Agilent Technologies 6890 Series User manual

Operating Manual
Volume 2. Inlets
Agilent 6890 Series Gas
Chromatograph

Agilent echnologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610
Agilent echnologies 2000
All rights reserved.
Reproduction, adaptation, or
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is prohibited, except as allowed
under the copyright laws.
Part No. G1530-90457
First edition, Jan 2000
Replaces Part No. G1530-90450
Operating Manual Volume 2.
Printed in USA
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Safety information
he 6890 Gas Chromatograph
meets the following IEC
(International Electrotechnical
Commission) classifications:
Safety Class 1, ransient
Overvoltage Category II, and
Pollution Degree 2.
his 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. he customer should
not attempt to replace the
battery or fuses in this
instrument. he 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 echnologies 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
his device complies with the
requirements of CISPR 11.
Operation is subject to the
following two conditions:
1. his device may not cause
harmful interference.
2. his 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
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 echnologies,
or an experienced technician
for assistance.
7. Changes or modifications not
expressly approved by
Agilent echnologies 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 ( ype
est)
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 . 19
( ypprüfung)
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. Introduction to Inlets
Inlet types....................................................................................................................................2
Using hydrogen...........................................................................................................................2
Procedure: Pressure units: Select psi, kPa, bar .....................................................................5
The inlet and column control tables ........................................................................................6
The column control tables.........................................................................................................
The column control table—defined capillary columns...................................................
The column control table—packed or undefined capillary columns............................9
What is gas saver?.....................................................................................................................11
Procedure: Using gas saver............................................................................................. 12
Pre Run and Prep Run..............................................................................................................13
The [Prep Run] key............................................................................................................13
Procedure: Auto Prep Run.............................................................................................. 14
Septum purge............................................................................................................................15
Chapter 2. The Split/Splitless Inlet
Part 1. Using a Split/Splitless Inlet .................................................................... 18
Standard and high-pressure versions.....................................................................................18
Septum tightening ..............................................................................................................18
Liners..........................................................................................................................................19
Procedure: Changing the liner........................................................................................ 19
Split mode pneumatics ............................................................................................................21
The control table—split operation.........................................................................................22
Procedure: Using the split mode with the column defined ........................................ 23
Procedure: Using the split mode with the column not defined ................................. 24
Splitless mode pneumatics......................................................................................................25
The control table—splitless operation ..................................................................................26
Operating parameters ..............................................................................................................2
Procedure: Using splitless mode with the column defined ........................................ 28
Procedure: Using splitless mode with the column not defined ................................. 29
Pulsed split and splitless modes.............................................................................................30
The control table—pulsed split mode....................................................................................31
Procedure: Using the pulsed split mode ....................................................................... 32
The control table—pulsed splitless operation......................................................................33
Procedure: Using the pulsed splitless mode................................................................. 34

ii
Contents
Part 2. Maintaining a split/splitless inlet .......................................................... 35
Changing septa ......................................................................................................................... 36
Procedure: Changing the septum................................................................................... 3
Changing the O-ring ................................................................................................................. 39
Procedure: Changing the O-ring..................................................................................... 40
Replacing the inlet base seal...................................................................................................42
Procedure: Replacing the inlet base seal...................................................................... 43
Replacing the split vent trap filter cartridge ................................................................. 45
Procedure: Leak testing the gas plumbing .......................................................................... 46
Procedure: Leak testing an EPC split/splitless inlet .......................................................... 4
Procedure: Leak testing a nonEPC split/splitless inlet ...................................................... 49
Procedure: Correcting leaks........................................................................................... 51
Procedure: Cleaning the inlet ............................................................................................... 52
Chapter 3. The Purged Packed Inlet
Part 1. Using a Purged Packed Inlet .................................................................. 5
Liners and inserts ..................................................................................................................... 55
Procedure: Installing liners ............................................................................................ 56
Procedure: Installing glass inserts................................................................................. 58
The control table ...................................................................................................................... 61
Packed columns or column not defined......................................................................... 61
Defined capillary columns................................................................................................ 61
Procedure: Using packed and undefined capillary columns...................................... 62
Procedure: Using defined capillary columns ............................................................... 62
Part 2. Maintaining a Purged Packed Inlet ....................................................... 63
Procedure: Changing septa ................................................................................................... 64
Procedure: Changing the O-ring ........................................................................................... 6
Procedure: Leak testing the gas plumbing .......................................................................... 69
Procedure: Leak testing an EPC purged packed inlet ....................................................... 69
Procedure: Leak testing a nonEPC purged packed inlet ................................................... 2
Procedure: Correcting leaks ................................................................................................. 3
Procedure: Cleaning the inlet ............................................................................................... 4

