Agilent Technologies 7673 Operating Manual
Operating Manual
Agilent 7673 Automatic Liquid Sampler
© Agilent Technologies 1995-2000
Target® is a registered trademark and DP™ is a
trademark of National Scientific Company.
HP-UX™ is a registered trademark of the
Hewlett-Packard Company.
All Rights Reserved.
Reproduction, adaptation, or translation without
permission is prohibited, except as allowed under
the copyright laws.
Part number G1513-90107
First edition, MAY 2000
Printed in USA
Safety Information
The Agilent Automatic Liquid Sampler meets the
following IEC (International Electrotechnical
Commission) classifications: Safety Class 1,
Transient Overvoltage Category II, and Pollutions
Degree 2. This unit has been designed and tested
in accordance with recognized safety standards
and designed for use indoors. Whenever the safety
protection of the Automatic Liquid Sampler has
been compromised, disconnect the unit from all
power sources and secure the unit against
unintended operation.
The recyclable carbon mono-fluoride lithium
battery is a BR-2/3 A 1,2OO mAh. Fuses F001 and
F002 are 3 A, 250 Vac, IEC 127 Type T. Fuses
F201 and F202 are 10 A, 250 Vac, IEC 127 Type
T. Fuse F101 is a 0.5 A, 250 Vac.
Warnings in this manual or on the instrument must
be observed during all phases of operation, service,
and repair of this instruments. 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. 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.
Safety Symbols
This manual contains safety information that
should be followed by the user to ensure safe
operation.
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.
Sound Emission Certification for Federal
Republic of Germany
If Test and Measurement Equipment is operated
with unscreened cables and/or used for
measurements in open set-ups, users have to
assure that under these operating conditions the
Radio Interference Limits are still met at the border
of their premises.The following information is
provided to comply with the requirements of the
German Sound Emission Directive dated
January 18, 1991:
Sound pressure Lp < 70db(A)
During normal operation
At the operator position
According to ISO 7779 (Type Test)
When operating the Automatic Liquid Sampler with
cryo valve option, the sound pressure ≈ 78 db(A)
during cryo valve operation for short burst pulses.
Schallemission
Werden Meß-und Testgeräte mit ungeschirmten
Kabeln und/oder in offenen Meßaufbauten
verwendet, so ist vom Betreiber sicherzustellen,
daß die Funk-Entströbedingungen unter
Betriebsbedingungen an seiner Grundstücksgrenze
eingehalten werden. Diese Information steht im
Zusammenhang mit den Anforderungen der
Maschinenlärminformation sverordnung vom
18 Januar 1991.
Schalldruckpegel LP < 70 dB(A)
Am Arbeitsplatz
Normaler Betrieb
Nach DIN 45635 T. 19
(Typprüfung)
Bei Betrieb des Automatischer
Slüssigkeitsprobengeber mit Cryo Ventil Option
treten beim Oeffnen des Ventils impulsfoermig
Schalldrucke Lp bis ca. 78 dB(A) auf.
Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 19808-1610
USA
Contents
Chapter 1 Setting Up
The modules of the automatic liquid sampler ....................................................... 3
Preparing the site ...................................................................................................... 5
Installing the injectors ..............................................................................................7
Installing the tray .....................................................................................................13
Installing the controller .......................................................................................... 17
Environmental considerations ......................................................................... 5
Space considerations ........................................................................................ 5
Electrical power requirements ........................................................................6
Connecting the controller power cord ...........................................................7
Behind the door to the control switches ........................................................9
Before you start ............................................................................................... 10
Mounting the injectors .................................................................................... 11
Checking your work ........................................................................................13
Before you start ............................................................................................... 14
Mounting the tray ............................................................................................ 15
Checking your work ........................................................................................16
Connecting cables to other instruments ...................................................... 18
Setting the configuration switches ................................................................19
Configuration switch definitions ................................................................... 19
Connecting the injector cables ......................................................................21
Connecting the tray cable ...............................................................................22
Connecting the controller power cord .........................................................22
Checking your work ........................................................................................23
Chapter 2 Preparing for Operation
Preparing sample vials ............................................................................................ 26
Selecting and labeling sample vials ...............................................................26
Specifications ...................................................................................................27
Sample caps and septum ................................................................................ 28
Filling sample vials .......................................................................................... 29
Crimp capping sample vials ........................................................................... 30
Placing sample vials in the standard injector turret ...................................32
Placing sample vials in a tray .........................................................................33
Using the injector fan .............................................................................................. 34
Turning the fan off ........................................................................................... 34
Preparing the solvent and waste bottles .............................................................. 36
Selecting the bottles ........................................................................................ 36
i
Contents
Filling and placing the bottles ........................................................................37
Do you need to read further? .........................................................................40
Estimating the maximum number of sample vials ......................................42
Controlling sample carryover .........................................................................47
Selecting and installing syringes ............................................................................49
Selecting syringes ............................................................................................49
Inspecting syringes ..........................................................................................51
Installing syringes ............................................................................................52
Checking your work ........................................................................................53
Maintaining the inlet ................................................................................................54
Changing septa .................................................................................................54
Changing or cleaning liners ............................................................................55
Suggestions for packed inlets with 530-µm columns ..................................55
Adapting for cool on-column injection .................................................................55
Chapter 3 Operation
Setting the run parameters .....................................................................................59
Description of the parameters .......................................................................59
Injection mode ...............................................................................................63
What happens during a run? ...................................................................................66
Checklist ...................................................................................................................68
Running the samples ...............................................................................................69
Starting a run or sequence ..............................................................................69
Stopping or interrupting a run or sequence ..................................................69
Using two injectors ..................................................................................................70
With a tray .........................................................................................................70
Without a tray ...................................................................................................72
Four methods of control .........................................................................................73
Examples of operation ............................................................................................74
Preparing the GC and controlling device ......................................................74
6890 Series GC Control ...........................................................................................75
Configure tower position ................................................................................75
Configure waste bottle position with a tray .................................................75
Configure the injector .....................................................................................75
Injector parameter setpoints ..........................................................................76
Sample tray setpoints ......................................................................................76
Storing injector setpoints ................................................................................77
Operating in cool on-column mode ...............................................................77
ii
Contents
Creating a sequence ........................................................................................78
Storing a sequence ..........................................................................................79
Starting/running a sequence ...........................................................................80
Special considerations when using an integrator with a 6890 Series GC ........ 81
3396 integrator with a 5890 GC .............................................................................. 83
Checking your work ........................................................................................85
Multitechnique ChemStation control with a 6890
Series GC ..................................................................................................................86
Injector parameters ......................................................................................... 86
Washes .............................................................................................................. 87
Position .............................................................................................................87
Extended Injector Parameters dialog box ...................................................88
Start a Run ........................................................................................................ 90
Start a sequence ...............................................................................................90
Chapter 4 Standalone Control
Setting the run parameters ..................................................................................... 92
