advertisement
Agilent 7697A
Headspace Sampler
Operation
Agilent Technologies
Notices
© Agilent Technologies, Inc. 2011
No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from
Agilent Technologies, Inc. as governed by
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.
2850 Centerville Road
Wilmington, DE 19808-1610 USA
安捷伦科技 （上海）有限公司
上海市浦东新区外高桥保税区
英伦路 412 号
联系电话：（800）820 3278
Warranty
The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.
Safety Notices
C A U T I O N
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.
WA R N I N G
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.
Contents
Method Development Workflow 15
The Agilent 7697A Headspace Sampler 9
Getting Familiar with the Headspace Sampler 11
The General Data Entry Keys 18
20
24
The Method Storage and Automation Keys 26
27
Keypad Functionality When the HS Is Controlled by an Agilent Data
29
30
30
31
32
Consumables for Headspace Analysis 34
Operation 3
4
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
50
51
52
56
57
59
To Determine the GC Cycle Time 60
To determine the GC cycle time
60
Validating the GC cycle time 61
Sequences, extraction modes, and vial punctures
64
How many sequences can the HS store? 65
How the HS processes priority samples 66
Priority samples using an Agilent data system
67
Sequences and Throughput (111 vial model) 68
Operation
Operation
To Run a Series (Sequence) of Samples
76
To Pause a Running Sequence 77
78
To Run a Priority Sample During a Sequence
79
To View Vial and Sequence Status 81
81
82
Sequence Control with an Agilent Data System
83
86
To Configure the Headspace Sampler
87
5
6 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
1
Introduction
The Agilent 7697A Headspace Sampler 9
Getting Familiar with the Headspace Sampler 11
This guide describes how to operate the Agilent 7697A
Headspace Sampler during typical operation.
Agilent Technologies
7
8
1 Introduction
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.
Operation
Introduction 1
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.
Operation 9
1 Introduction
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 .
10 Operation
Introduction 1
Getting Familiar with the Headspace Sampler
Tray gantry
Transfer line
Priority vial positions
On/Off switch
Tray lid
Sample loop cover
Figure 1 111 Vial model—front view
Vial racks
Tray
Display
Keypad
Transfer line
On/Off switch
Operation
Figure 2 12 Vial model—front view
Display
Keypad
11
1 Introduction
Gas connections
Communications connections
Voltage label
Power plug
Figure 3 12 Vial model—back view (111 vial model is similar)
12 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
2
The Operation Workflow
Method Development Workflow 15
This section describes the basic work flow for using the headspace sampler.
Agilent Technologies
13
2 The Operation Workflow
Routine Operation Workflow
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.
Start Up the Headspace
Sampler.
Load Method.
Prepare Samples.
Create Sequence.
Start.
Figure 4 Routine headspace analysis workflow
14 Operation
The Operation Workflow 2
Method Development Workflow
summarizes the workflow for developing methods.
For details about method development, refer to the
Advanced Operation Guide .
Start Up the Headspace
Sampler.
Start.
Configure.
Evaluate.
Create Method.
If Needed, Refine
Method.
Prepare Samples.
Re-evaluate.
Load Samples.
If needed, consider
MHE/MHC.
Create Sequence.
If Needed, Optimize.
Figure 5 Workflow for method development
Operation 15
2 The Operation Workflow
16 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
3
The Keypad
The General Data Entry Keys 18
The Method Storage and Automation Keys 26
Keypad Functionality When the HS Is Controlled by an Agilent Data
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 .
Agilent Technologies
17
3 The Keypad
The General Data Entry Keys
Use these keys to enter setpoints, make selections, and turn on or turn off HS components.
General data entry keys
18
Mode/Type
Clear
Enter
Numeric Keys
On / Yes
Off / No
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.
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.
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.
Use to enter settings for the method parameters.
(Press [Enter] to accept the changes.)
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).
Operation
The Run Keys
The Keypad 3
Use these keys to start sample preparation, stop preparation, and move the sample tray prior to loading sample vials.
Run keys
Operation
Stop
Start
Tray Park/Carousel
Advance
Priority Sample
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.
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.
• 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.
111 vial tray model only. Standalone use only.
Press to insert a sample vial into the running sequence. Disabled when using data system control.
19
3 The 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] .
Component keys
20
Temps
Times
Vial
Carrier
Press to set temperatures for the vial oven, sample loop, and transfer line.
Press to set the times for vial equilibration, injection duration, pressure equilibration, and the GC cycle time.
Press to set vial size, vial fill mode and parameters, loop fill mode and parameters, and vial shaking.
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.
Note that editing temperatures and times from the keypad
Operation
The Keypad 3 immediately changes that setting in the current method, and the HS will begin to adjust to the new setting, if appropriate.
Operation 21
3 The Keypad
The Adv Function Key
Use the [ Adv Function ] key to access advanced HS method parameters.
Adv
Function key
Adv Function Use to access parameters for:
• Sample loop and sample probe purge between sequences
• Headspace extraction mode
• Method sequence actions
• Barcode reader settings
• Parameters for method development
22 Operation
The Status Key
The Keypad 3
Use the Status key to learn about the current HS state.
Status key
Operation
Status Toggles between sequence, setpoint, and vial status information and messages. Also displays “ready,”
“not ready,” and “fault” information.
When the Not Ready status light is blinking, a fault has occurred.
The order in which items appear in the scrolling display window for setpoint status can be modified.
You may, for example, want to display the things you most frequently check in the top three lines so that you do not need to scroll to see them. To change the order of the Status display:
1 Press [Config] [Status] .
2 Scroll to the setpoint you want to appear first and press [Enter] . This setpoint will now appear at the top of the list.
3 Scroll to the setpoint you want to appear second and press [Enter] . This setpoint will now be the second item on the list.
4 Continue as above until the list is in the order you require.
23
3 The Keypad
The Info Key
For context- sensitive help, press [Info] . For example, if you press [Info] on a setpoint entry, the help provided would be similar to: Enter a value between 0.00 and 999.990 minutes .
Info key
Info Provides help for the currently shown parameter. For example, if Vial equib time is the active line in the display (has a < next to it), [Info] will display the valid range of times. In other cases, [Info] will display definitions or actions that need to be performed.
24 Operation
The Keypad 3
The Supporting Keys
Use these keys to view and set configuration parameters, to set options, and to view instrument history data.
Supporting keys
Operation
Logs
Options
Config
Toggles between the Sequence Log , the Event Log , and the Maintenance Log . The information in these logs can be used to support Good Laboratory
Practices (GLP) standards.
