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Agilent 7694 Headspace Sampler

1. Enter 7 2 Enter v vial equilibration step in a series VIAL NO AND Displays the vial number in each oven LOC carousel location i KEYBOARD LOCK Allows you to lock or unlock the keyboard KEYBOARD All keys are functional UNLOCKED 7 Enter v KEYBOARD LOCKED Numeric and enter keys are nonfunctional MANUAL The 0 and 1 keys control the motors and OPERATION valves to let you check their operation For a complete list of operations see page 48 P PRESSURE UNITS Changes the pressure units PSI Expresses pressure units in psi Enter v BAR Expresses pressure units in BAR x2 KPA Expresses pressure units in KPa 42 Table 5 continued Adv Fctn LLLA Key Sequence Display DEFAULT METHOD METHOD LOADED DEFAULT METHO Using the Adv Fctn Key List of Advanced Functions by Model Definition Function Loads the default method into active memory Notifies you know that the method is now loaded Enter v MULTI HS EXTR EXTR PER VIAL PUNCTURE 02S 1 M Sets parameters for multiple headspace extraction Specifies the number of extractions per vial 1 10 To access the next display you must specify 2 or more extractions Specifies single or multiple puncture mode Enter b d HAN
2. ae Em 3 Chapter 2 Introduction to Headspace and to the 7694 Headspace Sampler Overview of Headspace Analysis esses ener 6 The 7694 Headspace Sampler sess a nnn nnne nnns 7 Oven GI2Z89 GIZ90 iei eem t ie setts enim eee pte Er Eee yeasts 7 Heated Zones G1883 occ eeecescescecseceeeceeeeeacecsceesecesaececeeceeeeeesaecaeeeeeceeeeneeenes 8 G1289 G1290 9 Vial Transport Arm G1289 G1290 sess nente 9 Sampling System eee rece e eec P eee eR Reds 10 Transfer lane eee tea entera red er ener eren etae en ete ier Dea ELE RE 10 Keypad and Display eerte enne enhn nennen nennen 10 Prieuriatics 5 decet te ect et et te 11 Principles Operation citate eie weiter detis 13 General Operation eet eie e E Ete Ee ae 13 Power On Diagnostics 14 Standby Condition ct dex 14 Vial Pressu rlzatiOn eee ciet etre cette eee ena ae eode etna SEE eee Pea eso eade 15 Filling the Sample Loop enne nennen 16 Loop Equilibration aere e ete 17 Injecting the Sample 17 End of Cycle and Vial Recovery essen enne enne 18 Modes of Operation ise areia eene nnne tenen nnne nennen enter entes rennen 19 Standard Headspac
3. 112 Tightening the PTV Septumless Head Using the Leak Test Procedure 113 Chapter 10 Troubleshooting Chromatography Problems eese enne nennen nennen enne enne 116 DEDI c 116 Bad Data Bad Beaks ane 117 Unwanted Peaks Present eee eeeeee ee ee 119 Vial Handling Problems G1289 G1290 only essere 119 Gripper Arm Doesn t Pick Up Sample Vial seen 119 Sample Vial Doesn t Drop Down Into Oven eere 120 Vial Not Raised and Lowered in Oven essere 121 Vial Not Loaded Vial Retained Warning essen 121 Contents Vial Jam Problems G1289 G1290 only eese 121 Recovering from vial jam problems eese 122 Mechanical Electrical Problems 122 Instrument Resets Continuously esses eene 122 tein d mus 123 Oven Carousel Won t Rotate Properly essere 123 Oven Carousel Won t Agitate 123 Sample Tray Doesn t Stop at Correct Location G1289 G 1290 only 124 Sampling Sequence Won t Start essere 124 Second Method in Sequence Won t Start 125 Zones HEALS tt re here Neosat oett reete en ta e e Eee US 125 Pressures Are Wrong ccssccesse
4. 4 Enter Selecting Keyboard Lock displays the following message KEYBOARD UNLOCKED This is the default condition To lock the keyboard scroll to the following display KEYBOARD LOCKED Once the keyboard is locked scrolling to KEYBOARD UNLOCKED will unlock the keyboard 47 Using the Adv Fctn Key Advanced Function Descriptions MANUAL OPERATION G1883 Adv 8 Enter This function manually operates the vial carousel advance and valves to check for malfunctions Selecting Manual Operation displays the last operation used The cursor keys will scroll through the messages Selected Operation Key Pushed Result VIAL LOAD 1 To mid position from down position vial in heated zone 1 again To top position needle in vial Vial goes into carousel out of heat and needle PRESS VALVE 0 Off valve is open to flow 1 On valve is closed to flow VENT VALVE 0 Off valve is closed to flow 1 On valve is open to flow SAMPLE VALVE 0 Off the loop to pressure vent valves 1 On the loop is in the carrier stream CAROUSEL POSITION 0 Move location down 1 Move location up G1289 G1290 Adv 4 Enter This function manually operates the vial gripper arm tray advance oven advance vial loading and valves to check for malfunctions It is especially useful for checking that the gripper arm and gripper mechanism are properly aligned The cursor keys scroll through the following menu of items
5. Vial Not Loaded Vial Retained Warning Probable Causes e Robotic arm microswitch out of adjustment e Vial remains in robotic arm Suggested Actions Contact Agilent service Vial Jam Problems G1289 G1290 only In certain situations vials will jam when the unit attempts to drop one vial on top of another in the oven or tries to place a vial in the sample tray when a vial is already in that location Vial jam problems can also result from misalignment of the robotic arm or oven carousel This may cause the motor for the oven carousel or the robotic arm to jam 121 Troubleshooting Mechanical Electrical Problems WARNING Recovering from vial jam problems The headspace sampler attempts to recover from vial jams and continue where it left off Sometimes this is not possible The simplest way to recover from a vial jam problem is as follows 1 Determine which vial was the last one that was completed the sample was run and you have believable run data Vials removed from the oven are hot 2 Clear the jam Note that if the robotic arm jams in the x axis a protection circuit may engage disabling the arm for 10 to 15 minutes until the circuitry cools down After this time has elapsed press Adv 1 and Enter to reset the sampler Turn the sampler off then on again The sampler should return all vials back into the tray in their appropriate positions If it does you have recovered from t
6. GRIPPER Y AXIS UP GRIPPER X AXIS 1 TRAY ADVANCE OVEN ADVANCE 48 Note Using the Adv Fctn Key Advanced Function Descriptions VIAL LOAD DOWN PRESS VALVE ON VENT VALVE OFF SAMPLE VALVE OFF OVEN CALIBRATION The 0 and 1 keys activate the appropriate motors according to the display for x and y movement of the robotic arm movement of the sample tray and oven carousel and toggle the on off states for the valves When you exit Adv Fctn 5 all the motors are not reset to their default states Use Adv Fctn 1 Enter to reset If the operations do not work Troubleshooting on page 116 then call Agilent service Oven Calibration Contact Agilent service to recalibrate the oven MULTI HS EXTR G1289 G1290 Adv 8 Enter MHE is not allowed if Parameter Increment is on This function sets the parameters used for multiple headspace extraction MHE in single puncture or multiple puncture recommended mode Pressing Adv Fctn 8 and Enter brings up the following display EXTR PER VIAL 4 example The user selects a value of 1 10 followed by Enter for the number of extractions per vial If extractions per vial 1 default then other displays associated with MHE are not available with the scroll keys 49 Using the Adv Fctn Key Advanced Function Descriptions While not recommended you can also set single puncture mode for MHE by pressing the cursor key to bring up the follo
7. ON and the bubbling should stop within 10 15 seconds If the bubbling lasts much longer the vent valve or associated flowpath may be restricted Contact Agilent service Note that if the vent flow path is restricted you may be overpressurizing your sample vials When the problem is fixed your sensitivity may appear to decrease because you are now injecting the appropriate amount of sample for your method 112 Maintaining the Instrument Tightening the PTV Septumless Head Using the Leak Test Procedure Tightening the PTV Septumless Head Using the Leak Test Procedure If you are using a PTV inlet with a septumless head you can use the leak test procedure described in Carrier Gas Flow Path on page 105 or Carrier Gas Flow Path on page 110 to help you properly tighten the septumless head onto the needle As you tighten the fitting on the needle monitor the flow rate on the GC front display When the flow rate indicates there is no leak the connection is tight enough 113 Maintaining the Instrument Tightening the PTV Septumless Head Using the Leak Test Procedure 114 Troubleshooting Troubleshooting This chapter discusses the possible causes and the solutions for chromatography problems or instrument failures Chromatography Problems No Peaks Probable Causes e Vial cracked Vial cap leaking e Sample vial empty e 10m vial used without adapter e Method not sensitive enough e
8. 81 Pressure key Description 36 Using 36 Pressure Units Adv Fctn 6 Description 52 Pressure Valves Adv Fctn description 53 Pressurization time Description 62 Entering 62 Principles of operation End of cycle 18 Filling the sample loop 16 Index General operation 13 Injecting the sample 17 Loop equilibration 17 Standby condition 14 Vial pressurization 15 Vial recovery 18 Replacement parts common 85 Replacing Sample loop 92 Sampling needle 89 Robotic arm Description 9 Running a sample 78 S Sample injection time Description 62 Entering 62 Sample loop Changing 92 Equilibration description 17 Filling description 16 Locating 94 Sample tray Advancing 36 48 Home position 36 Loading vials 58 Malfunction 124 Moving 36 Using adapters 58 Sample running 78 145 Index Sampler cover Removing 89 92 Samples Preparing 56 Size effects of 73 74 Samples more than 44 G1290 G1289 66 Sampling needle Changing 89 Locating 91 Sampling system Description 10 Saving Methods 64 Sequence Entering methods 65 Method not starting 125 Not starting 124 Setpoints Clearing 37 Entering 26 37 Setting conditions Flow rates 78 Shaking vials Description 34 Using 34 Stabilize time Adv Fctn 2 Description 53 Standalone sampler Pneumatics description 11 Standard headspace extraction Description 19 Standby condition Description 14 Start stop key Using 30 Sta
9. Agilent 7694 Headspace Sampler Operating Manual 9 Agilent Technologies 2000 All Rights Reserved Reproduction adaptation or translation without permission is prohibited except as allowed under the copyright laws Part number 61290 90317 First Edition 3 2000 Replaces Part No 61290 90310 Operating and Service Manual and part No 61883 90310 Operating and Service Manual HP is a registered trademark of Hewlett Packard Co Silcosteel 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 Il 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 cu
10. Key Sequence Display Definition Function _ START or STOP Starts and or stops a run op Zone OVEN Sets oven equilibration temperature Temps LOOP toms J Y J ane 2 TR LINE Sets loop temperature Sets transfer line temperature Event GC CYCLE TIME Times CE VIAL EQ TIME mm J j E PRESSURIZ TIME m v Time to complete GC run Time vial spends heating in oven Time gas enters vial through needle 28 Table 3 continued Key Sequence Event mm v x3 Event mm Event ma Y xb Display FILL TIME LOOP EQ TIME INJECT TIME The Keypad The G1289 G1290 Keypad Definition Function Time when gaseous contents of vial pass through loop to vent Time when gases in loop equilibrate Time when gases in sample loop are swept into the GC Vial Parameters FIRST VIAL First vial analyzed during the method Vial Parameters Vial Parameters ivy X 2 LAST VIAL SHAKE 0 1 2 Last vial analyzed during the method Sets agitation level of oven carousel 0 off 1 low 2 high Load Method LOAD METHOD Moves a method from stored to active memory for current use Store Method STORE METHOD Moves a method in active memory into one of four memory storage locations Chain Methods METH 5 Strings methods together to form a sequence P
11. Probable Causes Chain Methods Off Parameter Increment on Incorrect sequence entered Vials not loaded correctly Setpoints for second method not reached Suggested Actions a ON Chain Methods On Turn off Parameter Increment Check the sequence entered Check that the vials are loaded in the sample tray correctly Check that the setpoints for the second method are reached Call Agilent service Zones Won t Heat Probable Causes Oven temperature sensor defective Heater band vial heater not working Fuse blown 125 Troubleshooting Mechanical Electrical Problems Suggested Actions 1 Measure R 111 ohms at connector pins 9 10 11 12 Replace the sensor if necessary See your service manual or contact Agilent service 2 Check the heaters line on J3 on the MK12 connector pins 9 10 11 12 Replace the heater if necessary Have a qualified service technician check the fuses Call Agilent service Pressures Are Wrong Probable Causes e Leaks in system e Gas supply exhausted Suggested Actions 1 Check the system for leaks 2 Replace the gas cylinder 3 Call Agilent service 126 Error Messages Error Messages This chapter describes various error messages that accompany machine failures and the means to correct the failures Most errors cause the sampler to stop running the current method You may need to remove vials from the carousel re loa
12. 4 Quick Reference of G1883 Advanced Functions Key Sequence A ae Display GC READY TYPE CONST HEATING TIME KEYBOARD LOCK PRESSURE UNITS STABILIZE TIME PARAMETER INCR MANUAL OPERATION PRESSURE VALVES VALVE COUNT Definition Function Indicates the current GC mode Indicates the GC is in constant heating time mode Not used Allows you to lock or unlock the keyboard Changes the pressure units Sets wait time between oven reaching initial setpoint and first vial loading During method development set to increment vial temperature or equilibration times between runs Manually operate carousel advance and valves Display current carrier gas or vial pressurization gas pressure Displays the number of times the sampling valve has actuated 41 Using the Adv Fctn Key List of Advanced Functions by Model Table 5 Quick Reference of G1289 G1290 Advanced Functions Key Sequence Display STABILIZE TIME Definition Function Sets wait time between oven reaching initial setpoint and first vial loading PARAM INCREMENT VIAL EQ STEP OVEN TEMP STEP Sets incremental time that the vials a series spend in the oven Sets increment in temperature of oven for
13. 61 Event times key Using 32 F Flow rates General rules 78 Setting auxiliary gas 73 Fuses locations 88 G GC cycle time Description 32 61 Entering 32 61 142 Gripper arm See Vial gripper arm 97 Gripper axis Changing 48 H Handshake mode Adv Fctn 9 Description 45 Headspace analysis Overview 6 Horizontal loader Adjusting gripper arm 97 Inject time Description 33 Entering 33 Injection Description 17 K Key functions G1289 G1290 28 Key operations Adv 37 Chain methods 36 Description 26 Enter 37 Event times 32 Link methods 36 Load method 35 Numeric keypad 37 Pressure 36 Start stop 30 Store method 35 Index Tray advance 36 Vial parameters 34 Zone temps 31 Keyboard lock Adv Fctn 4 Description 47 Keypad Description 26 Locking unlocking 47 Keypad and display Description 10 Keys functions G1883 27 L Link methods key Description 36 Using 36 Load method by Using 64 Load method key Using 35 Loading Methods 35 Loop equilibration time Description 33 62 Entering 33 62 Loop fill time Description 33 62 Entering 33 62 Optimizing 72 Loop temperature Entering 60 143 Index M Manifold cover Removing 90 93 Manual generation Adv Fctn 5 Description 48 Matrix effects For optimizing method 72 Mechanical electrical troubleshooting Carousel not agitating 123 Carousel not rotating 123 No power 122 Sample
14. GC CYCLE TIME The time required for the entire GC run to be completed It is the sum of the GC run time and GC equilibration time read from the GC front panel and an estimate of the cool down time required if any This time allows the 7694 Headspace Sampler microprocessor to introduce samples into the oven most efficiently and avoid injecting a sample before the GC is ready The allowed 32 The Keypad Keys and Their Functions range of values for the cycle time is 1 0 to 999 minutes The recommended minimum cycle time is 2 5 minutes VIAL EQ TIME Vial Equilibration Time Time the vial spends in the oven heating The length of time you should use depends on the type of sample solid liquid the amount of sample and the partition coefficient of the analytes The sample may or may not come to equilibrium e The allowed range of values is 0 00 to 999 9 minutes e sampler may extend the actual equilibration time if more time is needed to put the next vial into the carousel before starting the next run e The recommended minimum time is 5 0 minutes PRESSURIZ TIME Pressurization Time Time during which the vial pressurization gas is introduced into the sample vial The allowed range of values is from 0 00 to 99 99 minutes LOOP FILL TIME Time in which the headspace vial pressurization gas mixture passes through the sample loop to vent The allowed range of values is from 0 00 to 99 99 minutes LOOP EQ TIME L
15. GC EPC Gas saver Per method Gas type Per method Column Mode Per method Initial flow 4 0 ml min Initial pressure Per method Outlet pressure Ambient per detector Set the split flow to 4 ml min The GC total flow will read 11 ml min With an electronic flow meter connected to the GC split vent turn up the headspace carrier gas flow until the flow rate out the split vent equals the flow rate desired in the column Because the split ratio is 1 1 this flow rate equals the column flow rate See Figure 14 Remove the flow meter Note that the GC and Headspace pressure readings should be similar Record the headspace pressure reading you can use it to set up future checkout runs Caution The added flow of the headspace sampler will cause the flow calculations of the inlet to be incorrect If your added flow and pressure exceed the limits of the inlet the GC may go Not Ready 80 Running a Sample Setting Conditions Electronic flow meter Split vent 6850 GC shown Figure 14 Measuring the split vent flow rate Setting the Vial Pressurization Gas Pressure for the G1883 G1290 Control the gas pressure used for vial pressurization using the pressure regulator See Figure 3 on page 12 To read the actual pressure value press Pressure and use the cursor keys to scroll to the Vial Press PSI display Setting Carrier and Vial Pressurization Flows for the G1289 Set the