Sample size ....................................................................................................... 95
Injection ............................................................................................................ 96
Number of injections per vial ........................................................................ 97
Number of sample prewashes ....................................................................... 98
On-column injection mode .............................................................................99
Number of solvent postwashes ...................................................................100
Example of setting the injector switches ................................................... 101
Setting the position of the last vial ..............................................................102
Running the samples ............................................................................................. 103
Starting a run or sequence ............................................................................ 103
What happens during a run? ........................................................................ 103
Stopping or interrupting a run or sequence ............................................... 104
Using two injectors ............................................................................................... 106
Synchronous mode ........................................................................................106
Asynchronous mode ..................................................................................... 107
Example of standalone control setup ................................................................. 109
Checking your work ..............................................................................................112
Standalone control ........................................................................................ 112
iii
Contents
Chapter 5 Preventive Maintenance and Troubleshooting
Preventive maintenance ........................................................................................114
Regular basis (before you start a sequence ................................................114
Occasional basis .............................................................................................114
Turret exchange .............................................................................................115
Alignment procedure .....................................................................................116
Troubleshooting .....................................................................................................118
Bent syringe needle ...............................................................................................119
Dropped sample vial ..............................................................................................120
Chromatographic symptoms ................................................................................121
Variability ........................................................................................................121
Contamination or ghost peaks .....................................................................124
Peak area discrimination (smaller or larger peaks than expected) ........126
Sample carryover ...........................................................................................128
No signal/no peaks .........................................................................................129
Fault light symptoms .............................................................................................130
Fault light locations, colors, and patterns ..................................................131
Responding to the fault lights ......................................................................133
Power error .....................................................................................................133
Injector door open/not mounted ..................................................................134
Syringe error ...................................................................................................135
Turret error .....................................................................................................136
Plunger error ..................................................................................................137
Incomplete injection ......................................................................................138
Bottle in gripper .............................................................................................139
Hard tray/injector error .................................................................................140
Align LED is On ..............................................................................................141
Other patterns ................................................................................................142
Error messages ......................................................................................................145
Contacting Agilent Technologies .........................................................................147
Obtaining Agilent Technologies service .....................................................147
Shipment or storage ......................................................................................148
iv
Contents
Chapter 6 Special Topics
Performing cool on-column injection onto 250-µm and 320-µm columns ..... 151
Installing the needle into the syringe barrel ..............................................151
Checking the needle-to-column size ........................................................... 152
Preparing the cool on-column inlet .............................................................153
Using retention gaps and other precolumns ..............................................158
Preparing the injector ................................................................................... 160
Replacing the needle guide in the needle support foot ............................ 165
Troubleshooting 250-µm and 320-µm systems ........................................... 167
Controlling sample vial temperatures ......................................................... 168
Tray control commands ................................................................................ 174
Glossary ...................................................................................... 182
Index ........................................................................................... 191
v
Contents
vi
1
Setting Up
Setting Up
The purpose of this chapter is to:
• Introduce you to the names of the major parts associated with installing
• Help you set up the automatic liquid sampler and turn on the power.
You must complete the following tasks during installation to be ready to turn
on the power.
1. Install the mounting brackets for the injector and tray, along with any
2. Mount the injector and tray on the brackets.
3. Verify that the controller switch settings are correct.
4. Connect the cables for the injector and tray to the controller.
5. Connect the communication cables for the controller, the GC, and the data
the automatic liquid sampler and some preventive maintenance tips.
upgrade parts for the gas chromatograph (GC). Instructions for these
installations are contained in link manuals that are packaged with the
brackets or upgrade parts.
handling device.
6. Install the power cord for the controller.
The instructions for tasks 2 through 6 start on page 11.
2
Setting Up
"6890" [type C] tower, tray and controller
The modules of the automatic liquid sampler
The modules of the automatic liquid sampler
The automatic liquid sampler is made up of three modules:
The G1512A controller and communications module supplies
power and communications to the injector and tray.
The G1513A injector module removes a volume of sample from
a vial and injects it into the inlet.
The 18596C tray module moves sample vials to and from the
injector and the bar code reader.
The automatic liquid sampler works with the PrepStation system to automate
sample preparation procedures. The G1296A/G1926A bar code reader module
is also available. It reads the vial numbers and special instructions for running
a method. It can also be used for agitating the sample vial.
The automatic liquid sampler becomes part of your gas chromatography
system. It introduces sample to an inlet or a column on your GC.
The automatic liquid sampler, with or without the tray, can be controlled by a
variety of integrators and computers, including:
• 6890 Series GC
• Its own electronics (standalone control)
• 3396 integrators plus older models
• Most Agilent laboratory automation systems
• Most Agilent ChemStation systems
• Suitably programmed external computers
3
Setting Up
The modules of the automatic liquid sampler
Figure 1 illustrates how the automatic liquid sampler is an integral part of the
analytical system.
One or two injectors
With or without the tray
With or with out the bar
code reader
Controller
Controller configured to communicate with:
• 6890 Series GC
•Integrator
• Personal computer
• Workstation
• Lab data system
• Injector’s control switches
Figure 1. The automatic liquid sampler as part of your analytical system
4
Setting Up
Preparing the site
Preparing the site
The automatic liquid sampler has certain environmental, space, and electrical
power requirements.
Environmental considerations
The automatic liquid sampler is designed to operate within ranges of
temperature and relative humidity.