Accesses the instrument calibration, communications, and keyboard and display options.
Scroll to the desired line and press [Enter] to access the associated entries. See the Advanced Operation
Guide for details.
Use [Config] to set up components that are not automatically detectable by the HS but are essential to preparing the sample or running method, such as gas types, carrier gas mode, loop volume, and the clock.
25
3 The Keypad
The Method Storage and Automation Keys
These keys are for loading and storing methods and sequences locally on your HS. They cannot be used to access methods and sequences stored by your Agilent data system.
26
Method storage and automation keys
Load
Method
Store
Seq
Delete
Insert/Append
Use to load and store methods and sequences on your HS.
For example, to load a method, press [Load]
[Method] and select one from the list of methods
stored in the HS. See “To Load a Method” ,
, and
.
Removes a method, sequence, or sequence line. See
Use to add a sample vial to a new or existing sequence.
Operation
The Keypad 3
The Service Mode Key
Use this key to access service information and procedures.
Service Mode key
Service Mode Use to access maintenance functions and settings, service counters, vial leak tests, and diagnostics for the HS. See the Advanced Operation Guide for details.
Operation 27
3 The Keypad
Keypad Functionality When the HS Is Controlled by an Agilent Data System
While under data system control, the keypad may be locked for general use. This locking feature prevents a user from unintended changes to the headspace method while the data system controls the instrument. If locked, the following changes occur:
• Method parameters can be viewed, but not changed.
• You cannot load, edit, or save a method.
• You cannot load, edit, or save a sequence.
• You cannot change the instrument configuration or perform advanced functions.
While under data system control, the keypad can be used:
• To view sequence status, including time data, by selecting
[Status] .
• To view the method settings.
• To pause or abort a sequence by selecting [Stop] .
• To find which computer is controlling the HS by pressing
[Options] > Communication , then scrolling. The name of the computer controlling the HS is listed below the Enable
DHCP setting, along with the number of hosts connected to the HS.
28 Operation
The Keypad 3
Headspace Sampler Status
When the HS is ready to begin the current sequence, the display screen shows a Ready status, as shown below:
STATUS - Ready
Ready for start sequence
Alternatively, when a component of the HS is not ready to begin a run, the Not Ready indicator lights, and the status display shows Not Ready and explains why the HS is not ready.
STATUS - Not Ready
Oven is turned off
Operation
Alert tones
At any time, press [Status] to view messages explaining the current HS state, including whether the HS is ready to begin sample preparation or what conditions are currently preventing it from continuing.
Sequence status : Displays any status information related to the sequence.
Setpoint status : Displays general status information, such as readiness messages and faults states, and also lists the setting and current value data for HS setpoints.
Vial status : During sequence execution, displays details about the status of the selected vial. Use the arrow keys to select the desired vial.
One beep sounds when a problem exists, but the problem will not prevent the HS from executing the sequence. The HS will emit one beep and display a message. The HS can start the sequence and the warning will disappear when another sequence starts.
Fault messages indicate hardware problems that require user
29
3 The Keypad
WA R N I N G intervention. Depending on the type of error, the HS emits no beep or a single beep.
A series of warning beeps sounds before a flow shutdown occurs. After a short time the component with the problem shuts down, the HS emits one beep, and a brief message displays. For example, a series of beeps sounds if the vial pressurization gas flow cannot maintain setpoint. The flow shuts down after 5 minutes. A shutdown message briefly displays. Press [ Clear ] to stop any beep. Vials in the oven continue to equilibrate, but the HS handles no additional vials and will not perform an extraction or injection.
A continuous tone sounds if using HS carrier gas control and if hydrogen flow is shut down or if a thermal shutdown occurs. During a hydrogen shutdown, all HS heaters and motors turn off.
Before resuming operations, investigate and resolve the cause of the hydrogen shutdown. See Hydrogen Shutdown in the
Troubleshooting manual for details.
Error conditions
If a problem occurs, a status message appears. If the message indicates broken hardware, more information may be available.
Blinking setpoint
If the system shuts down a gas flow or the vial oven, Off will blink on the appropriate line of the component’s parameter listing.
30 Operation
Operation
The Keypad 3
Status indicators
The front panel display provides five (5) indicator LEDs to show instrument status.
STATUS - READY
Ready for start sequence
Tray Park
Run
Sleep
Not Ready
Service Due
When lit, indicates the tray is parked. (111 Vial model)
Lights when the HS is processing samples.
Lights when the HS is in sleep mode. See
.
Lights when the HS is not ready to process samples.
Lights when an early maintenance feedback (EMF) counter has traversed a threshold, and the counter has been set to light this indicator.
31
3 The Keypad
Logs
Three logs are accessible from the keypad: the run log, the maintenance log, and the system event log. To access the logs, press [Logs] to toggle to the desired log. The display will indicate the number of entries the log contains. Scroll through the list.
Sequence log
Maintenance log
The maintenance log contains entries made by the system when any of the user- defined component counters reach a monitored limit. The log entry contains a description of the counter, its current value, the monitored limits, and which of its limits has been reached. In addition, each user task related to the counter is recorded in the log, including resetting, enabling or disabling monitoring, and changing limits or units (cycles or duration).
Event log
The sequence log is cleared at the start of each new sequence. During the sequence, any deviations from the planned methods (including keypad intervention) are listed in the sequence log table.
The event log records significant events during HS operation.
Some of the events also appear in the sequence log if they occur during sequence execution.
32 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
4
Consumables
Consumables for Headspace Analysis 34
This section lists commonly- used parts, such as vials and sample loops, needed for routine operation of the Agilent
7697A Headspace Sampler. Procedures for replacing these parts can be found in this manual or in the Maintenance manual.
Agilent Technologies
33
4 Consumables
Consumables for Headspace Analysis
The following tables provide list common supplies for the headspace sampler and headspace analysis. For the latest parts available, visit the Agilent website at www.agilent.com/chem .
