
Procedure: Deleting run time events
1. Press [Run Table] to access the run time table.
2. From within this table press the [Delete] key to delete events
from the run time table. Pressing [Delete] while in an existing
time event table produces the following display.
3. Press [Enter] to delete the current timed event; press
[Clear] to cancel this operation.
172
Instrument Automation
Clock time programming
Clock time programming
Clock time programming allows certain setpoints to change
automatically at a specified time during a 24-hour day. Thus, an event
programmed to occur at 14:35 hours will occur at 2:35 in the afternoon.
A running analysis or sequence has precedence over any clock table
events occurring during this time. Such events are not executed.
Possible clock time events include:
•
Valve control
•
Method and sequence loading
•
Starting sequences
•
Initiating blank and prep runs
•
Column compensation changes
•
Adjustments of the detector offset
173
Instrument Automation
Using clock time events
Using clock time events
The Clock Table function allows you to program events to occur
during a day based on the 24-hour clock. Clock table events that would
occur during a run or sequence are ignored.
For example, the clock table could be used to start an analysis before
you even get to work in the morning.
Procedure: Programming clock time events
1. Press [Clock Table] to access the clock time control table.
The following message will be displayed if no events are
programmed.
2. Press [Mode/Type] to view the clock time program types.
These only show if the instrument
is equipped with valves.
174
Instrument Automation
Using clock time events
3. Scroll to select the parameter to be programmed.
For example, if the option “Load Method” is chosen for clock
time event #1, the display would look similar to the one
below.
4. Edit Time: and Method#: setpoints for this event.
Clock time for event to occur
Event type for entry #1
Setpoint parameter, varies
with event type
This allows you to program a specific time at which your GC
will load a predetermined method.
5. When the clock event is executed, the following screen
appears:
The instrument beeps when an
event is executed.
175
Instrument Automation
Using clock time events
Event 1 of 9
Event 2 of 9
Event 3 of 9
Event 4 of 9
Event 5 of 9
Event 6 of 9
Event 7 of 9
Event 8 of 9
Event 9 of 9
The clock table will resume at 01:25 the next
morning with the multiposition valve event.
Figure 28 A clock table example
Note: This is not a “realistic” clock table. It is intended to show the
variety of events that can be programmed and to demonstrate that the
size of any entry depends on the parameters required for that event
Up to 25 clock time events can be programmed.
176
Instrument Automation
Using clock time events
Procedure: Adding events to the clock table
1. Press [Clock Table].
2. To add new events to the clock table, press [Mode/Type].
When entries are added, they are automatically ordered
chronologically.
3. Select next event type.
4. Set appropriate parameters.
Repeat this process until all entries are added.
Procedure: Editing clock time events
1. Press [Clock Table] to view all events programmed.
2. Scroll to the event you want to change.
3. Edit the time for an event, move the cursor to the line labelled
Time: and type the desired time.
4. Edit a setpoint value by scrolling to the setpoint item and
pressing the [On] or [Off] key, or enter a numerical value for
the setpoint.
177
Instrument Automation
Using clock time events
Procedure: Deleting clock time events
1. Press [Clock Table].
2. Press the [Delete] key to remove events from the clock time
table. Pressing the [Delete] key while in an existing time table
produces the following display:
3. Press [Enter] to delete the current timed event; press
[Clear] to cancel this operation.
To delete the entire table, press [Delete][Clock Table].
The following display appears.
178
8
Analytical Methods
Saving an instrument setup as a
method. Restoring and using saved
methods.
Analytical Methods
What is a method?
An analytical method is a collection of setpoints required to run a single sample
on the 6890 Series GC. Methods make it possible to restore the instrument to a
desired setup without reentering all the setpoints.
You can think of a method as a collection of completed control tables, containing
information such as oven temperature programs, pressure programs, inlet
temperatures, etc. Actually, there is always an active method in the GC—it is
the set of conditions that are controlling the machine now. A method is created
by saving these conditions as a numbered method using the [Store] key.
There are three kinds of methods:
•
The active method—the setup that you are presently using.
•
Stored methods—one of the five methods that can be stored in the GC.
•
The default method—a set of default parameters for the GC. It can be
reloaded at any time.
What can you do with it?
Methods can be:
180
•
Created by setting the GC up the way you want it. This is the active method.
•
Stored by pressing [Store] and giving the method an identifying number
from 1 to 5.
•
Loaded by pressing [Load] and specifying the method number to be loaded.
Loading a method overwrites the setpoints of the active method.
•
Modified by loading, making the changes you want, and then storing using
the original number. The new version replaces the old one.
Analytical Methods
Creating a method
Methods are viewed in a method status control table, which shows the times
and dates when the methods were stored. Access this table by pressing [Method].
Method status. <empty>means that
no method is stored. If a method is stored
the time and date it was last stored are
shown.
Set default method. Replaces the active
method with the default setpoints.
Creating a method
Because a method is a set of control tables of setpoints used for analysis, it
depends on instrument configuration. The following is a list of parameters for
which you can store setpoints during method development:
•
Oven
•
Front/Back inlet
•
Column 1 & 2
•
Front/Back detector
•
Signals 1 & 2
•
Aux #1-5
•
Post run
•
Valve # 1-8
•
Run time table
•
Front and back injectors
•
Sample tray
These parameters are saved when the GC is turned off and reloaded
automatically when you turn the instrument back on. However, if the hardware
has been changed while the instrument was turned off, it may not be possible
to restore all setpoints in the method.
181
Analytical Methods
Creating a method
Procedure: Storing a method
To store a method:
1. Press [Method] and scroll to the method number you wish to use.
2. Press the [Store] key. You are then asked to confirm the store.
3. [Enter] stores the method using the chosen number. [Clear] returns to the
STORED METHODS status table without storing the method.
4. If a method with this number already exists, this screen appears:
182
•
[Enter] to replace the existing method with the new one and return to
the STORED METHODS status table.
•
[Clear] to return to the STORED METHODS status table without storing
the method.
Analytical Methods
Creating a method
Procedure: Loading a previously stored method
To load a stored method:
1. Press [Method] to access the STORED METHODS status control table.
2. Scroll to the method you wish to load.
3. Press the [Load] key.
You are prompted to either load the method by pressing [Enter] or to cancel
this function by pressing [Clear].
4. Press [Enter] to load the method. The selected method replaces the active
method.
[Clear] exits this function and returns to the STORED METHODS status table.
183
Analytical Methods
Creating a method
Procedure: Loading the default method
The GC default parameters can be reloaded at any time.
1. Press [Method].
2. Scroll to Set default method.
3. Press [Enter].
See chapter 2, Keyboard and Display, for more information.
184
Analytical Methods
Method mismatch
Method mismatch
Method mismatch messages appear when the method you load contains
parameters that do not match the GC’s current configuration. If this happens,
the setpoints that do not match may be ignored.
Mismatches are caused by user changes (different choice of carrier gas, etc.) or
by hardware changes (replace a TCD with an FID, etc.) that are made after the
method is stored.
User-entered configuration changes
You will be warned of user-entered configuration changes between the stored
method and the active method. The active method will overwrite the parameter
change.
Press [Status] to see which parameters are causing the method mismatch.
Method mismatch-—message will appear if
hardware or user-entered configuration has
changed.
Hardware configuration changes
If the hardware has changed, some parts of the method may be ignored. You are
warned if this happens. For example, suppose you replace the front FID with
an ECD. If you now load a method that uses the FID, the FID setpoints cannot
load. They will be ignored and current ECD setpoints will be retained. All other
setpoints that can be loaded, will be loaded.
185
Analytical Methods
Method mismatch
Procedure: Modifying a previously stored method
When a method is loaded it replaces the active method.
You can modify a previously stored method by:
1. Loading the desired method
2. Making the appropriate changes
3. Storing this method under the same method number (overwrite the original
method) or store as a different method number
186
Analytical Methods
Method listings
Procedure: Deleting a stored method
There are two ways to delete methods.
1. From within the method status control table, scroll to the appropriate
method and press [Delete]. You will be prompted with the following:
2. To delete this method, press [Enter].
3. To change your mind and not delete this method, press [Clear].
Method listings
When the 6890 transmits a formatted method listing to an external device, the
listing shows the pneumatics setpoints relative to the initial (start-of-run) oven
temperature, regardless of the current temperature.
This provides consistent method listings that depend only on the method content
and are not affected by the current state of the instrument.
As a result, the pneumatics setpoints listed on an integrator (or other products
that use the formatted method listing) may differ from the setpoints that appear
at the same time in the 6890 display.
187
Analytical Methods
Method listings
188
9
Valve Control
Using valves for flow path changes,
sample selection, and sample injection
Valve Control
The 6890 Series Gas Chromatograph (the GC) holds up to four valves in a heated
valve box on top of the oven.
The valve box is the preferred location because it is a stable temperature zone,
isolated from the column oven.
The valve box
Instrument rear
EPC pneumatics
Valve blocks
Detectors
Valve box,
cover removed
Figure 29 The valve box
Heating the valves
The valve box contains two heated blocks, each with two valve mounting
locations (shaded). The middle hole on each block is used to pass tubing into
the column oven.
If two valves are used, mount them on the same block. This allows them to be
heated using only one control channel (Aux 1 or Aux 2, depending on how the
heaters are wired). With more than two valves, both Aux 1 and Aux 2 must be
used for heating the two blocks. Set them at the same temperature.
190
Valve Control
The valve box
Valve temperature programming
Most valve applications are isothermal; however, you can define three
temperature ramps if desired. Press [Aux #], then [1] or [2]. Program this ramp
the same as an oven ramp. Refer to Making a temperature-programmed run
on page 88 for more information.
Configuring an Aux thermal zone
To configure a thermal Aux zone (1 or 2), press [Config], then [Aux #]. Press
[Mode/Type], then select the type of device to be controlled by the zone and
press [Enter].
191
Valve Control
Valve control
Valve control
Valves can be controlled manually from the keyboard or as part of a clock or
run time program. Note that if a valve position is changed during a run, it is not
reset automatically at the end of the run unless it is configured as a gas sampling
valve. For other valve types, you must include any desired resets in the program.
The valve drivers
A valve driver is the software and circuitry in the GC that controls a valve or
related function. There are eight drivers known as Valve 1 through Valve 8.
Table 22
Valve Driver Characteristics
Valve number
Type
Volts
Power or current
Use
1, 2, 3, and 4
Current
source
24 VDC
13 watts
Pneumatic valve
control
5 and 6
Current
source
24 VDC
100 mA
Relays and low-power
devices
7 and 8
Contact
closure
48 VDC or
48 VAC RMS
Control an external
current source
The internal valve drivers
Valve drivers 1 through 4 are usually used to control pneumatically operated
valves mounted in the valve box. The wiring for these appears at a set of
connectors inside the right cover of the GC.
Pneumatically driven valves are controlled by solenoids mounted near the
connectors that control the flow of air to the valve actuators.
192
Valve Control
The external valve drivers
Solenoid wiring bracket
Keyboard
Connector V1
or
Run time
program
Connector V2
Internal valve
drivers (1 through 4)
Connector V3
or
Connector V4
Clock time
program
Figure 30 Internal valve drivers
There is no direct relationship between the location of a valve in the valve box
and the driver that controls it. This depends on how the solenoids are wired and
the actuators are plumbed.
The external valve drivers
Valve drivers 5 and 6 control a current that may be used to drive a relay or other
low-power device. Valve drivers 7 and 8 switch a current from an external
source. Electrical details are in Table 22 on page 192.
These drivers, particularly Valve 7 and 8, may be used to control a motor driven
multiposition valve for stream selection.
All four of these drivers appear on the External Event connector on the back of
the GC.