16. INCR YES Press the 1 YES key to activate parameter incrementing or 0 NO to deactivate it When enabled you can use the cursor keys to scroll to the displays to set the vial temperature and vial equilibration time step increments VIAL TEMP INCR 0 0 51 Using the Adv Fctn Key Advanced Function Descriptions or VIAL EQ INCR 0 0 Change the increments from the numeric keypad and then press the ENTER key to execute the change in value G1289 G1290 Adv 2 Enter Select Parameter Incr and use the cursor keys to change the vial equilibrium time step increment and the oven temperature step VIAL EQUIL STEP 0 0 The cursor keys scroll to the next display OVEN TEMP STEP 0 PRESSURE UNITS G1883 Adv 5 Enter G1289 G1290 Adv 6 Enter This function changes the pressure units for the displays among psi kPa and bar Pressing Adv Fctn 6 and Enter displays the following message PRESSURE UNITS PSI Psi is the default for pressure units when the sampler unit is powered up Use the cursor keys to scroll to kPa or bar When units are shown on the display they are active 52 Using the Adv Fctn Key Advanced Function Descriptions PRESSURE VALVES 61883 Adv 9 Enter Press Adv Fctn 9 Enter to display the sampler s pressure sensor readings for either the vial pressurization gas or the carrier gas Use the cursor keys to scroll between the two choices The display is read
17. Leaks in the system e Needle broken clogged e Sample condensed in the loop or transfer line e Sample loop not filled with sample e Inject time too short e Sample did not create headspace e Incorrect vial sampled e Vial not punctured may be due to mechanical failure or vial elevator jam e Transfer line plugged Suggested Actions 1 Check that the proper vial is sampled and that the vial contains sample 2 Use adapters with 10 ml vials 116 10 11 12 13 14 15 Troubleshooting Chromatography Problems Edit the method parameters to increase the method sensitivity See Chapter 7 Developing Methods Check the system for leaks Check the sample vials for a proper seal see Sample Preparation on page 56 Check the condition of the needle Replace it if necessary see Changing the Sampling Needle on page 89 Check that the sample loop and transfer line temperatures are higher than the oven temperature Increase the vial pressurization to insure that the loop is filled Check the Event Times Increase the Inject Time Check that the oven temperature is set high enough to volatilize the compound of interest Make sure that the transfer line is hooked up to the GC and inlet in an appropriate manner Check the disk needle guide circle clip and spring in the injector slot for wear Replace them if necessary Make sure the transfer line is not plugged Make a syringe injection
18. Sampler Vial pressurization n Transfer line s Vial pressurization in Carrier gas in Power switch On 0 Off 61289 61290 G1883 Figure 2 Overview of the 7694 Headspace Sampler from back of instrument Vial Tray G1289 G1290 The 44 sample vial tray is located on top of the unit to the left of the oven The tray is constructed of a flexible belt with dividers for each vial compartment Tray rotation is controlled via the keypad to assist filling the tray with headspace vials The tray can move forward and backward When you use the keypad to move the tray from position 1 to 44 or from 44 to 1 the tray will rotate completely Adapters part no 300 305 HSP are needed in the sample tray when 10 ml vials are used Vial Transport Arm 61289 61290 A robotic arm moves samples from the vial tray into the oven and back Vials are lifted from the tray carried across the unit until centered above a port in the oven and then dropped into place The rail supporting the robotic arm swings away to allow access to the oven Use the switch on the back of the support rail to set the arm for either 10 or 20 ml vials Introduction to Headspace and to the 7694 Headspace Sampler The 7694 Headspace Sampler Sampling System The basic components include a 316 stainless steel single hole side port concentric vial sampling needle or probe with an internal diameter of 0 5 mm 316 55
19. Tray insert for 10 ml vial 25 pk For use in tray with 10 ml vials 300 301 HSP Oven carousel insert for 10 ml vial 1 each For use in carousel with 10 ml vials 301 017 HSP Wrenches 7 x 8 mm Set of 2 134 0407010 HSP Leak test fittings For capping the transfer line and other 325 0050010 HSP connections Vials and caps Flat bottom 20 ml 23 mm x 75 mm 144 pk 5182 0837 Flat bottom 10 ml 23 mm x 46 mm 144 pk 5182 0838 One piece silver aluminum crimp caps 20 mm with Preassembled Wider temperature range 5183 4477 PTFE silicone septa 100 pk septa need higher sensitivity One piece silver aluminum crimp caps 20 mm with Preassembled Wider temperature range 5183 4478 PTFE silicone septa and safety feature 100 pk septa need higher sensitivity One piece silver aluminum crimp caps 20 mm with Preassembled General purpose 5183 4479 PTFE butyl septa 100 pk One piece silver aluminum crimp caps 20 mm with Preassembled General purpose 45 psi 5183 4480 PTFE butyl septa and safety feature 100 pk 85 Maintaining the Instrument Common Replacement Parts and Consumables Table 7 Common Replacement Parts and Consumables continued Description Comment use Vial kits Part Number 20 ml flat bottom Headspace crimp top vials silver aluminum one piece crimp caps with safety feature molded PTFE butyl septa 144 pk 20 ml flat bottom Headspace crimp top vials silver aluminum one piece crimp caps with safety feature mo
20. adjustment see Checking carousel adjustment on page 101 e Elevator adjustment contact Agilent service e Sampler tray sensor adjustment contact Agilent service Checking carousel adjustment The surfaces of the oven carousel and oven lid may be hot and could burn you Before you begin set the oven and loop temperatures to 30 C swing the vial transport arm out of the way and open the oven cover Allow the oven to cool to a safe temperature Note that vials may remain hot even if the oven has cooled Check carousel adjustment to help prevent vial handling problems 1 Turn off the headspace sampler then turn it back on 2 During startup the sampler will reset the carousel position so that carousel position 1 is directly over the elevator rod and under the oven port in the cover If the position is off by a few degrees as shown below you may have intermittent vial handling problems when the vial is pushed up onto the sampling probe 101 Maintaining the Instrument Checking carousel adjustment O gt P Elevator rod o Ee j Rod bushing Figure 25 Misaligned carousel Hole in cylinder If the elevator rod and bushing do not line up exactly under the hole in the carousel cylinder call Agilent service 102 Maintaining the Instrument Leak Testing General Information Leak Testing General Information Refer to Figure 26 and Figure 27 which show the flow paths for
21. display shows the current value of the setpoint for that parameter Editing Setpoints To edit a setpoint 1 Press the key sequence for the parameter 2 the new value using the numeric keypad Aflashing appears to the left of the new value as you enter it 9 Press Enter to make the new value part of the active method If the new value is not within the allowed range the sampler displays a message showing the allowed range Press any non number key to remove the error message At any point in a menu press Clear to return to the top level display See Table 2 G1883 or Table 3 G1289 G1290 for a quick reference of the keys and their functions The G1883 Keypad The table below lists all the keys available on your instrument and summarizes their functions See Keys and Their Functions on page 30 for details about key functions 26 The Keypad The 61883 Keypad Table 2 Quick Reference of 61883 Keys and Functions Key Sequence Display Definition Function Stat START Starts a run Zone VIAL Sets heated zone equilibration temperature Im Y jJ LOOP Sets loop temperature Zone Y jJ x2 TR LINE Sets transfer line temperature GC CYCLE TIME Time to complete GC run Imes a v VIAL EQ TIME Time vial spends heating in oven imes fy 2 PRESSURIZ TIME Time gas enter
22. of 5 uL micro pipettes Material Safety Data Sheet Certificate of Analysis 87 Maintaining the Instrument Fuse Locations Fuse Locations Refer to Figure 15 and Table 8 below for fuse locations and part numbers WARNING Fuse replacement should be performed only by qualified service personnel PS 86 50 CS2006 A HSS pu t f A TA A oc too cs es AA peau 2002620 i gn F3 FA LE 081 VEN EM F6 amp R7 c1 25 ed 9 VER P osote T 12 0 19 0 15 0 15 0 15 ES 3 R4 PASSIO 45 2 1 2A 300mA n m Sog dc Sibel Power cord fuse e 3 fe JT e holder o 40 01 Dlo Power supply board Figure 15 Fuse locations on the power supply Table 8 Fuse Part Numbers Fuse Location Voltage Description Part No F1 230 0 5 A 5x20 384 1695004 HSP F1 115 5x20T 384 1595011 HSP F2 all 2 5 20 384 1695001 HSP F3 F4 all 0 5 A 5x20 384 1695004 HSP F5 all 2A 5x20T 384 1695001 HSP F6 all 5x20 F 384 1295001 HSP Power cord fuse holder 230 3A 5x20T 384 1695003 HSP Power cord fuse holder 115 6 A 5x20 F 384 1295001 HSP 88 Maintaining the Instrument Changing the Sampling Needle Changing the Sampling Needle 1 Remove the two screws on the sides of the sam
23. should substitute specific information For example setpoint means you should key in the numeric value you desire for the setpoint 2 Text in Bold means that you should press the key by that name Be careful how you enter information For example the key sequence Adv Fnct 1 Enter indicates that you should press the Adv Fnet key the key the 1 key and then Enter It does not mean that you should press a 66 comma There is no comma on the sampler s keypad 3 Text in Courier indicates the message you will read on the sampler display About This Manual Conventions Introduction to Headspace and to the 7694 Headspace Sampler Introduction to Headspace and to the 7694 Headspace Sampler This chapter briefly describes the theory and application of headspace analysis It describes the parts of the 7694 Headspace Sampler and its modes of operation Overview of Headspace Analysis Your new headspace sampler is a tool for introducing volatiles that are contained in liquid or solid samples into a gas chromatograph The analytical technique is called static headspace gas chromatography The term headspace refers to the space above the liquid or solid sample that you place in a sealed vial The term static means that the volatiles in the headspace of the vial are at equilibrium with the same compounds in the liquid or solid sample The instrument extracts a reproducible volume of the headspace an
24. six port valve nickel valve sample loop set of two miniature solenoid valves and nickel tubing You can program the system s temperature up to 200 C Also available is a fused silica lined stainless steel sampling path Accessory G1286A Transfer Line This line connects the headspace sampler with the GC Two types are available standard nickel and fused silica lined stainless steel The line is heated to a maximum temperature of 220 C There is a removable needle for easy interfacing through GC inlet septa Table 1 Transfer Lines Material Length cm Part Number Comment Nickel 68 301 011 HSP Nickel 82 301 152 HSP Standard transfer line Fused silica lined 82 301 211 HSP For applications requiring a stainless steel highly inert non metal flow path Keypad and Display The headspace sampler has a 25 key elastomeric keypad The display is a single line 20 character LED dot matrix design All functions of the sampler are controlled from the keypad with the exception of EPC which is controlled from the GC or ChemStation Introduction to Headspace and to the 7694 Headspace Sampler The 7694 Headspace Sampler Pneumatics The G1290 and G1883 headspace samplers use two flow paths GC carrier gas flow and flow for vial pressurization You control the GC carrier gas flow using a manual flow controller and the vial pressurization using a manual pressure regulator The G1289 samplers uses the same gas streams but all flow and pr
25. the Instrument Steam Cleaning the Pneumatic System Steam Cleaning the Pneumatic System Steam cleaning removes components of the sample that could stick to the surfaces of the flowpaths and valves For example polar compounds tend to stick to these surfaces and may appear as carryover when running solvent or air blanks after samples For safety reasons Agilent only recommends water as the cleaning agent The success of the cleaning procedure will vary depending on your application Check the results to assess the value of steam cleaning Disconnect the transfer line from the gas chromatograph or 5973 MSD Injecting water vapor into the GC will damage the column Injecting water vapor directly into the MSD may shorten the life of analyzer components You may have to cool down the GC or vent the MSD before disconnecting the transfer line Use vial septa that can handle the temperature and pressure associated with this procedure Agilent recommends septa part number 9301 0719 tan PTFE white silicone septa 60 C to 125 C These are the septa provided in the part number 5182 0840 preassembled 20 ml vial kits 1 Prepare the GC MSD Prepare 23 vials 20 vials with 1 ml of distilled water and 3 air blanks Disconnect the transfer line Set the carrier flow so that it is less than 100 ml min 4 Enter the following parameters on the headspace sampler keypad Function Parameter Settings Zone Temps 125 C 140 C 150 C Event
26. to be sure that the column and detector are working properly Call Agilent service Bad Data Bad Peaks Probable Causes GC conditions wrong for the sample type Sample not at equilibrium Too much sample injected into the GC Flow too low Sample condensing in the loop transfer line or valves Leaks in the system 117 Troubleshooting Chromatography Problems Sample contaminated Sample decomposing Oven temperature is too high Incomplete sample transfer System contaminated Suggested Actions EE CE E RO aE 10 11 12 13 14 15 16 Check the GC settings Increase the Vial Equilibration Time Use a smaller sample loop See Changing the Sample Loop on page 92 Use split injection Increase the Vial Pressurization Time to dilute the sample Check that the carrier gas flow rate is high enough for the column type See Developing Methods on page 70 Check that the loop and transfer line temperatures are higher than the oven temperature Check the system for leaks Lower the oven temperature Check the sample preparation procedure to check for sources of contamination See Chapter 5 Preparing a Sample for more information Increase the Inject Time Check the agitation level to prevent splashing material on the septum Use a heat gun to drive any contamination out of the valves or tubing while checking the detector response to confirm the location of contamination St
27. use is put into the specified memory location Parameters stored as parts of a method are Zone Temps Event Times Vial Parameters and the advanced functions for Oven Stabilization Time Pressure Units and Multiple Headspace Extraction G1289 G1290 only Storing overwrites any method already in that location There is no warning message that an overwrite is taking place When the 7694 HS is first turned on after a loss of the battery backed up RAM the default method is loaded into all four method storage locations Loading a Method You can retrieve a method from memory for use in the current analysis by using the Load Method key To bring a method up from memory 1 Press Load Method The sampler displays the following message G1289 and G1290 G1883 LOAD METH 1 4 LOAD METH 1 5 For the G1883 you can load method 5 the default method This method cannot be edited or chained 2 Enter the number of the method you desire to retrieve on the numeric keypad and press Enter 64 Note Entering a Method Chaining Methods The method stored in the specified location is now available for current use A method may not be loaded during a run Chaining Methods Chain Methods allows two to four stored methods to be used sequentially to run groups of samples It provides the user with some automation Once the chain or sequence is programmed in and the samples loaded the sampler will run the sequence without fu
28. 0 ml vial inserted upside down Servomotor on vertical loader defective Microswitch on fork defective Suggested Actions 1 Check that vials are loaded in the proper locations in the sample tray 2 Check that the method specifies the proper vial locations 3 Insert tray adapters part no 300 305 HSP in the sample tray for 10 ml vials 4 Check the setting of the vial size selector switch Adjust the height of the elevator assembly See your service manual or contact Agilent service Insert oven adapters correctly Check the operation of the servomotor Replace it if necessary See your service manual or contact Agilent service Check that the vial sensor microswitch is actuating properly Call Agilent service Sample Vial Doesn t Drop Down Into Oven Probable Cause Horizontal gripper arm movements are out of adjustment Suggested Actions 1 2 Adjust the arm movements See Aligning the Vial Loader G1289 G1290 only on page 97 Call Agilent service 120 Troubleshooting Vial Jam Problems G1289 G1290 only Vial Not Raised and Lowered in Oven Probable Causes e Belt on the vial elevator is loose or broken e Vial elevator motor is at fault Check the voltage on J9 pins and 9 on the main board V gt 20 V or lt 20 V Suggested Actions 1 Check the belt Replace it if necessary See your service manual or contact Agilent service 2 Exchange the motor 3 Call Agilent service