Table 1 Headspace sampler parts and standards
Description
Leak test kit. Includes:
• No hole ferrule
• 11 mm low bleed septa, 5/pk
• Headspace (blue) leak test vial
• 1/8-in. nylon tube fitting plug
• 1/16-in. stainless steel ZDV plug (6 port valve cap)
Tray vial rack set, 7697A (3 racks)
Part number
G4556-67010
5181-7458
5182-3413
G4556-20600
0100-2414
G6600-80039
G4564A
Tray vial rack
Tray vial rack labels
G4556-60019
G4556-90500
RDT-1020 Universal/external split vent trap with 3 cartridges,
1/8-inch Swagelok fitting
Column cutting wafer, ceramic
Sample probe, deactivated SN1030
Sample probe, deactivated SN2000
5181-8836
G4556-60690
G4556-60125
6-port valve, replacement rotor, WT series, 300 psi, 350 °C 1535-4952
Sample loop adapter:
1 ea. used with 0.025, 0.05, and 0.10 mL sample loops
2 ea. used with 0.5 and 1.0 mL sample loops
G4556-20177
Sample loop adapter:
1 ea. used with 0.025, 0.05, and 0.10 mL sample loops
G4556-20178
Standards
GC headspace evaluation standard, 1 x 1 mL
Headspace OQ/PV sample
8500-4328
5182-9733
Table 2 Headspace sampler transfer line parts
Description
Transfer line components
Part number
34 Operation
Operation
Consumables 4
Table 2 Headspace sampler transfer line parts (continued)
Description
Ferrule, polyimide Valcon, 5/pk
0.53 mm, 1/32 in. for tubing OD 0.50
0.80 mm
0.25, 0.32 mm, 1/32 in. for tubing OD 0.25
0.40 mm
Septum nut, transfer line, for split/splitless and multimode inlets
Blanking nut, 1/16-inch stainless steel
Part number
0100-2595
5190-1437
G3452-60835
01080-83202
Nut and reducing union for 6 port valve and transfer line connection
0100-2594
Transfer lines
Deactivated fused silica, 250 µm x 5 m
Deactivated fused silica, 320 µm x 5 m
Deactivated fused silica, 450 µm x 5 m
Deactivated fused silica, 530 µm x 5 m
ProSteel deactivated stainless steel, 5 m length
ProSteel sleeve for ProSteel, 5 m length
160-2255-5
160-2325-5
160-2455-5
160-2535-5
160-4535-5
4177-0607
Table 3 Headspace sampler sample loops
Description
Sample loops, SN 2000
0.025 mL
0.05 mL
0.1 mL
0.5 mL
1.0 mL
1.0 mL, Certified
3.0 mL
3.0 mL, Certified
5.0 mL
Sample loops, SN 1030
0.025 mL
0.05 mL
Part number
G4556-80101
G4556-80102
G4556-80103
G4556-80105
G4556-80106
G4556-80126
G4556-80108
G4556-80128
G4556-80109
G4556-80111
G4556-80112
35
4 Consumables
36
Table 3 Headspace sampler sample loops (continued)
Description
0.1 mL
0.5 mL
1 mL
3 mL
5 mL
Adapters for sample loops
Sample loop adapter:
1 ea. used with 0.025, 0.05, and 0.10 mL sample loops
2 ea. used with 0.5 and 1.0 mL sample loops
Sample loop adapter:
1 ea. used with 0.025, 0.05, and 0.10 mL sample loops
Part number
G4556-80113
G4556-80115
G4556-80116
G4556-80118
G4556-80119
G4556-20177
G4556-20178
Table 4 Headspace vials and caps
Description
Certified flat bottom vials
Certified flat bottom headspace vials, 20 mL, 100/pk
Certified flat bottom headspace vials, 10 mL, 100/pk
20 mm Headspace caps, with septa
Certified headspace Al crimp cap, PTFE/Si septum,
20 mm,100/pk
Headspace vial kits
Vial kit
20 mL Headspace crimp top, flat bottom vials, silver aluminum one-piece crimp caps with safety feature,
PTFE/white silicone septa, 100/pk
Cappers and decappers
Electronic crimper for 20 mm cap vials
Electronic decapper, for 20 mm crimp caps
Ergonomic manual crimper for 20 mm caps
Ergonomic manual decapper for 20 mm caps
Part number
5182-0837
5182-0838
5183-4477
5182-0840
5062-0208
5062-0210
5040-4669
5040-4671
Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
5
Sample Vials
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
This section discusses sample vial selection, sample preparation, and vial handling with the Agilent 7697A
Headspace Sampler.
Agilent Technologies
37
5 Sample Vials
Sample Vial Types
The headspace sampler accepts 10- mL, 20- mL, or 22- mL sample vials. Set the vial size in the method (see
“To Create a Method” ). The vial size can change with each new method
used in a sequence, but not within a method. Using a different vial size than expected by the method causes a run- time exception.
The headspace sampler uses clear or amber glass sample vials with crimp caps, or screw- cap vials. Use amber glass vials for light- sensitive samples. Both types are available with flat or rounded bottoms. Refer to your Agilent catalog for consumables and supplies for acceptable vial types, or visit the Agilent website at www.agilent.com/chem .
Incompatible sample vials can cause gripper errors (111 vial model).
Vials must conform to the specifications shown in Figure 6 .
18.0 mm maximum
47.0 mm minimum
79.0 mm maximum
5.0 mm maximum
22.40 to
23.10 mm
Figure 6 Supported vial dimensions
Avoid reusing vials.
Reused vials may crack when heated.
38 Operation
Sample Vials 5
Sample Vial Septa and Caps
There are two types of septa used with crimp caps and screw- on caps, each with different resealing characteristics and different resistance to solvents.
Septum material Compatible with Incompatible with Resealability Maximum temperature*
< 125 °C PTFE/butyl rubber
PTFE/silicone rubber
PTFE resistance until punctured, then septa or liner will have compatibility of rubber (ACN, acetone, DMF, alcohols, diethylamine, DMSO, phenols)
PTFE resistance until punctured, then septa will have compatibility of silicone (alcohol, acetone, ether,
DMF, DMSO)
ACN, THF, benzene chloroform, pyridine, toluene, hexane, heptane
* Approximate. Refer to manufacturer’s recommendations.
Chlorinated solvents, aromatics, hydrocarbons, carbon disulfide
Good
Average < 180 °C
Vial caps come with or without an internal safety feature that allows the vial to vent if the internal vial pressure exceeds about 310 kPa (45 psi).
In general, do not use crimp caps or septa more than once for headspace analysis.
Refer to your Agilent catalog for consumables and supplies for acceptable vial types, or visit the Agilent website at www.agilent.com/chem .
Operation 39
5 Sample Vials
Vial Labels
C A U T I O N
Make sure that any label and ink can withstand the oven heat without degrading.
If using labels with a 111 vial model, the label needs to conform to the dimensions below. If also using the optional barcode reader, the barcode labels must conform to the general dimensions for labels, plus the placement requirements shown.