193
Valve Control
Valve configurations
External event connector
on back panel
Keyboard
Valve 5 (pin 1) and
ground (pin 3 or 4)
or
Run time
program
External valve drivers
(5 through 8)
or
Clock time
program
Valve 6 (pin 2) and
ground (pin 3 or 4)
Valve 7
(pin 5 and pin 6)
Valve 8
(pin 7 and pin 8)
Figure 31 External valve drivers
Valve configurations
There are five possible valve types:
194
•
Gas sampling—a two-position (load and inject) valve. In load position, an
external gas stream flows through an attached 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, it starts a run if
one is not already in progress. See the example on page 198.
•
Switching—a two-position valve with four, six, or more ports. These are
general-purpose valves used for such tasks as column selection, column
isolation, and many others. For an example of valve control, see page 197.
•
Multiposition—also called a stream selection valve. It is usually used to
select one from a number of gas streams and feed it to a sampling valve for
analysis. It has a special actuator that advances the valve one position each
time it is activated, or it may be motor driven. An example that combines a
stream selection valve with a gas sampling valve is on page 199.
•
Other—could be anything.
•
Not installed—self-explanatory.
Valve Control
Valve configurations
Procedure: Configuring a valve
1. Press [Config] [Valve #].
2. Specify the valve driver to be configured.
Type the number (1 in this example) and
press [Enter].
3. The present type for this driver is shown.
4. Press [Mode/Type] for the valve choices.
or
5. Select a valve type and press [Enter].
or
195
Valve Control
Valve control
Valve control
Procedure: Controlling valves from the keyboard
Valves (except multiposition valves) have two positions controlled by the [On]
and [Off] keys. The keyboard commands for two-position valves are:
[Valve #] <scroll to the valve> [On](rotates valve to one stop)
and
[Valve #] <scroll to the valve> [Off](rotates valve to the other stop)
From the run or clock time tables
The Valve On and Valve Off commands can be run time or clock time
programmed. See chapter 7 for more information.
If a valve is rotated by a run time program, it is not automatically returned to its
initial position at the end of the run. You must program this reset operation
yourself.
196
Valve Control
Valve control examples
Valve control examples
Simple valve—column selection
This is the plumbing for a single valve, configured as a switching valve, that
selects one of two columns for analysis. It has no configuration parameters.
First column
First column
From inlet or
sampling valve
To detector
Back column
Back column
ON
OFF
Figure 32 A column selection valve
The column is selected by pressing [Valve #] <scroll to valve 2> [On] (for the
front column) or [Off] (for the back column). This run table ensures that the
valve is in the Off state between runs:
Ensure that the valve is in
the Off state between runs.
Gas sampling valve
If a valve is configured as a gas sampling valve, it starts a run automatically when
it is switched to the Inject position. This can be done with a keyboard command
or by a subsequence or clock table entry. You may have two gas sampling valves
installed.
197
Valve Control
Valve control examples
To column
To column
Carrier in
Inject
position
Load
position
Loop
Sample in
Sample out
Sample in
Sample out
Load position—the loop is flushed with a stream of the sample gas. The
column is flushed with carrier gas.
Inject position—the filled loop is inserted into the carrier gas stream. The
sample is flushed onto the column. The run starts automatically.
Figure 33 A gas sampling valve
Carrier gas may be provided by an (optional) auxiliary gas channel. To do this,
configure the column and specify an Aux # channel as the inlet. The Aux #
channel then becomes programmable with four operating modes.
Loop volume and Inlet: are
information only—they do not affect
operation.
Time in minutes that the valve remains in
the load position before becoming ready
Time in minutes that the valve remains
in the inject position before returning to
the load position
The sampling valve cycle is:
1. The sampling valve rotates to the Load position. Load time begins. Valve
is not ready.
2. Load time ends. The valve becomes ready.
3. If everything else is ready, the GC becomes ready.
If everything else is not ready:
198
Valve Control
Valve control examples
•
If you are using Clock Table or sequence control, the GC waits until
everything is ready, then executes the valve inject command.
•
If you are not using Clock Table or sequence control, the valve injection
can be made at any time from the keyboard.
4. The sampling valve rotates (keyboard command or sequence control) to the
Inject position. Inject time begins. The run begins.
5. Inject time ends. Return to step 1.
Multiposition stream selection valve and sampling valve
Several manufacturers provide multiposition stream selection valves that can
be driven by valve drivers 1 through 4. Only one multiposition valve can be
configured. See Table 22 on page 192 for the electrical details.
If a valve is configured as a multiposition valve and has a BCD position output
connected to the GC, the valve position can be selected directly.
To column
Multiposition
stream selection
valve
Carrier in
Load
position
Loop
Sample streams in
Selected
stream out
To waste
Figure 34 Multiposition valve with gas sampling valve
If the GC has one valve configured as a multiposition valve and another
configured as a gas sampling valve, it assumes that they are to be used as shown
in Figure 34. This “double configuration” can be used to replace an automatic
199
Valve Control
Valve control examples
liquid sampler and sample tray in an analytical sequence. The multiposition valve
becomes the sample tray; the gas sampling valve becomes the injector. See
chapter 11 for details.
Two configuration parameters provide mechanical and electrical compatibility
with most multiposition valve actuators.
Time between valve steps
If On, compliments BCD input
200
•
Switching time, in seconds, is a delay between successive actuator movements. It allows time for the actuator mechanism to prepare for the next
movement.
•
Invert BCD complements the BCD input—1’s become 0’s and 0’s become
1’s. This accommodates coding convention differences among manufacturers.
10
The Automatic Liquid
Sampler
The injector, the sample tray, and the
bar code reader
The Automatic Liquid Sampler
There are two Agilent automatic liquid sampler (ALS) systems available for the
6890 GC, the 7673 and the 7683. Refer to the ALS compatibility matrix below.
Table 23 ALS Compatibility Matrix
GC Serial
Number
G2612A ALS Interface
Board installed?
6890 or
6890 Plus
Any
No
6890 Plus
> 20,000
Yes
ALS
GC Type
7673
7683
Note that once a G2612A ALS Interface board is installed, that GC can use only
the 7683 ALS.
Part 1.
The 7673 ALS
This section contains information on how to configure and use your 7673 ALS.
The automatic liquid sampler system can include one or two injector towers, a
bar code reader, and a tray. You use the GC keyboard to enter injector and tray
setpoints and to control simple sequences. The system requires an G1512A
controller module. The parts of the sampler are:
•
Injector tower—houses a 5-µl or 10-µl syringe for sample injection. Two
towers can be mounted for injection into both inlets. The tower can be lifted
off the inlet and parked on posts at the back of the GC.
•
Sample tray—holds a maximum of 100 sample vials.
•
Injector turret—holds sample, waste, and wash vials.
•
Bar code reader—reads and decodes several different bar codes.
For more information on the 6890 automatic liquid sampler, refer to its
Operating Manual (Part no.07673-90187).
202
Part 1. The 7673 ALS
The Automatic Liquid Sampler
Tower
Tray
Bar code reader
Turret
Figure 35 The 7673 automatic sampler components
203
The Automatic Liquid Sampler
Injector control table
Part 1. The 7673 ALS
Injector control table
Press [Front Injector] or [Back Injector].
Appears only if Sampling offset is On
Injection volume—Each volume unit corresponds to one-tenth the syringe
capacity (enter 5 to inject half a syringe-full).
Number of sample pumps—How many times the syringe plunger is moved
up and down with the needle in the sample to expel air bubbles and improve
reproducibility.
Viscosity delay—How many seconds the plunger pauses at the top of the
pump and injection strokes. For viscous samples, the pause allows the sample
to flow into the vacuum created in the syringe.
Number of sample washes—How many times the syringe is rinsed with
sample before the injection. The injector lowers the needle into the sample vial,
fills the syringe to eight-tenths its full volume, and empties it into one of the
waste bottles.
Number of solvent A washes—How many times the syringe is rinsed with
solvent from the solvent A bottle.
Number of solvent B washes—How many times the syringe is rinsed with
solvent from the solvent B bottle.
204
Part 1. The 7673 ALS
The Automatic Liquid Sampler
Configuring the injector
Slow Plunger—The speed of the syringe plunger during injection. Enables you
to reduce the average speed of the plunger and hold the syringe needle in the
inlet for 4 seconds after the injection. Turning the setpoint On pushes at a rate
of about 5 µL/sec (with a 10 µL syringe)—Off is about 20 times faster. The
plunger speed during the pump and waste dispensing does not change.
Procedure: Editing injector setpoints
Accessing either of the injector keys allows you to edit injector control setpoints,
such as injection volumes, sample and solvent washes, etc.
To edit the injector setpoints:
1. Press [Front Injector] or [Back Injector].
2. Scroll to the desired setpoint.
3. Enter a setpoint value or turn the setpoint On or Off.
Configuring the injector
Tower position
Injector cables are connected to either the INJ1 or INJ2 port on the
controller. This setpoint indicates which tower is on which inlet. With only one
injector, you do not have to move cables when you move the tower, merely
reconfigure the tower position.
Waste bottle position
The turret waste bottle positions are controlled by entering a value of:
•
0 for the A position only
•
1 for the B position only
•
2 to alternate between the two waste bottles
205
The Automatic Liquid Sampler
Sample tray setpoints
Part 1. The 7673 ALS
Procedure: Configuring the injector
1. Press [Config][Front Injector] or [Config][Back Injector].
Specifies tower identity
Specifies turret waste bottles
2. With the cursor on a tower line, use the [On] or [Off] key to set the tower
position to either INJ1 or INJ2.
3. Enter a value for Waste bottle use.
Sample tray setpoints
The sample tray delivers sample vials to the front and rear injectors according
to the defined sequence parameters. There are a separate set of sequence
parameters for each injector. The sample tray delivers vials to the front injector
before the rear injector. Stored sequences and bar code configurations can be
used to tell the sample tray where to deliver and retrieve sample vials.
Enable tray—turn On for a tray sequence, Off for sample bottles in the
injector turret.
Enable bar code—turns the bar code reader on or off.
Procedure: Editing the sample tray setpoints
1. Press [Sample tray] to access the sample tray and bar code reader setpoints.
2. Press [On] or [Off] to enable or disable the tray.
3. Press [On] or [Off] to enable or disable the bar code reader.
206
Part 1. The 7673 ALS
The Automatic Liquid Sampler
Sample tray setpoints
Procedure: Configuring the bar code reader
The bar code reader can be configured to read specific codes on the bar code
label.
1. To edit the bar code reader setpoints, press [Config][Sample Tray].
[On] to use bar encoding, [Off] to disable
Bar code reader position on tray 1 to 19
2. Press [On] or [Off] to control the following bar code setpoints.
Enable 3 of 9—the 3 of 9 code offers the greatest versatility for
laboratory use. It can encode both letters and numbers, plus a few
punctuation marks, and message length can be varied to suit both the amount
of data to be encoded and the space available.
Enable 2 of 5—the 2 of 5 code is restricted to numbers but does allow
variable message length.
Enable UPC code—the Universal Product Code (UPC) is probably the
most well-known code in use today. UPC codes are numbers-only and have
fixed message length.
3. Enter a tray location to define the bar code reader position. The range is
1 to 19. Position 3 is the front of the tray.
For more information on the 18587A bar code reader, refer to its Operating
Manual (Part no.18587-90107) or Installation and Service Manual (Part no.
18587-90127).
207
The Automatic Liquid Sampler
Storing injector setpoints
Part 1. The 7673 ALS
Storing injector setpoints
After setting up injector setpoints, sample tray setpoints and bar code reader
configurations, store them as part of a method by following the procedures in
chapter 8, “Analytical Methods.” This method becomes a part of the sequence
used to run the samples.
For more information on injector sequences and sequence control, see
chapter 11, Analytical Sequences.
208
Part 2. The 7683 ALS
Part 2.
The Automatic Liquid Sampler
The 7683 ALS
This section describes how to configure and use your 7683 ALS.