• Temperature range: 0° to 55°C
• Relative humidity range: 5% to 95% at 40°C
• Altitude ranges: up to 2,300 m
Agilent Technologies recommends an environment comfortable for the
operators (reasonably constant temperature and humidity) for optimum
performance and instrument lifetime.
Caution Do not place any instruments that release heat on top of or underneath the
controller. For example, do not place an integrator on top of the controller.
The additional heat can cause damage to its electrical components.
Space considerations
The injector and tray increase the space requirements for the GC. The exact
amount depends on the model of the GC. Figure 2 shows the space
requirements for the components with a 6890 Series GC.
Installed on the 6890 Series GC, the injector adds 44 cm (17 in.) in height. The
tray adds 30.3 cm (9 in.) to the left side and 3 cm (2 in.) to the front. The
controller requires a clear surface about 33 cm (13 in.) wide and 38 cm
(15.2 in.) deep. About 20 cm (8 in.) of the depth is required for cabling. If you
place the controller on its right-hand side (i.e., power switch up), it needs a
clear surface of 38 cm (15.2 in.) deep and 14 cm (6 in.) wide.
5
Setting Up
Preparing the site
WARNING Place the G1512A controller where you can easily unplug it from the power
source.
Ventilation and cabling space
10
Top Views
Figure 2. Space considerations
Electrical power requirements
The controller is the power source for the injector and tray. The controller has
an autoranging power supply:
• 100–240 Vac single phase
• 48–66 Hz maximum
•320 VA maximum
The automatic liquid sampler requires a proper earth ground. To protect users,
the metal instrument panels and cabinet are grounded through the threeconductor power line cord in accordance with International Electrotechnical
Commission (IEC) requirements.
30
10
Ventilation space
33
All dimensions in centimeters
or
14
The power cord must be plugged into a receptacle connected to a suitable
earth ground. The receptacle ground should be verified.
6
Setting Up
Installing the injectors
WARNING Any interruption of the grounding conductor or disconnection of the power
cord could cause a shock that results in personal injury.
Connecting the controller power cord
1. Check the on/off button on the front of the controller. It must be off or
flush with the front panel before you plug in the power cord. The symbol
“ ” indicates standby. The symbol “|” indicates on.
2. Plug the female end of the power cord into the AC power receptacle on the
back of the controller.
3. Plug the male end of the power cord into the AC power receptacle of your
facility.
Installing the injectors
The injector contains the syringe, a syringe carriage, a six-position standard
turret, a cooling fan that you can turn off, parameter switches, and a last
sample vial switch.
The turret rotates sample vials and solvent and waste bottles into position
under the syringe. Without a tray, you load the sample vials manually into the
turret (maximum of three samples). With a tray, the robotic arm loads the vials
(up to 100 samples). You load the solvent and wash bottles manually (the
quantities of each depend on your controlling device). For more information on
the fan, see “Using the injector fan” on page 34.
7
Setting Up
Installing the injectors
Fan
Electronics assembly
Door to control switches
Start/stop buttons
Fault LEDs
Door to syringe
Turret
Base
Figure 3. G1513A injector module
8
Setting Up
Installing the injectors
Behind the door to the control switches
There are control switches behind the door on the injector’s front panel.
• You use the rotary switch to set the number of sample vials when no tray is
installed and the remaining ten switches to set six injector parameters
when the system cannot be controlled by the 6890 Series GC, a computer,
or an integrator. For example, you can set the number of injections per
sample vial or the number of syringe washes. For more information, see
“Setting the run parameters” on page 59.
• The injection switch can be used to set fast or slow injection with or
without an integrator or computer controlling the system having any affect
on that setting. However, it will be overridden by settings from the 6890
Series GC and the ChemStation.
• The Align LED is a diagnostic LED to warn users to perform the alignment
procedure. See Chapter 5, Preventive Maintenance and Troubleshooting.
9
Setting Up
Installing the injectors
Rotary switch
Align LED
Control switches
10
Figure 4. The parameter control switches
Before you start
To install an injector, you must first:
• Install the tray’s mounting bracket before mounting the injectors (if your
automatic liquid sampler includes a tray). The instructions and hardware
are packaged together with the tray.
• Open the front panel, and remove the foam packing materials.