1 mm skew maximum
4.0 mm high minimum
No label
17.5 mm minimum
Text
Bar code
Text
17.0 mm minimum
19 mm maximum
23.5 mm maximum, including label
Figure 7 Vial label and barcode specifications
C A U T I O N
Correct sample vial dimensions are critical for proper gripper operation. Vials and labels that do not meet these specifications may cause sampler errors. Service calls and repairs found to be due to vials and labels that do not meet these specifications are not covered under warranty or the service contract.
40 Operation
Sample Vials 5
Filling Sample Vials
In general, fill sample vials about half way. Although sample amounts can vary depending on the analysis, do not fill vials
more than the amount shown in Figure 8
. Filling the vial correctly ensures that the sampling probe will not contact with the matrix during sampling. If you need more sample, use a larger vial or optimize the method to improve results.
See the Advanced Operation Guide for recommendations.
17 mm
50% of height typical
50% of height maximum
75% of height maximum
20-mL and 22-mL vials
Figure 8 Vial fill limits
10-mL vials
Operation 41
5 Sample Vials
To Cap a Sample Vial
The vial must be sealed properly to insure that the headspace gases do not escape prematurely. For crimp top vials, use a crimper designed for headspace vials with
20- mm caps to seal the vials. Screw caps and screw top vials are also available. See
1 Before beginning, clean the inside surfaces of the crimper jaws.
2
3
If using separate septa and caps, place a septum in a vial cap with the
PTFE
side facing the vial. Take care not to contaminate the septum.
Place the cap upside down on a table.
4
5
6
7
Place the sample in the vial. (Most vials should not be more than 50% full, but some vials can reach 75% full. See
.)
Place the septum and cap assembly over the vial opening.
Lift the vial into the crimper.
With slow and steady pressure, squeeze the crimper handles to seal the vial. (Squeeze the handle until it reaches the adjustment screw.)
42
shows proper and improper vial caps.
Operation
Sample Vials 5
Centered
No folds or wrinkles
Off-center
Folds and wrinkles
Acceptable Unacceptable
Figure 9 Acceptable and unacceptable vial caps
Check each vial for proper crimping:
• Be sure there are no folds or wrinkles on the part of the cap that wraps under the neck of the vial. To remove folds or wrinkles, turn the vial about 10° and crimp it again. Adjust the crimper for a looser crimp by turning the adjusting screw clockwise.
• The cap should be finger- tight. If the cap is loose, adjust the crimper for a tighter crimp by turning the adjusting screw counterclockwise. Crimp the cap again. If the cap is too tight, the septum will distort and the vial may leak.
• Be sure that each cap has a flat septum centered over the top of the vial.
• If the septum is not flat, remove the cap, turn the crimper adjusting screw clockwise, and try again.
• If the cap is not centered, remove the cap and make sure the new cap is flat on the top of the vial before you squeeze the crimper.
Operation 43
5 Sample Vials
To Park or Unpark the Tray (111 Vial Model)
Parking the tray moves the tray gantry to a safe position.
When parked, you can load vials into the racks, or install and remove racks from the HS.
Press [Tray Park/Carousel Advance] to park the tray. The display reads:
TRAY PARKED
Tray Park - Unpark tray
Start - Start sequence
Press [Tray Park/Carousel Advance] to unpark the tray and ready it for use. The display reads:
SEQUENCE IDLE
Start - Start sequence
Tray Park - Park tray
You cannot start a sequence if the tray is parked.
Parking the tray during a sequence pauses the sequence.
Current vials continue to process, but no new vials are started.
44 Operation
Sample Vials 5
To Install a Vial Rack (111 Vial Model)
1 Press [Tray Park/Carousel Advance] to “park” the tray (move the gantry to a rest position for easy access to the vial rack area).
C A U T I O N
When loading a tray rack with sample vials, avoid excessive tray motion. If the sample coats the septum or coats the vial more than typical, this may change results.
2 While holding up the front end of the rack, slide the rack back and under the mounting clip on the HS top. Then, lower the front of the rack in place.
When installed correctly, a green LED on the tray rack lights.
Operation
Figure 10 Tray vial positions
3 Press [Tray Park/Carousel Advance] to prepare the tray for use.
45
5 Sample Vials
To Load a Sample into the Tray (111 Vial Model)
1
2
Press [Tray Park/Carousel Advance] to “park” the tray (move the gantry to a rest position for easy access to the vial racks).
Place the capped sample vials into the tray as desired.
See
.
36
108
111
110
109
1 73
Figure 11 Tray vial positions
3 Press [Tray Park/Carousel Advance] to prepare the tray for use.
46 Operation
To Load a Sample into the Tray (12 Vial Model)
1
Open the tray cover. See Figure 12 .
Tray cover
Sample Vials 5
Operation
Figure 12 Opening the tray cover
2 A label to the left of each vial position denotes the number of that position. See
.
47
5 Sample Vials
2
7
8 5
10
9
11
12
1
2
4
3
1
1
Figure 13 12 Vial tray positions
3
4
If the desired vial position is not available, press [Tray
Park/Carousel Advance] to rotate the tray.
Place the capped sample vials into the tray as desired.
48 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
6
Methods
To Determine the GC Cycle Time 60
This chapter defines the headspace sampler method, and describes how to load, save, create, and edit a method using the HS front keypad. If using an Agilent data system, most likely you will use the data system to create methods. Refer to the data system help and documentation for details, and to the Familiarization Guide .
Agilent Technologies
49
6 Methods
What Is a Method?
A method is the collection of setpoints needed for the headspace sampler to prepare a sample and inject it into the gas chromatograph. The Agilent 7697A Headspace Sampler can store up to 32 methods internally, plus several built- in methods. The primary parts of the method control the parameters for:
• Temperatures for the vial, sample loop, and transfer line
• Times for equilibration and injection, plus the GC cycle time (used for sample overlap and throughput calculations)
• Vial settings for vial size, filling, shaking, and venting after the injection
• Carrier gas settings, for controlling carrier gas flows during the injection and GC run (if using the optional
EPC module)
The parameters available depend on the instrument model and current configuration. For complete details about all possible method parameters, see the Advanced Operation
Guide .
Built-in methods
In addition to the 32 user- definable methods, the HS also stores 6 special methods:
Method
Default
Checkout
Qualification
MeOH in H2O
Sleep
Comments
A basic method, useful as a basis for new methods. Not editable.