The automatic liquid sampler system can include one or two injector towers, a
bar code reader, and a tray. You use the GC keyboard to enter injector and tray
setpoints and to control simple sequences. The system requires an accessory
board (G2612A) installed in the GC. The parts of the sampler are:
•
Injector tower—houses a syringe for sample injection. Two towers can be
mounted for injection into both inlets. The tower can be lifted off the inlet
and parked on posts at the back of the GC.
•
Sample tray—holds a maximum of 100 sample vials.
•
Injector turret—holds sample, waste, and wash vials.
•
Bar code reader—reads and decodes several different bar codes.
For more information on the 6890 automatic liquid sampler, refer to its
Operation Guide (Part no. G2612-90117).
209
The Automatic Liquid Sampler
Part 2. The 7683 ALS
Tower
Turret
Tray
Figure 36 7683 automatic sampler components
210
Part 2. The 7683 ALS
The Automatic Liquid Sampler
Injector control table
Injector control table
Press [Front Injector] or [Back Injector].
Appears only if Sampling offset is On
Injection volume—Each volume unit corresponds to an injection volume
as shown below.
Injection volume as percent of syringe size
Volume
unit
Nanoliter
adapter On
Nanoliter
adapter Off
1
2%
10%
2
10%
20%
3
20%
30%
4
30%
40%
5
40%
50%
Number of sample pumps—How many times the syringe plunger is moved
up and down with the needle in the sample to expel air bubbles and improve
reproducibility.
211
The Automatic Liquid Sampler
Injector control table
Part 2. The 7683 ALS
Viscosity delay—How many seconds the plunger pauses at the top of the
pump and injection strokes. For viscous samples, the pause allows the sample
to flow into the vacuum created in the syringe.
Number of sample washes—How many times the syringe is rinsed with
sample before the injection. The injector lowers the needle into the sample vial,
fills the syringe to eight-tenths its full volume, and empties it into one of the
waste bottles.
Number of solvent A washes—How many times the syringe is rinsed with
solvent from the solvent A bottle.
Number of solvent B washes—How many times the syringe is rinsed with
solvent from the solvent B bottle.
Slow plunger—The speed of the syringe plunger during injection. Enables
you to reduce the average speed of the plunger and hold the syringe needle in
the inlet for 4 seconds after the injection. Turning the setpoint On pushes at a
rate of about 5 µL/sec (with a 10 µL syringe)—Off is about 20 times faster. The
plunger speed during the pump and waste dispensing does not change.
Dwell times—How long, in minutes, the needle remains in the inlet before
or after the injection.
Sampling offset—Enables variable sampling depth.
Procedure: Editing injector setpoints
Accessing either of the injector keys allows you to edit injector control setpoints,
such as injection volumes, sample and solvent washes, etc.
To edit the injector setpoints:
1. Press [Front Injector] or [Back Injector].
2. Scroll to the desired setpoint.
3. Enter a setpoint value or turn the setpoint on or off.
212
Part 2. The 7683 ALS
The Automatic Liquid Sampler
Configuring the injector
Configuring the injector
Tower position
Injector cables are connected to either the INJ1 or INJ2 port on the
controller. This setpoint indicates which tower is on which inlet. With only one
injector, you do not have to move cables when you move the tower, merely
reconfigure the tower position.
Waste bottle position
The turret waste bottle positions are controlled by entering a value of:
•
0 for the A position only
•
1 for the B position only
•
2 to alternate between the two waste bottles
Nanoliter adapter enable
On the 6890 Plus, you can use this option to vary the injection volumes available
with your automatic liquid sampler. When On, injection volumes range from 2%
through 40% of syringe volume. When Off, the volume range is 10% through 50%.
Use B2 wash
On the 6890 Plus, you can enable this option to use two 4 mL vials of solvent B,
increasing the number of runs you can make before refilling solvent vials.
•
Use the same solvent in position B and in position B2. (This option does not
enable you to use a third solvent.)
•
Use the three sample vial position turret.
•
Because your solvent capacity is now 6 mL (2 mL each for solvent vials A,
B, and B2), you must use two waste vials. See Waste bottle position above.
•
Configure each injector separately.
Note that the number of solvent B washes for each injection does not change.
The injector simply alternates use between the two solvent B vials.
213
The Automatic Liquid Sampler
Sample tray setpoints
Part 2. The 7683 ALS
Procedure: Configuring the injector
1. Press [Config][Front Injector] or [Config][Back Injector].
Specifies tower identity
Specifies if two solvent B vials are used (6890 Plus)
Specifies turret waste bottles
Specifies 2% injection volume (6890 Plus)
2. With the cursor on a tower line, use the [On] or [Off] key to set the tower
position to either INJ1 or INJ2.
3. Enter a value for Waste bottle use.
Sample tray setpoints
The sample tray delivers sample vials to the front and rear injectors according
to the defined sequence parameters. There are a separate set of sequence
parameters for each injector. The sample tray delivers vials to the front injector
before the rear injector. Stored sequences and bar code configurations can be
used to tell the sample tray where to deliver and retrieve sample vials.
Enable tray—turn On for a tray sequence, Off for sample bottles in the
injector turret.
Enable bar code—turns the bar code reader on or off.
Procedure: Editing the sample tray setpoints
1. Press [Sample tray] to access the sample tray and bar code reader setpoints.
2. Press [On] or [Off] to enable or disable the tray.
3. Press [On] or [Off] to enable or disable the bar code reader.
214
Part 2. The 7683 ALS
The Automatic Liquid Sampler
Storing injector setpoints
Procedure: Configuring the bar code reader
The bar code reader can be configured to read specific codes on the bar code
label.
1. To edit the bar code reader setpoints, press [Config][Sample Tray].
[On] to use bar encoding, [Off] to disable
Bar code reader position on tray 1 to 19
2. Press [On] or [Off] to control the following bar code setpoints.
Enable 3 of 9—the 3 of 9 code offers the greatest versatility for
laboratory use. It can encode both letters and numbers, plus a few
punctuation marks, and message length can be varied to suit both the amount
of data to be encoded and the space available.
Enable 2 of 5—the 2 of 5 code is restricted to numbers but does allow
variable message length.
Enable UPC code—the Universal Product Code (UPC) is probably the
most well-known code in use today. UPC codes are numbers-only and have
fixed message length.
3. Enter 3 as the bar code reader position when it is installed in the front of the
tray.
For more information on the bar code reader, refer to its Operating Manual or
Installation Manual.
Storing injector setpoints
After setting up injector setpoints, sample tray setpoints and bar code reader
configurations, store them as part of a method by following the procedures in
chapter 8, “Analytical Methods.” This method becomes a part of the sequence
used to run the samples.
215
The Automatic Liquid Sampler
Storing injector setpoints
Part 2. The 7683 ALS
For more information on injector sequences and sequence control, see
chapter 11, Analytical Sequences.
216
11
Analytical Sequences
Performing multiple analyses
Analytical Sequences
What is a sequence?
A sequence specifies the samples to be run and the stored method to be used
for each. It is divided into subsequences, each of which uses a single method,
plus a priority sequence and post-sequence events.
A sequence can contain one to five subsequences, and can be either automatic
liquid sampler- or valve-driven.
What can you do with it?
Sequences can be:
•
Created by entering the sample and method information through the
keyboard.
•
Stored by pressing [Store] [Seq] and giving the sequence an identifying
number from 1 through 5.
•
Loaded by pressing [Load] [Seq] and specifying the sequence number.
•
Modified by loading, making the changes you want, and then storing using
the same number. The new version replaces the old one.
The stored sequence control table, Figure 37, shows the times and dates that
the sequences were stored. This table is accessed by pressing [Seq]. The [Seq]
key toggles between the stored sequence control table and the sequence
definition control table, Figure 38.
Sequence
number
1 to 5
Figure 37 Stored sequence control table
218
Sequence status
<empty> = no
sequence with this
number,
time and date =
when sequence
was stored.
Analytical Sequences
What can you do with it?
Title line—this title will change
depending on where the cursor is
placed within the control table
Priority sequence
Subsequences
Post-sequence events
Figure 38 Sequence definition control table
When in the sequence control table, you will find the [Info] key useful if an
explanation of sequence parameters is needed.
219
Analytical Sequences
Defining a sequence
Defining a sequence
A sequence may consist of the following parts (all three are optional):
220
•
Priority sequence—this is a special provision that allows you to interrupt a
sequence to analyze urgent samples.
•
Subsequences—each subsequence consists of the number of a stored
method and information that defines a set of samples and calibrators to be
analyzed using the method. There may be up to five subsequences.
•
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.
Analytical Sequences
Defining a sequence
Priority sequence
A priority sequence is a way to interrupt a running sequence to analyze one or
more urgent samples. It consists of a single subsequence, either sampler or valve
type, and a special Use priority parameter.
•
If Use priority is Off, the Priority Sequence does nothing. It can be
activated at any time, even when the sequence is running, by opening the
sequence and changing the value to Yes.
•
If Use priority is On, then:
1. The sequence pauses when the current run ends.
2. The priority method is loaded. The priority samples are run, as specified
in the priority sequence.
3. The Use priority parameter is turned Off.
4. The main sequence resumes where it paused.
Sampler
Valve
Figure 39 Priority sequences
Subsequences
A subsequence can use either an automatic liquid sampler or a sampling valve
for injection. It uses one method to analyze a group of samples.
221
Analytical Sequences
Defining a sequence
Post Sequence
Post Sequence is a pair of events that may be applied after the last
subsequence. Post Sequence may load a method—usually to shut down gases
and lower temperatures—and may repeat the set of subsequences.
Procedure: Creating a sequence
1. Press [Seq] to open the sequence control table.
2. Create a Priority Sequence, if desired. This is either a valve or sampler subsequence, with two differences. The method line is labeled Priority
meth #. An additional line, labeled Use priority, may be set either On
or Off.
3. Create one to five subsequences. Subsequences may be either valve subsequences (page 223) or sampler subsequences (page 222). Both types can be
used in the same sequence.
4. Change the Post Sequence events, if desired.
5. Store the completed sequence.
Procedure: Creating a sampler subsequence
To create a sampler subsequence:
1. Press [Seq] to open the sequence control table.
2. Scroll to a subsequence Method # line. If this is the Priority Sequence,
the line is labeled Priority meth #.
3. Enter a method number. Use 0 for the currently active method, 1 to 5 for the
stored methods, or Off to end the sequence.
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.
222
Analytical Sequences
Defining a sequence
4. Press [Mode/Type] and select one of the three injector types.
Sampler sequence
Press [Mode/Type] to select the type.
5. Supply the rest of the subsequence parameters. If you are using both injectors, there will be two sets of parameters.
•
#Injections/vial—the number of repeat runs from each vial. Enter
0 if no samples are to be injected.
•
Samples—the range (first-last) of sample vials to be analyzed.
6. If this is the Priority Sequence, set Use priority to On.
7. Proceed to the next subsequence or to the Post Sequence.
Procedure: Creating a valve subsequence
If your GC is equipped with a gas sampling valve and an (optional) multiposition
valve, a valve subsequence can be created.
1. Press [Seq] to open the sequence control table.
2. Scroll to a subsequence Method # line. If this is the Priority Sequence,
the line is labeled Priority meth #.
3. Enter a method number. Use 0 for the currently active method, 1 to 5 for the
stored methods, or Off to end the sequence.
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.
4. Press [Mode/Type] and select Valve.
223
Analytical Sequences
Defining a sequence
With multiposition valve
Without multiposition valve
Figure 40 Valve subsequences
5. Enter the valve sequence parameters (the first three appear only if a multiposition valve is configured):
#inj/position
number of injections at each position, (0-99)
Position rng
first-last valve positions to sample, (1-32)
Times thru range number of times to repeat the range, (1-99)
# injections
number of injections for each sample
Procedure: Setting the Post Sequence events
1. Scroll to the Post Sequence title section.
2. Method # is the method to be loaded and run once at the end of a sequence.
Enter 1 through 5 for stored methods. If there is no method to be loaded,
enter 0.