Setting Up
Installing the injectors
• Install the injector mounting posts in the front and back locations of the
injection bracket on the GC.
Mounting the injectors
The first part of each step describes how to mount the injector over the front
inlet (injection port).
1. Hold the injector with both hands so the cable points toward you. Line up
the hole in the base of the injector that is nearest the cable with the
mounting post on the bracket. Lower the injector about an inch on to the
post.
Cable
Hole
Front mounting post
Figure 5. Lining up the injector with the mounting post
Door
Turret
Injector base
Mounting pin
Back disk
Front disk
11
Setting Up
Installing the injectors
2. Turn the injector so that the turret is facing toward you. Lower the injector
Turret
so that the pin in the base enters the hole in the disk on the mounting
bracket.
Mounting pin
Front mounting post
Disk
Figure 6. Lowering the injector. The injector in this diagram is angled back to illustrate
the position of the mounting pin.
12
Setting Up
Installing the tray
Checking your work
❐ Be sure the mounting pin is seated in the hole of the disk. The injector’s feet
should touch the mounting bracket. Be sure the gas lines are not routed
under the feet or the mounting pin.
❐ Turn the turret so you can see the inlet of the GC, and open the door to the
syringe. Be sure the inlet is flush with the surface of the hole in the injector’s
base. This check does not apply to on-column inlets.
❐ If your system does not include a tray, read “Placing sample vials in the
standard injector turret” in chapter 2.
For information on installing syringes, see “Selecting and installing syringes” in
chapter 2. See this section for instructions on how to align the syringe to the
inlet. Alignment is critical when injecting onto a 320- or 250-µm column.
Chapter 6, “Special Topics,” contains more information on use of 320- and
250-µm columns.
Installing the tray
The tray delivers samples to one or two injectors depending on the
configuration of the gas chromatography system. The arm and gripper
mechanism in the center of the tray loads sample vials into the injector turret
and then returns them to the tray after each injection. It can also transport
sample vials to and from the G1296A/G1926A bar code reader.
Each of the four removable tray quadrants holds 25 vials. Each is hollow and
has fittings so that you can circulate a temperature-controlled fluid through it.
13
Setting Up
Installing the tray
Quadrant
Arm
Gripper
Gripper jaws
Sample vial
Figure 7. 18596B tray module
Before you start
Caution Do not remove the tray’s arm back and forth. Do not move the tray’s gripper up
and down. These movements could damage the tray arm. If you need to move
the arm, turn it in a clockwise or counterclockwise direction.
To install a tray, you must first install the tray mounting bracket. The mounting
bracket for the tray attaches to the injector mounting bracket and the GC. The
instructions and hardware are packaged together with the tray.
14
Setting Up
Installing the tray
Mounting the tray
1. Thread the cable through the hole in the mounting bracket. Lower the tray
onto the bracket. Position the tray so that it sits flat on the bracket with
the raised arrow pointing toward the right (the front injector). Move the
injector cable out of the way.
Arrow
Figure 8. Threading the tray cable
2. Line up the arrow on the tray base with the alignment pin on the mounting
bracket. Slide the tray to the right until the edge is under the two tray
locks.
Arrow
Tray locks
Alignment pin
Figure 9. Attaching the tray
15
Setting Up
Installing the tray
3. Lock the tray into place by pulling each lock up (A), turning each lock (B),
and inserting each tab into a slot in the tray (C).
A B C
Figure 10. Locking the tray
4. Snap the tab of each tray quadrant into a slot on the base of the tray. The
numbers on the quadrants should match the numbers on the base.
16
Ta b
Slot
Figure 11. Inserting the tray quadrants
Checking your work
❐ Be sure the tray base is all the way to the right and locked into place.
❐ Be sure the quadrants are seated on the tray base.
Setting Up
Installing the controller
Installing the controller
The G1512A controller provides power and the communication interface for
18593A/B or G1513A injectors and for the 18596A or 18596B/C tray.
There are 11 connectors and two sets of switches for defining the
communication type.
Fault LED
Serial number
On/off button
Injector connectors
Figure 12. G1512A controller and communications module
Configuration switches
AC power receptacle
17
Setting Up
Installing the controller
This section covers connecting the injector and tray cables to the controller,
connecting the controller to the GC, connecting the controller to the data
handling device, and plugging in the controller.