The parameters needed for initial performance verification. Not editable.
The parameters needed for Agilent’s performance verification and qualification service. Not editable.
Basic starting parameters for analyzing methanol in water. Not editable.
Use the Sleep method to load settings for periods of inactivity. The sleep method is editable. To schedule the instrument to load the sleep method at a given time of day, see the Advanced Operation Guide .
50 Operation
Operation
Methods 6
Method
Wake
Comments
Use the Wake method to load settings after the sleep period ends, for example, to warm the vial oven or increase gas flows. If desired, the wake method can be simply the last analytical HS method run. The wake method is editable. To schedule the instrument to load the wake method at a given time of day, see the
Advanced Operation Guide .
Data system methods
If using an Agilent data system, you will primarily use the data system methods, rather than the methods stored locally in the HS. Data system methods save parameters for all associated instruments and devices, such as the GC and HS, plus all data analysis and reporting settings.
When running a sequence, the data system will download the setpoints to the HS as needed. HS data system method parameters appear on the HS display as a HOST method. The
HS does not permanently store HOST methods. HOST methods only remain until overwritten or until the HS is turned off.
51
6 Methods
Method Parameter Summary
This section lists method parameters, along with a brief description of each one. For more detailed information, see the Advanced Operation Guide .
Table 5 Common method parameters
Enabled in modes Parameter
[Temp] key
Oven
Loop/Valve
Transfer line
[Time] key
GC cycle time
Vial equib time
Pres equib time
Inject time
[Vial] key
Fill mode
Fill pressure
Fill flow
Fill volume, mL
Loop fill mode
Loop ramp fill rate
Loop final pressure
Loop equilibration
Vent after extraction
Description
Oven temperature for vial equilibration.
Temperature of the sample loop and valve.
Temperature of the transfer line (isothermal).
Time for the GC to become ready after an injection.
Time for the vial to equilibrate in the oven.
Time to allow for the pressure in the vial to stabilize after initial vial pressurization.
Amount of time to sweep the sample loop vapors into the GC inlet.
Fill modes: Flow to pressure and Fill to pressure
Fill mode: Flow to pressure
Fill mode: Constant volume
Loop fill mode: Advanced
Loop fill mode: Advanced
Loop fill mode: Advanced
Select how to pressurize the vial.
Target sample vial final pressure.
Flow rate used to pressurize the vial.
Specific volume of gas with which to pressurize the vial.
Select how the HS will fill the sample loop with gas after pressurizing and puncturing the sample vial.
How quickly to fill the sample loop.
Final target pressure for the filled sample loop.
Time set for the sample loop to stabilize after pressurization.
After the last extraction, and while the sample transfers to the GC, vent residual vial pressure to atmosphere.
(Other venting is provided during concentrating extractions under the [ Adv Function ] key.)
52 Operation
Methods 6
Table 5 Common method parameters (continued)
Parameter
Vial size
Enabled in modes
Shaking
[Carrier] key
Pressure (read only display)
[Adv Function] key
Extraction mode
# of extractions
Vent between extractions
Purge flow
Carrier control: GC Control
Concentrated extractions
Concentrated extractions
Purge time
Barcode reader
Sequence actions
Method development
[Adv Function] > Barcode reader
BCR action
BCR symbology
Enable BCR checksum
Description
Select the sample vial size for all vials using this method.
Set the level of shaking for the sample during equilibration in the oven. (111 vial model only)
For other carrier parameters, see the Advanced
Operation Guide .
See the Advanced Operation Guide .
Set the type of extraction for the method, Single,
Multiple, or Concentrated.
Enter the number of extractions to concentrate.
On or Off. Vent vial between concentrating extractions.
Purge sample probe and loop with vial pressurization gas after removing the vial from the probe.
Requires the 111 vial tray and optional barcode reader.
Select to set barcode reader parameters.
Set how the HS should handle unexpected sequence issues, such as a missing vial or vial size mismatch.
Access parameters to use when developing methods.
Requires the 111 vial tray and optional barcode reader.
Set whether and how to proceed if a barcode error occurs.
Set the expected symbology for barcodes used with this method.
Expect barcodes to use a checksum feature (availability also depends on barcode symbology).
Operation 53
6 Methods
To Create a Method
N O T E
To create a basic method, you will access the method parameters using the 4 component keys, in order: [Temps] ,
[Times] , [Vial] , and [Carrier] . For a listing of commonly- used
parameters, see “Method Parameter Summary”
.
1 When the HS is not processing samples, press [Temps] . The display shows the current oven, loop/valve, and transfer line temperature setpoints and actual temperatures.
a b c d
Scroll to Oven .
Use the keypad to enter the new oven setpoint, then press [ Enter ].
Enter the desired Loop/Valve temperature, then press
[ Enter ].
Enter the desired Transfer line temperature, then press
[ Enter ].
2
Temperature setting is complete.
Press [ Time ].
a Scroll to GC cycle time . b Use the keypad to enter the new GC cycle time , then press [ Enter ]. To determine the correct value to input, see
“To Determine the GC Cycle Time” .
c d e
Enter the desired Vial equib time , then press [ Enter ].
Enter the desired Pres equib time , then press [ Enter ].
Enter the desired Inject time , then press [ Enter ].
3
Time setting is complete.
Press [ Vial ].
a b c
Scroll to Fill mode .
Press [ Mode/Type] to display the selections for the vial fill mode. Scroll to the desired fill mode, then press
[ Enter ].
Enter any vial fill mode parameters, pressing [ Enter ] after each.
If using Constant volume
loop fill, the HS determine loop fill. Skip steps d
and
54 Operation
Operation
Methods 6 f d e g h
Scroll to Loop fill mode , then press [ Mode/Type] to display the selections for the sample loop fill mode. Select the desired loop fill mode.
Enter any sample loop fill mode parameters, pressing
[ Enter ] after each.
Scroll to Vent after extraction . Press [ On/Yes ] to vent the sample loop after the last each extraction, or [ Off/No] to leave the loop as- is.
Scroll to Vial size . Press [ Mode/Type ] to select the vial size from a list, then press [ Enter ].
Scroll to Shaking . Press [ On/Yes] to enable, then press
[ Mode/Type ] to select the level of shaking desired. Press
[ Off/No] to disable shaking for this method.
4
Vial settings are complete.
Press [ Carrier ]. If not using an optional EPC carrier gas module, these settings are disabled and the HS uses GC carrier gas control. If using the optional EPC carrier gas module, you can set parameters as defined by the configured carrier gas control mode.