3. Repeat sequence—On keeps repeating the sequence. This function is
useful for valve sequences. Off halts the sequence at the end. Turn Repeat
sequence On or Off.
224
Analytical Sequences
Defining a sequence
Procedure: Storing a sequence
1. Press [Store][Seq] to open the Store Sequence control table.
2. Enter an identifying number for the sequence.
3. Press [Enter] to store the sequence.
If the sequence number you specified already exists, you will be prompted to
either:
•
Overwrite the existing sequence, which will replace the existing sequence
with the new sequence
•
Cancel the store and return to the STORED SEQUENCES status table.
Sequences can also be stored from within the STORED SEQUENCES status
setpoint table by scrolling the cursor to the appropriate sequence number and
pressing the [Store] key.
225
Analytical Sequences
Defining a sequence
Procedure: Loading a previously stored sequence
1. Sequences can be loaded by pressing [Load][Seq].
2. Press a number key to select the sequence to be loaded.
3. Press [Enter] to load the sequence or cancel this by pressing [Clear].
4. If you press [Enter], the load is confirmed. This is now the active sequence.
If the sequence number you specified has not been stored previously, you
will be informed by an ERROR: message.
226
Analytical Sequences
Defining a sequence
Procedure: Modifying a previously stored sequence
1. Load the sequence you wish to edit.
2. Open the sequence control table. Scroll to the parameter within the subsequence or Post Sequence you wish to edit.
3. Make the changes.
4. To save the new values, store the sequence under its original number.
227
Analytical Sequences
Sequence control
Procedure: Deleting a sequence
1. To delete a sequence, press [Delete] [Seq]. You will be prompted with:
2. Press one of the indicated number keys to select one of the five possible
sequences to be deleted.
3. To delete the sequence, press [Enter]. You will see this display:
Sequence control
To access the Sequence Control table, press the [Seq control] key. This displays
the current status of the active sequence.
228
Analytical Sequences
Sequence control
Sequence status
There are six possible sequence status modes:
•
Start/running
•
Ready wait
•
Paused/resume
•
Stopped
•
Aborted
•
No sequence
Sequence Control—diplays the
current status of the sequence,
shows which subsequence is
currently active, current sample # or
valve position, and which injection
number of multiple runs is currently
executing.
Procedure: Starting/running a sequence
To start a sequence, scroll to the Start sequence line and press [Enter].
Pressing [Enter] changes the sequence status to Running.
The sequence continues to run until all subsequences are executed, or until one
of the events described on page 231 occurs.
229
Analytical Sequences
Sequence control
Ready wait
If a sequence is started and the instrument is not ready (due to oven temp, equib
times, etc), the sequence will not start until all instrument setpoints are ready.
Procedure: Pausing and resuming a sequence
1. A running sequence can be paused by scrolling to Pause sequence and
pressing [Enter]. Pressing [Enter] changes sequence status to paused, and
you are given the option to resume or stop the paused sequence.
When a sequence is paused, it stops when the current sample run is complete.
2. To continue the paused sequence, scroll to Resume sequence and press
[Enter].
When a sequence is resumed, it starts with the next sample.
Procedure: Stopping a sequence
To halt a sequence, scroll to Stop sequence and press [Enter].
When a sequence is stopped, it can only be restarted from the beginning and the
sampler tray is halted immediately.
A sequence stops at the end of the last active subsequence unless Repeat
sequence is On in the Post Sequence events.
230
Analytical Sequences
Sequence control
Aborting a sequence
When a sequence is aborted, it stops immediately without waiting for the current
run to finish. These will cause a sequence to abort:
A run is stopped by
pressing the [Stop] key.
A sampler error occurs
producing an error message.
The GC detects a configuration
mismatch during a method load
(see chapter 8, "Analytical
Methods").
A running sequence tries to
load an empty method.
The sampler is turned off.
You can correct the problem and then resume the sequence. The aborted sample
run will be repeated.
231
Analytical Sequences
Special considerations when using an integrator
No sequence
If the sequence is off or not defined, the sequence control status will state no
sequence.
To correct this, use the [Seq] key to define a sequence or turn the sequence
parameters on.
Special considerations when using an integrator
The definitions of sequence are not the same in the 6890 Series GC and in the
3396 integrator. The following points must be considered when sequences are
used with this GC/integrator combination:
232
•
The integrator has only one subsequence plus the priority sequence. Only
one GC method can be used within an integrator sequence.
•
The ALS method parameters are prepared using the [Front injector] and
[Back injector] keys on the 6890 keyboard.
•
The sample information table is prepared on the integrator.
•
The injection sequence parameters can be prepared either with the [Seq]
key on the 6890 keyboard or in the [PREP][SEQ] dialog of the 3396. Setting
sequence parameters on either instrument changes the sequence in both
places.
•
The Start sequence function on the GC is inactive.
•
A sequence must be started from the integrator using [SEQ][START].
•
If you use INET, pressing the stop key on either instrument stops the run
and aborts the sequence.
•
If you use cable # 03396-61010 instead of INET, the two stop keys have
different effects. The [STOP] key on the integrator stops the current run and
aborts the sequence. Stop on the GC stops the current run, but the sequence
continues as soon as the GC becomes Ready.
12
Messages
What a message means,
and what to do about it.
Messages
The GC regularly monitors the state of its detectors, pneumatics, oven, PC
boards, and other components. If a problem exists, the GC displays a message,
beeps or activates an LED, and puts itself in a “safe state” if the problem could
be dangerous to the user.
In addition to the information in this chapter, there is device-specific
troubleshooting and maintenance information in many of the chapters in this
and the Inlets and Detectors volumes.
There are six message types:
Not Ready
A Not Ready message means that some component of the GC is not ready to
begin a run. When the GC is not ready, the Not Ready LED lights but there is no
popup message on the display. Press [STATUS] to see a message that explains
why the GC is not ready. Not ready messages are recorded in the run log.
Method Mismatches
These messages appear if you load a method that contains parameters that do
not match the current GC configuration. One of two things occurs if the method
and configuration do not match:
234
•
If the parameter that does not match is set from the keyboard, the method
overwrites the current parameter; the message states that the current parameter has been replaced. For example, if the gas type currently configured
differs from the one in the method, the current gas type is overwritten with
that of the method.
•
If the parameter that does not match is hardware dependent, the method is
ignored and the current setpoints remain; the message states that the method
parameter is being ignored. For example, if the method indicates that the
front detector is an NPD but you have replaced it with an FID, the method
NPD information is ignored and the current FID parameters remain.
Messages
Warning
A Warning message means that a problem exists but that the problem will not
prevent the instrument from executing the run. The GC emits one beep and a
Warning message appears on the display. The GC can start the run and the
warning disappears when a run starts. The warning is not recorded in the run log.
Shutdown
Shutdown occurs when there is a hardware problem that could compromise the
safety of the user or damage the instrument. Before shutdown occurs, the GC
emits a series of warning beeps. After a length of time specific for the component
elapses, the component with the problem shuts down, the GC emits one beep,
and a warning message appears. The GC is still in a ready state. No additional
information appears under the [STATUS] key and the error is not recorded in
the run log.
Faults
Fault messages indicate hardware problems that require user intervention.
Depending on the type of error, the GC emits no beep or a single beep. The Not
Ready LED lights because the GC is unable to begin a run and an error message
appears. Press [STATUS] for more information. The error is recorded in the run
log.
Two faults can occur that shut down the entire GC; they are a pneumatics
problem for an inlet configured for hydrogen gas and a thermal runaway
condition for the GC oven. In these cases, the GC beeps continuously until you
press [Clear].
Bad mainboard and Fatal error messages
These messages almost always indicate that the mainboard is malfunctioning
and must be replaced. These messages are not numbered and usually appear
when the instrument is first turned on. See Table 24 for a list of messages. With
a few exceptions which are listed in the table, if you get a Bad mainboard or
Fatal error message, you will need to contact your Agilent service representative
to replace the board.
235
Messages
Table 24 Bad Mainboard and Fatal Error Messages
Popup message
Comments
BAD MAINBOARD
Main FPGA Failure
Static RAM Failure
Contact your Agilent service representative.
Boot ROM Checksum
ROM #2 Checksum
Either EEPROM 2 or 3 is malfunctioning. Contact your Agilent
service representative.
ROM #3 Checksum
Incorrect ROM #2
Incorrect ROM #3
ROM #2 wrong version
ROM #3 wrong version
EEPROM 2 or 3 is installed in the wrong position. Change the
position the EEPROM is installed in; contact your Agilent service
representative for more information.
The version of either EEPROM 2 or 3 is different than that of
the other EEPROMs. Contact your Agilent service
representative.
DMA FPGA Failure
DRAM Failure
Contact your Agilent service representative.
FATAL ERROR
Exception Vector
Bus Error
Address Error
Illegal Instruction
Divide by Zero
No 512Hz Interrupt
236
Contact your Agilent service representative.
Part 1. Not Ready messages
Part 1.
Messages
Not Ready messages
A listing of the Not Ready messages is given in Table 25 below.
Table 25 Not Ready Messages
Status message
Run log entry
Comments
Temperature zone not ready messages
Oven temp
Not ready:
Oven temp
See page 240.
####
Front inlet temp
Not ready:
F inlet temp ####
Back inlet temp
Not ready:
B inlet temp ####
Front det temp
Not ready:
Front det temp ####
Back det temp
Not ready:
Back det temp ####
Aux 1 temp
Not ready:
Aux 1 temp
####
Not ready:
Aux 2 temp
####
Aux 2 temp
See page 240.
Pressure or flow not ready messages
Front inlet pressure
Not ready:
Front inlet flow
Not ready:
F inlet flow ##.#
Back inlet pressure
Not ready:
Back inlet flow
Not ready:
B inlet flow ##.#
Front det H2 flow
Not ready:
Front det air flow
Not ready:
F det makeup gas
Not ready:
Back det H2 flow
Not ready:
See page 241.
237
Messages
Part 1. Not Ready messages
Table 25, continued
Status message
Run log entry
Back det air flow
Not ready:
B det makeup gas
Not ready:
Aux 3 pressure
Not ready:
Aux 4 pressure
Not ready:
Aux 5 pressure
Not ready:
Comments
See page 241.
Detector not ready messages
238
Front det waiting
Not ready:
Front det on wait
See page 241.
Back det waiting
Not ready:
Back det on wait
See page 241.
Front det igniting
Not ready:
Front det ignite
See page 242.
Back det igniting
Not ready:
Back det ignite
See page 242.
Front det adjusting
Not ready:
Front det adjust
See page 242.
Back det adjusting
Not ready:
Back det adjust
See page 242.
Front det equib time
Not ready:
Front det equib
See page 242.
Back det equib time
Not ready:
Back det equib time
See page 242.
Front det shutdown
Not ready:
Front det shutdown
See page 242.
Back det shutdown
Not ready:
Back det shutdown
See page 242.
F NPDBead slewing
Not ready:
Front NPD slewing
See page 243.
F NPDBead slewing
Not ready:
Back NPD slewing
See page 243.
Part 1. Not Ready messages
Messages
Table 25, continued
Status message
Run log entry
Comments
Gas saver
Not ready:
Gas saver active
The inlet is in Gas Saver mode.
Press [Prep Run].
Front inlet purging
Not ready:
F inlet purge
Inlet in split mode is purging.
Press [Prep Run]. See page 244.
Back inlet purging
Not ready:
B inlet purge
Inlet in split mode is purging.
Press [Prep Run]. See page 244.
F inl pulse inactive
Not ready:
F inlet pres pulse
Press [Prep Run].
B inl pulse inactive
Not ready:
B inlet pres pulse
Press [Prep Run].
F inl VI flow idle
Not ready:
F inlet VI flow
Press [Prep Run].
B inl VI flow idle
Not ready:
B inlet VI flow
Press [Prep Run].