29. DSHAKE MODE CHECK GC READY NO CHECK GC READY YES Tells the 7694 whether or not to look for a ready signal from the GC before injecting The 7694 will not look for a signal The 7694 will look for a signal 1 Erer 7694 RESET Displays ready message until setpoints are reached 7694 RESET can be used to recover from error conditions listed in Error Messages on page 128 E VALVE COUNT Use this function to view reset the number of valve cycles ERIT BAUD RATE Use this function to adjust the sampler communications rate 43 Using the Adv Fctn Key Advanced Function Descriptions Advanced Function Descriptions CONSTANT HEATING TIME 61883 Adv Fetn 2 Enter This function indicates that the 7694 is always in the constant heating time mode DEFAULT METHOD G1289 G1290 Adv 7 Enter Pressing Adv Fctn 7 and Enter displays the following message LOAD DEFAULT METHOD Pressing Enter again loads a default method into the headspace sampler The display shows the following flashing message METHOD LOADED before returning to a top level display The following parameters are loaded in the default method Oven Temp 70 C Loop Temp 80 C Tr Line Temp 90 C GC Cycle Time 25 min Vial 15 min Pressuriz Time 0 2 min Loop Fill Time 0 2 min Loop Eq Time 0 05 min Inject Time 1 0 min First Vial 1 Last Vial 10 Shake O
30. Messages on page 128 Standby Condition During standby the pressurization valve is open and auxiliary gas flushes the sample valve the sample loop and the sampling needle Carrier gas is also flowing to the GC injection port through the sample valve Do not use hydrogen as a gas in the 7694 HS Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation When the sampler is started it moves the first vial into the oven Equilibration time begins To shorten the required equilibration time agitate the vial in the oven See Setting Vial Parameters on page 63 Pressure Vent transducer Carrier gt I ERE a ee EE eee dil I ER gas flow d Mass flow controller Pressure transducer Auxiliary gas Sen I uc fiw flow forvial gt pressurization Pressure Flow regulator restrictor Needle Carrier gas Auxiliary gas Headspace vial Figure 4 Standby condition S1 is open Vial Pressurization At the end of the vial equilibration time agitation stops the vial moves in line with the sampling needle and is raised by the mechanical rod onto the needle The pressurization valve closes The sampling needle pierces the septum of the Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation vial The pressurization valve opens allowing gas to enter the vial for the pressurization time The valve then closes again Pre
31. Pressure G1883 G1290 36 Tray Advance G1289 G1290 only essent nente 36 Enter 37 iz she PO 9T Numeric Keypad a ER Ree eg 37 Adv TEA D h SESA eerte eorr re eo E ets ved pet eed 37 Chapter 4 Using the Adv Fctn Key Using an Advanced Function 40 List of Advanced Functions by Model essen 41 Advanced Function Descriptions esses eene nnne 44 Chapter 5 Preparing a Sample Sample Preparatioh 56 Loading the Sample Tray and or Carousel eese 58 Contents Chapter 6 Entering a Method Entering a Method naino OPE en eet dene ELE aevo deno 60 Entering Zone Temps eter ee te eere edet 60 Setting Event Times 0 c cc cccceceseesssesseceeeceececeeeceeceeeceeeeeececeeeaeecsaeeeeeeeaeeeeeeees 61 Setting Vial Parameters s sessseeeeseeeeeeeee eterne nennen nnne tenentes 63 Storing and Loading Methods eese entente neret 64 SLOTING a Method ect tete er eno PR ER epe e casa doe enne ed 64 Loading a Method imie 5 eene iet ete 64 Chaining Methodi icerisine ieres oeie reii entren entis enne testen enne 65 Activate a Method Chain eese eene eene nennen entren 65 Deactivate a Method Chain essen enne 66 Using a Method Chain fo
32. Probable Causes The temperature sensor for the heated zone noted is failed shorted or disconnected The temperature for the zone is too high indicating a bad PC board or sensor Oven gt 220 C Loop gt 240 C Tube gt 240 C Suggested Actions Call Agilent service 129 Error Messages Error Message Listing The microprocessor immediately switches off the heater associated with the failed sensor You must correct the problem before you can continue to use the sampler CAROUSEL RESET Probable Causes The sampler was reset Suggested Actions See Agilent 7694 or 7694 RESET Agilent 7694E or 7694E RESET on page 128 PRESS STOP TO CONFIRM The sampler is waiting for confirmation before changing a setpoint RAM CHECK ERR PRESS CLEAR TO RESET Probable Causes The RAM check value is different from the stored value Suggested Actions Press Clear to continue The instrument is stopped and you must totally reset it This resets the microprocessor and automatically initializes all the data method parameters advanced function values flags and all the variables with default values If the unit fails to reset try turning the power off then on If this fails contact Agilent service 130 Error Messages Error Message Listing REMOVE ALL VIALS Probable Causes The sampler was reset The sampler does not know if the vials still in the carousel are the ones originally associated with your me
33. Set the GC conditions See your GC operating manual Load the method or set the method chain you want to use See page 64 or page 65 Prepare the samples See 5Preparing a Sample Load the samples into the tray G1289 G1290 or carousel G1883 See page 58 When the GC and HS are ready press Start Setting Conditions Flow Rates Refer to your GC operating manual for details about its flow systems Two distinct versions of the 7694 Headspace Sampler exist Models G1883 and G1290 are supplied with mechanical pneumatic controls model G1289 is designed for use with a GC with EPC control and so it contains no pressure regulator or flow controller The procedure for setting flow rates differs for these two versions As a general rule when you are setting flows for the headspace sampler most of the flow should come through the transfer line from the headspace sampler 78 Running a Sample Setting Conditions Pressure regulator Flow controller Figure 13 Location of flow controller and pressure regulator 61883 and G1290 only 79 Running a Sample Setting Conditions Setting the Carrier Gas Flow Rate for the G1883 G1290 Set the carrier gas flow as follows 1 Set the following GC parameters Inlet Volatiles Interface or Split Splitless Mode Split Initial temperature Per method Pressure Per method Split ratio 1 1 G1290 Split flow 4 ml min G1290 G1883 at
34. Table 9 Vial Loader Potentiometer Adjustments Potentiometer Position Display Reads Desired Results Adjustment P1 Fork Down GRIPPER Y AXIS DOWN Fork grabs center of vial neck Clockwise UP P2 Fork Up GRIPPER Y AXIS UP Vial clears all obstacles during Clockwise UP delivery P3 Oven Load 4 GRIPPER X AXIS 4 Successfully drops or picks up Clockwise LEFT vial at oven port P4 Oven Wait 3 GRIPPER X AXIS 3 Loader waits between oven and Clockwise LEFT tray no interferences P5 Tray Load 2 GRIPPER X AXIS 2 Successfully drops or picks up Clockwise LEFT vial at sample tray P6 Rest Set 1 GRIPPER X AXIS 1 Loader rests over center of tray Clockwise LEFT no interferences Procedure 1 Place a capped sample vial in sampler tray position 1 2 Press Adv Fctn 5 Enter 3 Check vial pickup from the tray a Scroll until the display reads Y AXIS Press 0 to lower the fork b Scroll down until the display reads X AXIS Press 1 to move the fork to the right It should snap onto the middle of the vial s neck Observe this movement by pressing 0 and 1 to move the fork back and forth If the fork is too high or too low adjust potentiometer P1 If the fork moves too little or too far to the left adjust P5 c Scroll up until the display reads Y AXIS Press 1 to raise the vial If the vial does not clear the tray when lifted adjust potentiometer P2 The bottom of the vial should not strike anything 4 Check vial delivery to the oven
35. The same vial sequence is assigned to each method A given vial is placed in the oven sampled then removed from the oven and placed in the sample tray It is returned to the oven for the next extraction Usually four extractions per vial are adequate to allow you to obtain a good log area versus extraction number graph for quantitative work 22 Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation Multiple Headspace Extraction with Single Vial Puncture The use of single puncture mode is not recommended Agilent recommends using multiple vial puncture mode Multiple Headspace Extraction for Analyte Concentration G1289 G1290 only In this multiple headspace extraction mode multiple vials are sampled to concentrate the analytes at the head of the GC column or in a cryo trap at the GC inlet A start signal is sent to the GC only after the last vial sampling is complete This feature is available only through ChemStation control 23 Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation 24 The Keypad The Keypad Accessing Functions Use the instrument keypad on the lower left front section of the instrument to view and change all settings Pressing a key once brings up the first item in a menu of parameters connected with that key Use the cursor keys A V to scroll through the menu items available for control As you scroll to each item the instrument
36. Times minutes 2 5 15 0 0 0 0 2 0 2 1 Vial 1 1 23 0 off 5 Start It takes about 70 minutes to complete 95 Maintaining the Instrument Installing the Transfer Line onto the Volatiles Interface Installing the Transfer Line onto the Volatiles Interface If you are using your headspace sampler with a 6890 and a volatiles interface install the transfer line onto the interface as follows 1 Install an appropriate sized male nut and steel ferrule onto the transfer line 2 Connect the transfer line to the interface Tighten the nut 1 4 turn past finger tight Do not overtighten If the nut leaks tighten an additional 1 8 turn Volatiles interface 3 Check for leaks See your 7694 Headspace Sampler Site Prep and Installation Guide for details 96 Maintaining the Instrument Aligning the Vial Loader G1289 G1290 only Aligning the Vial Loader 61289 G1290 only Every three months Agilent recommends that you check the vial loader to see if it needs adjustment This helps prevent vial handling problems This procedure uses the Advanced Function keys to pick up and move a vial from the sample tray to the oven port At the steps where the fork picks up or releases the neck of a sample vial you will check to see if the fork and vial are lined up properly If there is a misalignment between the vial and the fork you will adjust one or more of the six potentiometers that control the positioning of
37. all gases used in each type of headspace installation Carrier gas in Total flow Vial pressure 200 ml min gas m EPC Flow Module ZDV union PCV1 1 H E Aux EPC S Hors ue k Split vent flow M 4 e PCV2 Aux bleed i ee ee fitting 047 Sample t Flow loop restrictor Needle ZDV s union Split vent trap Headspace vial J Column flow 4 ml min Lagcnid Headspace Sampler 9 Column FS Flow sensor PS Pressure sensor GC S1 Pressurize valve S2 Vent valve Flow paths before GC prep run Figure 26 Flow paths for a 61289 to 6890 GC installation 103 Maintaining the Instrument Leak Testing General Information Carrier gas EPC Flow Module PCV1 1 Carrier gas in FS 40 60 psi 1 q ny gt lt 1 Septum purge Q Split vent Purge pey2 flow Flow e restrictor s2X valve pa bw gt lt t Vial 1 E ps pressure oop adm gas in 4 Needle Headspace vial Split vent trap FS PS 1 52 Legend Flow sensor Headspace Sampler Pressure sensor Column GC Pressuri
38. ample Preparation on page 56 2 Manually install the headspace vial in the oven slot under the headspace probe 3 Using MANUAL OPERATION load the vial onto the probe and make sure the Pressurize Valve is ON and the Vent Valve is OFF Pressurize the vial to 20 psi using the Aux control on the GC Wait at least one full minute then cap off the aux bleed fitting 108 Maintaining the Instrument Leak Testing a 61289 to 6890 GC Interface Cap on open end of fitting Figure 28 Cap the aux bleed fitting 6 Monitor the pressure on the front panel display it should equilibrate at some pressure lower than 20 psi and then hold The pressure will drop slightly at first then stabilize At this point it should drop less than 1 psi in 5 minutes If the unit cannot maintain pressure there is a leak in the vial pressurization flow path Using MANUAL OPERATION switch the sample valve and repeat steps 2 6 If the unit cannot maintain pressure there is a leak at the sample tube fittings De pressurize the system by opening the vent valve from MANUAL OPERATION Correcting leaks 1 If the headspace sampler GC system failed the test isolate the source of the leak by using MANUAL OPERATION to toggle the Pressurize Valve to OFF Repeat steps 4 6 under Leak test on page 108 above If the unit passes the test the leak is in the headspace unit at either the Vent Valve the co
39. area Lift front cover Rear cover Remove screws Manifold cover Figure 19 Removing the sampler cover 2 Loosenthe two screws on the manifold cover the stainless steel box and remove it and the insulation inside it from the valve compartment 92 Maintaining the Instrument Changing the Sample Loop Manifold cover a L and insulation oosen Front cover not shown for clarity SEA Figure 20 Removing the manifold cover and insulation 3 Use a 7 mm wrench to loosen the two nuts connecting the sample loop to the six port valve See Figure 21 93 Maintaining the Instrument Changing the Sample Loop Sample loo Insulator P P Loop mandrel Manifold body Disconnect sample loop fittings from valve Figure 21 The Sampling System 4 Use 7 mm wrench to loosen the bolt holding the loop mandrel to the manifold body and remove the loop mandrel Slide the loop off the mandrel Slide the new loop over the mandrel and tighten the nuts to the six port valve Reinstall the mandrel Position the fiberglass insulator between the manifold body and the loop mandrel Note When installing a Silcosteel treated sample loop take care not to bend the loop when installing it or you will break the coating and compromise inertness 7 Perform a leak test on fittings before replacing the box and cover 94 Caution WARNING Maintaining
40. carrier gas flow rate directly using the GC or GC data system Set the vial pressure directly using the appropriate auxiliary channel in your 6890 GC 81 Running a Sample Setting Conditions 82 Maintaining the Instrument Maintaining the Instrument This chapter describes the procedures for maintaining the instrument Table 6 lists routine maintenance activities that should reduce unplanned repairs and maintenance The maintenance frequency appropriate for your instrument will vary significantly depending on the sample matrix solvents temperatures and sample throughput Table 6 Recommended Maintenance Schedule Maintenance Activity Frequency Replace sample probe 3 month Steam clean flow path 3 months Check vial transport alignment and adjust if necessary 3 months Check carousel alignment and adjust if necessary 6 months PM Service and inlet maintenance 12 months Flowpath vent parts replacement 24 months These tasks and frequencies are based on experience They are not based on life time testing or benchmark testing 84 Maintaining the Instrument Common Replacement Parts and Consumables Common Replacement Parts and Consumables Below is a list of commonly used parts Also refer to the Agilent catalog for consumables and supplies Table 7 Common Replacement Parts and Consumables Description Comment use Part Number Adapters and tools Decapper 20 mm 5181 1214 Crimper 20 mm 9301 0720
41. ce The partition coefficient K is related to the degree of solubility that the analyte has in the matrix For example benzene is not very soluble in water and has a K of approximately seven Ethanol which is very soluble in water has a K of 7000 A high value of K implies it is difficult for the analyte to leave the matrix and go into the headspace K is also very dependent on temperature as demonstrated by the following equation dK _ 1 aT Processes that reduce the value of will increase the sensitivity of the headspace analysis The following operations can be used to decrease K 1 Add mineral salts to the matrix aqueous samples 2 Add another liquid to the matrix 3 Increase the temperature 70 Note Note Developing Methods Varying Oven Temperature Varying Oven Temperature The oven temperature can have a profound effect on the concentration of analyte that passes into the headspace gas In general as the oven temperature increases the amount of gas entering the headspace from the sample increases increasing the pressure in the vial and delivering more analyte to the GC This increases the sensitivity of the analysis When you pick an oven temperature consider the following e Over pressurization of the headspace vial could be dangerous e Unstable compounds could degrade at elevated temperatures There are two ways you can program the 7694 HS to increase oven temperature in steps e Use Chain M