Contents
iii
Chapter . The Cool On-Column Inlet
Part 1. Using a Cool On-Column Inlet ............................................................... 78
Hardware ................................................................................................................................... 9
Automatic or manual injection with septum nut..................................................................81
Septum nuts........................................................................................................................81
Septa ....................................................................................................................................81
Manual injection with a cooling tower and duckbill septum..............................................82
Procedure: Changing the septum nut or cooling tower and septum ...............................83
Procedure: Installing an insert ..............................................................................................84
Procedure: Check the needle-to-column size .....................................................................85
Procedure: Manual injection with septum nut ....................................................................86
Procedure: Manual injection with cooling tower ...............................................................86
Retention gaps ..........................................................................................................................88
Inlet temperature......................................................................................................................88
CryoBlast (optional)..........................................................................................................88
Track oven mode ...............................................................................................................88
Temperature programming mode....................................................................................88
Cryogenic considerations .................................................................................................89
Setpoint ranges...................................................................................................................89
Procedure: Programming the temperature................................................................... 90
Procedure: Operating the cool on-column inlet .................................................................91
Part 2. Maintaining a Cool On-Column Inlet ..................................................... 92
Cool on-column inlet hardware problems.............................................................................94
The inlet cools very slowly ...............................................................................................94
The inlet is unable to reach a temperature setpoint......................................................94
The syringe needle bends during injections ...................................................................94
Procedure: Replacing the fused silica syringe needle .......................................................95
Procedure: Installing a fused silica needle ..........................................................................96
Changing septa..........................................................................................................................9
Procedure: Changing septa............................................................................................. 98
Procedure: Cleaning the inlet ..............................................................................................100
Procedure: Leak testing the gas plumbing ........................................................................103
Procedure: Leak testing a cool on-column inlet ...............................................................104
Procedure: Correcting leaks ...............................................................................................105

iv
Contents
Chapter 5. The Programmable Temperature Vaporization Inlet
Part 1. Introducing the Agilent PTV ................................................................ 108
Operating modes .................................................................................................................... 108
System requirements .............................................................................................................108
System components...............................................................................................................109
Sampling heads ................................................................................................................ 110
Heating the inlet ..................................................................................................................... 111
Additional temperature ramps.......................................................................................111
Cooling the inlet ..................................................................................................................... 112
Configuring the PTV ........................................................................................................ 112
Shutdown behavior.......................................................................................................... 113
Part 2. Using the Split Modes ........................................................................... 115
Flow pattern............................................................................................................................ 115
Temperature considerations................................................................................................. 116
Cold split introduction .................................................................................................... 116
Hot split introduction...................................................................................................... 116
Control table parameters—split mode operation .............................................................. 11
Procedure: Using split mode with the column defined............................................. 11
Procedure: Using split mode with the column not defined...................................... 118
Pulsed modes.......................................................................................................................... 120
Control table parameters—pulsed split mode.................................................................... 121
Procedure: Using pulsed split mode with the column defined................................ 122
Procedure: Using pulsed split mode with the column not defined ......................... 123
Part 3. Using the Splitless Modes .................................................................... 12
Flow patterns.......................................................................................................................... 124
Temperature considerations................................................................................................. 128
Cold splitless introduction ............................................................................................. 128
Hot splitless introduction ............................................................................................... 128
Control table parameters—splitless operation .................................................................. 129
Starting values.................................................................................................................. 129
Procedure: Using splitless mode with the column defined...................................... 131
Procedure: Using splitless mode with the column not defined............................... 132
Pulsed splitless mode operation........................................................................................... 133
Control table parameters—pulsed splitless operation ............................................... 133
Procedure: Using pulsed splitless mode with the column defined ......................... 134
Procedure: Using pulsed splitless mode with the column not defined................... 135

