Agilent Technologies 6890 Series User manual

Operating Manual
Volume 3. Detectors
Agilent 6890 Series Gas
Chromatograph

Agilent Technologies Inc.
2850 Centerville Road
Wilmington DE 19808-1610
Agilent Technologies 2000
All rights reserved.
Reproduction adaptation or
translation without permission
is prohibited except as allowed
under the copyright laws.
Part No. G1530-90467
First edition Jan 2000
Replaces Part No. G1530-90460
Operating Manual Volume 3.
Printed in USA
The information contained in
this document is subject to
change without notice.
HP® is a registered trademark
of Hewlett-Packard Co.
Microsoft® Windows® and
Windows NT® are registered
trademarks of Microsoft
Corporation.
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 radio-active
hazard.
Indicates explosion
hazard.
Electromagnetic
Compatibility
This device complies with the
requirements of CISPR 11.
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.
Sound Emission
Certification for
ederal 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
i
Chapter 1. Using Detectors
Using hydrogen.......................................................................................................................... 2
Procedure: Setting up detector control tables...................................................................... 3
Makeup gas flow........................................................................................................................ 6
Makeup gas and EPC detectors .........................................................................................6
Procedure: Defining the makeup gas .............................................................................7
Procedure: Changing makeup gas flow mode ...............................................................7
Makeup gas and nonEPC detector.....................................................................................8
Maximum flow rates ................................................................................................................. 9
[Det Control] shortcut key ..................................................................................................... 10
Chapter 2. The lame Ionization Detector
Part 1. General Information
FID pneumatics........................................................................................................................ 12
Special considerations............................................................................................................ 13
Conditions that prevent the detector from operating ...................................................13
Detector shutdown ............................................................................................................13
Jets............................................................................................................................................. 14
Automatic reignition—Lit offset............................................................................................ 15
Procedure: Changing the auto-reignite setpoint .........................................................15
Electrometer ............................................................................................................................ 16
Data rates............................................................................................................................16
Procedure: Using fast peaks ..........................................................................................16
Part 2. Operating the ID
Gas pressures........................................................................................................................... 18
Operating with EPC................................................................................................................. 19
Procedure: Using the FID with EPC .............................................................................20
Operating without EPC........................................................................................................... 21
Procedure: Using the FID without EPC .......................................................................22
Part 3. Checkout Conditions and Chromatogram
FID checkout conditions ........................................................................................................ 24
Typical FID checkout chromatogram................................................................................... 26
Part 4. Maintaining a lame Ionization Detector
Correcting FID hardware problems...................................................................................... 28
Replacing or cleaning the jet.................................................................................................. 28
Procedure: Removing and inspecting the jet ...............................................................29

ii
Contents
Procedure: Cleaning the jet ........................................................................................... 32
Procedure: Installing the jet .......................................................................................... 33
Cleaning the collector............................................................................................................. 35
Procedure: Removing the collector .............................................................................. 36
Procedure: Cleaning the collector ................................................................................ 38
Procedure: Reassembling the detector ........................................................................ 39
Procedure: Replacing the FID ignition wire ....................................................................... 40
Part 5. The Nickel Catalyst Tube
Gas flows.................................................................................................................................. 44
Temperature............................................................................................................................. 45
Repacking the catalyst............................................................................................................ 45
Chapter 3. The Thermal Conductivity Detector
Part 1. General Information
TCD pneumatics...................................................................................................................... 52
Conditions that prevent the detector from operating......................................................... 53
Filament passivation............................................................................................................... 54
Carrier reference and makeup gas...................................................................................... 54
Negative polarity ..................................................................................................................... 55
Analyzing for hydrogen........................................................................................................... 55
Part 2. Operating the TCD
Gas pressures........................................................................................................................... 57
Operating with EPC ................................................................................................................ 58
Procedure: Using the TCD with EPC ........................................................................... 59
Operating without EPC........................................................................................................... 60
Procedure: Using the TCD without EPC ...................................................................... 61
Part 3. Checkout Conditions and Chromatogram
TCD checkout conditions....................................................................................................... 63
Typical TCD checkout chromatogram ................................................................................. 65
Part 4. Maintaining a Thermal Conductivity Detector
Correcting TCD performance problems............................................................................... 66
Procedure: Thermal cleaning................................................................................................ 66