Find the power cord in the controller box. Check the shape of the plug and the
source voltage listed on the packing contents sheet. Verify that the power cord
is appropriate for the power source at your facility.
Connecting cables to other instruments
The automatic liquid sampler communicates to other instruments via cables
that connect to the various connectors on the controller. Figure 13 shows the
connectors on the back of the controller and what they are used for.
RS-232-C to computer
Connect to a
computer
Connect to the
Instrument
Network
Figure 13. Common cable connections
18
Connect to the
bar code reader
Connect to the injector modules
Connect to the tray module
Setting Up
Installing the controller
Setting the configuration switches
There are 16 switches on the back of the controller. Figure 14 and Figure 15
show the switches and settings for five common types of communications.
When you are using ChemStation software, you must set the GPIB address
switches to a unique address. The address for the first sampler is usually set to
“8.” For a complete list of address switches, see Table 3.
Configuration switch definitions
The following tables describe the configuration switches and their settings.
Table 1. Left-hand Switch Settings
Switch Description Possible Values
MM Communication mode type 00—INET, standalone
10—3365 ChemStation, MS ChemStation
(Rev 3.65 and lower)
11—ChemStation, MS ChemStation
(Rev 3.71 and higher)
01—Asynchronous standalone
PP The bar code reader position 00—Front
01—Back
10—Right
11—Left
H RS-232-C host handshake 0—XON/XOFF
1—RTS/CTS
BB RS-232-C host baud rate 00—2400
01—9600
10—19.2 K
11—38.4 K
Table 2. Right-hand Switch Settings
Switch Description Possible Values
LF Controller termination
message
16,8,4,2,1 GPIB address of controller 00000=0, 00001=1, 00010=2, 00011=3, etc.
0—Line feed only
1—Carriage return and line feed
(see Figure 14)
19
Setting Up
Installing the controller
Communication mode Baud rate
Bar code reader position Handshake
Figure 14. Setting the address switches
ChemStation
6890 Series GC
MSD ChemStation
(rev 3.70 and above)
3365 ChemStation
MSD ChemStation
(rev 3.65 and below)
HP-UX ChemStations
Integrator with INET
Synchronous standalone
1
0
LFBBHPPMM124816
1
0
LFBBHPPMM124816
1
0
LFBBHPPMM124816
1
0
LFBBHPPMM124816
GPIB address
1
0
1
Address = 10
0
1
Address = 8
0
1
0
Asynchronous standalone
35900 Loop
RS-232-C, described in
serial interface manual,
part no. 18594-90300
Figure 15. Examples of switch settings
20
1
0
1
0
1
0
1
0
LFBBHPPMM124816
1
0
LFBBHPPMM124816
1
0
LFBBHPPMM124816
Table 3. Possible GPIB Address Switch Settings
Setting Up
Installing the controller
Switch
GPIB Address
0 00000 15 01111
1 00001 16 10000
2 00010 17 10001
3 00011 18 10010
4 00100 19 10011
5 00101 20 10100
6 00110 21 10101
7 00111 22 10110
8 01000 23 10111
9 01001 24 11000
10 01010 25 11001
11 01011 26 11010
12 01100 27 11011
13 01101 28 11100
14 01110 29 11101
Settings GPIB Address
Switch
Settings
Connecting the injector cables
With the power off, plug each injector cable into the connector on the back
panel of the controller associated with the position of the injector, front or
21
Setting Up
Installing the controller
back. Be sure the spring clamps on either side of the plug snap onto the
connector. Note the TOP label on the connector for orientation purposes.
22
Tray Injector
Figure 16. Connecting the injector and tray cables
Connecting the tray cable
Plug the cable into the tray connector on the back panel of the controller.
Secure the plug to the connector with a small flathead screwdriver.
Connecting the controller power cord
1. Check the on/off button on the front of the controller. It must be off or
flush with the front panel before you plug in the power cord.
2. Plug the female end of the power cord into the AC power receptacle on the
back of the controller.
3. Plug the male end of the power cord into the AC power receptacle of
your facility.
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