HS-TD G1290_2.qxp
Contents
1. HS TD G1290 Headspace Thermal Desorption System Operators Manual May 2008 QUI 1050 VERSION 1 0 MARKES international a D 4 A O 3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International This page left intentionally blank QUI 1050 V1 0 May 08 a D 4 A O 3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Table of Contents 1 0 Introduction 5 2 0 Packing List 5 3 0 Installing UNITY e onto G1888 headspace system 6 4 0 Software Instructions 16 5 0 Operation 19 Table of Figures Figure 1 PTFE block with aluminium tube inserted 6 Figure 2 UNITY HS link tube assembly 6 Figure 3 Link tube inserted into PTFE block 7 Figure 4 Connecting the HS transfer line to the inert zero dead volume union and stabilizing with the fixing screws 7 Figure 5 The assembled transfer line interface tube 8 Figure 6 Interface tube in position 8 Figure 7 Extending the carrier gas inlet line 9 Figure 8 Removing the HS valve cover 9 Figure 9 Removing the silcosteel tubing 10 Figure 10 Removing the silcosteel tubing from the 6 port valve 10 Figure 11 Removing sample line connection from valve 11 Figure 12 Connecting the union to transfer line outlet 11 Figure 13 Connecting2. UNITY Link tube Brass sleeve NA ds Zero dead E volume union Figure 2 UNITY HS link tube assembly QUI 1050 V1 0 6 May 08 E z 3 Q x D n A e Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International UNITY Link tube PTFE block Zero dead 7 volume union Figure 3 Link tube inserted into PTFE block Connect the HS transfer line into the union and secure with the screws as shown figure 4 Figure 4 Connecting the HS transfer line to the inert Zero dead volume union and stabilizing with the fixing screws The transfer line and interface tube assembly is now ready to be secured into position in the UNTTY tube oven figure 5 E z 3 a x D n A e QUI 1050 V1 0 J May 08 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Figure 5 The assembled transfer line interface tube Seal the UNITY link tube into the UNITY oven and fit the perspex cover supplied p n SERMTD 1368 onto UNITY as shown figure 6 Figure 6 Interface tube in position a D 4 A O 3 QUI 1050 V1 0 8 May 08 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Connect the 1 16 inch stainle
3. Sampling Re collection C AirServer and Ltr all E AirServer C Autosecure Auto v C UaTD Auto Manual Manual Ut Load Unload Temperatures r Blank Tubes Arserver Channels AirServer Internal Std Co Ult has ISDP Accy e No ISDP or Unity DP Accy Figure 22 UNITY Options menu displaying selection to operate direct mode with HP7694 9 Open HS operating software and check that the system is communicating with the operating PC 10 Open UNITY software When you select Direct sampling from the drop down menu a new window Should appear which says HP 694DDE figure 23 If the headspace sampler is correctly configured then this window should reflect what is shown on the HS display If this window shows intializing continuously then the COM port has not been properly set see above QUI 1050 V1 0 7 _ May 08 17 HS TD G1290 User Manual Markes International This completes the software installation and setup 2 i f a ou 39 psi Figure 23 UNITY operating software displaying status of HS system in new window QUI 1050 V1 0 7 May 08 18 HS TD G1290 User Manual 5 0 Operation Markes International There are two sets of parameters to set up for headspace sampling the headspace parameters and the Unity method parameters The system has been configured to use the HS in the simplest manner possible it is there to automatically deliver vials to the oven and retain them at a specifie
4. on the system Tab and setting the COMs port to either 1 or 2 figure 20 Comm Port instrument Pressure Linits C Offline 6290 Heady E a None C 1 amp a2 om 5690 C Wait Com 2 35900 O Other e psi O kPa C Abort O bar Lock HP 694 keypad Pressure Control Oven Stabilization CO Yes FERE 1 0 E Hin Default Headspace Method CAHPZ694AMETHODSADEFAULT HSM Figure 20 Setting the communication ports on the HS unit The HS system is now being controlled from the PC and the status can be monitored using the monitor funcion on the HP7694Link programme figure 21 SU HP7694 System Monitor Not Ready U 0 S cal Transter Line j J Vials B Figure 21 The HS monitor window QUI 1050 V1 0 _ May 08 16 HS TD G1290 User Manual Markes International Setting up UNITY for operation with G1290 HS system 1 Select the Unity opt file in the UNITY program folder 2 Open this file using notepad 3 In this text file change the following line Direct off should be changed to Direct on 4 Check that the following information is correct Syncstatdisplay Probe in 5 Save the changes to this file close and restart UNITY 6 From the View gt Options menu select the configuration tab 7 Tick the box which says operate direct mode with HP7694 figure 22 8 Close software Options Methods has Sequence Ports Configuration Reporting Miscellaneous Automation