Contents
v
Part . Using the Solvent Vent Mode ............................................................... 136
Flow patterns..........................................................................................................................136
Temperature, pressure, and flow considerations...............................................................138
Sequence of operations..........................................................................................................139
Timelines .................................................................................................................................140
When is Start Run? .................................................................................................................141
Control table parameters—solvent vent operation............................................................141
Procedure: Using solvent vent mode with the column defined ............................... 143
Procedure: Using solvent vent mode with the column not defined ........................ 144
Large volume injection ..........................................................................................................145
Gas chromatograph requirements .................................................................................145
Automatic sampler requirements...................................................................................145
ChemStation requirements .............................................................................................146
Calculated values.............................................................................................................14
Possible adjustments.......................................................................................................151
Part 5. Maintaining a PTV ................................................................................. 15
Inlet adapters ..........................................................................................................................154
Procedure: Replacing inlet adapters ........................................................................... 154
Procedure: Installing columns ............................................................................................155
The septumless head..............................................................................................................156
Procedure: Removing the septumless head................................................................ 156
Procedure: Cleaning the septumless head.................................................................. 15
Procedure: Replacing the Teflon ferrule..................................................................... 159
The septum head ....................................................................................................................160
Procedure: Removing the septum head ...................................................................... 160
Procedure: Changing the septum................................................................................. 162
Glass inlet liners .....................................................................................................................163
Procedure: Replacing liners.......................................................................................... 164
Replacing the split vent trap filter cartridge................................................................ 166
Procedure: Leak testing the gas plumbing .........................................................................16
Procedure: Leak testing the PTV inlet ................................................................................168
Correcting leaks ...............................................................................................................1 1
Potential leak points........................................................................................................1 1
Consumables and replaceable parts ....................................................................................1 2

vi
Contents
Chapter 6. The Volatiles Interface
Part 1. Using a volatiles interface ................................................................... 176
Split mode ............................................................................................................................... 1
Understanding the pneumatics...................................................................................... 1 8
Using the control table.................................................................................................... 1 8
Operating parameters...................................................................................................... 180
Split ratio .......................................................................................................................... 180
Procedure: Operating in the split mode with the column defined .................................181
Procedure: Operating in the split mode with the column not defined.................... 182
Splitless mode......................................................................................................................... 183
Understanding the pneumatics ...................................................................................... 183
Using the control table.................................................................................................... 184
Operating parameters...................................................................................................... 18
Procedure: Operating in the splitless mode ............................................................... 188
Direct mode............................................................................................................................. 189
Understanding the pneumatics ...................................................................................... 189
Preparing your interface for direct sample introduction ........................................... 191
Procedure: Disconnecting the split vent line ............................................................. 191
Procedure: Configuring for a direct injection ............................................................ 194
Using the control table.................................................................................................... 194
Operating parameters...................................................................................................... 196
Procedure: Operating in direct mode.......................................................................... 196
Part 2. Maintaining a Volatiles Interface ........................................................ 197
Procedure: Installing columns ............................................................................................ 198
Procedure: Replacing or cleaning the interface ............................................................... 203
Replacing the split vent trap filter cartridge ............................................................... 206
Procedure: Leak testing the gas plumbing ........................................................................ 20
Procedure: Leak testing the system ................................................................................... 208
Procedure: Preparing the interface for a leak test ........................................................... 210
Procedure: Correcting leaks ............................................................................................... 211
Part 3. Connecting to an External Gas Sampler ............................................. 212
Procedure: Connecting the 694 headspace sampler ...................................................... 213
Procedure: Connecting the 695 purge and trap concentrator ...................................... 21

