Agilent Technologies 7697A User manual

Agilent Technologies
Agilent 7697A
Headspace Sampler
Operation

Notices
© Agilent Technologies, Inc. 2011
No part of this manual may be reproduced
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United States and international copyright
laws.
Manual Part Number
G4556-90015
Edition
Second edition, November 2011
First edition, January 2011
Printed in USA
Agilent Technologies, Inc.
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Wilmington, DE 19808-1610 USA
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Safety Notices
CAUTION
A CAUTION notice denotes a hazard. It
calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in damage to the product
or loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are fully
understood and met.
WARNING
A WARNING notice denotes a hazard.
It calls attention to an operating
procedure, practice, or the like that, if
not correctly performed or adhered to,
could result in personal injury or
death. Do not proceed beyond a
WARNING notice until the indicated
conditions are fully understood and
met.

Operation 3
Contents
1 Introduction
Introduction 8
The Agilent 7697A Headspace Sampler 9
About This Manual 10
Getting Familiar with the Headspace Sampler 11
2 The Operation Workflow
Routine Operation Workflow 14
Method Development Workflow 15
3 The Keypad
The General Data Entry Keys 18
The Run Keys 19
The Component Keys 20
The Adv Function Key 22
The Status Key 23
The Info Key 24
The Supporting Keys 25
The Method Storage and Automation Keys 26
The Service Mode Key 27
Keypad Functionality When the HS Is Controlled by an Agilent Data
System 28
Headspace Sampler Status 29
Alert tones 29
Error conditions 30
Blinking setpoint 30
Status indicators 31
Logs 32
Sequence log 32
Maintenance log 32
Event log 32
4 Consumables
Consumables for Headspace Analysis 34

4Operation
5 Sample Vials
Sample Vial Types 38
Sample Vial Septa and Caps 39
Vial Labels 40
Filling Sample Vials 41
To Cap a Sample Vial 42
To Park or Unpark the Tray (111 Vial Model) 44
To Install a Vial Rack (111 Vial Model) 45
To Load a Sample into the Tray (111 Vial Model) 46
To Load a Sample into the Tray (12 Vial Model) 47
6 Methods
What Is a Method? 50
Built-in methods 50
Data system methods 51
Method Parameter Summary 52
To Create a Method 54
To Save (Store) a Method 56
To Edit a Method 57
To Load a Method 58
To Delete a Method 59
To Determine the GC Cycle Time 60
To determine the GC cycle time 60
Validating the GC cycle time 61
7 Sequences
What Is a Sequence? 64
Sequences, extraction modes, and vial punctures 64
How many sequences can the HS store? 65
Priority samples 66
Priority sample locations 66
How the HS processes priority samples 66
Priority samples using an Agilent data system 67
Sequences and Throughput (111 vial model) 68
To Create a Sequence 69
To Save (Store) a Sequence 70

Operation 5
To Load a Sequence 71
To Edit a Sequence 72
To Delete a Sequence 73
Method Sequence Actions 74
8 Running Samples
To Run a Series (Sequence) of Samples 76
To Pause a Running Sequence 77
To Stop a Running Sequence 78
To Run a Priority Sample During a Sequence 79
To View Vial and Sequence Status 81
Readiness status 81
Setpoint status 81
Vial status 82
Sequence Control with an Agilent Data System 83
9 Configuration
What is Configuration? 86
To Configure the Headspace Sampler 87
Resource Conservation 88

6Operation

7
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
Agilent Technologies
1
Introduction
Introduction 8
The Agilent 7697A Headspace Sampler 9
About This Manual 10
Getting Familiar with the Headspace Sampler 11
This guide describes how to operate the Agilent 7697A
Headspace Sampler during typical operation.

8Operation
1Introduction
Introduction
Headspace analysis is a technique for analyzing volatile
organic compounds using gas chromatography. Headspace
analysis samples the ambient volume above a sample matrix,
where the volatile compounds exist in gaseous form at
predictable levels.
Headspace analysis is useful for situations where:
•The analyte of interest is volatile at temperatures below
285 °C (111 vial model) or 195 °C (12 vial model).
•The sample matrix is a solid, paste, or a liquid that is not
easy to inject into a GC inlet.
•Sample preparation to allow easy liquid injection is
currently difficult.
Headspace analysis provides several advantages over
traditional injections:
•Simpler sample preparation. The sample does not need to
be processed into an injectable liquid.
•Directly analyze a wide range of sample matrices (liquids,
solids, and pastes).
•Solvent peak is smaller or nonexistent compared to
traditional liquid injection GC techniques.
•Columns last longer, with less maintenance. The
headspace volume above the sample matrix is more clean
than the matrix. By injecting fewer contaminants, the
analytical column lasts longer and requires less
maintenance (trimming, bakeout, guard column
replacement, and so forth).
•High precision.

Introduction 1
Operation 9
The Agilent 7697A Headspace Sampler
The Agilent 7697A Headspace Sampler (HS) is a
pressure- loop headspace sampling system with either a
12- vial or 111- vial capacity. If configured for 12 sample
vials, the HS uses a single- vial oven to equilibrate the
sample at the desired temperature. If configured with the
111 sample vial tray, the HS uses a 12 vial oven for
equilibrating samples at temperature. Since the longest hold
time in headspace analysis is typically the equilibration time,
using a multi-vial oven allows the higher capacity HS to
increase throughput by equilibrating multiple vials at once.