5. that has just been edited Clicking Start run in the UNITY software will aurtomatically trigger the HS method to start The UNITY status should display waiting for HS sync figure 26 Figure 26 UNITY software showing waiting for HS sync status Once the HS system reaches the probe in status i e the needle is piercing the HS vial the UNITY sampling sequence begins IMPORTANT If multiple vials are to be analysed then you must ensure that Unity is set up to Link i e to sequence the same number of runs as there are vials Leak testing In order to leak test the system place an empty headspace vial into position 1 Set the HS method to have a long Vial Pressurisation time sufficient to allow full leak testing Open the leak test dialogue in the UNITY software pressurise the system and use a helium leak detector to look for any leaks in the newly inserted flow path interface tube HS valve T piece etc QUI 1038 V1 0 SA Apr 07 24
6. 1 16 inch silcosteel tubing to union 12 Figure 14 Connecting 1 16 inch silcosteel tubing to Valco T piece 12 lt Figure 15 Connecting 1 16 inch silcosteel tubing to the headspace needle 13 Figure 16 Connecting 1 16 inch silcosteel tubing to the Valco T piece 13 Figure 17 T piece in position with connections to headspace needle and transfer fab line 14 Figure 18 Connecting the UNITY line into the T piece 14 Al Figure 19 Gas line protruting from HS system 15 N A O ou V1 0 _3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Figure 20 Setting the communication ports on the HS unit 16 Figure 21 The HS monitor window 16 Figure 22 UNITY Options menu displaying selection to operate direct mode with HP7694 17 Figure 23 UNITY operating software displaying status of HS system in new window 18 Figure 24 Typical TD method conditions for operation in HS TD mode 19 Figure 25 Method parameter window for controlling HS sampler 22 Figure 26 UNITY software showing waiting for HS sync status 23 a V1 0 4 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a D 4 A O 3 HS TD G1290 User Manual Markes International 1 0 Introduction Markes International s HS TD system brings together two of the most powerful GC introduction techniques equilibr
7. Figure 17 T piece in position with connections to headspace needle and transfer line Connect the 1 16 inch stainless steel tubing from the UNITY link tube into the final remaining port on the silcosteel T piece as shown figure 18 Figure 18 Connecting the UNITY line into the T piece a D 4 A O 3 QUI 1050 V1 0 E z May 08 14 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Replace the metal cover over the headspace valve system Finally feed the carrier gas inlet line to the front right hand corner of the Headspace unit figure 19 and carefully shut the headspace cover taking care to ensure that the cover does not crimp the gas line Figure 19 Gas line protruting from HS system This completes all the flow path connections Note Before use the system will need to be fully leak tested follow the sofware instructions in section 4 and leak test as described at the end of section EE QUI 1050 V1 0 z _ May 08 15 HS TD G1290 User Manual Markes International 4 0 Software Instructions Prior to configuring with UNITY the Headspace system should be connected to the operating PC via a serial connection cable and its HP7694Link programme Software running The headspace is limited to running on either COM1 or COM2 The COM ports settings may be accessed by running the HP7694Link programme clicking
8. ating it in the tick box This flow will determine the flow rate of split in standby prepurge line flush if split is activated split during trap desorption Set trap desorb flow by entering set flows mode and when prompted Set flows with split on click No This flow will determine sampling flow when pressure is released during pulsed sampling or continuous sampling flow during dynamic sampling It will also determine the trap purge flow during post sampling trap purge QUI 1050 V1 0 a K3 May 08 21 HS TD G1290 User Manual Markes International 5 1 Headspace settings The HS parameters are controlled via the Method Editor window in the HP7694Link programme see fig 25 When the UNITY software is running but UNITY is in standby open the HP7694LINK application Select the Method Edit option from the main screen If the screen shows Under DDE Control then you must exit the UNITY software and re open it Once in method edit figure 25 open an exisiting method or create a new method NB there is no way of downloading the current HS parameters from the instrument however it is possible to view them from the method edit screen by clicking on View Monitor fi Method Editor C HP7694 METHODS LARA HSM DD Temperature Setpoints deg E Sample Properties Oven 54 E Matrix Water sample Valve 0 E Boiling Point 100 Transter Line 80 Val R 2 ial Range Timing Parameters Hinutes star