Contents
iii
Chapter 4. The Nitrogen-Phosphorus Detector
Part 1. General Information
Software requirements............................................................................................................ 70
NPD pneumatics...................................................................................................................... 71
Conditions that prevent the NPD from operating ............................................................... 72
Gas purity ................................................................................................................................. 72
The bead ................................................................................................................................... 73
Adjust offset........................................................................................................................73
Aborting adjust offset........................................................................................................75
Turning off the detector....................................................................................................75
Setting adjust offset on the clock table...........................................................................75
Equilibration time ..............................................................................................................75
Procedure: Changing equilibration time ......................................................................76
Turning hydrogen off during a solvent peak ..................................................................76
Turning hydrogen off between runs................................................................................76
Bead voltage .......................................................................................................................76
Extending the life of the bead ..........................................................................................77
Temperature programming .................................................................................................... 77
Electrometer ............................................................................................................................ 78
Data rates............................................................................................................................78
Procedure: Setting data rate for NPD ...........................................................................78
Jets and collectors................................................................................................................... 79
Part 2. Operating the NPD
Gas pressures........................................................................................................................... 81
Operating with EPC ............................................................................................................... 82
Procedure: Using the NPD with EPC ...........................................................................83
Operating without EPC........................................................................................................... 84
Procedure: Using the NPD without EPC ......................................................................85
Part 3. Checkout Conditions and Chromatogram
NPD checkout conditions....................................................................................................... 87
NPD checkout chromatogram ............................................................................................... 89
Part 4. Maintaining a Nitrogen-Phosphorus Detector
NPD illustrated parts breakdown.......................................................................................... 90
Correcting NPD hardware problems .................................................................................... 91
Procedure: Replacing the bead assembly............................................................................ 93
Procedure: Cleaning detector and collector; changing insulators and rings.................. 99
Replacing or cleaning the jet................................................................................................ 107
Procedure: Removing and inspecting the jet .............................................................108

iv
Contents
Procedure: Cleaning the jet ......................................................................................... 110
Procedure: Replacing the jet and reassembling the detector ................................. 111
Chapter 5. The Electron Capture Detector
Part 1. Regulatory and Safety Information
The 63Ni isotope .................................................................................................................... 115
ECD licenses.......................................................................................................................... 115
Specific License ............................................................................................................... 115
General License................................................................................................................ 115
ECD warnings........................................................................................................................ 116
Safety precautions when handling ECDs........................................................................... 118
Part 2. General Information
Detector pneumatics............................................................................................................. 119
Sensitivity............................................................................................................................... 120
Linearity.................................................................................................................................. 121
Gases....................................................................................................................................... 121
Temperature........................................................................................................................... 121
Electrometer .......................................................................................................................... 121
Adjust offset........................................................................................................................... 122
Aborting adjust offset...................................................................................................... 123
Reference current.................................................................................................................. 123
Output—pulse interval ......................................................................................................... 124
Part 3. Operating the ECD
Gas pressures......................................................................................................................... 126
Operating with EPC .............................................................................................................. 127
Procedure: Using the ECD with EPC ......................................................................... 128
Operating without EPC......................................................................................................... 129
Procedure: Using the ECD without EPC ................................................................... 130
Part 4. Checkout Conditions and Chromatogram
ECD checkout conditions .................................................................................................... 132
Typical ECD checkout chromatogram............................................................................... 134
Part 5. Maintaining the Detector
Correcting performance problems...................................................................................... 136
Procedure: Checking for gas leaks..................................................................................... 138
Procedure: Thermal cleaning.............................................................................................. 139
Performing a wipe test (radioactivity leak test)................................................................ 142

Contents
v
Chapter 6. The Micro-Cell Electron Capture Detector
Part 1. Regulatory and Safety Information
The 63Ni isotope..................................................................................................................... 145
ECD licenses .......................................................................................................................... 145
Specific License................................................................................................................145
General License................................................................................................................145
µ-ECD warnings..................................................................................................................... 146
Safety precautions when handling µ-ECDs........................................................................ 148
Part 2. General Information
Linearity.................................................................................................................................. 149
Detector gas ........................................................................................................................... 150
Temperature........................................................................................................................... 150
Electrometer .......................................................................................................................... 150
Part 3. Operating the µ-ECD
Procedure: Operating the µ-ECD........................................................................................ 152
Part 4. Checkout Conditions and Chromatogram
µ-ECD checkout conditions ................................................................................................. 154
Typical µ-ECD checkout chromatogram............................................................................ 156
Part 5. Maintaining the Detector
Correcting performance problems...................................................................................... 158
Checking for gas leaks.......................................................................................................... 160
Thermal cleaning ................................................................................................................... 162
Performing a wipe test (radioactivity leak test)................................................................ 164
Chapter 7. The lame Photometric Detector ( PD)
Part 1. General Information
Linearity.................................................................................................................................. 166
Quenching effects.................................................................................................................. 167
PMT saturation ...................................................................................................................... 168
Optical filters.......................................................................................................................... 168
Fused silica liner.................................................................................................................... 168
Conditions that prevent the detector from operating....................................................... 168
Detector shutdown................................................................................................................ 169
Compatibility requirements.................................................................................................. 169
The dual wavelength FPD .................................................................................................... 169