10 Operation
1Introduction
About This Manual
This manual described the concepts and tasks needed for
routine headspace sampler operation.
For information needed to perform more advanced tasks and
method development, see the Advanced Operation Guide.

Introduction 1
Operation 11
Getting Familiar with the Headspace Sampler
Figure 1 111 Vial model—front view
Figure 2 12 Vial model—front view
Tray gantry
Transfer line
Tray
Vial racks
On/Off switch
Keypad
Display
Priority vial positions
Tray lid
Transfer line
On/Off switch
Keypad
Display
Sample loop cover

12 Operation
1Introduction
Figure 3 12 Vial model—back view (111 vial model is similar)
Communications
connections Power plug
Voltage label
Gas connections

13
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
Agilent Technologies
2
The Operation Workflow
Routine Operation Workflow 14
Method Development Workflow 15
This section describes the basic work flow for using the
headspace sampler.

14 Operation
2The Operation Workflow
Routine Operation Workflow
Figure 4 summarizes the normal operating workflow for
headspace analysis. This workflow assumes that the
headspace sampler is set up and that the methods and
samples are known.
Figure 4 Routine headspace analysis workflow
Start Up the Headspace
Sampler.
Load Method.
Prepare Samples.
Create Sequence.
Start.

The Operation Workflow 2
Operation 15
Method Development Workflow
Figure 5 summarizes the workflow for developing methods.
For details about method development, refer to the
Advanced Operation Guide.
Figure 5 Workflow for method development
Start Up the Headspace
Sampler.
Configure.
Create Method.
Prepare Samples.
Load Samples.
Create Sequence.
Start.
Evaluate.
If Needed, Refine
Method.
Re-evaluate.
If needed, consider
MHE/MHC.
If Needed, Optimize.

16 Operation
2The Operation Workflow

17
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
Agilent Technologies
3
The Keypad
The General Data Entry Keys 18
The Run Keys 19
The Component Keys 20
The Adv Function Key 22
The Status Key 23
The Info Key 24
The Supporting Keys 25
The Service Mode Key 27
The Method Storage and Automation Keys 26
Keypad Functionality When the HS Is Controlled by an Agilent Data
System 28
Headspace Sampler Status 29
Logs 32
This section describes the basic operation of the Agilent
7697A HS keypad. The keypad provides access to all
instrument functionality. For additional details on keypad
functionality, see the Advanced Operation Guide.

18 Operation
3The Keypad
The General Data Entry Keys
Use these keys to enter setpoints, make selections, and turn
on or turn off HS components.
Mode/Type Accesses a list of possible parameters associated
with a component’s nonnumeric settings. For
example, when selecting the vial fill mode, press
[Mode/Type] to list the vial fill mode options.
Clear Removes a misentered setpoint before pressing
[Enter]. It can also be used to return to the top line of
a multiline display, return to a previous display, cancel
a function during a sequence or method, or cancel
loading or storing sequences and methods.
Enter Accepts changes you enter or selects an alternate
mode.
Scroll keys. Use to scroll up and down through the
display one line at a time. The < in the display
indicates the active line.
Numeric Keys Use to enter settings for the method parameters.
(Press [Enter] to accept the changes.)
On / Yes
Off / No
Use when you are setting up parameters, such as the
warning beep, method modification beep, and key
click, or for turning on or off a parameter or device
(such as the transfer line heater).
General data
entry keys

The Keypad 3
Operation 19
The Run Keys
Use these keys to start sample preparation, stop preparation,
and move the sample tray prior to loading sample vials.
Stop During a sequence:
•Press once to pause the sequence. Current
samples continue processing, but no new samples
will be started. Press [Start] to resume.
•Press twice (within 5 seconds) to abort the
sequence. Any vials in the vial oven will be
returned to the tray.
Start Begin processing the next sample or sequence of
samples. When processing is complete for a sample,
the HS performs an injection to the GC and sends a
Start Run signal.
Tray Park/Carousel
Advance
•For the 111 vial model, press to park or unpark the
tray. (Park the tray to load/unload vials or vial
racks.) If pressed during a running sequence, the
sequence pauses until the tray is unparked.
•For the 12 vial model, press to advance the
carousel one position.
Priority Sample 111 vial tray model only. Standalone use only.
Press to insert a sample vial into the running
sequence. Disabled when using data system control.
Run keys

20 Operation
3The Keypad
The Component Keys
Use these keys to access method temperatures, timing events,
flows and pressures, vial fill modes, and similar parameters.
To display the current settings, press any one of these keys.
More than three lines of information may be available. Use
the scroll keys to view additional lines, if necessary.
To change settings, scroll to the line of interest, enter the
change, and press [Enter].
Note that editing temperatures and times from the keypad
Temp s Press to set temperatures for the vial oven, sample loop, and
transfer line.
Times Press to set the times for vial equilibration, injection duration,
pressure equilibration, and the GC cycle time.
Vial Press to set vial size, vial fill mode and parameters, loop fill mode
and parameters, and vial shaking.
Carrier If using optional HS carrier gas EPC module, press to set the
carrier gas control mode and the parameters for the carrier flow
or pressure program.
If the optional HS carrier gas control is not available, then the GC
controls the carrier gas flow.
Component
keys