Contents
vii
Chapter 7. NonEPC Inlets
Purged packed inlet................................................................................................................222
Split/splitless inlet—split mode............................................................................................222
Split/splitless inlet—splitless mode .....................................................................................222
Configuration ..........................................................................................................................222
Procedure: Configuring a nonEPC inlet...................................................................... 223
Inlet control tables .................................................................................................................224
Column control tables............................................................................................................225
Procedure: Setting carrier flow for the purged packed inlet ..........................................225
Procedure: Setting flows for the split mode inlet .............................................................226
Procedure: Setting flows for the splitless mode ...............................................................22
Chapter 8. The Pneumatics Control Module
Using a Pneumatics Control Module....................................................................................232
Operating the PCM .................................................................................................................234
With an inlet......................................................................................................................234
With a valve or other device ...........................................................................................235
The control tables...................................................................................................................236
Packed column or column not defined .........................................................................236
Defined capillary columns ..............................................................................................23
Procedure: Using packed and undefined capillary columns ............................................23
Procedure: Using defined capillary columns .....................................................................238
Maintaining a PCM .................................................................................................................239
Procedure: Leak testing the gas plumbing ........................................................................239
Materials needed: .............................................................................................................239
Appendix A GC Operating Information
Preparing for analysis ............................................................................................................242
To configure the carrier gas..................................................................................................243
To select a column mode.......................................................................................................244
To set the initial flow or pressure or average linear velocity ...........................................245
To enter a pressure or flow program ...................................................................................246

viii
Contents

1
Introduction to Inlets

2
Chapter 1
Introduction to Inlets
Inlet types
he 6890 GC has five types of inlets available. All are offered with electronic
pneumatics control (EPC) and two are offered without.
Table 1 Inlet Types
Using hydrogen
WARNING When using hydrogen (H2), as the carrier gas, be aware that hydrogen (H2) gas
can flow into the oven and create an explosion hazard. herefore, 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.
Inlet type Gas control
Split/splitless EPC and nonEPC
Purged packed EPC and nonEPC
Cool on-column EPC only
Programmed temperature vaporization EPC only
Volatiles interface EPC only

3
Introduction to Inlets
Using hydrogen
Table 2 An Overview of Inlets
Inlet Column Mode
Sample
concentration Comments Sample to column
Split/splitless Capillary Split
Pulsed split
Splitless
Pulsed splitless
igh
igh
Low
Low
May be useful with large
injections
Useful with large injections
Very little
Very little
All
All
Cool
on-column Capillary n/a Low or labile Minimal discrimination
and decomposition
All
Purged
packed Packed
Large capillary
n/a
n/a
Any
Any OK if resolution not critical
All
All
Programmed
temperature
vaporization
Capillary Split
Pulsed split
Splitless
Pulsed splitless
Solvent vent
igh
igh
Low
Low
Low Multiple injections concentrate
analytes and
vent solvent
Very little
Very little
All
All
Most
Vo la t il es
interface Capillary Direct
Split
Splitless
Low
igh
Low
Lowest dead volume
Max flow = 100 mL/min
All
Very little
All

Introduction to Inlets
Using hydrogen
4
Table 3 Column Size and Carrier Gas low Rate
Column type Column size Carrier gas flow rate
ydrogen elium
Packed 1/8 inch 30
1/4 inch 60
Capillary 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.