Need F inl Solv vent
Not ready:
F inlet Solv. vent
Press [Prep Run].
Need B inl Solv vent
Not ready:
B inlet Solv. vent
Press [Prep Run].
24V pneu valve drive
Not ready:
24V pneu valve drive
See page 243.
Multiposition valve
Not ready:
Multiposition valve
See page 243.
Gas sampling valve 1
Not ready:
Gas sampling valve 1
See page 243.
Gas sampling valve 2
Not ready:
Gas sampling valve 2
See page 243.
Inlet not ready messages
Valve not ready messages
239
Messages
Temperature zone not ready
Part 1. Not Ready messages
Table 25, continued
Status message
Run log entry
Comments
Diagnostics mode
Not ready:
Diagnostics active
See page 244.
Test in progress
Not ready:
Test in progress
A diagnostic test is in progress.
Wait until it is completed.
Front injector
Not ready:
Front injector
Back injector
Not ready:
Back injector
Host system
Not ready:
Host system
Other not ready messages
External device
Power on in progress
See page 244.
An device connected to the
Remote Start connector is not
ready.
Power-on restart:
Blank run
See page 245.
Temperature zone not ready
Oven temp
The GC is not ready to begin a run until the oven temperature is within ±1 degree
of the setpoint for the equilibration time. The GC is not ready if the oven is not
turned on.
If the oven is unable to reach the setpoint, the GC remains not ready indefinitely
unless the oven temperature is out of the oven range, which will cause a
shutdown.
Other heated zones
The GC has a number of heated zones in addition to the oven. These are inlets,
detectors, and auxiliary, or “aux,” zones. The GC is not ready to start a run until
240
Part 1. Not Ready messages
Messages
Pressure and/or flow not ready
all the zones are within ± 1°C of the setpoint and have maintained the setpoint
temperature for 30 seconds. A zone that is turned off is considered ready.
If a temperature zone is unable to reach the setpoint, the GC remains not ready
indefinitely. The GC does not shut down unless a temperature is out of the range
for the zone.
Pressure and/or flow not ready
The GC will not start a run until all pressurized areas have reached their setpoints
and maintained them for 6 seconds. The acceptable pressure range of an area
is between 0.05 and 0.5 psi, depending on its sensor type.
Likewise, the GC is not ready to begin a run until flows are within 1 mL/min of
the setpoint and remain in the range for 6 seconds. Pressure zones that are turned
off are considered ready.
If the zone does not become ready within a specified time, the GC goes into
shutdown mode. See the Shutdown messages for more information.
When a pressure or flow cannot become ready, check that the gas supply is on
and has enough gas.
Detector not ready
Front det waiting
Back det waiting
To prevent condensation, FID and NPD temperatures must be at least 150°C
before they can ignite. The FPD must be at 120°C or higher before it can ignite.
The TCD must be at 100°C or higher before the filament current turns on. If
temperatures are below the minimum, the GC is not ready.
If a detector is unable to reach its minimum temperature, the GC remains not
ready indefinitely.
•
Verify that the detector temperature setpoint is high enough for operation.
Raise it if it is too low.
241
Messages
Detector not ready
Part 1. Not Ready messages
•
If the temperature setpoint is high enough but the detector is unable to reach
it, the heater may have failed or the sensor or mainboard may be bad. Contact
your Agilent service representative.
Front det igniting
Back det igniting
The GC is not ready while the FID or FPD is going through the flame ignition
sequence. The messages clear if the detector is turned off.
If the FID or FPD is unable to ignite, the detector may eventually shutdown. See
the FID or FPD section of the Detectors volume.
Front det adjusting
Back det adjusting
The GC is not ready because the NPD or ECD is adjusting its baseline to reach
the offset (FID) or output (ECD) setpoint. The ECD adjustment is usually
complete in 30 seconds. The NPD may require an hour to adjust.
The NPD may be unable to reach the setpoint if there is contamination in the
system (for example, if the gas is not pure enough or the bead is damp) or if the
bead is worn out. If it cannot reach the setpoint, you will not receive an error
message; the GC simply does not become ready.
Turning the detector off clears the message.
Front det equib time
Back det equib time
The NPD has completed adjusting the offset and is waiting for the value to remain
at the setpoint for the equilibration time.
The NPD may not be able to equilibrate if the system is contaminated or the
bead is worn out. In addition, changes in the room temperature could prevent
equilibration. The GC becomes ready if the detector is turned off.
You can change the equilibration time from the Detector control menu.
Front det shutdown
Back det shutdown
The FID, FPD, NPD, or TCD shut down if they experience a pneumatics failure
or if the TCD experiences a filament failure.
242
Part 1. Not Ready messages
Messages
Valve not ready
The GC remains not ready until the detector with the failure is turned off. Turning
off the FID or FPD turns off the igniter, hydrogen flow, and air flow. Turning off
the NPD turns off bead voltage, hydrogen flow, and air flow. Turning off the TCD
turns off filament voltage and reference flow.
F NPD bead slewing
B NPD bead slewing
The NPD bead voltage is adjusting to a new setpoint.
Valve not ready
24V pneu valve drive
This Not Ready state means that the +24 V supply to the pneumatics valves is
actually less than +16.5 V. All valves are disabled to prevent improper operation.
When full voltage is restored, the GC becomes ready.
This Not Ready state could indicate a hardware problem.
Gas sampling valve 1
Gas sampling valve 2
The GC is not ready because the inject time or load time has not elapsed. It
becomes ready when the specified load or inject time has passed.
Multiposition valve
The multiposition valve is causing the GC to be in a not ready state for one of
the following reasons:
•
The multiposition valve is not at the setpoint position. The GC remains not
ready until the valve reaches the setpoint.
•
The BCD cable is missing or not plugged into the receptacle. If the cable is
missing, the valve will never become ready.
•
The BCD setpoint is incorrect for the valve BCD output polarity. The valve
will most likely shutdown with Illegal Position or Not Switching shutdown
errors.
243
Messages
Other not ready messages
•
Part 1. Not Ready messages
If the valve is plugged or the sample is viscous, the switching time may be
too short for the valve to switch. Increase the switching time.
Other not ready messages
Diagnostics mode
The GC is not ready when it is in diagnostics mode. The instrument is in
diagnostics mode whenever a Diagnostics control table has been accessed
through the [Options] key.
Exit the Diagnostics section of the keyboard for the GC to become ready.
External device
An instrument that is part of the start/stop bus is not ready. For example, the
automatic liquid sampler is not ready to begin injecting. The GC becomes ready
when the other instruments on the bus are ready.
Host system
The GC is not ready if the integrator, Agilent ChemStation, or other controller
is not ready to begin a run. It becomes ready when the host does.
Front inlet purging
Back inlet purging
This applies only if you have a split/splitless inlet. The message appears if you
try to start a run while the inlet purge valve is still in the split mode.
The inlet remains not ready and purging continues until you press the [Prep Run]
key. Pressing [Prep Run] closes the valve (it also turns off the gas saver mode
and increases pressure for a pressure pulse, if selected).
244
Part 1. Not Ready messages
Messages
Other not ready messages
Power on in progress
This message appears when:
•
Power is restored after a power failure during a run or while the oven was
turned on and the GC was not performing a run.
• Power is turned on again after a user turned it off while the oven was turned
on.
The GC heats all the other thermal zones and then heats the oven. When the
oven temperature reaches the setpoint for equilibration time, the GC becomes
ready.
If the power failure occurred during a run, upon power restoration the GC heats
all the thermal zones and the oven and automatically performs a blank run. When
the blank run is completed, the GC becomes ready.
245
Messages
Part 2.
Part 2. Shutdown messages
Shutdown messages
When the GC encounters a Shutdown condition, a popup message appears on
the display. The popup message is numbered and briefly explains the problem.
This chapter provides more thorough information about the problems that cause
the GC or a component of the GC to shut down.
Table 26 Shutdown Messages
246
Shutdown no.
Popup message
Comments
1
Oven shut off
See page 247.
2
Oven cryo shutdown
See page 247.
3
Front inlet pressure shutdown
See page 248.
4
Front inlet flow shutdown
See page 248.
5
Back inlet pressure shutdown
See page 248.
6
Back inlet flow shutdown
See page 248.
7
Front detector fuel gas shutdown
See page 248.
8
Front detector air/ref shutdown
See page 248.
9
Front detector makeup shutdown
See page 248.
10
Back detector fuel gas shutdown
See page 249.
11
Back detector air/ref shutdown
See page 249.
12
Back detector makeup shutdown
See page 249.
13
Pres aux 3 shutdown
See page 249.
14
Pres aux 4 shutdown
See page 249.
15
Pres aux 5 shutdown
See page 249.
16
Multiposition valve is not switching
See page 249.
17
Can’t reach setpoint of multipos valve
See page 250.
18
Front inlet cryo shutdown
See page 250.
19
Back inlet cryo shutdown
See page 250.
20
Aux 1 cryo shutdown
See page 251.
21
Aux 2 cryo shutdown
See page 251.
22
Front inlet heating too slowly: temperature shut off
See page 251.
23
Back inlet heating too slowly: temperature shut off
See page 251.
Part 2. Shutdown messages
Messages
Shutdown 1—Oven shut off
The power required to keep the oven at setpoint exceeds the expected power
for that temperature. The GC becomes not ready. The oven flaps open half-way
(if they are operating correctly). Turn the GC off and then on again or change
the oven temperature to restore operation. Possible causes include:
•
Malfunctioning oven flap. Check the oven flap on the back of the GC. It
should be open when cooling (for temperatures between 50 and 250°C) or
closed completely to reach temperature setpoints. If the flap is stuck
completely or partially open, it is not operating correctly. Contact your
Agilent service representative.
•
Look for thermal leaks in the oven (for example, missing insulation around
an inlet or detector location or a leak in the door).
•
Check for excessive load in the oven (for example, a very large packed
column).
•
The oven heater or the heater electronics are not operating correctly.
Contact your Agilent service representative.
Shutdown 2—Oven cryo shutdown
The GC oven has shut down. Cryogenic shutdowns conserve liquid coolant when
the GC is unable to start a run. A cryo shutdown does not mean that the cryogenic
cooling system is malfunctioning. Instead, one of the following could be the
cause:
•
A “cryo timeout” has occurred. This happens if the GC oven has reached its
temperature setpoint but the amount of time you specified for the cryo timeout setpoint has elapsed without a run beginning.
Turn the oven off and then on again or change the setpoint to restore normal
operation. Then turn the timeout option off to prevent another shutdown or
lengthen the timeout period.
•
A “cryo fault” has occurred. Cryogenic cooling has been on for over
16 minutes but the oven has not reached its temperature setpoint.
Check the level of the cryogenic fluid and replace the supply if it is too low
for proper cooling. The cryo valve may be stuck open or closed. If your fluid
supply is adequate, the valve may be broken or the electronics driving it may
247
Messages
Part 2. Shutdown messages
be malfunctioning (this is a less likely cause). Contact your Agilent service
representative.
Shutdown 3—Front inlet pressure shutdown
The front inlet failed to reach its setpoint in the allotted time. The time varies
with the type of inlet; it is 2 minutes for purged packed and cool on-column inlets
and 5.5 minutes for the split/splitless inlet. The GC is not ready until the problem
is corrected and the inlet reaches the setpoint.
Shutdown 4—Front inlet flow shutdown
The front inlet failed to reach its flow setpoint in the allotted time. In flow-control
mode, the inlet has 2 minutes to reach the setpoint before shutdown. The GC is
not ready until the problem is corrected and the inlet reaches the flow setpoint.
Shutdown 5—Back inlet pressure shutdown
The back inlet can not reach or maintain the pressure setpoint. See Shutdown 3.
Shutdown 6—Back inlet flow shutdown
The back inlet can not reach or maintain the flow setpoint. See Shutdown 4.