Set carrier gas parameters using the same process as the other method parameters.
5
Carrier gas settings are described in the Advanced
Operation Guide .
Basic method parameters are complete. Save the method.
(See
In addition, the Adv Function key provides access to other method parameters, including multiple headspace extraction modes and functions useful during method development.
See the Advanced Operation Guide for more information.
55
6 Methods
To Save (Store) a Method
To save a method:
1 Press [ Method ].
2
3
Scroll to the method number to save.
Press [ Store ]. When prompted, press [ On/Yes ] to save, or
[ Off/No] to return to the selection list.
Alternately:
1 Press [ Store ].
2 When prompted, press [ Method ].
3
4
5
When prompted, scroll to the desired method number to save.
Press [ Enter ].
When prompted, press [ On/Yes ] to save, or [ Off/No] to return to the selection list.
56 Operation
To Edit a Method
Methods 6
To edit a method:
1
Load the desired method. See “To Load a Method”
.
2
3
Edit the method parameters as desired. See “To Create a
When done, save the method. See “To Save (Store) a
Operation 57
6 Methods
To Load a Method
To load a method:
1 Press [ Load ].
2 When prompted, press [ Method ].
3
4
When prompted, select the method to load from the list, then press [ Enter ].
When prompted, press [ On/Yes ] to load the selected method, or [ Off/No] to return to the selection list.
Alternately:
1
2
3
Press [ Method ].
Scroll to the desired method.
Press [ Load ]. When prompted, press [ On/Yes ] to load the selected method, or [ Off/No] to return to the selection list.
58 Operation
Methods 6
To Delete a Method
You can delete only the internal, user- defined methods. To delete a method:
1
2
3
Press [ Method ].
Scroll to the user- defined method to delete.
Press [ Delete ]. When prompted, press [ On/Yes ] to confirm.
Alternately:
1 Press [ Delete ].
2 When prompted, press [ Method ].
3
4
When prompted, scroll to the method number to delete, then press [ Enter ].
When prompted, press [ On/Yes ] to delete the selected method, or [ Off/No] to return to the selection list.
Operation 59
6 Methods
To Determine the GC Cycle Time
The HS uses the GC cycle time to calculate throughput and timing. An accurate GC cycle time is crucial to optimizing throughput and for correctly processing samples.
If the GC cycle time is too long, this can cause:
• Lowered throughput. Vials wait longer than needed before processing.
If the GC cycle time is too short, this can cause:
• Sequence faults. Vials may be processed too early and may sit too long while waiting for the GC to become
Ready.
It is better to enter a longer time than needed than to enter too short a time and possibly reduce sample quality.
The GC cycle time is the GC run time plus any additional time needed for the GC to execute any post- run program, then return to a ready state.
To determine the GC cycle time
To determine the GC cycle time , program the GC to perform a sequence of two or three blank (no injection) runs.
• If using a data system, you can determine the cycle time from the data system sequence log. Compare the start times for the runs. A good GC cycle time is the average difference between the start times, plus 0.2 to 0.5 minutes.
• If not using a data system, watch the GC. Count the time between the start of the first run and when the GC becomes Ready for the second run. Then, add 1 to 2 minutes.
You can also estimate the GC cycle time without making a run.
By adding the GC oven program duration and the duration of any post- run programs, you can get close to the true cycle time. However, temperature programming and cryogenic operation can make estimation more difficult. Add extra time.
Also consider time for data processing. While in most cases data processing is not a problem, a very busy data system may need extra time between samples.
60 Operation
Methods 6
Validating the GC cycle time
Look at the GC run time. The GC cycle time cannot be less than the total run time.
Look at the GC post run program duration. The GC cycle time cannot be less than the total run time plus the post run program duration.
Operation 61
6 Methods
62 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
7
Sequences
Sequences and Throughput (111 vial model) 68
This chapter defines the headspace sampler sequence, and describes how to load, save, create, and edit a sequence.
Agilent Technologies
63
7 Sequences
What Is a Sequence?
A sequence for the 7697A Headspace Sampler is an ordered series of sample vials to prepare and inject, including the method needed to prepare each vial. For the 7697A HS:
• All sample processing occurs in a sequence. To run a sample, there must be a sequence defined.
• A sequence can skips vials.
• A sequence can run a vial more than once.
• A sequence does not require any particular vial order.
Running vials 1, 49, 5, 2, 3, and 101 is valid.
A sequence consists of a series of lines . Each line contains a range of vials, the method number to use for these vials, and the number of injections to make using each vial.
To view a sequence, press [ Seq ].
SEQUENCE (line 1 of 6)
Method: Stored method #1<
Vials 1-1
Injections per vial 1
Current line
Use the scroll keys to view all lines in the sequence.
Sequences, extraction modes, and vial punctures
In the sequence you can specify the same vial in as many entry lines as desired. How the HS sampler processes the vial depends on the method Extraction mode and the sequence:
• Extraction mode is Single .
If a vial appears more than once in a sequence, or if the number of injections is greater than one, the vial is completely reprocessed for each entry or injection.
• Extraction mode is Multiple .
If the number of injections per vial is greater than 1, the
HS will puncture the vial once, then make the extractions and injections. The HS will not perform multiple vial punctures.
64 Operation
Operation
Sequences 7
When more than one consecutive entry exists for a vial, and the entries use the same method, the HS will puncture the vial once, then make the extractions and injections. The HS will not perform multiple vial punctures.
• Extraction mode is Concentrated .
If a vial appears more than once in a sequence, or if the number of injections is greater than one, the vial is completely reprocessed for each entry or injection.
See also “To Create a Sequence”
.
How many sequences can the HS store?
The HS can store up to 9 sequences internally. In addition, the HS can temporarily store sequences that are downloaded from the data system.
65
7 Sequences
Priority samples
A priority sample is a vial that you want to run as soon as possible, before other vials in the currently- running sequence. Use the priority sample feature to insert one or more special vials into the current sequence without stopping the sequence, editing it, and restarting it.
This feature is available only for the 111 vial model, and only when operating in standalone mode. (The feature is not
needed when using an Agilent data system. See “Priority samples using an Agilent data system”
.)
Priority sample locations
The priority sample locations are vial locations 109, 110, and
66
Priority sample 3 (111)
Priority sample 2 (110)
Priority sample 1 (109)
Figure 14 Priority sample locations
How the HS processes priority samples
The first time you press [ Priority Sample ] during a running sequence, the HS checks the first priority sample location
(
). It takes the vial from that location and inserts it into the current sequence at the next appropriate time. (The
HS does not interrupt any ongoing vial moves or processing.)