42. ced into the column and the major part is allowed to escape splitless injection An injection with the entire injected volume applied to the column standard addition See internal standard Thermal Conductivity Detector TCD A gas phase detector based upon changes in the thermal conductivity of the gas stream The thermal 138 Glossary conductivities of hydrogen and helium are six to ten times greater than most organic compounds The presence of even small amounts of organic materials causes a large decrease in the thermal conductivity of the column effluent thermostated Control of the temperature is provided by a thermostat top level display The main item in a menu This is the display that appears first when the menu item is first accessed vapor pressure The pressure exerted by a vapor in equilibrium with its solid or liquid form 139 Glossary 140 Index Numerics 7694 Reset Description 46 A Adapters Description 58 Loading in carousel 58 Loading in tray 58 Adv Fctn Key Description 37 40 Using 40 Advanced functions Adv Fctn 1 Description 46 Adv Fctn 2 Description 53 Adv Fctn 1 Description 53 Adv Fctn 2 Description 50 Adv 3 Description 54 Adv Fctn 4 Description 47 Adv 5 Description 48 Adv Fctn 6 Description 52 Adv Fctn 7 Description 44 Adv Fctn 8 Description 44 45 49 Adv Fctn 9 Description 45 Key description 37 List 97 Using 40 Auto
43. cifies the location of the last vial to be analyzed by this method Use the numeric keypad to enter the vial location followed by Enter The number of the last vial cannot be lower than the first vial number The headspace sampler gives an error message and you will have to re enter the vial number Use the down cursor key V to scroll to the last display SHAKE 0 1 2 This specifies the agitation level of the oven carousel during vial equilibration 0 off 1 low 2 high Specify the level desired by keying in 0 1 or 2 followed by Enter G1883 sampler only After turning on agitation set the agitation time Use the down cursor key to scroll to SHAKE LOW MIN setpoint Enter the desired setpoint of number of minutes and press Enter to save At this point all the parameters in a method necessary to run a sample are entered To save this method use Store Method To run a sample make sure that vials are loaded into the proper spots in the sample tray then press Start 63 Entering a Method Storing and Loading Methods Caution Note Storing and Loading Methods Storing a Method Store Method places the method in active memory into one of four storage locations for future use To store the method currently in use 1 Press Store Method This displays the following message STORE METH 1 4 2 Enter the storage location desired 1 4 on the numeric keypad followed by Enter The method currently in
44. d injects it into the carrier gas flowing into the gas chromatograph Food packaging pharmaceutical products soil and water are often tested to see if they meet quality criteria or regulatory standards Fragrances and consumer products are analyzed using headspace in order to understand their composition Forensics laboratories use headspace for measuring the percent of ethanol in human blood to see if a driver is legally intoxicated The ease with which a sample forms a gaseous headspace depends on the sample s partition coefficient See Developing Methods on page 68 for a more thorough explanation After a programmed heating time the headspace gas is extracted from the vial and injected into a GC for analysis There are two means of extracting the headspace gas from the vial single or multiple headspace extraction MHE With single headspace extraction only one sample of gas is taken from each sample vial Single headspace extraction is the standard method It is used for samples that are readily volatile or for Introduction to Headspace and to the 7694 Headspace Sampler The 7694 Headspace Sampler which there are no matrix effects Quantitative analysis can be performed by using suitable internal or external standards MHE is available only in models G1289 and G1290 MHE is used for headspace samples for which no calibration standard can be prepared easily for example solid samples or for highly volatile compounds in liq
45. d vials into the carousel or change the method if you want to continue your analysis from the point at which it stopped Error Message Listing Agilent 7694 or 7694 RESET Agilent 7694E or 7694E RESET Probable Causes The sampler rebooted due to a power failure or user input Comments Power to the 7694 Headspace Sampler may be lost during a run The sampler contains a battery backup which will retain methods in storage When power is restored the headspace sampler runs through a series of diagnostic tests See Power on Diagnostics on page 14 for more information The method in use when the power was lost will be reloaded into the active memory If you press Start the sampler will run the method starting with the first vial specified If you wish to start the run from the point at which the run was interrupted you will have to edit the number entered for First Vial 128 Error Messages Error Message Listing ALARM STEPPER errors Probable Causes Carousel jammed because of mishandled vial or broken glass or other foreign bodies Carousel out of alignment See Checking carousel adjustment on page 101 Carousel drive mechanism failed Suggested Actions 1 Remove all vials from the carousel and gripper Clean out the oven carousel Power cycle the headspace sampler and hold down the clear key until the tray is reset Call Agilent service ALARM TEMP1 OVEN ALARM TEMP2 LOOP ALARM TEMP3 TUBE
46. dit 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 About This Manual Intended User Chapter 7 Developing Methods describes the parameter changes that can affect sensitivity precision and accuracy Chapter 8 Running a Sample summarizes operation of the headspace sampler to run a sample Chapter 9 Maintaining the Instrument describes maintenance procedures including changing the sample loop transfer line needle valves and EPROM Chapter 10 Troubleshooting lists the possible causes and solutions for chromatography problems or instrument failure Chapter 11 Error Messages describes the various error messages that accompany machine failures and the means to correct the failures Intended User This manual is intended for users who understand the basics of gas chromatography Although the manual contains some headspace theory it primarily provides operating maintenance and troubleshooting information for the 7694 Headspace Sampler Conventions The following conventions are used in this manual 1 Braces jenclose a generic name for which you
47. e squeeze the crimper handles to seal the vial Remove the crimper 8 Checkthat the seal is adequate by trying to twist the cap on the vial It should be difficult or impossible to turn the cap If you can easily turn the cap on the vial re crimp the cap You may need to adjust the crimping tool 9 decap vials use a decapper for vials with 20 mm caps part no 5181 1214 Note Vials will contain laboratory air which may be contaminated with things such as solvents or Freon leaking from air conditioners If contaminants will adversely affect your results use argon to purge the vials just before capping and sealing Handle Adjusting screw Jaws Sample vial Figure 9 Position of crimper and vials for proper capping 57 Preparing a Sample Loading the Sample Tray and or Carousel WARNING Loading the Sample Tray and or Carousel G1883 Press Carousel Advance and Scroll until the carousel rotates to the desired position G1289 G1290 Press Advance Tray position 4 and Enter to move the desired loading position to the very front of the sample tray If you are using 10 ml vials be sure to place inserts into the spaces in the oven carousel Be sure the inserts are placed in the carousel with the closed end down see Figure 10 Finally be sure to set the vial size switch on the back of the horizontal loader to the proper size Using the cursor keys advance tray positions one by one wh
48. e Extraction esses 19 Multiple Headspace Extraction with Multiple Vial Puncture 1289 GT1290 60nly 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 1289 GT1290 0nly ees ee ace eee eae 23 Contents Chapter 3 The Keypad Accessing Eunictioris de eret pee heo ipae Eee tee devas encore in re eae Lee ep cess 26 Editing 5 reser eot eee rene e Pe Eee te Pee eo eed 26 The G T1883 Keypad ies te e ER ERR OE CREE 26 The G1289 G1290 Keypad esses ener enne enne nnne nennen nnn enn 28 Keys and Their FunctLiornis eere te eee Ce aec op een 30 Start G1883 Only Jannina a a r a EE E TT 30 Stop Reset G1883 only e esesesseressesrssresereresesseresessestrsseneraresseseresessereresesessers 30 Start Stop G1289 G1290 only sees eene 30 200E Temps iair nan a 31 Event Times ndn dier ri err e ina i eer uH eL FCR 32 Vial EY COId ERREUR 34 Load Method 2 eiue redeem esce dene neue eee op Roe e Le E 35 Store Method us voeem vara un met ot tait ot e 35 Chain Methods iss sec en eee ii 36 Tank Method ied rete 36 Carousel Advance 61883 only eese treten 36
49. e loop and transfer line temperatures should be set higher than the oven temperature Set the loop temperature 15 C higher than the oven and set the transfer line 25 C higher than the oven Setting Event Times Using this key you enter values in minutes for the timed events which make up the vial sampling sequence Pressing Event Times displays the first timed event GC CYCLE TIME From the numeric keypad enter a value for this event which is the time for the total GC run to complete Total run includes the GC run and cool down time and the vial equilibration time Press Enter after keying in the numeric value Use the down cursor key V to bring you to the next timed event VIAL EQ TIME The Vial Equilibration Time is the time which the sample vial spends heating in the oven to form the headspace gas Enter the desired time from the numeric keypad followed by Enter 61 Entering a Method Entering a Method The down cursor V brings you to the next display PRESSURIZ TIME Pressurization Time specifies the time that gas is allowed to enter the vial through the sampling needle to build up additional pressure in the vial Key in the desired time on the numeric keypad followed by Enter Use the down cursor W to scroll to the next display LOOP FILL TIME The Loop Fill Time is the time during which the vent valve is open The gases in the sample vial travel through the sample loop and are vented to the outside This
50. e oven carousel Agitation is used to homogenize the sample at room temperature Settings are as follows 0 off 1 low 2 high Default is off The stepper motor rotates the carousel at a constant frequency to agitate the vials Agitation takes place at the beginning of a method before the first vial is heated If Shake 1 or 2 low or high is selected then a shake time parameter will be available from the Vial Parameter function key The display will show SHAKE LOW or HIGH MIN 34 Caution The Keypad Keys and Their Functions where is the number of minutes from 1 to 999 If 0 is entered in the first Shake screen it will turn shaking off When a multi vial method is started the carousel shakes for the number of minutes selected then the first vial is lifted into the heating zone After injection the vial immediately returns to the carousel If the vial heating time is shorter than the run cycle time then shaking resumes until the run cycle expires Under these circumstances the shaking time setpoint only applies to the period before the first vial begins heating The additional shaking cannot be controlled or changed by the operator G1289 G1290 Sets the agitation level of the oven carousel Agitation mixes the sample in the vial for potentially faster equilibration and is used most often with liquid samples Settings are as follows 0 off 1 low 2 high The stepper motor in the oven rotates the caro
51. eam clean the system See Steam Cleaning the Pneumatic System on page 95 Change the valves regulators and tubing Refer to your service manual or contact Agilent service Call Agilent service 118 Troubleshooting Vial Handling Problems G1289 G1290 only Unwanted Peaks Present Possible Causes Dirty vials or septa Dirty laboratory air sealed in the vial with sample Carryover from the previous sample Contaminated GC system Dirty column and or ferrules Suggested Actions 1 2 3 4 5 D Bake the vials and septa in oven Flame the vials before use Wash the vials and septa and then dry them in the oven Purge the vial with argon during sample preparation Steam clean the headspace sampler See Steam Cleaning the Pneumatic System on page 95 Perform a blank GC run clean or bake out the GC Heat the graphite GC column ferrules with a flame before use Call Agilent service Vial Handling Problems G1289 G1290 only Gripper Arm Doesn t Pick Up Sample Vial Probable Causes Arm movements out of adjustment Spring lock and spacer out of adjustment Carousel out of adjustment See Checking carousel adjustment on page 101 10 ml vials used without adapters 119 Troubleshooting Vial Handling Problems G1289 G1290 only Selector switch on the back of the horizontal loader not set for the vial size being used Elevator assembly height incorrect Oven adapter for 1
52. ems that represent commands for the software to execute method The parameters defined for conducting the sample equilibration and sampling 136 Glossary multiple headspace extraction An analytical technique that takes more than one headspace sample from each sample vial followed by chromatographic analysis of each extracted sample By summing up the peak area for each compound the total amount of that compound in the sample can be determined eliminating the effect of the matrix See single headspace extraction multiple puncture Multiple headspace extraction performed by puncturing the septum separately for each extraction See single puncture partition coefficient K in gas chromatography The ratio of the amount of a component per unit volume of the stationary phase g cm 3 to its amount per unit volume of the mobile phase at constant temperature and at equilibrium The partition coefficient is assumed to be independent of concentration at the concentration prevailing in gas chromatography and is related to the volume VN by O VN VN a VTS K m m where Vi volume of the liquid stationary phase density of the liquid my mass of the liquid Vg specific retention volume phase ratio The ratio of the volume of the mobile phase to the volume of the stationary phase in a column precision The agreement between the results of repeated data quantitative analysis Analysis performed for the purpo
53. essure control is provided by the 6890 GC In all models two 1 8 inch Swagelok bulkhead fittings are provided at the rear of the pneumatic compartment for connecting lines for vial pressure and carrier gas Introduction to Headspace and to the 7694 Headspace Sampler The 7694 Headspace Sampler Pressure regulator standalone units only Model G1289 units do not have pressure regulators or flow controllers Flow controller standalone units only Stainless steel tubing BW Solenoid valves Vial sampling needle tt Sample loop Transfer line Figure 3 Pneumatic system for the 7694 Headspace Sampler Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation Principles of Operation General Operation When the instrument is switched on the sampler moves the first vial into position For models with a tray the vial tray moves to the start position placing the vial located in position one next to the robotic arm For models without a tray G1883 the carousel moves vial one to the start position The oven sample loop and transfer line begin heating to reach the setpoint values Until the oven sample loop and transfer line setpoints are reached the display reads 7694 Not Ready and the red Not Ready light is lit If you press Start Stop before the machine is ready the display reads Waiting for Ready and the Not Ready li
54. ethods see Chaining Methods on page 65 and setting the oven temperature higher in each method in the chain e Use Param Increment see Advanced Function Descriptions on page 44 Do not set the oven temperature within 10 C of the boiling point of any solvents in the sample except in special cases Loop and transfer line temperatures should be set higher than the highest temperature the oven will reach in a programmed sequence Varying Event Times Vial Equilibration Time The time that the sample vial spends in the oven determines the amount of analyte in the headspace gas and the presence or absence of equilibrium The 7694 HS can be programmed to analyze a series of samples to determine if equilibrium is reached 71 Developing Methods Matrix Effects Figure 12 To determine if equilibrium is reached use Chain Methods see Chaining Methods on page 65 to increase the Vial Equilibration Time for each method in the chain or use Param Increment see Advanced Function Descriptions on page 44 to increase the Vial Equilibration Time for each successive sample in the series Then plot the peak area versus equilibration time for a certain peak The system is at equilibrium when this curve flattens out See Figure 12 Equilibrium Condition L N Where X is the component of interest X g is the concentration of X IX g Heating Time Equilibration curve Lo
55. f 106 Caution Maintaining the Instrument Leak Testing a 61289 to 6890 GC Interface Observe the column flow rate from the GC front panel The flow rate should be close to the nominal approximately 4 ml min The inlet Total Flow at the GC front panel should read the sum of the purge flow 200 ml min the column flow 4 ml min the septum purge flow 3 ml min or approximately 207 ml min Press the Prep Run key on the 6890 If another temperature or flow is not ready you may need to press Prep Run twice The capillary inlet purge valve shuts off and the inlet switches to forward pressure control The inlet EPC module flow sensor becomes read only Check the total flow reading for the inlet Now that the purge flow is turned off the total flow should drop to the column flow 4 ml min the septum purge flow 3 ml min or approximately 7 ml min If the flow rate is much higher there is a leak in the carrier gas flow path between the 6890 inlet flow module and the detector column fitting Continue with the next step to get more information On the headspace sampler press Adv Fctn 5 Enter and scroll to Sample Valve Turn it on using keys 0 and 1 Observe the total flow rate If the flow rate changes when the sample loop is taken out of the flow path then one or both of the fittings on the sample loop is leaking Tighten any leaking fitting If the total flow rate indicates a leak check each connection in the pa
