Agilent Technologies G1289 User manual

Agilent 7694 Headspace Sampler
Operating Manual
View More Agilent Manuals at
www.Chromatography.co

Agilent Technologies, Inc.
2850 Centerville Road
Wilmington, DE 1 808-1610
USA
© Agilent Technologies 2000
All Rights Reserved. Reproduction,
adaptation, or translation without
permission is prohibited, except as
allowed under the copyright laws.
Part number 1290-90317
First Edition, 3/2000
Replaces Part No. 1290-90310,
Operating and Service Manual, and part
No. 1883-90310, Operating and
Service Manual.
HP® is a registered trademark of
Hewlett-Packard Co.
Silcosteel® is a registered trademark of
Restek Corp.
Swagelok® is a registered trademark of
Swagelok company.
Printed in USA
Safety Information
The Agilent Technologies 7694
Headspace Sampler 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 Agilent 7694 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.
WAR I G
A warning calls attention to a condition
or possible situation that could cause
injury to the user.
CAUTIO
A caution calls attention to a condition
or possible situation that could damage
or destroy the product or the user’s
work.
+Indicates a hot surface
*Indicates earth (ground) terminal
Sound Emission Certification for
Federal Republic of Germany
Sound pressure Lp < 68 dB(A)
During normal operation
At the operator position
According to ISO 7779 (Type Test)
Schallemission
Schalldruckpegel LP < 68 dB(A)
Am Arbeitsplatz
Normaler Betrieb
Nach DIN 45635 T. 19 (Typprüfung)

i
Contents
Chapter 1 About This Manual
Manual Overview ....................................................................................................... 2
Intended User ............................................................................................................ 3
Conventions ............................................................................................................... 3
Chapter 2 Introduction to Headspace and to the
7694 Headspace Sampler
Overview of Headspace Analysis ............................................................................ 6
The 76 4 Headspace Sampler .................................................................................. 7
Oven (G128 /G12 0) ......................................................................................... 7
Heated Zones (G1883) ...................................................................................... 8
Vial Tray (G128 /G12 0) ...................................................................................
Vial Transport Arm (G128 /G12 0) .................................................................
Sampling System ............................................................................................. 10
Transfer Line .................................................................................................... 10
Keypad and Display ......................................................................................... 10
Pneumatics ....................................................................................................... 11
Principles of Operation ........................................................................................... 13
General Operation ........................................................................................... 13
Power on Diagnostics ..................................................................................... 14
Standby Condition ........................................................................................... 14
Vial Pressurization ........................................................................................... 15
Filling the Sample Loop .................................................................................. 16
Loop Equilibration ........................................................................................... 17
Injecting the Sample ........................................................................................ 17
End of Cycle and Vial Recovery .................................................................... 18
Modes of Operation ................................................................................................. 1
Standard Headspace Extraction .................................................................... 1
Multiple Headspace Extraction with Multiple Vial Puncture–
G128 /G12 0 only ............................................................................................ 21
Multiple Vial Puncture with Constant Heating Time–G128 /G12 0 only . 22
Multiple Headspace Extraction with Single Vial Puncture ........................ 23
Multiple Headspace Extraction for Analyte Concentration–
G128 /G12 0 only ............................................................................................ 23

Contents
ii
Chapter 3 The eypad
Accessing Functions ................................................................................................26
Editing Setpoints ......................................................................................................26
The G1883 Keypad ...................................................................................................26
The G128 /G12 0 Keypad .......................................................................................28
Keys and Their Functions .......................................................................................30
Start (G1883 only) ............................................................................................30
Stop/Reset (G1883 only) .................................................................................30
Start/Stop (G128 /G12 0 only) .......................................................................30
Zone Temps .....................................................................................................31
Event Times .....................................................................................................32
Vial Parameters ...............................................................................................34
Load Method ....................................................................................................35
Store Method ...................................................................................................35
Chain Methods ................................................................................................36
Link Methods ..................................................................................................36
Carousel Advance (G1883 only) .....................................................................36
Pressure (G1883/G12 0 only) .........................................................................36
Tray Advance (G128 /G12 0 only) ................................................................36
Enter ................................................................................................................37
Clear .................................................................................................................37
Numeric Keypad ...............................................................................................37
Adv Fctn { } ......................................................................................................37
Chapter 4 Using the Adv Fctn ey
Using an Advanced Function .................................................................................40
List of Advanced Functions by Model ...................................................................41
Advanced Function Descriptions ..........................................................................44
Chapter 5 Preparing a Sample
Sample Preparation .................................................................................................56
Loading the Sample Tray and/or Carousel ...........................................................58