Operation
Operation
Sequences 7
• If the vial is not present, a vial not found error occurs.
(See the Advanced Operation Guide for information about how to set HS handling of missing vials.)
• The HS continues to process any vial it is handling before it looks for the new priority sample vial.
• The HS uses the method of the last vial placed in the oven to process the priority sample vial. If you wish to use another method, you must interrupt the current sequence.
• You may insert only three priority samples per sequence.
• Avoid using sample vial positions 109–111 if you might use priority samples. If you use positions 109–111 in your normal sequences, you will need to replace the normal sequence vials with the priority vials, run the priority vials, then put the normal sequence vials back.
Consecutive presses of [ Priority Sample ] cycle through the priority locations.
1
2
3
The first time you press [ Priority Sample ], the HS checks for and runs the vial in position 1.
• The Vial Status names this vial P 1 .
The second time you press [ Priority Sample ], the HS checks for and runs the vial in position 2.
• The Vial Status names this vial P 2 .
The third time you press [ Priority Sample ], the HS checks for and runs the vial in position 3.
• The Vial Status names this vial P 3 .
If you press of [ Priority Sample ] a fourth time, an error message appears. You may only insert 3 samples into the sequence using this feature. If you need to make a fourth change, stop the sequence and edit it to add the needed sample.
Priority samples using an Agilent data system
The Agilent data system already provides flexibility for editing a running sequence. When using an Agilent data system, the priority samples feature is disabled. To insert a new sample into the running sequence, simply edit the sequence to insert the new sample(s). Refer to the data system’s online help for details.
67
7 Sequences
Sequences and Throughput (111 vial model)
The HS optimizes throughput by checking the temperature and shaking parameters for the vials specified in the current sequence. When consecutive vials share the same temperature and shaking settings, the HS will examine the timing parameters for the samples, then calculate the best times to place each vial into the oven. This approach maximizes the number of vials equilibrating at a time.
Vials without the same temperature and shaking parameters will not be handled until the preceding samples leave the oven.
For more information, see the Advanced Operation Guide .
68 Operation
Sequences 7
To Create a Sequence
To create a new sequence:
1 Press [ Seq ].
2 Select the method for the first vial range.
a Press [ Mode/Type ].
3
4 b c
Scroll to the desired method.
Pres [ Enter ] to select this method.
Enter the range of vial to prepare with this method.
• For a simple range, for example vials 1 through 5, press [ 1 ][–][ 5 ][ Enter ].
• For a single vial, enter the vial twice, for example,
[ 6 ][ – ][ 6 ][ Enter ].
Enter the number of injections per vial, then press [ Enter ].
5
6
7
The sequence is created. You can now store the sequence
(see
), run it (see
Series (Sequence) of Samples” ), or continue to add
additional lines as described below.
To enter another range of vials, press [ Insert/Append ].
When prompted, select where to add the new sequence line then press [ Enter ]:
• Append to sequence : add the new line to the end of the sequence
• Insert into sequence : add the new line before the current sequence line
Enter the method, vial range, and number of injections per vial for the new line.
Repeat
as needed.
You can now store the sequence (see “To Save (Store) a
) or run it (see “To Run a Series (Sequence) of
).
Operation 69
7 Sequences
To Save (Store) a Sequence
Storing a sequence saves the current sequence to nonvolatile memory. You do not have to be viewing the current sequence to save it.
If editing the sequence, save it as follows:.
1
2
3
4
5
Press [ Store ].
When prompted, press [ Sequence ].
When prompted, scroll to the desired sequence number to save.
Press [ Enter ].
When prompted, press [ On/Yes ] to save, or [ Off/No] to return to the selection list.
Alternately:
1 Press [ Seq ].
2
3
Scroll to the sequence number to save.
Press [ Store ]. When prompted, press [ On/Yes ] to save, or
[ Off/No] to return to the selection list.
70 Operation
Sequences 7
To Load a Sequence
To load a sequence:
1 Press [ Load ].
2 When prompted, press [ Seq ].
3
4
When prompted, select the sequence to load from the list, then press [ Enter ].
When prompted, press [ On/Yes ] to load the selected sequence, or [ Off/No] to return to the selection list.
Alternately:
1
2
3
Press [ Seq ].
Scroll to the desired sequence.
Press [ Load ]. When prompted, press [ On/Yes ] to load the selected sequence, or [ Off/No] to return to the selection list.
Operation 71
7 Sequences
To Edit a Sequence
To edit a sequence:
1 If desired, load the sequence to edit.
2 Scroll through each line of the sequence.
• Change the method, vial range, and injections per vial for each line as desired.
• Delete the entire current line by pressing [ Delete ].
Press [ On/Yes] to confirm, or [ Off/No ] to cancel.
72 Operation
Sequences 7
To Delete a Sequence
To delete a sequence:
1 Press [ Delete ].
2 When prompted, press [ Seq ].
3
4
When prompted, scroll through the list of sequences to the desired sequence. Press [ Enter ] to select this sequence.
When prompted, press [ On/Yes ] to confirm and delete the sequence, or [ Off/No ] to cancel.
Alternately:
1
2
3
Press [ Seq ].
Scroll to the user- defined sequence to delete.
Press [ Delete ]. When prompted, press [ On/Yes ] to confirm, or [ Off/No ] to cancel.
Operation 73
7 Sequences
Method Sequence Actions
When the HS encounters certain problems during a sequence, it has the ability to skip vials, continue anyway, or pause the sequence. The settings to control HS behaviors during sequence execution are called sequence actions .
Sequence actions are part of the HS method, and therefore can change from sample to sample during sequence execution. Use Sequence Actions to specify what the HS should do when it encounters issues such as a vial size mismatch, missing vial, barcode error, and similar issues. For more details, see the Advanced Operation Guide .
74 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
8
Running Samples
To Run a Series (Sequence) of Samples 76
To Pause a Running Sequence 77
To Run a Priority Sample During a Sequence 79
To View Vial and Sequence Status 81
Sequence Control with an Agilent Data System 83
To run samples on the Agilent 7697A Headspace Sampler, create and run a sequence.
Agilent Technologies
75
8 Running Samples
To Run a Series (Sequence) of Samples
2
3
1
4
5
Create or load the first method. (This prepares the HS temperatures and flows for the first sample.)
• If needed, create the method. See
.