56. ff 44 Using the Adv Fctn Key Advanced Function Descriptions GC READY TYPE 61883 Adv 1 Enter This function indicates the GC mode Pressing Adv Fctn 1 and Enter displays the following message GC IS 6890 orthe current set state Use the scroll key to choose a different mode The following modes are available GC1 GC2 5890 4890 NO GC READY HANDSHAKE MODE G1289 G1290 Adv 9 Enter A hardwired connection is built into the remote start cable between the 6890 or 6580 GC and the 7694 HS Press Adv Fctn 9 and Enter to display the active mode Use the scroll key to choose a different mode The following modes are available CHECK GC READY NO The sampler will not wait for the GC ready signal CHECK GC READY WAIT L 5890 The sampler waits for 5890 GC ready signal before beginning the sequence The headspace sampler s Sample Equilibration Time is ignored the sequence is controlled by GC readiness CHECK GC READY WAIT H 6890 45 Using the Adv Fctn Key Advanced Function Descriptions The sampler waits for 6850 6890 GC ready signal before beginning the sequence The headspace sampler s Sample Equilibration Time is ignored the sequence is controlled by GC readiness CHECK GC READY YES L 5890 The sequence aborts if the HP 5890 GC is not ready after the Vial Equib time has expired CHECK GC READY YES H 6890 The sequence aborts if the 6850 6890 GC is not ready after the Vial Equ
57. fills the sample loop with a precise aliquot of headspace gas Key in the desired time with the numeric keypad followed by Enter Use the down cursor key V to scroll to the next display LOOP EQ TIME The Loop Equilibration Time is the time after the vent valve closes during which the gases in the sample loop equilibrate with the pressure and temperature of the sample loop Key in the desired value using the numeric keypad followed by Enter Use the down cursor key V to scroll to the last display INJECT TIME The Inject Time is the time in which the sample valve is open and the gases in the sample loop are swept into the GC Key in the desired value from the numeric keypad followed by Enter These times may be checked on the display and changed while the headspace sampler is running samples Changes are applied to the next vial analyzed You cannot change parameters for a vial currently being sampled The keys involved are locked 62 Entering a Method Entering a Method Setting Vial Parameters Using this key you specify the locations in the sample tray from which vials will be taken for headspace analysis 1 Press Vial Parameters to bring up the first display FIRST VIAL First Vial specifies the location of the first vial to be analyzed by this method Use the numeric keypad to key in the vial location followed by Enter Use the down cursor key to scroll to the next display LAST VIAL Last Vial spe
58. for the duration of the GC Cycle Time between each incrementation If Vial Temp is incremented the display reads WAITING FOR READY until the new setpoint is reached The default values for both displays are 0 0 which means that the parameter increment is off The two parameters are mutually exclusive if a nonzero number is entered into one the other must be set to zero e Donotallow the maximum vial temperature to be closer than 10 to the boiling point of any solvent in the sample e The Vial Temp Incr function increases the temperature from run to run in the headspace vial only The loop and transfer line temperatures remain at their original setpoints Be sure to set the loop and transfer line temperatures so they exceed the highest temperature the vial is programmed to reach Take note of any maximum temperature on the transfer line you are using e Chain methods are not allowed if either the Vial Temp Incr or the Vial Equilibration Incr is set to a non zero value e If your combination of vial temperature step and number of vials to run would set the oven temperature above it maximum for example the open temperature is 155 C the step is 10 C and you run 6 vials you will see a warning message If you start the run anyway the analysis will stop when the oven reaches 200 C 61883 Adv 7 Enter To activate deactivate Parameter Increment press Adv Fctn 7 and Enter You will see PARAMETER INCR NO or PARAMERTER
59. ght flashes When setpoints are reached the display changes to 7694 Ready and the Not Ready light goes out During normal operation when a run is in progress the Not Ready light may light depending on the values specified for the GC Cycle Time and the Vial Equil Time When the Not Ready light goes on during a run it simply means that the headspace sampler is not ready to insert the next vial into the oven because of timing restraints to maintain constant heating time Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation WARNING Power on Diagnostics When the instrument is powered on or reset see page 30 and page 46 it runs through a series of checks to make sure it is operating properly The messages displayed will vary depending on your model but will be similar to G1289 and G1290 G1883 Agilent 7694 or 7694 RESET Agilent 7694E or 7694E RESET FIRMWARE REV X Y FIRMWARE REV X Y ROM CHECK ROM CHECK OK RAM CHECK RAM CHECK OK TRAY RESET CAROUSEL RESET VIAL TEMP OK VIAL TEMP PROBE OK LOOP TEMP OK LOOP TEMP PROBE OK TR LINE TEMP OK TUBE TEMP PROBE OK 7694 NOT READY 7694E NOT READY 7694 READY 7694E READY Other messages may appear as well If your sampler has a tray the sampler may move remaining vials from the carousel and display a message such as RETURNING VIALS or VIALS RETURNED If you receive other messages see Error
60. h has been heated and is ready for injection with the GC s readiness for another injection For simplicity the two cases are Situation A total preparation time of 30 minutes with run cycle time of 15 minutes Situation B total preparation time of 15 minutes with run cycle time of 30 minutes Sequence of events G1883 The normal sequence of events is 20 Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation 1 The run method is started bo If agitation shaking is set the carousel will shake for the entered amount of minutes The vial is lifted into the heated zone 3 4 The vial is heated for the preset time 5 A headspace injection is made 6 The vial is returned to the carousel Sequence of events G1289 61290 When a vial uses a different method from the preceding vial maximum throughput may be effected Runs for all vials using a particular method must be completed and the vials removed from the carousel before the new method is loaded The following events take place during standard headspace extraction 1 Method loaded 2 Vial placed in oven 9 Vial heated for vial equilibration time 4 Vial sampled 5 GC started 6 Vial returned to tray Multiple Headspace Extraction with Multiple Vial Puncture G1289 G1290 only In multiple headspace extraction mode up to 10 extractions can be made per vial With multiple vial puncture the needle is removed from the v
61. he 7694 Headspace Sampler The 7694 Headspace Sampler motor driven fan in the center of the carousel circulates the air to maintain constant and uniform temperature The carousel can be shaken to help components elute into the headspace quicker Mechanical rods move vials up for removal by a robotic arm or for sampling Adapters part no 301 017 HSP are required in the carousel when 10 ml vials are used Heated Zones 61883 There are three heated zones They are the vial oven the loop and the transfer line The vial oven is where the vial is heated during thermal and chemical stabilization Setpoint temperature range is between 40 and 200 C At this point the needle has not pierced the septum The loop zone is controlling the temperature of the upper chamber the valve and the sample loop The setpoint range of the loop is between 50 and 200 C It is recommended that the loop temperature is kept 15 C higher than the vial temperature for most operations Carrier gas flow control Vial pressurization control Vial transport arm Vial tray Standalone unit only G1289 G1290 Figure 1 Pneumatic Grn Cy Vial pressurization control p Carrier gas flow control compartment Keypad and display G1883 Overview of the 7694 Headspace Sampler from front of instrument Introduction to Headspace and to the 7694 Headspace Sampler The 7694 Headspace
62. he oven assembly 123 Troubleshooting Mechanical Electrical Problems e Check the stepper motor Measure R across the left or right pair of wires in the motor connector R 6 7 ohms Suggested Actions 1 Set agitation on with Vial Parameters 2 Tighten or replace the belt in the oven assembly See your service manual or contact Agilent service Replace the stepper motor if necessary Call Agilent service Sample Tray Doesn t Stop at Correct Location G1289 G1290 only Probable Causes e Optical sensor is blocked or broken e Faulty chip on the mother board e Faulty encoder on the tray motor Suggested Actions 1 Make sure that the tab is in contact with the optical sensor 2 Clean the sensor with an alcohol swab 3 Call Agilent service Sampling Sequence Won t Start Probable Causes e The 7694 Headspace Sampler not ready e Oven stabilization time not expired e No vial in tray G1289 G1290 only e Setpoints not reached Suggested Actions 1 Check the 7694 Headspace Sampler setpoints 124 6 Troubleshooting Mechanical Electrical Problems Oven stabilization time may be set too long Check the STABLIZE TIME advanced function Check that the vials are loaded into the proper locations in the tray or carousel Check that the method specifies the proper vial locations Wait for the 7694 READY display before pressing Start Call Agilent service Second Method in Sequence Won t Start
63. he vial jam If it does not turn the sampler off and continue with the next step Remove all vials from the oven and the gripper Place into the tray any vials from the oven or gripper that still need to be run Press the Clear key and turn the power on Continue to hold the Clear key until you see the message Remove all vials Atthis point the instrument is reset Adjust the method for the new range of vial locations then restart the run Mechanical Electrical Problems Instrument Resets Continuously Probable Causes Shorted temperature sensor 122 Troubleshooting Mechanical Electrical Problems Suggested Actions Call Agilent service No Power Probable Causes e No power to the unit Suggested Actions l Verify that the power cord is connected to the 7694 Headspace Sampler and to a live power source 2 Call Agilent service Oven Carousel Won t Rotate Properly Probable Causes e Loose or broken belt in the oven assembly e Check the stepper motor Measure R across the left or right pair of wires in the motor connector R 6 7 ohms e Dirty carousel sensor eye Suggested Actions 1 Tighten or replace the belt in the oven assembly See your service manual or contact Agilent service Replace the stepper motor if necessary Clean the sensor eye with an alcohol swab 4 Call Agilent service Oven Carousel Won t Agitate Probable Causes e Agitation set off e Loose or broken belt in t
64. ial and the vial is returned to its original position in the oven after an extraction For the first extraction the vial is heated for the programmed vial equilibration time For each successive extraction the vial is heated for the GC cycle time The GC is started after each sampling Vial agitation is allowed during this mode Sample throughput is optimized during this mode 21 Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation Multiple headspace extraction is not allowed if Parameter Increment Advanced Function 2 is on The following events take place during multiple headspace extraction with multiple vial puncture 0 90 SOR cg PESCE OBS cS mM 4 12 Multiple Vial Puncture with Constant Heating Time G1289 61290 only Multiple extraction method loaded Vial placed in oven Vial heated for vial equilibration time Vial sampled according to event times GC started Vial returned to slot in oven carousel Second heating time started time GC cycle time Vial sampled according to event times GC started Vial returned to oven Continue from Step 7 up to number of extractions per vial Vial returned to tray To perform multiple headspace extraction with multiple vial puncture where the heating time for each extraction equals the vial equilibration time you must chain together identical methods The number of methods equals the extractions per vial desired maximum four
65. ib time has expired Note that L stands for Low and H stands for High If CHECK GC READY YES is active then the sampler will check for the presence of a ready signal from the GC just prior to injection If a GC ready signal is not found the sampler will abort the run or sequence return all vials to the tray and display the message GC NOT READY If CHECK GC READY NO is active the headspace sampler will inject regardless of the ready state of the GC 7694 RESET G1289 G1290 Adv Fetn 1 Enter Select 7694 Reset to force the sampler to abort whatever it is doing and re run its startup routine See Power on Diagnostics on page 14 for more information Note e The instrument remains Not Ready until all setpoints for the method are reached e last method in use before reset remains in effect 46 Using the Adv Fctn Key Advanced Function Descriptions Adv Fctn 1 can be used to recover from certain error conditions These include the following VIAL NOT FOUND VIAL NOT LOADED VIAL RETAINED See Error Messages on page 128 for descriptions of these error conditions KEYBOARD LOCK This function disables the numeric keypad and Enter keys 61883 Adv Fctn 4 Enter Selecting Keyboard Lock displays the following message KEYBOARD UNLOCKED This is the default condition To lock the keyboard press 1 Yes KEYBOARD LOCKED To unlock a locked keyboard press 0 No G1289 G1290 Adv
66. ile adding vials and inserts until all samples are loaded into the tray Open end faces up Adapter for tray if equipped Adapter for carousel Part No 300 301 HSP Part No 301 017 HSP up to 44 needed up to 6 needed for G1289 G1290 up to 12 needed to G1883 Figure 10 Adapters for use with 10 ml vials When loading a tray if equipped or carousel e Do not mix 10 ml and 20 ml vials in a tray if equipped e Be sure to insert the oven adapters with the closed end down e To remove oven adapters bend a large paper clip to make a hook and insert the hook into the lip on the inside of the adapter Oven adapters are hot when first removed Place them on a heat resistant surface Do not touch them with bare hands until they are cooled 58 Entering a Method Entering a Method Caution This chapter details the procedure for entering a method including storing and retrieving a method and chaining methods Entering a Method To enter a method for the 7694 Headspace Sampler via the keypad setpoints must be set for the keys labeled Zone Temps Event Times and Vial Parameters Each of these keys has a number of setpoints associated with it The cursor keys A V scroll up and down through the list of setpoints To enter a value for a setpoint scroll to that setpoint key in the value using the numeric keypad then press Enter If the value keyed in is not within the allowed range the sampler displays a mes
67. ing 56 Running more than 44 66 Shaking 34 63 Uncapping 56 Z Zone temperatures See Temperatures 31 Zone temps Entering 60 Zone temps key Using 31 147 Index 148
68. ion curve A graph showing the relationship between the amount of a compound and its response from an analytical technique In gas chromatography that response is the peak area carrier gas The gas that flows through the chromatographic column and moves the sample components when they are not retained by the stationary phase chromatographic column A tube e g of glass stainless steel or plastic generally cylindrical containing the stationary phase and provided with an inlet and an outlet for the mobile phase chromatography A separation method in which the sample components different affinities toward two phases one of which is immobile the stationary phase and the other which moves the mobile phase are taken advantage of column See chromatographic column constant heating mode In HS sampling a setting which heats the contents of each sample vial for an identical length of time for each extraction distribution coefficient See partition coefficient elastomeric displaying elastic qualities similar to rubber Electron Capture Detector ECD A gas phase detector that uses a radioactive source and detects a component by its ability to capture low energy electrons eluate The material exiting a column in chromatography equilibrium In HS sampling the point at which molecules diffuse out of the sample into the headspace at the same rate at which they diffuse from the headspace back into the sample 135 Glossary external s
