Agilent Technologies G1289 Manuale utente

Agilent 7694 Headspace Sampler

Operating Manual

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Agilent Technologies, Inc.

2850 Centerville Road

Wilmington, DE 1 808-1610

USA

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)

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

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

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

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

About This Manual

Manual Overview

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.

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