5
Introduction to Inlets
Procedure: Pressure units: Select psi, kPa, bar
Procedure: Pressure units: Select psi, kPa, bar
You can display pressure in psi, bar, or kPa. o check the units you are using,
pressing the [Info] key while the cursor is on the Pressure line of a control table.
o change the display units:
Table 4 Pressure Unit Conversions
To convert to Multiply by
psi bar 0.0689476
kPa 6.89476
bar psi 14.5038
kPa 100
kPa psi 0.145038
bar 0.01
1. Press [Options].
2. Scroll to Keyboard & Display and press [Enter].
3. Scroll to Pressure units: and press [Mode/Type].
4. Choose a new pressure unit and press [Enter].

Introduction to Inlets
The inlet and column control tables
6
The inlet and column control tables
he tables for the inlet and column are interrelated. If you set a pressure at the
column control table, that same pressure setting is active on the inlet control
table, and vice versa. Although pneumatics can be controlled from either the
column or the inlet, the column should be considered first.
Note that the pressure readings—both setpoint and actual—are identical on the
column and inlet control tables.

7
Introduction to Inlets
The column control tables
The column control tables
he control tables change depending on your column configuration. he next
few pages describe the column control tables for the two types of columns,
capillary and packed.
The column control table—defined capillary columns
If your column is defined, your control table will be similar to Figure 1.
The title his heading identifies the column—Column 1 or Column 2— and
the type of carrier gas configured to the inlet (in parentheses).
Dim his line shows the column dimensions you have specified. Column length
is in meters (m) and column inside diameter is in microns (µ).
Pressure, flow, and velocity are related. If the column is defined, enter any one
of them and the GC computes and displays the other two.
Pressure he setpoint appears at the far right. he number at the left shows
the actual pressure value. When you enter a pressure value, the values for flow
and average linear velocity are calculated and displayed.
Flow If you enter a flow (in mL/min) here, pressure and velocity are calculated
and adjusted.
Velocity If you enter average linear velocity (in cm/sec), pressure and flow
are calculated.
Mode: here are four column modes: constant flow, constant pressure,
ramped flow, and ramped pressure. o change the mode, scroll to Mode: and
press [Mode/ ype].
he “Flow and Pressure Control” chapter of the General Information volume
explains how to set pressure and flow programs.

Introduction to Inlets
The column control tables
8
igure 1 Column display — defined capillary columns
Press [Col 1] or [Col 2]
Carrier gas type
Column dimensions
Actual pressure
Pressure setpoint
Column flow (mL/min)
—actual and setpoint
Calculated average linear
velocity (cm/sec)
—actual and setpoint
Press [Mode/Type]
Mode: Your control table also has one of these, depending on Mode:

9
Introduction to Inlets
The column control tables
The column control table—packed or undefined capillary columns
If you have not defined your column or if your inlet selection is Unspecified,
your column control table will be similar to Figure 2.
The title his heading identifies the column—Column 1 or Column 2— and
the type of carrier gas configured to the inlet (in parentheses).
Dimensions unknown his line tells you that you have not defined your
column.
Pressure he split/splitless inlet and the cool on-column inlet are pressure
controlled. Because the column is unknown, flow and average linear velocity
cannot be computed.
he purged packed inlet is flow controlled. he actual pressure is displayed, but
is not controllable by the user.
Mode:You have a choice of three modes if using a split/splitless or cool on-
column inlet—constant pressure, constant flow, and ramped flow. he packed
inlet gives you only the two flow modes—constant and ramped.
he “Flow and Pressure Control” chapter of the General Information volume
explains how to set pressure and flow programs.

Introduction to Inlets
The column control tables
10
igure 2 Column display — Packed or undefined capillary columns
Split/splitless or cool on-column inlets
Carrier gas type
Indicates that your column is not defined
Pressure (in psi, bar, or KPa)
Press [Mode/Type]
Purged packed inlet
Carrier gas type
Indicates that your column is not defined
Pressure
Flow to inlet, setpoint and actual
Press [Mode/Type]