69. l models is 40 C or 15 C above ambient whichever is greater Do not enter a value below the minimum oven operating temperature even though temperatures between 0 39 C are accepted e Ifa Zone Temp is changed during a run the sampler will not display NOT READY but it will adjust the zone to the new temperature value e Asa general rule the temperatures for the loop and transfer line should be set higher than the oven temperature to avoid condensation Set the loop 31 The Keypad Keys and Their Functions Caution temperature 15 C higher than the oven and set the transfer line 25 C higher than the oven e To set the oven temperature at 40 C set the loop temperature at 40 C The minimum oven temperature is approximately 15 C above ambient Oven temperature should not exceed 10 C below the boiling point of any solvents in the vial Exceeding this may cause the cap and septum to leak or to pop off the vial pressure line could also become contaminated Event Times Pressing Event Times brings up the first menu item Setpoint GC CYCLE TIME The cursor keys allow scrolling through the list of events They are the following Allowed Setpoint Range Default Value Event min increments min GC CYCLE TIME 1 0 999 9 in 0 1 25 VIAL EQ TIME 0 999 9 in 0 1 15 PRESSURIZ TIME 0 99 99 in 0 01 0 20 LOOP FILL TIME 0 99 99 in 0 01 0 20 LOOP EQ TIME 0 99 99 in 0 01 0 05 INJECT TIME 0 99 99 in 0 01 1 00
70. lded PTFE silicone septa 144 pk Sample loops General purpose Wider temperature range septa need higher sensitivity 5182 0839 5182 0840 0 25 ml nickel 169 0011 HSP 0 5 ml nickel 169 0012 HSP 1 ml nickel 321 055 HSP 2 ml nickel 169 0013 HSP 3 ml nickel 321 056 HSP 1 ml Silcosteel 9 321 058 HSP 3 ml Silcosteel 321 059 HSP Probes unions Nickel needle assembly for G1289 or G1290 301 013 HSP Silcosteel needle assembly for 61289 or G1290 301 220 HSP Nickel needle assembly for G1883 232 2790010 EHS Silcosteel needle assembly for 61883 232 2790012 EHS Zero dead volume union for G1290 G1289 325 045 HSP Union elbow for G1883 998 0000053 EHS 86 Maintaining the Instrument Common Replacement Parts and Consumables Table 7 Common Replacement Parts and Consumables continued Description Comment use Part Number Transfer line needles and unions Transfer line needle dia 0 5 for on column inlet Nickel 301 016 HSP Transfer line needle dia 0 7 for split splitless inlet Nickel 301 015 HSP Transfer line needle dia 0 7 for split splitless inlet Silcosteel 301 221 HSP Union M5 D1 6 SS assembly Zero dead volume union 325 961 DAN Strain relief Supports needle through GC inlet 301 205 HSP septum Manuals Site Preparation and Installation 61290 90307 Operating 61290 90317 Service CD ROM 61290 90327 Standards Headspace 0Q PV Standard kit 5182 9733 1 ampoule of standard 1 ml 1 pkg
71. mation error recovering from 133 Auxiliary gas Setting flow rates 73 Auxiliary gas flow setting G1883 G1290 81 Auxiliary gas setting G1289 81 C Carousel Advancing 48 Loading vials 58 Using adapters 58 Carousel advance 36 Carrier gas 9 Carrier gas setting G1289 81 G1883 G1290 80 Chain methods key Description 36 65 Using 36 65 Chaining methods Description 65 Key description 36 Multiple headspace extraction 65 To run more than 44 vials 66 Using 65 Chromatography troubleshooting Bad peaks 117 141 Index No peaks 116 Unwanted peaks 119 Clear Key operations 37 Clear key Description 37 Using 37 Constand heating time With multiple vial puncture 22 Consumables 85 Contamination Pneumatic system cleaning 95 Conventions Description 3 D Default method Parameters 44 Default method Adv Fctn 7 Description 44 E Enter key Using 37 Entering data Setpoints 26 40 EPC ready sampler Pneumatics description 11 Equilibrium Curve 72 Determining 72 Error messages 7694 RESET 128 7694E RESET 128 Agilent 7694 128 Agilent 7694E 128 ALARM STEPPER 129 ALARM TEMP 129 CAROUSEL RESET 130 FIRMWARE REV 128 Power failure 128 130 PRESS STOP TO CONFIRM 130 RAM CHECK ERR 130 Recovering from 47 REMOVE ALL VIALS 131 ROM CHECK ERR 131 TRAY RESET 132 UP MOTOR ERROR 132 VIAL NOT FOUND 132 VIAL RETAINED 133 Error automation 133 Event times Entering
72. method Store this method in one of the four storage locations Press the following Chain Methods X X X X where X is the location where your method is stored Using a Method Chain for Running More Than 44 Samples By chaining the same method to itself you can run up to 88 vials To run more than the 44 sample vials in the tray do the following 66 Entering a Method Using a Method Chain for Running More Than 44 Samples Key in the vial parameters First Vial 1 Last Vial 44 Press the following Chain Methods X X X X where X is the location where your method is stored Manually change the vials in the tray at the appropriate time so that you do not re sample the same vials 67 Entering a Method Using a Method Chain for Running More Than 44 Samples 68 Developing Methods Developing Methods This chapter discusses various parameters that can affect the sensitivity precision and accuracy of an analysis m E J x G E x xX X x Equilibration X y xxxi x X XXxx XX x Ix X x C x Xx X Xx x XX Ix X x Xyx Cy Figure 11 Illustration of partition coefficient The tendency of a material to go into the gaseous phase is the partition coefficient K where C is the concentration of the analyte in the condensed phase the sample matrix and C is the concentration of the analyte in the gaseous phase the headspa
73. n for trace analysis might be desired A 3 ml loop is available See Changing the Sample Loop on page 92 A larger sample injection may broaden some peaks especially on a capillary column Sample Size A larger sample size may give greater sensitivity Peak areas are often strongly influenced by the relative amount of the gas and condensed phases in the sample vial Increasing the sample size may give corresponding increases in peak areas If sensitivity is not an issue small samples may be preferred because the required equilibration time is shorter Vial Pressurization and Time Vial Pressurization With many liquid e g aqueous samples the pressure developed in the vial may be sufficient to ensure filling the valve loop without additional pressure 73 Developing Methods Optimizing Carrier Gas Flow Note Note Some samples e g dry plastics may not create enough head pressure and do require more in the method In general 1 5 2 atmospheres pressure in the vial will be appropriate for filling the valve loop It may be possible to make or buy a pressure gauge fitted with a needle that could be used to determine the actual vial pressure developed under your time and temperature conditions Set the method vial pressurization at a slightly higher value e g 3 5 psi if your measured pressure is not enough to ensure adequate loop filling To optimize your selection of vial pressurization run a series of vial
74. nnections on the sampling valve probe connections or vial cap septum If the unit fails the test the leak is in the Aux control module the Swagelok fittings on the back of the sampler or the auxiliary bleed fitting 109 Maintaining the Instrument Leak Testing a G1290 G1883 to GC Interface WARNING Leak Testing a G1290 G1883 to GC Interface For the G1290 G1883 you can check the carrier gas flow system for leaks by performing a pressure decay test The heated zones of the unit can burn your skin Allow the zones to cool off before performing the test Prepare the Sampler 1 Set the three heated zones to ambient temperature 2 Detachthe transfer line from the inlet or interface and plug it with either a new inlet septum or a leak test fitting as shown in Figure 29 ES Io Leak test fitting b 3 4 325 0050010 HSP A new inlet septum Figure 29 Plug the transfer line 3 Remove the pneumatics cover and loop oven cover to give you access to all of the tubing valve and manifold connections Carrier Gas Flow Path 1 Open the Mass flow controller full counter clockwise CCW until the carrier flow path pressurizes to line pressure The carrier pressure should read between 40 to 60 psi about 4 bar 2 Shutoffthe ball valve installed between the source and the headspace sampler An alternative would be to turn the Mass Flow Controller full clockwise CW 110 WARNING Maintaining the Instrume
75. nt Leak Testing a G1290 G1883 to GC Interface Turning the valve may not completely shut off flow depending on the setting of the knob on the stem Also excessive pressure on the stem can damage the flow controller if the knob is set to allow full travel 3 Using MANUAL OPERATION switch the sample valve to 0 or OFF See MANUAL OPERATION on page 48 for details Monitor the pressure on the front panel display it should equilibrate at some pressure close to the line pressure and then hold It should drop less than 2 psi in 5 minutes If the pressure drop is much greater there is a leak Using MANUAL OPERATION switch the sample valve to 1 or ON to include the sample loop Repeat steps 2 5 After the test remove the septum or plug The flow path should instantaneously de pressurize If it does not there may be a restriction Using MANUAL OPERATION switch the sample valve to 0 or OFF to reset the sample loop Vial Pressurization Flowpath 1 Prepare a new empty 20 ml headspace vial Make sure that it is capped properly See Sample Preparation on page 56 Manually install the headspace vial in the oven slot under the headspace probe Using MANUAL OPERATION load the vial onto the probe and make sure the Pressurize Valve is ON and the Vent Valve is OFF Pressurize the vial to 20 psi by adjusting the pressurize regulator Wait at least 1 minute to allow the system to equilibrate then shut off the
76. oller The vial pressurization is measured at the outlet of the pressure regulator before the in line restrictor It is a read only display no editing is allowed Use the cursor keys to scroll the display from the carrier gas to the vial pressurization gas Tray Advance G1289 G1290 only This key is used to move the sample tray for vial insertion and removal Keying in vial position and Enter moves that vial position to the position The home position in the tray is pointed out by an arrow silk screened on the oven For easier access to vials for inserting and removing them key in position 4 and Enter to bring that position to the very front of the sample 36 The Keypad Keys and Their Functions tray The cursor keys move the tray forward or backward by increments of one position Enter This key is used after choosing a numeric value for a setpoint Pressing Enter after making a set point change incorporates the change into the active method Clear The Clear key has two functions During editing pressing Clear returns the value to its previous setpoint If not editing Clear returns the display to the menu top level You may need to press Clear more than once to reach the top level Numeric Keypad The numbered keys are used to enter setpoint values for the variable conditions of the headspace sampler After a numeric value is keyed in press Enter to make the value part of the active method Adv Fe
77. only VIAL PRESS PSI XX example CARR PRESS PSI YY example STABILIZE TIME 61883 Adv 6 Enter G1289 G1290 Adv 1 Enter This function changes the length of time the oven equilibrates after reaching its initial setpoint before vials are loaded into the oven Selecting Stabilize Time displays the following STABILIZE TIME 1 0 One minute is the default time The allowed range of values is 0 0 to 99 9 minutes VALVE COUNT G1883 Adv 2 Enter G1289 G1290 Adv 2 Enter Displays the number of times the sampling valve has actuated Agilent service personnel may refer to the valve count to get an idea of the extent of the sampler s use 53 Using the Adv Fctn Key Advanced Function Descriptions VIAL NO AND LOC G1289 G1290 Adv Fetn 3 Enter Selecting Vial No and Loc displays the following 05 06 07 08 09 10 EXAMPLE It tells the user what vial number is in which position in the oven carousel The first number on the left is the first oven carousel position the last number on the right is the sixth oven carousel position In this example vial number five is in oven carousel position one and vial number 10 is in position six This is a read only display No editing is possible 54 Preparing a Sample Preparing a Sample Note This chapter describes the steps necessary to prepare a sample for analysis including filling and sealing a sample vial and loading
78. oop Equilibration Time Time to allow the analytes in the sample loop to equilibrate to the higher loop temperature and to allow pressure and flow in the loop to stabilize The allowed range of values is from 0 00 to 99 99 minutes INJECT TIME Time in which the gases in the sample loop are injected into the GC This time must be sufficient for complete sample transfer If the time is too short the analysis will lose sensitivity because not all the sample will be transferred It is 33 The Keypad Keys and Their Functions not a problem if the time is longer than necessary The allowed range of values is from 0 00 to 99 99 minutes Vial Parameters This key specifies the vial s analyzed during a method Use the cursor keys to Scroll through the following set of parameters FIRST VIAL Designates the first vial 1 44 for the G1289 G1290 1 12 for the G1883 analyzed by the current method LAST VIAL Designates the last vial 1 44 for the G1289 G1290 1 12 for the G1883 analyzed by the current method The last vial number cannot be lower than the first vial number The headspace sampler will give an error message and you will need to re enter the vial number For models G1289 G1290 if one or more sample tray slots is left empty between the first vial and the last vial the instrument will check the empty positions for a vial and then move on to the next tray position SHAKE 0 1 2 G1883 Sets the agitation level of th
79. op Fill Time Normally set the loop fill time to 10 seconds A very short loop fill time one or two seconds may help increase sensitivity in headspace analysis The headspace gas purges the sample loop but the vent valve is closed before the sample vial falls to atmospheric pressure The loop is maintained at the vial s still elevated pressure Because the loop pressure is greater the analyte will be more concentrated and consequently more sample will be injected into the GC Matrix Effects The composition of the sample matrix can affect the amount of analyte that escapes into the headspace Adding an inorganic salt to aqueous samples increases the concentration of organic molecules in the headspace by making them less soluble in the sample matrix increasing sensitivity For nonaqueous 72 Note Developing Methods Changing the Sample Loop but water miscible systems dilute the sample with water This decreases the solubility of most organic molecules in the sample and increases their concentration in the headspace Matrix effects are important when developing external standards The composition of the matrix in the standard should closely resemble that of the sample or accuracy suffers The effect of the matrix on a standard can be compensated for by using the standard addition method or by quantifying results using MHE Changing the Sample Loop Although the 1 ml sample loop is usually adequate a larger sample injectio
80. p Equilibration Both pressure and vent valves are closed for the length of time assigned to this setpoint Injecting the Sample The sample valve brings the sample loop in line with the carrier gas flow The carrier gas flows through the sample loop and the transfer line into the GC inlet port This sweeps the sample into the GC Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation Pressure Vent transducer Carrier gt gt I et ee p gt ON Lem gas flow EL Mass flow controller L Pressure transducer Auxiliary gas flow for vial Pressure pressurization regulator restrictor Needle P lt Open gt Closed Carrier gas g Headspace Auxiliary gas vial Figure 7 Injection S1 and S2 are closed End of Cycle and Vial Recovery The sample vial is lowered back into the carousel For models with a vial tray the carousel rotates and the robotic arm returns the vial to the tray The vent valve opens to purge the vent line The sampler returns to the standby configuration Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation Pressure Vent transducer Carrier gt gt M Sa eee aa es fo L AY gas flow Mass flow I controller J Pressure transducer 32 Auxiliary gas Ab 51 t soe ST Po EE flow for vial Sample ressurization loo P regulator Flow a Oop
81. play reads PRESS STOP TO CONFIRM This prevents an inadvertent run interruption To stop press the key again To continue the run press Clear e Ifyou press the Start Stop key while the robotic arm is moving the display shows the message Wait End of Movement Press the Stop key again after the movement is completed e When you stop the sampler during a run the robotic arm automatically returns the vials in the oven to the sample tray The method cannot be resumed from the point at which you stopped it If you want to continue the analysis from the last vial sampled you must change the method so that it starts with the correct vial 30 Zone Temps The Keypad Keys and Their Functions Press Zone Temps to set temperature values for various heated zones in the sampler Pressing Zone Temps brings up the following top level display Actual Setpoint G1289 G1290 OVEN 100 120 Actual Setpoint G1883 VIAL 100 120 Use the cursor keys to scrollto LOOP or TR LINE Transfer Line to set these temperature values The allowed range of values is as follows Heated Zone Allowed Setpoint Range G1883 Vial 40 200 in 1 C increments Loop 50 200 in 1 C increments Tr Line 50 220 in 1 C increments G1289 G1290 Oven 0 200 in 1 C increments Loop 0 220 in 1 C increments Tr Line 0 220 in 1 C increments Default Value C 70 50 50 70 80 90 The minimum oven temperature for al