Shutdown 7—Front detector fuel gas shutdown
The front detector (EPC version) fuel gas is unable to reach or maintain the
pressure setpoint in the allotted 2 minutes. The GC is not ready until the problem
is corrected and the detector reaches the setpoint.
Shutdown 8—Front detector air/ref shutdown
The front detector (EPC version) air or reference gas is unable to reach or
maintain the pressure setpoint. All the detector gases are shut off and the GC is
not ready. See Shutdown 7.
Shutdown 9—Front detector makeup shutdown
The front detector (EPC version) makeup gas is unable to reach or maintain the
pressure setpoint. All the detector gases are shut off and the GC is not ready.
See Shutdown 7.
248
Part 2. Shutdown messages
Messages
Shutdown 10—Back detector fuel gas shutdown
The back detector (EPC version) fuel gas is unable to reach or maintain the
pressure setpoint. All the detector gases are shut off and the GC is not ready.
See Shutdown 7.
Shutdown 11—Back detector air/ref shutdown
The back detector (EPC version) air or reference gas is unable to reach or
maintain the pressure setpoint. All the detector gases are shut off and the GC is
not ready. See Shutdown 7.
Shutdown 12—Back detector makeup shutdown
The back detector (EPC version) makeup gas is unable to reach or maintain the
pressure setpoint. All the detector gases are shut off and the GC is not ready.
See Shutdown 7.
Shutdown 13—Pres aux 3 shutdown
The pneumatics aux 3 module can not maintain the pressure setpoint. All the
detector gases are shut off and the GC is not ready. See Shutdown 3.
Shutdown 14—Pres aux 4 shutdown
The aux 4 module can not maintain the pressure setpoint. See Shutdown 3.
Shutdown 15—Pres aux 5 shutdown
The aux 5 module can not maintain the pressure setpoint. See Shutdown 3.
Shutdown 16—Multiposition valve is not switching
The multiposition valve has tried to switch twice without success. The valve
shuts down and reports that it is not ready (not at setpoint). Clear the shutdown
by entering a new setpoint. Possible causes include:
•
The valve is not connected to the correct valve driver or is not connected at
all. Connect the valve to the correct valve driver.
•
The valve is stuck.
•
The switching time is too short for the speed of the valve. The valve could
be switching more slowly than usual because it is sticking slightly or the
sample is viscous. Increase the switching time.
249
Messages
Part 2. Shutdown messages
Shutdown 17—Can’t reach setpoint of multipos valve
The valve is switching to the wrong position or is unable to switch to the setpoint
position. The valve will shut down. Clear the shutdown by entering a new
setpoint. Possible causes include:
•
The valve position is incorrect. A setpoint was entered that the valve is
unable to reach. For example, position ten was entered for an eight-port
valve. Enter a correct valve position setpoint.
•
The Invert BCD setpoint is incorrect. With most valves, the invert should be
On. If the BCD setpoint is already On and you experience a shutdown, set it
to Off.
Shutdown 18—Front inlet cryo shutdown
Shutdown 19—Back inlet cryo shutdown
The inlet is shut down. A cryogenic shutdown conserves liquid coolant when
the GC is unable to start a run. A cryo shutdown does not mean that the cryogenic
cooling system is malfunctioning. Instead, one of the following could be the
cause:
•
A “cryo timeout” has occurred. This happens if the GC inlet has reached its
temperature setpoint but the amount of time you specified for the cryo timeout setpoint has elapsed without a run beginning.
Turn the inlet off and then on again or change the setpoint to restore normal
operation. Then turn the timeout option off to prevent another shutdown or
lengthen the timeout period.
•
A “cryo fault” has occurred. Cryogenic cooling has been on for over 16
minutes but the inlet has not reached its temperature setpoint.
Check the level of the cryogenic fluid and replace the supply if it is too low
for proper cooling. The cryo valve may be stuck open or closed. If your fluid
supply is adequate, the valve may be broken or the electronics driving it may
be malfunctioning (this is a less likely cause). Contact your Agilent service
representative.
250
Part 2. Shutdown messages
Messages
Shutdown 20—Aux 1 cryo shutdown
Shutdown 21—Aux 2 cryo shutdown
The Auxiliary temperature zone equipped with cryo cooling has shut down. A
cryogenic shutdown conserves liquid coolant when the GC is unable to start a
run. A cryo shutdown does not mean that the cryogenic cooling system is
malfunctioning. Instead, one of the following could be the cause:
•
A “cryo timeout” has occurred. This happens if the GC Aux zone has reached
its temperature setpoint but the amount of time you specified for the cryo
timeout setpoint has elapsed without a run beginning.
Turn the zone off and then on again or change the setpoint to restore normal
operation. Then turn the timeout option off to prevent another shutdown or
lengthen the timeout period.
•
A “cryo fault” has occurred. Cryogenic cooling has been on for over
16 minutes but the Aux zone has not reached its temperature setpoint.
Check the level of the cryogenic fluid and replace the supply if it is too low
for proper cooling. The cryo valve may be stuck open or closed. If your fluid
supply is adequate, the valve may be broken or the electronics driving it may
be malfunctioning (this is a less likely cause). Contact your Agilent service
representative.
Shutdown 22—Front inlet heating too slowly:
temperature shut off
Shutdown 23—Back inlet heating too slowly:
temperature shut off
The inlet heater has been full on for a long time but the inlet temperature is not
at setpoint. Either the temperature sensor for the zone has failed, or the zone’s
heater is defective.
251
Messages
Part 3.
Part 3. Warning messages
Warning messages
Table 27 lists the Warning messages for the GC. Most require Agilent service
intervention. Those that users can correct are indicated along with the corrective
procedures.
Table 27
Warning Messages
Warning no.
Status message
Popup message
100
Oven sensor missing
Oven sensor missing
101
Invalid heater power
Invalid heater power for
front detector, inlet, and
aux 1
Run log entry
Comments
If using an MSD, make
sure the Aux zone is
configured for an MSD
transfer line..
102
Invalid heater power
Invalid heater power for
front detector, inlet, and
aux 2
103
Sig 1 buffer full
Sig 1 buffer full
Possible data loss:
Sig 1 buffer full
See page 255.
104
Sig 2 buffer full
Sig 2 buffer full
Possible data loss:
Sig 2 buffer full
See page 255.
105
Analog out data loss
Analog out data loss
Possible data loss:
Analog out data loss
Contact Agilent service.
106
Signal data loss
Non-recoverable data loss.
Data corrupt.
Possible data loss:
Signal data loss
Contact Agilent service.
107
F det config changed
Front det: config changed,
method defaulted
Correct the method to
match your hardware.
108
B det config changed
Back det: config changed,
method defaulted
Correct the method to
match your hardware.
109
F inl config changed
Front inlet: config changed,
method defaulted
Correct the method to
match your hardware.
110
B inl config changed
Back inlet: config changed,
method defaulted
Correct method to
match your hardware.
111
Col 1 config changed
Column 1: config changed,
method defaulted
Correct method to
match your hardware.
252
Part 3. Warning messages
Messages
Table 27, continued
Warning no.
Status message
Popup message
112
Col 2 config changed
Column 2: config changed,
method defaulted
Correct method to
match your hardware.
113
Aux 3 method changed
Aux 3 config changed
Method defaulted
Correct method to
match your hardware.
114
Aux 4 method changed
Aux 4 config changed
Method defaulted
Correct method to
match your hardware.
115
Aux 5 method changed
Aux 5 config changed
Method defaulted
Correct method to
match your hardware.
116
Run log entry
Log overflow
Comments
Run log capacity is 50
entries.
117
F inl calib deleted
F inl calib deleted
118
B inl calib deleted
B inl calib deleted
119
F det calib deleted
F det calib deleted
120
B det calib deleted
B det calib deleted
121
P aux calib deleted
P aux calib deleted
122
Comm data overrun
Host communications:
data overrun
Possible data loss:
Comm data overrun
Contact Agilent service.
123
Comm data error
Host communications:
data error
Possible data loss:
Comm data error
Contact Agilent service.
124
Comm abnormal break
Host communications:
abnormal break
Possible data loss:
Comm abnormal break
Check connection.
125
Sampler data overrun
Sampler communications:
data overrun
Possible data loss:
Sampler data overrun
Check your sampler
settings. Contact
Agilent service.
126
Sampler data error
Sampler communications:
data error
Possible data loss:
Sampler data error
Check your sampler
settings. Contact
Agilent service.
127
Sampler abnormal com
Sampler communications:
abnormal break
Possible data loss:
Sampler abnormal com
Check connection.
Inlet module is returned
to default calibration.
Detector module is
returned to default
calibration.
Module is returned to
default calibration.
253
Messages
Part 3. Warning messages
Table 27, continued
Warning no.
Status message
Popup message
128
F inl flow cal fail
Front inlet flow sensor
auto zero calib failed.
Contact Agilent service.
129
B inl flow cal fail
Back inlet flow sensor
auto zero calib failed.
Contact Agilent service.
130
Aux 1 cryo disabled
Aux 1 & front inlet on
same cryo valve drive:
aux1 disabled
Reconfigure aux or inlet
cryo drive.
131
Aux 2 cryo disabled
Aux 2 & back inlet on
same cryo valve drive:
aux2 disabled
Reconfigure Aux or inlet
cryo drive.
132
Chgd Col 1 Init time to
###.## ; avoids Sampling
End problem
133
Chgd Col 2 Init time to
###.## ; avoids Sampling
End problem
134
Chgd FI Saver time to
###.## ; avoids Sampling
End problem
135
Chgd BI Saver time to
###.## ; avoids Sampling
End problem
136
Chgd FI Purge time to
###.## ; avoids Sampling
End problem
137
Chgd BI Purge time to
###.## ; avoids Sampling
End problem
254
Run log entry
Comments
For Volatiles interface, a
setpoint conflicted with
the Sampling End time
parameter. Check your
method. See the Inlets
volume for more
information.
Part 3. Warning messages
Messages
Warning 103–Sig 1 buffer full
Warning 104–Sig 1 buffer full
Usually, this error occurs when your data collection device (for example, a PC
running an Agilent ChemStation) goes off-line while the GC is still collecting
data.
Possible causes and solutions:
•
There is a problem with the PC, the cabling to the PC, or the local network
that links the GC to the PC. Check the PC, cabling, and network.
•
The PC was turned off without closing the Agilent ChemStation instrument
session. The GC collects and stores real-time plot data until the buffer overflows and the warning appears. Next time, close the instrument session
before turning off the PC so that the GC stops collecting data.
•
The PC entered power saver mode. When the PC enters power saver mode,
its processor slows down and cannot collect data fast enough for normal
communications, eventually causing the warning to appear. If the PC stays
in power saver mode overnight, for example, there will be an error on the
GC but the Agilent ChemStation will show a Ready status. Close and restart
the instrument session, and disable the PC’s power saver feature.
•
There was a software problem on the PC that stops data collection.
•
There is a hardware problem in the GC. If the problem persists, contact
Agilent for service.
255
Messages
Part 4.
Part 4. Fault messages
Fault messages
Table 28 lists the Fault messages for the GC. Most require Agilent service
intervention. Those that users can correct have a page reference for the
corrective procedures.
Table 28
Fault Messages
Fault no.
Status message
Popup message
Run log entry
200
Pneu board FPGA
Pneumatics shutdown:
faulty pneumatics board
Not ready:
Pneu board FPGA
201
Pneumatics board
Pneumatics shutdown:
faulty pneumatics board
Not ready:
Pneumatics board
202
Hydrogen shutdown
Hydrogen safety
shutdown
Not ready:
Hydrogen shutdown
203
Signal DSP faulty
Signal DSP faulty
Not ready:
Signal DSP faulty
204
Sig DSP ROM broken
Sig DSP ROM broke
Not ready:
Sig DSP ROM broken
205
Sig DSP RAM broken
Sig DSP RAM broken
Not ready:
Sig DSP RAM broken
206
Sig DSP registers
Sig DSP registers
Not ready:
Sig DSP registers
207
Sig DSP data corrupt
Sig DSP data corrupt
Not ready:
Sig DSP data corrupt
208
0-1 mV out #1
Signal path test failed
Not ready:
0-1 mV out #1
209
0-1 mV out #2
Signal path test failed
Not ready:
0-1 mV out #2
210
Analog out #1
Signal path test failed
Not ready:
Analog out #1
256
Comments
See page 262.