• If already created, load the existing method. See
.
Prepare the sample vials.
Load the sample vials into the tray. See “To Load a
Sample into the Tray (111 Vial Model)” or
Sample into the Tray (12 Vial Model)”
.
Create or load the sequence to run.
• If needed, create the sequence. See
• If already created, load the existing sequence. See
Press [ Start ].
When the HS becomes ready (all temperatures and flows are at method setpoint), the HS will begin processing the samples.
To view the progress of the vials, press [ Status ]. See also
“To View Vial and Sequence Status” .
76 Operation
Running Samples 8
To Pause a Running Sequence
Press [ Stop ] once.
• All vials currently in process will continue processing through injection (and return to the tray).
• No more vials will start processing.
Operation 77
8 Running Samples
To Stop a Running Sequence
To stop a running sequence, press [ Stop ] twice within 5 seconds. The current sample immediately aborts. All processing stops. All vials are returned to the tray (111 vial model). No further vials are processed.
78 Operation
Running Samples 8
To Run a Priority Sample During a Sequence
N O T E
This feature is available only with the 111 vial model, and only when operating in standalone mode. If using an Agilent data system, edit the running sequence instead.
You may run only 3 priority samples during a sequence. You should avoid using sample vial positions 109–111 if using priority samples.
To run a priority samples during a sequence:
1 Check the status of the sequence. Find the vial last placed into the oven. (Press [ Status
]. See “To View Vial and Sequence Status” .) The HS will use this vial’s method
to process the new sample.
2 Place the new sample vial in the next priority sample position. Start with priority sample position 1. See
Priority sample 3 (111)
Priority sample 2 (110)
Priority sample 1 (109)
Figure 15 Priority sample locations
3 Press [ Priority Sample ].
Operation 79
8 Running Samples
4 The new vial will be processed using the method for the last vial placed into the oven.
• The tray will check the first priority sample position for a sample vial as soon as it is ready to load another sample into the oven.
• To track the vial status, press [ Status ] until the display reads VIAL STATUS . The vial number will show as P n , where n is 1, 2, or 3.
Priority sample
VIAL STATUS
1: Completed
2: Equilibrating 15:18
P 1: Equilibrating 18:35
80 Operation
Running Samples 8
To View Vial and Sequence Status
While a sequence is running, press [ Status ] to view the status of the sequence and the individual vials. The [ Status ] key cycles through displays for readiness state, temperatures and setpoints, and vial status.
Readiness status
This display shows the overall state of the headspace sampler, along with messages regarding system readiness.
These messages can include warnings, faults, or other conditions that prevent the HS from becoming ready.
STATUS - Ready
Ready for start sequence
Setpoint status
This display lists the setpoints and current values for HS temperatures, flows, and pressures. To change the information shown in this list, see the
.
STATUS
Oven temp 100.0 100.0
Loop temp 110.0 110.0
Transfer line 115.0 115.0
Operation 81
8 Running Samples
Vial status
This display shows the status information for the next few vials listed in the sequence. The HS will display:
• Time until a vial operation is scheduled to occur.
• Current or next vial operation (for example, equilibrating, injecting, loading, and so forth).
• Completed.
VIAL STATUS
1: Completed
2: Equilibrating 15:18
P 1: Equilibrating 18:35
82 Operation
Running Samples 8
Sequence Control with an Agilent Data System
In general, when using an Agilent data system, use the data system for starting, stopping, and pausing a sequence.
However, an Agilent data system can deactivate the [ Start ] key.
Otherwise, pressing the [ Start ] and [ Stop ] keys on the HS provides the same functionality when in standalone control or data system control. Note that
Operation 83
8 Running Samples
84 Operation
Agilent 7697A Headspace Sampler
Agilent 7697A Operation
9
Configuration
To Configure the Headspace Sampler 87
This section describes how to configure the Agilent 7697A
Headspace Sampler before use.
Agilent Technologies
85
9 Configuration
What is Configuration?
Most of the hardware used in the headspace sampler (HS) is known by the programs that control it. For example, the HS can detect whether or not a transfer line is installed, and it knows whether it has a 12 vial or 111 vial tray. However, some settings, such as gas types, sleep and wake modes, sample loop size, and similar are not detected. The HS stores your inputs for these items as settings. Configuration is the process of making these settings. The current configuration is the collection of these settings at any given time.
As part of installation, you configured the HS. However, you will need to reconfigure the HS whenever you want to do any of the following:
• Change a gas type
• Add an accessory, such as the optional EPC module or barcode reader
• Change the sample loop
• Change the carrier gas control mode
• Enable, disable, or change the resource conservation settings
• Change the standby flow (the purge flow used to keep the system clean when between sequences)
86 Operation
Configuration 9
To Configure the Headspace Sampler
Press [ Config ] to access the configuration parameters.
lists the most common parameters, along with brief descriptions. Refer to the Advanced Operation Guide for complete information.
Table 6 Most common configuration parameters
Setting
Vial Gas type
Loop Volume (mL)
Carrier Gas type
Comments
Use the [ Mode/Type ] key to select the correct gas type.
Enter the sample loop volume, in mL, and press
[ Enter ].
If available. Use the [ Mode/Type ] key to select the correct gas type.
Carrier
Standby flow
Status
Clock
Use the [ Mode/Type ] key to select the desired carrier gas control mode. If the optional EPC module is not installed, this mode is automatically set to GC
Control .
Input the desired flow used to purge the sampling probe between sequences, then press [ Enter ]. To turn the flow off completely (not recommended), press
[ Off/No ].
Scroll to each setpoint that you want to appear and press [ Enter ]. Select parameters in the order you wish them to appear. For example, select the parameter you want to appear at the top of the list first,
Select [ Clock ] to access of list of parameters that allow you to set the current time, current date, time zone, and desired date format. See the Advanced
Operation Guide .
APG polarity See Installation and First Startup .
Instrument Schedule
and the Advanced
Operation Guide .
Operation 87
Agilent Technologies
Resource Conservation
The Agilent 7697A Headspace Sampler provides the following features to conserve resources:
• Instrument schedule (sleep and wake methods): Load a method at a specified time during the day to reduce flows and temperatures, then load another method to restore them before operation.
• Control over standby purge flow.
• More advanced resource conservation features are available if using an
Agilent data system. See the data system help.
For details, refer to the Advanced Operation Guide .
©
Agilent Technologies, Inc. 2011
advertisement
* Your assessment is very important for improving the workof artificial intelligence, which forms the content of this project