82. pler cover shown below and lift the cover Support the cover while working in the sampler area Lift front cover Rear cover Remove screws Manifold cover Figure 16 Removing the sampler cover 2 Loosen the two screws on the manifold cover it is a stainless steel box and insulation from the valve compartment 89 Maintaining the Instrument Changing the Sampling Needle Manifold cover Loosen and insulation Sampler cover removed for clarity Figure 17 Removing the manifold cover and insulation 3 sampling needle is located inside the square aluminum block It is connected to the sampling valve through a 1 16 inch nickel tube and hexagonal union 4 Support the hexagonal union with a 7 mm wrench and remove the nut with another 7 mm wrench Then loosen and remove the hexagonal union Lift out the needle 90 Maintaining the Instrument Changing the Sampling Needle Union D Hexagonal union Sampling needle Sampling needle TDA G1289 G1290 G1883 Figure 18 Position of vial sampling needle 5 Replace the sampling needle tighten the fittings and perform a leak test before replacing the insulation and cover 91 Maintaining the Instrument Changing the Sample Loop Changing the Sample Loop 1 Remove the two screws on the sides of the sampler cover shown below and lift the cover Support the cover while working in the sampler
83. port a Scroll down until the display reads X AXIS Press 1 to move the vial to the left Press 1 again to position the vial over the oven port b Scroll up until the display reads Y AXIS Press 0 to lower the vial into the oven port The vial should be placed in the center of the oven port 99 Maintaining the Instrument Aligning the Vial Loader G1289 G1290 only and should not touch the walls Press 1 then 0 to move the fork up and down and watch the motion Repeat several times If the vial appears to be too far right or left from the oven port adjust P3 5 Check vial release and pickup at the oven port Scroll down until the display reads VIAL LOAD Press 1 to move the elevator to the up position Scroll up until the display reads Y AXIS Press 0 to move the vial down into the oven port Scroll down until the display reads X AXIS Press 0 then 1 to move the fork left and right The fork should cleanly release the vial then grab it again If the fork is too high or too low adjust the spring lock and spacer on the top of the oven cover If you make an adjustment to the spring lock repeat step 3b Spring lock and spacer Figure 24 Spring lock and spacer 100 WARNING Maintaining the Instrument Checking carousel adjustment Other vial handling adjustments In addition to the potentiometers also check or adjust the following e Vial size selection switch on the back of the vial transport arm e Carousel
84. pressurize regulator full CCW Monitor the pressure on the front panel display It should equilibrate at some pressure lower than 20 psi and then hold dropping less than 5 psi in 10 minutes If the pressure drop is much greater there is a leak Using MANUAL OPERATION switch the sample valve and repeat steps 2 6 111 Maintaining the Instrument Flow Testing the Vent Valve and Associated Flow Path 8 De pressurize the system by opening the vent valve from MANUAL OPERATION Flow Testing the Vent Valve and Associated Flow Path Perform this test only after the system all models passes the carrier and pressurize vial tests 1 Prepare a new empty 20 ml headspace vial Make sure that it is capped properly See Sample Preparation on page 56 Manually install the headspace vial under the probe in the headspace oven Set the Vial Pressure to 20 psi Place the vent exit tube from back of headspace in a beaker of water e If needed extend the tube using 1 8 inch PTFE or similar tubing Using MANUAL OPERATION load the vial onto the probe set the vent valve to OFF and set the pressurize valve to ON See MANUAL OPERATION on page 48 for details Wait at least 20 seconds for the vial to pressurize Using MANUAL OPERATION turn Pressurize Valve OFF and set the vent valve to ON Observe the vent tube in the water The vent tube should produce bubbles immediately when the vent is turned
85. r MHE enne 66 Using a Method Chain for Running More Than 44 Samples 66 Chapter 7 Developing Methods Varying Oven Temperature esessssseeseeeee eterne nennen nennen senes 71 Varying Event TIMES e eina pea sid pue 71 Vial Equilibration Time 71 Loop Fill Time iiec ete eerte erae eh re eee eon ee eor ee race reads 72 Matris Eee EE ER 72 Changing the Sample Loop tenete enne nennen tenente 73 Sample Size 73 Vial Pressurization and Time esses eene 73 Vial PrESSUTIZALION dita cas este Pee 73 Vial Pressuri zation EE S 74 Optimizing Carrier Gas Flow 74 Recommended 6890 6850 Liner esses enne nnn 75 Chapter 8 Running a Sample Setting Conditions treo Ee nete Ese ei 78 Flow Rates E 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 Contents Chapter 9 Maintaining the Instrument Common Replacement Par
86. ressure Lada v CARR PRESS VIAL PRESS Displays current carrier gas pressure setpoint Displays current vial pressurization pressure setpoint Tray Advance TRAY POSITION Moves slots in sample tray to their home position Use cursor keys to move slots forward or backward by one position Enter Adds keyboard entry to current method Clear Cancels a keyboard entry Displays menu top level Adv Fctn ADV FCTN Accesses nonroutine parameters See Using the Adv Fctn Key on page 40 29 The Keypad Keys and Their Functions Keys and Their Functions Start 61883 only Press this key to start a run Stop Reset 61883 only Press this key once to stop a run To reset the unit press the key again The sampler aborts whatever it is doing and re runs its startup routine See Power on Diagnostics on page 14 e The method cannot be resumed from the point at which you stopped it If you want to continue the analysis from the last vial sampled you must change the method so that it starts with the correct vial e If this key is pressed when the unit is not in a run the unit will be reset e The last method in use before reset remains in effect The instrument is not ready until it reaches all setpoints Start Stop G1289 G1290 only Press this key to start or stop a run To start a run press once To stop a run press the key again The dis
87. restrictor 4 Needle i y 3 To GC Carrier gas Auxiliary gas Headspace J vial Figure 8 Purge S1 and S2 are open S2 is open for 30 seconds Modes of Operation The 7694 Headspace Sampler has two modes of operation standard headspace extraction and multiple headspace extraction Standard Headspace Extraction In standard headspace extraction mode one extraction is made per vial The GC run starts when the sample is injected into the GC inlet In order to Introduction to Headspace and to the 7694 Headspace Sampler Modes of Operation Minutes maintain the same incubation interval during the gas chromatographic run vials are transferred one by one into the oven and recovered after sampling The sampler analyzes the event times and the GC cycle time then adjusts vial delivery and recovery times to optimize overall process time Vial agitation is allowed in this mode Note that the GC run cycle time is the time from injection until the system is READY for another injection Occasionally the time for data handling will become a factor 15 30 60 90 130 Run 1 Run 2 Run 3 Vial 1 prepared Vial 2 prepared Vial 3 prepared Vial 4 prepared Run 1 Run 2 Run 3 Vial 1 Vial 2 Vial 3 Vial 4 prepared prepared prepared prepared The diagram above shows how the instrument actually synchronizes the availability of a vial whic
88. rther operator intervention Method chaining is also a means of performing multiple headspace extraction MHE Activate a Method Chain To activate a method chain 1 Press Chain Methods The display reads as follows METH Ss 2 Press a method number 1 4 A flashing appears on the display followed by the method number chosen Key in the method sequence in the order to be run 4 Press Enter The following flashing message is displayed METH CHAIN ON Methods are run in order from left to right on the display For example keying in the following 2413 Enter would have the sampler run method two followed by method four then methods one and three Press Chain Methods again to display the current chain sequence This method sequence is active until you edit it or press Load Method 65 Entering a Method Using a Method Chain for MHE Note Deactivate a Method Chain To deactivate a method chain l Press Chain Methods The display shows METH where is the number of a method 2 Press 0 NO to display METH CHAIN OFF If Parameter Increment is active Chain Methods is inactive Turn off Parameter Increment to use the method chain feature Using a Method Chain for MHE Use Chain Methods to perform a multiple headspace extraction with multiple punctures and constant equilibration time for each extraction To run an MHE 1 Key in the parameters for Zone Temps Event Times and Vial Parameters for the
89. rting Runs 30 Steam cleaning pneumatics Procedure 95 Stopping Runs 30 Store method key Using 35 Storing Methods 35 64 T Temperatures Entering values 31 Optimizing with 71 Setting values 31 Times Entering setpoints 32 GC cycle time 32 Injecting sample into GC 33 Loop equilibration 33 Loop filling 33 Setting values 32 Vial equilibration 33 Vial pressurization 33 Transfer line Description 10 Entering temperature 60 Transfer line location 9 Tray advance key Using 36 146 V Valve count Adv Fctn 2 Description 53 Vial elevator assembly Failure error message 132 Vial equilibration time Description 33 61 Entering 33 61 Optimizing 71 Vial gripper arm Adjusting motion 97 Troubleshooting 119 Vial handling troubleshooting Vial gripper arm malfunction 119 Vial jam 121 Vial not loading 121 Vial positioning 120 Vial heating time See Vial equilibration time 33 Vial No and Loc Adv Fctn 3 Description 54 Vial parameters key Using 34 Vial Pressure setting G1289 81 G1883 G1290 81 Vial pressurization 9 Description 15 Vial pressurization time Description 33 Entering 33 Vial sampling needle See Sampling needle 91 Index Vial transport arm Description 9 Vial tray Descripton 9 Vials Agitating 34 63 Capping 56 Crimping 56 Description 56 Entering parameters 34 63 Error messages 132 133 Filling 56 Loading carousel 58 Loading tray 58 Prepar
90. s using different pressures and interpret the optimum conditions from peak areas versus vial pressurization Optimization is valid only for analysis of a specific sample at a specific oven temperature Vial Pressurization Time Typical vial pressurizations times range from 10 to 30 seconds Optimizing Carrier Gas Flow The 7694 Headspace Sampler carrier gas flow rate should be set high enough to sweep the headspace sample out of the sample loop into the GC without causing peak broadening For example for a packed GC column that gives 15 second wide peaks flow would be at least 6 ml min for a 1 ml loop This will sweep out the loop in 10 seconds Some detectors such as ECDs and TCDs are more sensitive at lower detector flow rates 74 Developing Methods Recommended 6890 6850 GC Liner Recommended 6890 6850 GC Liner For the split splitless inlet Agilent recommends using the deactivated splitless liner part no 5181 8818 75 Developing Methods Recommended 6890 6850 GC Liner 76 Running a Sample Running a Sample To run a sample perform the following 1 If the transfer line is not connected to the GC connect it e If using a needle through the septum see your installation manual e If using a volatiles interface see page 96 Check your gas supplies to make sure you have sufficient gas available for all your analyses Set the flow and pressures for the headspace sampler See page 78
91. s vial through needle Imes x3 FILL TIME Time when gaseous contents of vial pass EE through loop to vent mo y 4 LOOP EQ TIME Time when gases in loop equilibrate Times X v x5 INJECT TIME Time when gases in sample loop are swept MELDE into the GC Vial FIRST VIAL First vial analyzed during the method Parameters Vil un LAST VIAL Last vial analyzed during the method V eters x2 SHAKE 0 1 2 Sets agitation level of oven carousel 0 off 1 low 2 high Load LOAD METHOD Moves a method from stored to active ma memory for current use pun STORE METHOD Moves a method in active memory into one of ethol H four memory storage locations om METH S Strings chains methods together to form a lethods sequence 27 The Keypad The G1289 G1290 Keypad Table 2 continued Key Sequence Display top Reset Definition Function Stops and or resets a run Carousel Advance Moves carousel ahead one position Enter Adds keyboard entry to current method Clear Cancels a keyboard entry Displays menu top level EU ADV FCTN Fctn Accesses nonroutine parameters See Using the Adv Fctn Key on page 40 The G1289 G1290 Keypad The table below lists all the keys available on your instrument and summarizes their functions See Keys and Their Functions on page 30 for details about key functions Table 3 Quick Reference of G1289 G1290 Keys and Functions
92. sage showing the allowed range Pressing any non number key removes the error message If the value keyed in is not the one desired pressing Clear returns you to the top level of the display Entering Zone Temps This key allows you to enter values for the oven temperature loop temperature and transfer line temperature Press Zone Temps The sampler displays the following G1289 and G1290 G1883 OVEN VIAL Key in the desired value for the oven temperature setting followed by Enter The allowed range for this setting is 0 200 C 40 200 C for G1883 The oven temperature should not exceed 10 C below the boiling point of any solvent in the vial Exceeding this may cause the cap and septum to leak or to pop off 60 Note Note Entering a Method Entering a Method Although the sampler may allow you to enter temperatures from 0 C to 39 C the minimum oven temperature is 40 C or 15 C above ambient whichever is greater Use the down cursor key to scroll to the following display LOOP Key in the desired sample loop temperature within the allowed range of 0 220 C for the G1289 G1290 50 220 C for the G1883 followed by Enter Use the down cursor key to scroll to the last setpoint display TR LINE Key in the desired setpoint on the numeric keypad for the transfer line temperature followed by Enter The allowed range is 0 220 C for the G1289 G1290 or 50 220 C for the G1883 As a general rule th
93. se of determining the amount of a compound in a sample 137 Glossary retention time The time interval from the moment of injection of a sample into the column to the appearance of the peak maximum of the given component in the eluate sampling sequence In headspace analysis the steps involved in removing the sample from the vial and injecting it into the GC column These steps include puncturing the septum pressurizing the vial venting the vial and injecting the headspace gas into the GC scroll To move text or graphics to see parts of the file that cannot be seen on the display sensitivity ofanalytical method The ratio of the analytical signal increment to the corresponding increment of concentration or contents of the determinant setpoint Numerical value for an analytical step entered into a method single headspace extraction The standard method of headspace analysis One headspace sample is taken from each sample vial being analyzed See multiple headspace extraction single puncture Multiple headspace extraction performed by piercing the septum with the needle only once The needle remains in the vial for all the heating and sampling steps until it is withdrawn after the last extraction See multiple puncture split injection A injection method that allows very small amounts of sample to be introduced to capillary columns A homogeneous sample is split into two portions in a known ratio the smaller portion is introdu
94. ssscncsensecncsenscetscenceenseenscsaaceneeectacsasenteenesensees 126 Chapter 11 Error Messages Error Message Listing set nca eem eed eire a GE 128 Recovery from an Automation Error G1289 G1290 133 I pM 135 nr e 141 Contents vi About This Manual About This Manual Manual Overview About This Manual The 7694 Headspace Sampler Operating Manual explains how to use the 7694 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 Keypad describes the keypad the functions each key controls and how to enter new setpoints for each function Chapter 4 Using the Adv Fctn Key describes the advanced functions controlled by the Adv Fctn key how to e
95. ssure Vent transducer Carrier gt gt Musis a ee PON gas flow TV Mass flow controller L poe ee 3 Pressure transducer 52 s1 ly Auxiliary gas i dd BRI eeu EV LL flow for vial gt ressurization Flow restrictor PI Open Needle p lt Closed Carrier gas Auxiliary gas Headspace vial Figure 5 Vial pressurization S1 is closed vial raised on needle Filling the Sample Loop The vent valve opens and the headspace gas fills the sample loop it then vents to atmospheric pressure through the vent outlet A short loop fill time 2 to 5 seconds may leave pressure in the loop equilibrated to the vial pressure and allow more analyte to be injected A longer loop fill time 10 to 15 seconds will equilibrate the loop pressure to atmospheric pressure Introduction to Headspace and to the 7694 Headspace Sampler Principles of Operation Pressure Vent transducer Carrier gt T gt T ue Se ee Se eee Nea gas flow i EL Mass flow 4 controller L ee Pressure r transducer 52 Auxiliary gas En 51 t V M e U p flow for vial Sample ressurization Flow N a4 restrictor NUN SOM t Needle i pen b u x d Closed i To GC Carrier gas Headspace i Auxiliary gas vial PERDRE 2j Figure 8 Loop fill S1 is closed S2 is open to fill loop Loo
96. stomer 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 WARNING A warning calls attention to a condition or possible situation that could cause injury to the user CAUTION A caution calls attention to a condition or possible situation that could damage or destroy the product or the user s Work A Indicates a hot surface L 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 Typpr fung Agilent Technologies Inc 2850 Centerville Road Wilmington DE 19808 1610 USA Contents Chapter 1 About This Manual Manual Overview eese ess etes esses stessi etes sitit e 2 Intended Ser titre rece ette aeo oe Dese veo decret eU 3