9. d temperature whilst Unity takes care of all the sampling parameters The recommended procedure for setting all method parameters is to define the Unity sampling parameters first and then adjust the headspace method accordingly 5 1 UNITY settings Note Pulsed direct sampling works by pressurising a sealed sample vessel for a set period of time and then shutting off the gas supply and allowing the carrier gas pressure to be released out through the cold trap of UNITY This process may be repeated multiple times on a single sample to enhance the concentration of trapped analytes before desorbing the cold trap and beginning the GC MS analysis Figure 24 shows a typical direct sampling method for HS TD operation Rc program Files Unity methods Example Headspace meth Urect Sampling Purge 1 0 Prepung Time Direct Samplin amenng Pressurisalion Time 30 Sampling Cucles munido Trap Decor Trap Low Trap Held E Trap High Trap Heating Rate ICs 300 120 Flow Path Temp 0 0 GC Cycle Time 5 0 Minimum Caner Pressure Split On E Standby T Split On LO Trap Purge Time Flush Time 1 0 Leak test W Tiap ln Line Spit On Figure 24 Typical TD method conditions for operation in HS TD mode QUI 1050 V1 0 May 08 19 HS TD G1290 User Manual Markes International Sampling parameters Split on in standby This option allows a continuous purge of the standby flow path through the spl
10. in the sampling vial is allowed to re equilibrate before it is repressurised and resampled Sampling cycles Sets the number of times that the pressurisation sampling and equilibration steps will be repeated for any particular sample before desorption of the focusing trap triggers the GC MS analysis Flush time A similar step to prepurge this stage permits carrier gas purge of the sample lines to remove any residual sample and transfer to the trap or out of the split or both Trap low temperature When sampling on line from vials there is a high probability that the sample will contain water it is therefore advisable to set the trap low temperature to above freezing Or more typically above ambient to prevent condensation or formation QUI 1050 V1 0 E _ May 08 20 HS TD G1290 User Manual Markes International of ice in the trap Trap high and trap hold The two parameters govern the time for and temperature to which the trap will be heated to release the sample These parameters are set as would be normally set for desorption of the sample from the cold trap GC Cycle time The GC cycle time should be set to 0 1 for all HS TD operation Flow path temperature Defines the temperature to which the heated interface tube is heated the temperature to which the heated valve in Unity is heated and the temperature of the transfer line to the GC Setting flows on Unity Set the split flow whilst Unity is in standby by activ
11. it vent it prevents ingress of air and water into the Unity flow path and is thus most commonly used in conjunction with GCMS Pre purge Defines the time for which gas from the sample travels through the flow path bypassing the trap and out through the split at the flow rate set on the split needle valve This prepurge cleans out the sampling lines and thus helps minimise carryover from previous runs and avoids systematic error in the Sampled volume when sampling in dynamic mode However as there is no overall flow in the sampling vessel prepurge does not flush the vessel Trap Purge Defines the time for which carrier gas is purged through the cold trap in the Sampling direction following the completion of the sampling cycles This stage purges the trap of any oxygen prior to heating and under certain conditions allows selective purge of unwanted solvents such as water or ethanol Pressurisation time Governs the amount of time for which carrier gas is sent from Unity to the headspace vial to build up pressure prior to releasing that pressure through the cold trap No sample is taken at this point Sampling time Defines the amount of time for which the trap valve is opened so that sample is transferred from the previously pressurised vial to the UNITY focusing trap The pressure drops as soon as sampling begins until it eventually reaches atmospheric pressure Equilibration time Governs the amount of time for which the sample
12. ition and connect the zero dead volume union as shown p n SERZ 0691 and connect this union to the sample outlet line as shown figure 12 Figure 12 Connecting the union to transfer line outlet a D 4 A O 3 QUI 1050 V1 0 _ _ May 08 11 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Connect 100 mm length of 1 16 inch silcosteel tubing supplied p n SERZ 0679 to the zero dead volume connector and the other end of the tubing to the silcosteel zero dead volume Valco T piece p n SERZ 0699 as shown Figure 13 amp 14 Figure 14 Connecting 1 16 inch silcosteel tubing to Valco T piece a D 4 A O 3 QUI 1050 V1 0 _ E May 08 12 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Connect the 170 mm length of 1 16 inch silcosteel tubing supplied p n SERZ 0679 to the headspace needle and bend the tubing as shown in figures 15 amp 16 Figure 16 Connecting 1 16 inch silcosteel tubing to the Valco T piece a D 4 A O 3 QUI 1050 V1 0 E _ May 08 13 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International The set up should now resemble that in Figure 17 below