vi
Contents
Part 2. Using the Detector
Detector temperature considerations................................................................................. 171
Heater configuration............................................................................................................. 171
Lit offset.................................................................................................................................. 172
Procedure: Changing the Lit offset setpoint .............................................................. 172
Flame ignition sequence....................................................................................................... 173
Lighting the flame.................................................................................................................. 174
Electrometer on/off............................................................................................................... 174
Electrometer data rates........................................................................................................ 175
Procedure: Using fast peaks ............................................................................................... 175
Operating the FPD................................................................................................................. 176
Procedure: Using the FPD ............................................................................................ 178
Part 3. Checkout Conditions and Chromatogram
FPD checkout conditions..................................................................................................... 179
Typical FPD checkout chromatograms.............................................................................. 181
Part 4. Maintaining the Detector
Flame ignition problems....................................................................................................... 182
Changing wavelength filters................................................................................................. 183
Leak testing............................................................................................................................ 184
Parts identification................................................................................................................ 185
Cleaning/replacing windows filters and seals ................................................................. 189
Cleaning/replacing the jet..................................................................................................... 191
Replacing the transfer line fused silica liner ..................................................................... 193
Replacing the photomultiplier tube .................................................................................... 196

1
Using Detectors

2
Chapter 1
Using Detectors
The 6890 Series gas chromatograph (the GC) has several detector systems
available. Others will be added in the future. See your Agilent sales
representative for the latest information.
Using hydrogen
WARNING When using hydrogen (H2) as the carrier gas or fuel gas be aware that hydrogen
(H2) gas can flow into the oven and create an explosion hazard. Therefore be
sure that the supply is off until all connections are made and ensure that the
inlet and detector column fittings are either connected to a column or capped
at all times when hydrogen (H2) gas is supplied to the instrument.
WARNING Hydrogen (H2) is flammable. Leaks when confined in an enclosed space may
create a fire or explosion hazard. In any application using hydrogen (H2) leak
test all connections lines and valves before operating the instrument. Always
turn off the hydrogen (H2) supply at its source before working on the instrument.
Name Sensitivity Responds to Comments
Thermal conductivity,
TCD Medium Everything except the carrier gas The “Universal Detector” for everything
lame ionization,
ID High Almost all organic compounds The “Universal Detector" for organics
Electron capture,
ECD and µ-ECD Very high Limited range of compounds, mostly
halocarbons
Used for trace level pesticide
and herbicide analysis
Nitrogen-phosphorus,
NPD Very high Compounds with nitrogen or phosphorus Used in pharmaceutical and environmental analysis
lame photometric,
PD High Compounds with sulfur or phosphorus Used in environmental and bioscience analysis

3
Using Detectors
Procedure: Setting up detector control tables
Procedure: Setting up detector control tables
You must be familiar with this set of control tables to operate your detector.
Follow these three steps when setting up all types of detectors.
1. Check your column configuration. (This is normally done when you set up
your inlet but it does not hurt to check this information again.)
• You must tell the instrument which detector your column is connected
to front or back. If you have only one detector it is best to have only
one column configured to it—unless you actually do have two columns
attached to that detector.
• If you have an EPC inlet and detector and are using a capillary column
you must enter the column length and diameter if you want to have a
choice of makeup gas flow modes. This is called column defined. If you
do not enter these values it is called column not defined and your
control choices are limited.
1. Press [Config] [Col 1] or [Config] [Col 2]:
Press [Mode/Type]
2. Scroll to Detector: Press [ ront] or [Back] or
Press [Mode/Type] and choose Front or Back
3. Enter column dimensions, if necessary.