97. tandard A sample containing a known quantity of the component to be quantified Flame Ionization Detector FID An ionization detector consisting of a hydrogen burner whose flame burns between two electrodes with potential difference between them When the column effluent gas is burned with air or oxygen in the hydrogen flame an increased ionization current is obtained as a result of ionization of the solute molecules flow rate The amount of the carrier gas passing through the column per unit time Flame Photometric Detector FPD A detector that measures the intensity of the light at fixed wavelength that accompanies the combustion of the eluate in a hydrogen rich flame gas chromatography GC Chromatography in which a gas is the mobile phase headspace HS The gaseous space in a sealed vial above the solid or liquid sample in that vial The headspace is composed of volatile compounds contained in the sample injection In chromatography introduction of a sample to a column See also split injection and splitless injection internal standard A compound added in known concentration to the sample for example to eliminate the need to measure the size of the sample in quantitative analysis matrix The main constituents of a sample other than the detected and or determined component matrix effect The disturbing influence of other components of the analyzed sample on the detection and or determination of an analyte menu A list of it
98. th and tighten if necessary Do not tighten Swagelok fittings more than approximately 1 4 turn If needed remake the connection Carrier Flow Path Pressurization Test This test is an alternate to the test described above 1 2 Set the three heated zones to ambient temperature De configure the GC column assigned to the inlet used with the headspace sampler Cap the column fitting with a no hole ferrule part no 5181 7458 Cap the inlet s septum purge fitting with a 1 8 inch Swagelok cap 107 Maintaining the Instrument Leak Testing a G1289 to 6890 GC Interface 5 Setthe following GC conditions Setting Value Inlet PTV or split splitless Mode Splitless Total flow 60 ml min Pressure 25 00 psi Allow the system at least 60 seconds to equilibrate Turn the inlet pressure Off Monitor the pressure on the GC front panel display It should equilibrate close to the setpoint pressure and then hold It should drop less than 2 psi in 5 minutes 9 Using MANUAL OPERATION switch the sample valve to 1 or ON to include the sample loop 10 Repeat steps 5 8 11 After the test remove the plug in the column fitting The flow path should instantaneously de pressurize 12 Using MANUAL OPERATION switch the sample valve to 0 or OFF to reset the sample loop Vial Pressurization Gas Aux Flow Path Leak test 1 Prepare anew empty 20 ml headspace vial Make sure that it is capped properly See S
99. the loaders and the vial gripper fork These potentiometers are located in the horizontal loader arm You will need to remove the horizontal loader back cover to adjust them The procedure to adjust the potentiometers is described below The procedure to check vial loader operation starts on page 99 Adjusting the potentiometers Remove the back cover by removing the three screws Remove screws Back cover Figure 22 Removing the horizontal loader back cover 97 Maintaining the Instrument Aligning the Vial Loader G1289 G1290 only The potentiometers are located on a small printed circuit board and are labelled P1 through P6 See Figure 23 Use the procedure on page 99 to identify which potentiometer you need to adjust P1 and P2 adjust the height of the fork these are the y axis adjustments P3 through P6 adjust the horizontal position of the fork at four different locations these are x axis adjustments Horizontal loader assembly Potentiometers Vial size selection switch Horizontal loader PC board The potentiometers are located on the PC board for the horizontal loader Figure 23 Potentiometers controlling the vial gripper arm To determine if you need to turn a potentiometer clockwise or counterclockwise refer to Table 9 Then use a small flathead screwdriver to turn the adjusting screw 98 Maintaining the Instrument Aligning the Vial Loader G1289 G1290 only
100. the sample tray Sample Preparation The 7694 Headspace Sampler can accept either 10 or 20 ml sample vials You cannot mix vial sizes when loading the tray Before using 10 ml vials you must insert adapters into the spaces in the sample tray and in the oven carousel Samples that will undergo headspace extraction are placed in the sampler in glass vials You also must flip the switch on the back of the horizontal loader to the proper size setting In general sample vials should be filled only about half way although vials can be filled to the 3 4 level This ensures that the needle will not come into contact with the solid or liquid phase during the sampling step The vial must be sealed properly to insure that the headspace gases do not escape prematurely Use a crimper designed for headspace vials with 20 mm caps to seal the vials Agilent part no 9301 0720 Sampling from an incorrectly capped vial may cause the 7694 Headspace Sampler to jam during septum puncture Do the following to prepare a vial for sampling 1 Place a septum in a vial cap with the Teflon side facing the vial Take care not to contaminate the septum Place the cap upside down on a table Place the sample in the vial The vial should not be more than 50 full Place the septum and cap together over the vial opening a amp ON Place the crimper over the cap and vial 56 Preparing a Sample Sample Preparation 6 With slow and steady pressur
101. thod Suggested Actions Remove all vials from the carousel and re load the carousel according to the current method See also Agilent 7694 or 7694 RESET Agilent 7694E or 7694E RESET on page 128 Vial Jam Problems G1289 G1290 only on page 121 ROM CHECK ERR PRESS CLEAR TO RESET Probable Causes The ROM check value is different from the stored value Suggested Actions Press Clear to continue The instrument is stopped and you must totally reset it This resets the microprocessor and automatically initializes all the data method parameters advanced function values flags and all the variables with default values If the unit fails to reset try turning the power off then on If this fails contact Agilent service 131 Error Messages Error Message Listing WARNING TRAY RESET Probable Causes The sampler was reset Suggested Actions See Agilent 7694 or 7694 RESET Agilent 7694E or 7694E RESET on page 128 UP MOTOR ERROR Probable Causes The elevator assembly that lifts the vial onto the sampling needle is unable to reach the needle Suggested Actions Remove all vials from the oven and the gripper Power cycle the headspace sampler and hold down the clear key until the tray is reset VIAL NOT FOUND Probable Causes e The robotic arm is unable to retrieve a vial from the oven e headspace sampler is unable to load a vial into the oven Suggested Actions 1 Manually remo
102. tn Makes available a series of advanced functions that are not used in routine applications These functions are accessed by pressing Adv a number code and Enter See Using the Adv Fctn Key on page 40 for more information 37 The Keypad Keys and Their Functions 38 Using the Adv Fctn Key Using the Adv Fctn Key Using an Advanced Function Using the Adv Fctn Key This chapter describes the nonroutine functions controlled by the Adv Fctn key It describes the displays value ranges and how to edit the setpoints for these functions Using an Advanced Function To access an advanced function setpoint or reading 1 2 3 Press Adv Fctn 1 9 1 2 3 and Enter Scroll to the desired subfunction if applicable Key in the new value using the numeric keypad A flashing appears to the left of the new value as you enter it Press Enter to make the new value part of the active method If the new value is not within the allowed range the sampler displays a message showing the allowed range Press any non number key to remove the error message At any point in a menu press Clear to return to the top level display See Table 4 G1883 or Table 5 G1289 G1290 for a quick reference of the advanced functions and Advanced Function Descriptions on page 44 for details 40 Using the Adv Fctn Key List of Advanced Functions by Model List of Advanced Functions by Model Table
103. tray malfunction 124 Zones not heating 125 Methods Chaining 36 65 Changing 62 Default 44 Entering 60 Entering temperature 60 Entering times 61 Entering vial parameters 63 Loading 35 64 Retrieving 64 Saving 64 Sequencing 36 65 Storing 35 64 Multi HS Extr Adv Fctn 8 Description 44 45 49 Multiple headspace extraction Analyte concentration 23 Chaining methods 66 Multiple vial puncture Constand heating 22 Description 21 Overview 6 Setting parameters 44 45 49 Single vial puncture Description 23 Technique 66 0 On off switch 9 Operating principles See Principles of operation 13 Optimizing methods Changing sample loop 73 Changing sample size 73 74 Reaching equilibrium 71 Varying loop fill time 72 Varying oven temperature 71 Varying vial equilibration time 71 Oven Description G1289 G1290 7 Description G1883 8 Entering temperature 60 Not heating 125 Oven carousel No agitation 123 No rotation 123 P Param Increment Adv Fctn 2 Description 50 Parameters Clearing 37 Entering 37 144 Partition coefficient K Description 70 Equation 70 Parts consumables 85 Pneumatics Description 11 Steam cleaning 95 Potentiometers Adjusting 98 Locating 98 Power Error message 128 130 Failure 128 130 Power switch 9 Pressure Displaying 36 Setpoints not reached 126 Units changing 52 Vial pressuzation setting G1289 81 Vial pressuzation setting G1883 G1290
104. ts and Consumables eese 85 FUSE LOCATIONS meor e terrere eget Ded eet pede 88 Changing the Sampling Needle sss enne nre ene 89 Changing the Sample Loop eee netten enhn enne testen 92 Steam Cleaning the Pneumatic System eese nennen 95 Installing the Transfer Line onto the Volatiles Interface 96 Aligning the Vial Loader G1289 G1290 only essere 97 Adjusting the potentiometers 97 Brocedu re sons areni e 99 Other vial handling adjustments 101 Checking carousel adjustment rennen 101 Leak Testing General Information eeeessesseeseeeeeeeeennr enne enne 103 Leak Testing a G1289 to 6890 GC Interface essere 105 Carrier Gas Flow 105 Carrier Flow Path Pressurization Test sss 107 Vial Pressurization Gas Aux Flow Path esee 108 Leak Testing a G1290 G1883 to GC Interface sess 110 Prepare the Sampler nennen nennen nnne nnns 110 Carrier Gas Flow Path esses nennen enne nene nnne 110 Vial Pressurization Flowpath 111 Flow Testing the Vent Valve and Associated Flow Path
105. uids where the method of standard addition is difficult because of losses due to evaporation MHE takes several headspace samples from each vial With each extraction the concentration of the volatile compound in both the gas phase and the sample becomes smaller although the ratio remains constant The logs of the peak areas versus the extraction number are plotted to obtain quantitative data about the compound of interest MHE is often used as a calibration tool Once the peak area versus the concentration is established for a given sample matrix quantitative measurements of samples with a similar matrix can be carried out using a single extraction The 7694 Headspace Sampler The 7694 Headspace Sampler provides an automated method to run up to 44 samples consecutively without operator attention The sampler s microprocessor optimizes the time spent for each run according to the values programmed in by the operator Up to four different methods can be stored and used to analyze a series of samples Models G1289 and G1290 can also be used for multiple HS extraction using multiple septum punctures with up to 10 extractions per sample You can also automate optimization routines The unit is made up of the following components Oven G1289 G1290 The oven contains a circular aluminum sample carousel that can hold up to six 10 or 20 ml sample vials A resistance band heater is used for heating A Introduction to Headspace and to t
106. usel at a constant frequency to agitate the vials Agitation takes place during the entire vial equilibration time Load Method Retrieves one of four stored methods and places it into active memory for use in the current analysis See Loading a Method on page 64 Store Method Stores the current method in one of four method storage areas See Storing a Method on page 64 Storing a method overwrites any method already stored there There is no warning message that an overwrite is taking place 35 The Keypad Keys and Their Functions Chain Methods Allows two to four methods to be used sequentially to analyze groups of samples in the tray See Chaining Methods on page 65 Chaining methods is not allowed if Parameter Increment is on For the G1289 G1290 chaining methods is one means of performing multiple headspace extraction MHE See also MULTI HS EXTR on page 49 Link Methods Press this key to sequentially chain two to four method together See Chaining Methods on page 65 Chaining methods is not allowed if Parameter Increment is on Carousel Advance 61883 only This key is used to move the sample tray for vial insertion and removal The cursor keys move the tray forward or backward by increments of one position Pressure 61883 G1290 only This key displays the pressure of the carrier gas or the vial pressurization gas The carrier gas pressure is measured at the outlet of the flow contr
107. ve any vials that are in the oven carousel Vials in the oven may be hot 132 WARNING Error Messages Recovery from an Automation Error 61289 G1290 2 Power cycle the headspace sampler and hold down the clear key until the tray is reset To remove a vial from the robotic arm see Vial Not Loaded Vial Retained Warning on page 121 See also Vial Jam Problems G1289 G1290 only on page 121 VIAL RETAINED Probable Causes The 7694 HS was reset with a vial still held by the robotic arm This may happen after a power failure or a manual reset Suggested Actions 1 Manually remove the vial that is held in the robotic arm See Vial Not Loaded Vial Retained Warning on page 121 or remove the cover from the vertical loader and pull the vial out of the gripper Vials in the oven may be hot 2 Power cycle the headspace sampler and hold down the clear key until the tray is reset Recovery from an Automation Error G1289 G1290 If an automation error occurs there are two recovery modes If you want to reload the default method hold Clear during power up The following message is displayed LOAD DEFAULT METHOD TRAY RESET If you want to reset the counter hold Adv Fetn during power up 133 Error Messages Recovery from an Automation Error G1289 G1290 134 Glossary accuracy The difference between a measured quantity and its true value analyte The compound of interest in an analysis calibrat
108. wing display PUNCTURE 0 S 1 M 1 example Press 0 Enter to enable single puncture mode or 1 Enter to disable it The display reads SINGLE PUNCTURE ON or MULTI PUNCTURE ON Default is multipuncture mode The following are definitions for terminology used with Adv Fctn 8 Multi HS Extr Multiple headspace extraction Multi Puncture On Recommended Multiple headspace extraction with multiple needle punctures of the septum This is the default mode of the sampler Single Puncture On Do not use MHE with single vial puncture Extract Per Vial Number of extractions per vial for either the multiple or single needle puncture mode PARAMETER INCR Parameter increment is a method development tool that makes stepwise increases in either vial equilibration time or oven temperature automatically Entering a value for the Vial Equilibration Increment increases the Vial Equilibration Time by that many minutes for the second vial and each subsequent vial in the present method The value range is 0 0 to 99 9 minutes Entering a value for the Vial Temp Incr increases the Vial Temperature during vial equilibration by that many degrees for the second vial and each subsequent vial in the present method The value range is from 0 to 99 minutes 50 Using the Adv Fctn Key Advanced Function Descriptions During parameter incrementing each vial is sampled and returned to the carousel The sampler displays 7694 NOT READY
109. ze valve Vent valve Flow paths before GC prep run Figure 27 Flow paths for a G1290 G1883 to GC installation In general if there is a leak check the following locations e Zero dead volume ZDV unions e Auxiliary bleed fitting 104 Maintaining the Instrument Leak Testing a 61289 to 6890 GC Interface e Sample loop connections e Connections to the sampler from the GC or gas supply e Remaining valve connections Leak Testing a G1289 to 6890 GC Interface Carrier Gas Flow Path Perform this leak test to check the integrity of the entire carrier gas flow path between the GC and the headspace sampler 1 Install a checkout column part number 19091J 413 in the GC 105 Maintaining the Instrument Leak Testing a G1289 to 6890 GC Interface 2 Set the following conditions on the 6890 GC Setting Value ven Initial temp 40 C Ramps Off Equilibration time 0 10 min Run time 10 min Inlet PTV or split splitless Mode Splitless Initial temp 250 C Pressure 25 00 psi Purge flow 200 0 ml min Purge time 1 00 min Gas saver Off Column Model number 19091J 413 Max temperature 325 C Nominal length 30m Nominal diameter 320 00 Nominal film thickness 0 25 um Mode Constant pressure Pressure 25 psi Outlet pressure Ambient Nominal initial flow 3 9 ml min Aux Pressure Vial Pressurization channel Gas type Initial pressure Initial time Rate 1 Helium 15 psi On 0 00 min 0 0 Of

Agilent 7694 Headspace Sampler

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