安捷伦7694 顶空进样操作说明（英文版）

仪器资料 · 发表于 2017-6-8 16:45:49

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 7694 Headspace Sampler . ................................................................................. 7
Oven (G1289/G1290)  . ................................................................................................ 7
Heated Zones (G1883)  . ............................................................................................. 8
Vial Tray (G1289/G1290) . .......................................................................................... 9
Vial Transport Arm (G1289/G1290) . ........................................................................ 9
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 . ................................................................................................ 19
Standard Headspace Extraction . ................................................................... 19
Multiple Headspace Extraction with Multiple Vial Puncture–
G1289/G1290 only . ........................................................................................... 21
Multiple Vial Puncture with Constant Heating Time–G1289/G1290 only . 22 Multiple Headspace Extraction with Single Vial Puncture . ....................... 23
Multiple Headspace Extraction for Analyte Concentration–
G1289/G1290 only . ........................................................................................... 23
Chapter 3 The Keypad
Accessing Functions . ................................................................................................26
Editing Setpoints . ......................................................................................................26
The G1883 Keypad . ..................................................................................................26
The G1289/G1290 Keypad . ......................................................................................28
Keys and Their Functions . ......................................................................................30
Start (G1883 only) . ...........................................................................................30
Stop/Reset (G1883 only)  . ................................................................................30
Start/Stop (G1289/G1290 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/G1290 only) . ........................................................................36
Tray Advance (G1289/G1290 only)  . ...............................................................36
Enter . ................................................................................................................37
Clear . ................................................................................................................37
Numeric Keypad . ..............................................................................................37
Adv Fctn { } . .....................................................................................................37
Chapter 4 Using the Adv Fctn Key
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
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 6890/6850 GC Liner  . ..................................................................... 75
Chapter 8 Running a Sample
Setting Conditions . .................................................................................................. 78
Flow Rates . ....................................................................................................... 78
Setting the Carrier Gas Flow Rate for the G1883/G1290 . ........................... 80
Setting the Vial Pressurization Gas Pressure for the G1883/G1290    . ...... 81
Setting Carrier and Vial Pressurization Flows for the G1289  . ................... 81
Chapter 9 Maintaining the Instrument
Common Replacement Parts and Consumables . ...............................................85
Fuse Locations . .......................................................................................................88
Changing the Sampling Needle  . .............................................................................89
Changing the Sample Loop . ....................................................................................92
Steam Cleaning the Pneumatic System . ................................................................95
Installing the Transfer Line onto the Volatiles Interface . ...................................96
Aligning the Vial Loader (G1289/G1290 only)  . .....................................................97
Adjusting the potentiometers . ................................................................................97
Procedure . .................................................................................................................99
Other vial handling adjustments  . .........................................................................101
Checking carousel adjustment . ............................................................................101
Leak Testing: General Information . .....................................................................103
Leak Testing a G1289 to 6890 GC Interface . .......................................................105
Carrier Gas Flow Path . ..........................................................................................105
Carrier Flow Path Pressurization Test . ...............................................................107
Vial Pressurization Gas (Aux) Flow Path  . ..........................................................108
Leak Testing a G1290/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 . .....................................................................................119
Vial Handling Problems (G1289/G1290 only) . ....................................................119
Gripper Arm Doesn’t Pick Up Sample Vial . ................................................119
Sample Vial Doesn’t Drop Down Into Oven  . ..............................................120
Vial Not Raised and Lowered in Oven . ........................................................121
Vial Not Loaded/Vial Retained Warning . .....................................................121
Vial Jam Problems (G1289/G1290 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 (G1289/G1290 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 (G1289/G1290) . ...................................... 133
Glossary  . .................................................................................... 135
Index  . ......................................................................................... 141