Contents
iii
Chapter 6 Entering a Method
Entering a Method ................................................................................................... 60
Entering Zone Temps ...................................................................................... 60
Setting Event Times ........................................................................................ 61
Setting Vial Parameters .................................................................................. 63
Storing and Loading Methods ................................................................................ 64
Storing a Method ............................................................................................. 64
Loading a Method ............................................................................................ 64
Chaining Methods .................................................................................................... 65
Activate a Method Chain ................................................................................ 65
Deactivate a Method Chain ............................................................................ 66
Using a Method Chain for MHE ............................................................................. 66
Using a Method Chain for Running More Than 44 Samples .............................. 66
Chapter 7 Developing Methods
Varying Oven Temperature .................................................................................... 71
Varying Event Times ............................................................................................... 71
Vial Equilibration Time ................................................................................... 71
Loop Fill Time .................................................................................................. 72
Matrix Effects .......................................................................................................... 72
Changing the Sample Loop .................................................................................... 73
Sample Size .............................................................................................................. 73
Vial Pressurization and Time ................................................................................ 73
Vial Pressurization .......................................................................................... 73
Vial Pressurization Time ................................................................................. 74
Optimizing Carrier Gas Flow ................................................................................. 74
Recommended 68 0/6850 GC Liner ...................................................................... 75
Chapter 8 Running a Sample
Setting Conditions ................................................................................................... 78
Flow Rates ........................................................................................................ 78
Setting the Carrier Gas Flow Rate for the G1883/G12 0 ............................ 80
Setting the Vial Pressurization Gas Pressure for the G1883/G12 0 ....... 81
Setting Carrier and Vial Pressurization Flows for the G128 .................... 81

Contents
iv
Chapter 9 Maintaining the Instrument
Common Replacement Parts and Consumables ................................................85
Fuse Locations ........................................................................................................88
Changing the Sampling Needle ..............................................................................8
Changing the Sample Loop ..................................................................................... 2
Steam Cleaning the Pneumatic System ................................................................. 5
Installing the Transfer Line onto the Volatiles Interface .................................... 6
Aligning the Vial Loader (G128 /G12 0 only) ...................................................... 7
Adjusting the potentiometers ......................................................................... 7
Procedure ..........................................................................................................
Other vial handling adjustments ..................................................................101
Checking carousel adjustment .............................................................................101
Leak Testing: General Information ......................................................................103
Leak Testing a G128 to 68 0 GC Interface ........................................................105
Carrier Gas Flow Path ...................................................................................105
Carrier Flow Path Pressurization Test ........................................................107
Vial Pressurization Gas (Aux) Flow Path ...................................................108
Leak Testing a G12 0/G1883 to GC Interface .....................................................110
Prepare the Sampler ......................................................................................110
Carrier Gas Flow Path ...................................................................................110
Vial Pressurization Flowpath .......................................................................111
Flow Testing the Vent Valve and Associated Flow Path ..................................112
Tightening the PTV Septumless Head Using the Leak Test Procedure ..........113
Chapter 10 Troubleshooting
Chromatography Problems ..................................................................................116
No Peaks .........................................................................................................116
Bad Data (Bad Peaks) ...................................................................................117
Unwanted Peaks Present ..............................................................................11
Vial Handling Problems (G128 /G12 0 only) .....................................................11
Gripper Arm Doesn’t Pick Up Sample Vial .................................................11
Sample Vial Doesn’t Drop Down Into Oven ...............................................120
Vial Not Raised and Lowered in Oven .........................................................121
Vial Not Loaded/Vial Retained Warning ......................................................121

Contents
v
Vial Jam Problems (G128 /G12 0 only) ............................................................. 121
Recovering from vial jam problems ............................................................ 122
Mechanical/Electrical Problems .......................................................................... 122
Instrument Resets Continuously ................................................................. 122
No Power ........................................................................................................ 123
Oven Carousel Won’t Rotate Properly ........................................................ 123
Oven Carousel Won’t Agitate ....................................................................... 123
Sample Tray Doesn’t Stop at Correct Location (G128 /G12 0 only) ...... 124
Sampling Sequence Won’t Start ................................................................... 124
Second Method in Sequence Won’t Start ................................................... 125
Zones Won’t Heat .......................................................................................... 125
Pressures Are Wrong .................................................................................... 126
Chapter 11 Error Messages
Error Message Listing ........................................................................................... 128
Recovery from an Automation Error (G128 /G12 0) ....................................... 133
Glossary ...................................................................................... 135
Index ........................................................................................... 141

Contents
vi

1
About This Manual

About This Manual
Manual Overview
2
About This Manual
The 7694 Headspace Sampler Operating Manual explains how to use the 76 4
Headspace Sampler. It includes all the basic information the user needs to
develop methods, use the sampler to carry out analyses, and maintain and
troubleshoot the sampler.
For site preparation requirements and checkout procedures, see the 7694
Headspace Sampler Site Preparation and Installation Manual.
Manual Overview
This manual contains ten chapters, a glossary, and an index.
Chapter 1: About This Manual provides the purpose of this manual and an
overview of its contents. It identifies the intended reader and lists the
conventions used throughout the manual.
Chapter 2: Introduction to Headspace and to the 7694 Headspace
Sampler provides an overview of headspace theory and practice. It describes
the instrument and its modes of operation.
Chapter 3: The eypad describes the keypad, the functions each key
controls, and how to enter new setpoints for each function.
Chapter 4: Using the Adv Fctn ey describes the advanced functions
controlled by the Adv Fctn key, how to edit setpoints for these functions, and
the displays that accompany each function.
Chapter 5: Preparing a Sample describes the preparation of a sample for
analysis, including filling and sealing the sample vial, loading the sample tray,
and running a checkout sample.
Chapter 6: Entering a Method describes the steps to follow in entering a
method, including changing setpoints, storing and retrieving a method, and
chaining methods.