Part 4. Fault messages
Messages
Table 28, continued
Fault no.
Status message
Popup message
Run log
Comments
211
Analog out #2
Signal path test failed
Not ready:
Analog out #2
212
F det electrometer
Front detector
electrometer out of
specification
Not ready:
F det electrometer
213
B det electrometer
Back detector
electrometer out of
specification
Not ready:
B det electrometer
214
Front det flame out
Front detector flame out
Not ready:
Front det flame out
See page 263.
215
Back det flame out
Back detector flame out
Not ready:
Back det flame out
See page 263.
216
F TCD filament open
Front TCD filament open
Not ready:
F TCD filament open
See page 263.
217
B TCD filament open
Back TCD filament open
Not ready:
B TCD filament open
See page 263.
218
F TCD filament short
Front TCD filament
shorted
Not ready:
F TCD filament short
See page 264.
219
B TCD filament short
Back TCD filament
shorted
Not ready:
B TCD filament short
See page 264.
220
Heater overcurrent
Heater overcurrent.
Thermal shutdown.
221
Thermal shutdown
Not ready:
See page 264.
222
Oven temp too hot
Oven thermal shutdown
Not ready:
Thermal shutdown
See page 264.
223
Oven temp too cool
Oven thermal shutdown
Not ready:
Thermal shutdown
See page 264.
224
Oven temp sensor
Oven thermal shutdown
Not ready:
Thermal shutdown
See page 264.
225
F det temp too hot
Front detector thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
257
Messages
Part 4. Fault messages
Table 28, continued
Fault no.
Status message
Popup message
Run log
Comments
226
F det temp sensor
Front detector thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
227
B det temp too hot
Back detector thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
228
B det temp sensor
Back detector thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
229
F inl temp too hot
Front inlet thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
230
F inl temp sensor
Front inlet thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
231
B inl temp too hot
Back inlet thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
232
B inl temp sensor
Back inlet thermal
shutdown
Not ready:
Thermal shutdown
See page 264.
233
Aux l temp too hot
Aux 1 thermal shutdown
Not ready:
Thermal shutdown
See page 264.
234
Aux l temp sensor
Aux 1 thermal shutdown
Not ready:
Thermal shutdown
See page 264.
235
Aux 2 temp too hot
Aux 2 thermal shutdown
Not ready:
Thermal shutdown
See page 264.
236
Aux 2 temp sensor
Aux 2 thermal shutdown
Not ready:
Thermal shutdown
See page 264.
237
No line interrupt
No line interrupt
thermal shutdown
Not ready:
Thermal shutdown
238
Line interrupt
Faulty line interrupt
thermal shutdown
Not ready:
Thermal shutdown
239
No mux ADC response
Mux ADC thermal
shutdown
Not ready:
Thermal shutdown
240
Mux ADC offset value
Mux ADC thermal
shutdown
Not ready:
Thermal shutdown
258
Part 4. Fault messages
Messages
Table 28, continued
Fault no.
Status message
Popup message
Run log
241
Invalid line sense
Line sense reading
thermal shutdown
Not ready:
Thermal shutdown
242
Aux3 faulty fact cal
Pneu aux module invalid
constants from factory
calibration
Not ready:
Aux3 faulty fact cal
243
Aux4 faulty fact cal
Pneu aux module invalid
constants from factory
calibration
Not ready:
Aux4 faulty fact cal
244
Aux5 faulty fact cal
Pneu aux module invalid
constants from factory
calibration
Not ready:
Aux5 faulty fact cal
245
F det module rev
Front det module:
obsolete EEPROM
Not ready:
F det module rev
246
B det module rev
Back det module: obsolete
EEPROM
Not ready:
B det module rev
247
F inlet module rev
Front inlet module:
obsolete EEPROM
Not ready:
F inlet module rev
248
B inlet module rev
Back inlet module:
obsolete EEPROM
Not ready:
B inlet module rev
249
Aux module rev
Pres aux module: obsolete
EEPROM
Not ready:
Aux module rev
250
F det wrong module
Front det: non-det module
Not ready:
F det wrong module
251
B det wrong module
Back det: non-det module
Not ready:
B det wrong module
252
F inlet wrong module
Front inlet: non-inlet
module
Not ready:
F inlet wrong module
253
B inlet wrong module
Back inlet: non-inlet
module
Not ready:
B inlet wrong module
254
Aux wrong module
Non-aux module in pneu
aux position
Not ready:
Aux wrong module
Comments
259
Messages
Part 4. Fault messages
Table 28, continued
Fault no.
Status message
Popup message
Run log
255
F det invalid type
Front detector: invalid det
module
Not ready:
F det invalid type
256
B det invalid type
Back detector: invalid det
module
Not ready:
B det invalid type
257
F inlet invalid type
Front inlet: invalid inlet
module
Not ready:
F inlet invalid type
258
B inlet invalid type
Back inlet: invalid inlet
module
Not ready:
B inlet invalid type
259
F det type mismatch
Front detector: det board
not the same as module
Not ready:
F det type mismatch
260
B det type mismatch
Back detector: det board
not the same as module
Not ready:
B det type mismatch
261
MIO board defective
Host communications:
MIO board defective
Not ready:
MIO board defective
262
RS232 defective
Host communications:
RS232 defective
Not ready:
RS232 defective
263
GPIB defective
Host communications:
GPIB defective
Not ready:
GPIB defective
264
Sampler RS232 defect
Sampler communications:
RS232 defective
Not ready:
Sampler RS232 defect
265
F inlet invalid pid
Front inlet: invalid pids
266
B inlet invalid pid
Back inlet: invalid pids
267
F det invalid pid
Front detector:
invalid pids
268
B det invalid pid
Back detector:
invalid pids
269
Pneu aux invalid pid
Pneu aux module:
invalid pids
270
F inlet bad cksum
Front inlet:
invalid module checksum
260
Comments
If you installed a new
detector, check that the new
detector’s electronics board
and module are installed in
the proper locations.
Part 4. Fault messages
Messages
Table 28, continued
Fault no.
Status message
Popup message
Run log
271
B inlet bad cksum
Back inlet: invalid module
checksum
272
F det bad cksum
Front detector: invalid
module checksum
273
B det bad cksum
Back detector: invalid
module checksum
274
Pneu aux bad cksum
Pneu aux module: invalid
module checksum
275
F inlet bad fact cal
Front inlet: invalid
constants from factory
calibration
276
B inlet bad fact cal
Back inlet: invalid
constants from factory
calibration
277
F det bad fact cal
Front detector: invalid
constants from factory
calibration
278
B det bad fact cal
Back detector: invalid
constants from factory
calibration
279
P aux bad fact cal
Pneumatics aux invalid
constants from factory
calibration
280
F inlet i/o failure
281
B inlet i/o failure
282
F det i/o failure
283
B det i/o failure
284
Pneu aux i/o failure
285
F det adjust failure
Front detector offset
adjustment failed
Not ready:
F det adjust failure
286
B det adjust failure
Back detector offset
adjustment failed
Not ready:
B det adjust failure
Comments
261
Messages
Part 4. Fault messages
Fault 202—Hydrogen safety shutdown
An inlet configured for hydrogen gas did not reach the pressure setpoint within
2 minutes. Because hydrogen presents an explosion hazard, the following
occurred:
•
The GC oven fan and heaters are turned off.
•
The oven flaps are fully opened.
•
Both pressure and flow controls are turned off and the control parameters
are flashing when viewed.
•
The small zone heaters for inlets and detectors are turned off and the control
parameter are flashing when viewed.
•
The warning beep continues until the [Clear] key on the keypad is depressed.
•
The oven cannot be turned on unless the instrument is power failed. Turn
the GC power off and on again to restore operation.
The sequence would continue until the fault is fixed. To find the fault, check for
the following possible causes:
262
•
Check the gas supply pressure. Increase the pressure at the initial supply if
it is too low to reach the setpoint.
•
Check for a leak somewhere in the system. Leak test the gas supply tubing,
the inlet, and the inlet column fittings. Leak test procedures are found with
each inlet section.
•
The column may be broken. Use the leak detector to check the column for
leaks and replace the broken column or break off the cracked portion.
•
An inlet proportional control valve may be stuck open or closed because of
contamination or other fault. Contact your Agilent service representative.
Part 4. Fault messages
Messages
Fault 214—Front detector flame out
Fault 215—Back detector flame out
This message appears when the FID or FPD is not able to ignite or if the flame
goes out during a run. During the ignition process or the run, the detector will
try to ignite the flame twice; if both attempts fail, the hydrogen, air, and ignitor
will shut off, and the error message will appear. The detector will be in a not
ready state.
•
Make sure the hydrogen and air are turned on and that the flow rates are
high enough for the flame to ignite.
•
Use an electronic leak detector to search for and correct leaks around the
detector column fitting.
•
See the discussion of your detector in the Detectors volume to make sure
that you are using the correct jet for your column.
•
Change the Lit Offset to 0.5 for the FID or 0.2 for the FPD (the default value).
•
If problem persists, contact your Agilent service representative.
Fault 216—Front TCD filament open
Fault 217—Back TCD filament open
The TCD filament bridge voltage indicates that the filament resistance is too
high (or “open,” in the electrical sense). The resistance may be too high because
the filament is broken or worn thin from use, or the wires from the TCD are not
connected on the detector board, or if the cell temperature sensor (∆PRT) is
shorted.
The detector will not be ready until the condition is corrected.
•
Check that the wires from the detector are connected on the detector board.
•
Check the cell temperature sensor (∆PRT).
•
The TCD cell must be replaced. Contact your Agilent service representative.
263
Messages
Part 4. Fault messages
Fault 218—F TCD filament shorted
Fault 219—B TCD filament shorted
The TCD filament bridge voltage indicates that the resistance of the filament is
too low, indicating a shorted filament. This could be caused by a worn or sagging
filament or if the wires from the TCD (including the cell temperature sensor
wires) are not connected properly to the detector board or are touching each
other.
The detector will not be ready until the condition is corrected.
•
Check that the wires from the cell are connected on the detector board
properly.
•
The TCD cell must be replaced. Contact your Agilent service representative.
Faults 221 to 236—Thermal shutdown
These faults cause the GC to shut down entirely. A thermal fault is detected if
the oven or another heated zone is not within its allowable temperature range
(lower than minimum temperature or greater than maximum temperature by
25°C). Several things could cause this error:
• A problem with the electrical supply to the instrument.
• A malfunction of the zone control electronics.
• A shorted temperature sensor.
• A shorted heater.
No power reaches the oven and other heated zones. The GC is not ready.
Any of the following components can experience a thermal shutdown: the oven,
the inlets, the detectors, and the aux zones. In addition, problems with
electronics on the main PC board can cause a thermal shutdown.
•
264
If you see any thermal shutdown message, turn the GC off and on. If the
error was caused by a power supply problem, the error will disappear and
the instrument will become ready. If the error reappears, the main board or
one or more of the heater/sensor assemblies must be replaced. Contact your
Agilent service representative.