Using Detectors
Procedure: Setting up detector control tables
4
2. Check your detector configuration (makeup gas type).
The main reason for doing this is to verify that the makeup gas entered (or
makeup and anode gas on the ECD reference and makeup on the TCD) is
the same as the gas plumbed to your detector.
This is important because:
• When the actual and configured gas types are different for an EPC detec-
tor the calculated flow rate is not correct and the flow rate stability is
affected.
• The electronics for some detectors change depending on the gas type
configuration. The detector does not operate properly when the actual
and configured gas types are different.
• Good laboratory practice. Keep a record of the gas used.
Most of the detectors have other configurable items. These will be described
later in this section.
3. Set up your detector control table. The following is a brief description of
each line item for the FID. If you have EPC flow setpoints (right number)
and actual values (left number) are displayed. NonEPC detectors have
on/off control.
Press [ ront Det] or [Back Det].
EPC (column not de ined) NonEPC

5
Using Detectors
Procedure: Setting up detector control tables
FRONT DET (FID) The title indicates the detector position and the type
of detector installed.
Temp This is where you set the temperature. The control is identical on
EPC and nonEPC detectors and includes setpoint (right number) and actual
(left number) values.
H2 flow, Air flow These are the detector gases for the FID.
Mkup (N2) This is where you set your makeup gas flows. The gas type is
displayed in parentheses. The lines of the display vary depending on your
instrument and the way you have configured it.
Flame This is the on/off control for the FID—also called the Detector
Control line. Each detector has its own type of on/off control.
Output This is the actual detector output value. You cannot enter a
setpoint here.

Using Detectors
Makeup gas low
6
Makeup gas flow
Makeup gas enters the detector close to the end of the column. Its purpose is to
speed the peaks through the detector—especially with capillary columns—so
that the peak separation achieved by the column is not lost through remixing in
the detector.
Makeup gas and EPC detectors
The makeup gas line of your detector control table changes depending on your
instrument configuration.
If you have a nonEPC inlet or an EPC inlet with the column not defined, the
makeup flow is constant. The control table for the EPC detector looks like this:
If you have an EPC inlet configured to your detector and you are operating with
column defined you have a choice of two makeup gas modes.
The Const makeup mode provides a constant flow of makeup gas to the
detector. If you choose it your control table looks like this:
You can enter a flow or press
[On] to get the default flow.
You can enter a flow or press
[On] to get the default flow.

7
Using Detectors
Makeup gas low
The Col+mkup=const mode provides a variable flow of makeup gas to the
detector. As column flow increases or decreases the makeup flow changes to
provide a constant combined flow to the detector. If you choose this option
enter a value under Combined flow. The Combined flow line always
displays the same value while the Mkup line of the control table changes as the
actual makeup flow changes.
Procedure: De ining the makeup gas
Procedure: Changing makeup gas low mode
You can enter a flow or press
[On] to get the default flow.
This number will change as flow
from the column changes.
1. Press [Config] [ ront Det] or
[Config] [Back Det]: 2. Scroll to Mkup gas type and press [Mode/Type].
3. Scroll to the correct gas and press [Enter].
1. Scroll to Mode: 2. Press [Mode/Type].
3. Choose a flow mode and press [Enter].

Using Detectors
Makeup gas low
8
Makeup gas and nonEPC detector
If you have a nonEPC detector your makeup gas must be measured and adjusted
manually from a pressure regulator located in the pneumatics carrier. The control table
only displays one flow mode — On/Off.
NonEPC detector makeup gas low mode
Turn the gas on or off.

9
Using Detectors
Maximum low rates
Maximum flow rates
The maximum flow rates that can be set with EPC detectors are:
Detector and gas Maximum low rate, mL/min
lame ionization
Hydrogen 100
Air 800
Makeup (nitrogen, helium, argon) 100
Thermal conductivity
Nitrogen reference 100; makeup 10
Helium reference 100; makeup 12
Hydrogen reference 100; makeup 18
Argon reference 100; makeup 10
Electron capture
Nitrogen anode purge 12; makeup 200
Argon/methane anode purge 12; makeup 200
Nitrogen-phosphorus
Hydrogen 30
Air 200
Makeup (nitrogen, helium, argon) 100
lame photometric
Hydrogen 250
Air 200
Makeup (nitrogen, helium, argon) 130

Using Detectors
[Det Control] shortcut key
10
[Det Control] shortcut key
This is another way to open a Detector control table. Press [Front Det] [Det
Control] or [Back Det] [Det Control] to open a Detector control table. If you
have only one detector [Det Control] opens that table.
When you use [Det Control] your table opens at the On/Off control for your
detector—FID and FPD Flame, TCD Filament NPD and ECD Adjust
offset.
Press [Det Control]
Turns the detector on or off

2
The lame Ionization
Detector