13. ium headspace HS and thermal desorption TD The combined system offers users optimum sensitivity for trace VOCS in solid liquid and vapour phase samples all on one versatile analytical platform This manual gives details of the Markes HS TD system for the following models Agilent G1888 Headspace system Markes UNITY e Thermal desorption system 2 0 Packing List Remove the contents from the U HSTD G1888 shipping box inspect and check each item against the packing list below ma GE SERZ 0690 Tubing Aluminium 0 5 OD x 9 5 mm ID E esmes mm po ES E CO SERZ 0699 Zero dead volume Valco T piece 1 16 silcosteel Em smroo mma sere raner sone mena QUI 1050 V1 0 ala May 08 a D 4 A O 3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International 3 0 Installing UNITY e onto G1290 headspace system Take the aluminium tube p n SERZ 0690 and insert into the PTFE block p n SERUTD 1229 Also insert the PTFE collar UTD 1382 into the sleeve and secure with the three screws supplied p n SERZ SM416PPSS as shown in figure 1 PTFE Block Aluminium tube inserted inside PTFE block Figure 1 PTFE block with aluminium tube inserted Take the UNITY HS link tube assembly p n SERUTD 5132 figure 2 and insert the end with the zero dead volume silcosteel union attached into the PTFE block as shown figure 3
14. me on Unity to avoid losing any of this sample Vial pressurization Must be the sum of the following steps U Prepurge U Sampling total U Flush time 0 5 minutes Where U Sampling total is the result of the following equation U Sampling cycles x U Pressurize U Sampling U Equilibration Sample Loop Fill Not used Set to zero Loop equilibration Not used Set to zero Sample injection Not used Set to zero Sample Properties These parameters may be filled in as they can be useful for future reference Vial Range Put in the number of the first and last vial that will be injected in the sequence Shaking If your sample requires shaking during the headspace equilibration stage then select that here Parameter Increment Not used Extractions per vial Setto1 Once the headspace method is set up SAVE it under an appropriate name 8 3 characters max GC Cycle Sets interval between runs to allow overlap of samples For HS TD operation the total GC cycle time should be calculated as follows GC runtime GC equilibration cooldown time HS injection time QUI 1050 V1 0 E _ May 08 23 HS TD Gi888 User Manual Markes International Launching the combined methods Once the Unity and the HS sampler parameters are set then the sequence may be launched Go back into the Unity software and double click in the Headspace Status window this will prompt you to choose the appropriate Headspace method Select the method
15. ss steel union supplied p n SERZ 0386 to the carrier gas inlet tube on the UNITY link tube Then connect the 500 mm piece of 1 16 inch stainless steel tubing supplied p n SERZ 0175 to the union in order to extend this inlet gas line figure 7 Figure 7 Extending the carrier gas inlet line Open the top cover of the HS unit and remove the stainless steel cover over the valve system figure 8 Figure 8 Removing the HS valve cover QUI 1050 V1 0 9 May 08 a D 4 A O 3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Remove the silcosteel tubing from the union at the top of the headspace needle assembly as shown figure 9 Figure 9 Removing the silcosteel tubing Also remove the silcosteel tubing from the 6 port headspace valve and retain for use if you wish to return to standard headspace operation in the future Figure 10 Removing the silcosteel tubing from the 6 port valve a D 4 A O 3 QUI 1050 V1 0 _ _ May 08 10 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD G1290 User Manual Markes International Remove the HS fitting which connects the 6 port valve to the HS transfer line figure 11 Figure 11 Removing sample line connection from valve Position the sample outlet line in a vertical pos
16. t Vial 1 5 End Vial 10 E GC Cycle 75 0 Shaking Faigmete o on chain UE Vial Equilibration 50 Che ne Step E C Low Vial Pressurization 25 00 E C Oven Temperature C High C ial Equilibration Time Sample Loop Fill 0 00 E Sampling Mode 0 00 7 E Extractions Per Vial 1 E Loop Equilibration Sample Injection 0 00 O qm veea Figure 25 Method parameter window for controlling HS sampler Sampling parameters Temperature Set Points Represent the conditions for the sample in the vial during sampling Oven temperature Vial temperature during equilibration and sampling Sample valve First part of the sample flow path inside the Headspace must be hotter than the sample vial Transfer line Temperature of HS transfer line through which sample passes to the UNITY TD system Typically set a little higher than sample valve temperature QUI 1050 V1 0 E 7 May 08 22 HS TD G1290 User Manual Markes International Timing parameters These represent really key parameters errors here may cause problems in Unity HS synchronisation GC cycle time Must be equal to GC cycle time GC Run time plus cool down time equilibration time assuming that the GC cycle time is the longest step Vial equilibration The amount of time for which the vial will be maintained at the oven temperature before the septum is pierced This may be set to any required value but care must be taken with the prepurge ti
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