Index
A
Actual value, 18
Adapter
bubble meter, 77
detector
installation, 128
Ambient temp
oven setpoint, 97
Analog
zero, 154
Analog output
attenuation, 156
range, 155
Asterisk, 17
Attenuation, 156
Automatic liquid sampler
7673
bar code reader, 207
components, 202
configuring injector, 206
control table, 204
injector setpoints, 205
sample tray setpoints, 206
7683
bar code reader, 215
components, 209
configuring injector, 214
control table, 211
injector setpoints, 212
sample tray setpoints, 214
Aux # keys, 23
Auxilary temperature programming, 191
Auxiliary channels, 66
B
Back Det key, 23
Back Injector key, 39
Back Inlet key, 23
Bar code reader
with 7673, 207
with 7683, 215
Baseline shifts
digital signal, 157
Batteries, 9
Beep, 18, 34
Bubble meter, 76
C
Calibration
EPC, 70
option, 33
Capillary columns
conditioning, 138
Caution message, 19
Channels
auxiliary, 66
changing frits, 69
ChemStation
signal processing, 159
Clear key, 37
Click
key, 34
Clock Table
LED, 20
Clock Table key, 39
Clock time
adding events, 177
deleting events, 178
editing events, 177
programming, 174, 175
Col Comp n keys, 23
Col n keys, 23
Column
capillary
ferrules, 121
hanger, 100
preparation, 101
compensation, 160
making a run, 162
plotting profile, 164
compensation profile, 162
265
Index
conditioning, 136
configuration, 48
modes, 52
packed
conditioning, 139
packed glass
installation, 133
packed metal
ferrules, 130
fittings, 122
installation, 129
installing ferrules, 127
making a spacer, 125
preparation, 124
selecting mode, 53
size and flow rate, 55
Column shutdown, 43
Communication
option, 33
Compensation
column, 160
profile
creating, 162
Conditioning
capillary columns, 138
column
preliminary steps, 137
columns, 136
packed columns, 139
traps, 140
Config key, 35
Configuration
carrier gas, 51
column, 48
definition, 46
injector
7673, 206
7683, 214
instrument, 35
oven, 86
setpoint status table, 29
266
valve, 194
Constant flow, 52
Constant pressure, 52
Control table
automatic liquid sampler
7673, 204
7683, 211
definition, 3
keyboard and display, 34
sequence, 228
sequence definition, 218
signal, 150
split/splitless inlet, 61
stored sequence, 218
use, 4
Cool on-column inlet
installing capillary columns, 105
Cooling
oven, 97
Creating
method, 181
sampler subsequence, 222
sequence, 222
valve subsequence, 223
Cryo
oven setpoint, 97
Cryo fault
oven setpoint, 98
Cryo shutdown, 98
Cryo timeout
oven setpoint, 98
Cryogenic
oven, 97
Cursor, 17
D
Data rate
ChemStation, 159
INET, 160
Data rates
definition, 157
Index
Date
setting, 30
Default method, 184
Default parameters, 40
Delete key, 37
Deleting
method, 187
sequence, 228
Det Control key, 25
Detector
ECD
plumbing, 64
ECD and µ-ECD
installing capillary columns, 114
FID
installing capillary columns, 109
FID and NPD
plumbing, 62
FPD
installing capillary columns, 118
installing adapters, 128
nonEPC, 73
NPD
installing capillary columns, 109
TCD
installing capillary columns, 113
plumbing, 63
Diagnostics
option, 34
Digital zero, 157
Display, 17
blinking, 18
LED, 20
E
Editing
method, 186
sequence, 227
Electron capture detectors
installing capillary columns, 114
Electronic Pneumatic Control
definition, 42
EPC
calibration, 70
definition, 42, 45
Equilibration time
oven, 86
Error, 19
External Event
connector, 193
F
Fast peaks, 157
Ferrules
capillary columns, 121
glass packed columns, 135
packed metal columns, 130
installing, 127
Final Temp
LED, 20
Final temp
oven programming, 89
Final time
oven programming, 89
Flow
constant, 52
initial, 54
interpretation, 79
measuring with bubble meter, 76
problems, 80
programming, 57
ramped, 52
sensor calibration, 70
Flow key, 24
Front Det key, 23
Front Injector key, 39
Front Inlet key, 23
Fuses, 9
267
Index
G
Gas
carrier flow and column size, 55
configure carrier, 51
Gas sampling valve, 197
Gas Saver
LEDs, 20
Gases
on/off control, 44
Glass columns
installation, 133
H
Hanger
capillary columns, 100
Hydrogen shutdown, 43
I
INET
data rate, 160
Info key, 27
Init temp
oven programming, 89
Init time
oven programming, 89
Initial flow, 54
Initial pressure, 54
Initial Temp
LED, 20
Injector
configuring
7673, 206
configuring 7683, 214
Inlet
cool on-column
installing capillary columns, 105
nonEPC, 72
parameters, 59
PTV
installing capillary columns, 109
268
purged packed
installing capillary columns, 106
split/splitless
control table, 61
installing capillary columns, 103
Volatiles Interface
installing capillary columns, 109
Installing capillary columns
cool on-column inlet, 105
ECD and µ-ECD, 114
FPD, 118
NPD and FID, 109
PTV inlet, 109
purged packed inlet, 106
split/splitless inlet, 103
TCD, 113
Volatiles Interface, 109
Installing packed glass columns, 133
Installing packed metal columns, 129
Isothermal oven, 87
K
Key click, 34
Keyboard, 21
lock, 34
L
Linear velocity, 54
Listing a method, 187
Load key, 39
Loading
default method, 184
default parameters, 40
method, 183
sequence, 226
Lock
keyboard, 34
Index
M
Maintenance, schedule, 10
Manuals, 2
Messages, 19
Method
creating, 181
definition, 180
deleting, 187
editing, 186
listing, 187
loading, 183
loading default, 184
mismatch, 185
storing, 182
Method key, 39
Mode/Type key, 36
N
Nitrogen-phosphorus detector
installing capillary columns, 109
Not Ready
LED, 20
O
Options key, 33
O-ring
glass packed columns, 135
Output
analog, 154
zeroing, 154
Oven
configuration, 86
cryogenic, 97
equilibration time, 86
fast rates, 90
isothermal, 87
maximum temperature, 86
safety, 85
specifications, 84
Oven key, 23
Oven shutdown, 85
P
Packed metal columns
installation, 129
Parameters
default, 40
inlet, 59
Post Run
LED, 20
setting up, 31
Post Sequence, 220, 224
Pre Run
LED, 20
Prep Run key, 22
Preparing capillary columns, 101
Preparing packed metal columns, 124
Pres correct, 50
Pres key, 24
Pressure
auxiliary channels, 66
constant, 52
initial, 54
Normal, 45
problems, 80
program, 57
ramped, 52
selecting units, 34
sensor calibration, 70
Priority sequence, 221
Procedure
Adding events
Clock table, 177
Run table, 171
Changing
Auxiliary channel frit, 69
Conditioning columns
Capillary columns, 138
Packed columns, 139
Preliminary steps, 137
269
Index
Configuring
bar code reader
7673, 207
7683, 215
Capillary column, 49
Carrier gas, 51
injector
7673, 206
7683, 214
Setpoint status table, 29
Valves, 195
Controlling valves from the keyboard,
196
Creating
Column compensation profile, 162
Sampler subsequence, 222
Sequence, 222
Valve subsequence, 223
Deleting
Clock table events, 178
Run table events, 172
Stored method, 187
Stored sequence, 228
Editing
Clock table events, 177
injector setpoints
7673, 205
7683, 212
Run table events, 172
sample tray setpoints
7673, 206
7683, 214
Stored method, 186
Stored sequence, 227
Installing capillary columns
Cool on-column inlet, 105
ECD and µ-ECD, 114
FID, 109
FPD, 118
270
NPD, 109
Preparing the column, 101
PTV inlet, 109
Purged packed inlet, 106
Split/splitless inlet, 103
TCD, 113
Volatiles Interface, 109
Installing packed columns
Detector adapters, 128
Ferrules for metal columns, 127
Glass columns, 133
Making a spacer, 125
Metal columns, 129
Loading
Default method, 184
Default parameters, 40
Stored method, 183
Stored sequence, 226
Pausing and resuming a sequence, 230
Plotting
Column compensation profile, 164
Programming
Clock table events, 174, 175
Column flow, 57
Column pressure, 57
Isothermal oven, 87
Multiple-ramp oven temperature, 92
Run table events, 170
Single-ramp oven temperature, 91
Selecting
Column mode, 53
Fast peaks, 157
Setting, 31
Average linear velocity, 56
Initial flow, 56
Initial pressure, 56
Inlet parameters, 60
Post Run events, 31, 224
Time and date, 30
Index
Starting/running a sequence, 229
Stopping a sequence, 230
Storing
Method, 182
Sequence, 225
Using
Bubble flow meter, 78
Column compensation, 162
Stopwatch, 31
Zeroing
Analog signal, 154
Flow and pressure sensors, 71
Programming
Auxilary temperature zone, 191
clock time, 174, 175
flow, 57
oven temperature, 88
pressure, 57
run time, 168, 170
PTV inlet
installing capillary columns, 109
Purged packed inlet
installing capillary columns, 106
Q
Quick cryo cool
oven setpoint, 97
R
Radix type, 34
Ramp # key, 26
Ramped flow, 52
Ramped pressure, 52
Range
analog output, 155
Rate
data, 157
fast oven, 90
INET, 160
LED, 20
oven programming, 89
Reader
bar code, 207, 215
Remote LED, 20
Run LED, 20
Run Log key, 32
Run Log LED, 20
Run Table key, 39
Run time
adding events, 171
deleting events, 172
editing events, 172
maximum, 89
programming, 168, 170
Running a sequence, 229
S
Sample Tray key, 39
Scrolling, 17
Selecting a column mode, 53
Septum purge
nonEPC, 72
Seq Control key, 39
Seq key, 39
Sequence
aborting, 231
control table, 218, 228
creating, 222
definition, 218
control table, 218
deleting, 228
editing, 227
integrator, 232
loading, 226
pausing & resuming, 230
post, 220
post sequence, 224
priority, 221
sampler subsequence
creating, 222
starting & running, 229
271
Index
stopping, 230
storing, 225
subsequence
definition, 221
valve subsequence
creating, 223
Setpoint
7673
injector, 205
sample tray, 206
7683
injector, 212
sample tray, 214
status table, 29
Setpoint value, 18
Setpoints
oven programming, 89
Setting
Post Run, 31
time and date, 30
Shutdown
column, 43
cryo, 98
hydrogen, 43
oven, 85
Signal
analog, 154
ChemStation, 159
control table, 150
conversion, 151
output scaling, 155
store digital, 158
type, 150
value, 150
zeroing, 154
Signal n keys, 23
Single column compensation, 160
Spacer for packed metal columns, 125
Split/splitless inlet
installing capillary columns, 103
Starting a sequence, 229
272
Status key, 28
Status table, 28
Stop key, 22
Stopping
sequence, 230
Stopwatch, 31
Store key, 39
Storing
method, 182
sequence, 225
Strategy, 8
Stream selection valve, 199
Subsequence
definition, 221
sampler
creating, 222
T
Temp
oven programming, 89
Temp key, 24
Temperature
isothermal, 87
Normal, 45
oven maximum, 86
programmed, 88
Test plot, 164
Thermal conductivity detector
installing capillary columns, 113
Time
setting, 30
Time key, 30
Traps
conditioning, 140
U
Units
pressure, 34
Index
V
Vacuum correct, 50
Value
actual, 18
setpoint, 18
Valve
box, 190
column selection, 197
configuration, 194
control
keyboard, 196
run or clock table, 196
drivers, 192
external drivers, 193
gas sampling, 197
heating, 190
internal drivers, 192
multiposition, 199
stream selection, 199
subsequence
creating, 223
temperature programming, 191
Valve # key, 39
Velocity
average linear, 54
W
Warnings, 11
Z
Zero
analog, 154
digital, 157
flow and pressure sensors, 70
signal output, 154
273
Index
274
Was this manual useful for you? yes no
Thank you for your participation!

* Your assessment is very important for improving the work of artificial intelligence, which forms the content of this project

Download PDF

advertisement