Ultra manual v3.0.qxd
Contents
1. HS TD G1888 Headspace Thermal Desorption System Operators Manual JANUARY 2011 QUI 1043 VERSION 1 2 MARKES Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a a D 4 A O HS TD Gi888 User Manual Markes International This page left intentionally blank QUI 1043 V1 2 Jan 2011 a a D A O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Table of Contents 1 Introduction 2 Packing List 3 Installing UNITY e onto Gi888 headspace system 4 4 Software Instructions 13 5 Operation 15 Table of Figures Figure 1 PTFE block with aluminium tube inserted Figure 2 UNITY HS link tube assembly 5 Figure 3 Link tube inserted into PTFE block 5 Figure 4 Connecting the HS transfer line to the inert zero dead volume union 6 Figure 5 Secure the transfer line into the PTFE block 6 Figure 6 Fit the Perspex cover supplied 7 Figure 7 Extending the carrier gas inlet line 7 Figure 8 Removing the HS valve cover 8 Figure 9 Removing the black needle cover 8 Figure 10 Removing the silcosteel tubing 9 Figure 11 Removing the silcosteel tubing from the 6 port valve 9 Figure 12 Connecting 1 16 inch Silcosteel tubing 10 Figure 13 Position sample outlet line vertically 10 Figure 14 Connecting the sample out2. HS TD Gi888 User Manual Markes International Figure 19 UNITY operating software displaying status of HS system 5 Operation 5 1 Headspace settings The HS parameters are controlled via the Method Parameter window in the G1888 controlling software see figure 20 QUI 1043 V1 2 _ _ Jan 2011 15 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a a D 4 O O HS TD Gi888 User Manual Markes International Method Parameter Temperature Setpoints Deg T Actual Oven ET Ea E Sample Valve 704 7 Transfer Line es S gg Timing Parameters Minutes gt Temperature Mal Eguilibration Time Vial Equilibration Vial Pressurization LS LM Loop Fill Time Peer 00 amp Potractionsper Via 2 4 Tee time 3000 6 15 pre Pine Su nt i Figure 20 Method parameter window for controlling HS sampler Oven Controls temperature of HS vial oven Sample Valve Controls temperature of sample valve Transfer line Controls temperature of HS transfer line 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 Vial equilibration Sets time for equilibration of vial in HS oven Vial pressurization Not used in HS TD operation L
3. O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International From the View gt Options menu select the configuration tab Tick the box which says operate direct mode with HP7694 Close software Open HS operating software and connect to the unit as above Open UNITY s w When you select Direct sampling from the drop down menu a new window Should appear which says HP7694DDE This completes the software installation and setup E Options Methods Gas Sequence Ports Configuration Reporting Miscellaneous Automation Sampling Recollection C AirServer and UMA C AiServer C Autosecure Auto UtATD Auto 7 50 50 Same ATO Manual Manual Ult Load Unload Temperatures Load emp UrLoadT emp Blank Tubes Sampling HIHA Recollection Uta AirServer Channels E Estermalvalve Eesen Number Of Channel Peery oy ri i AirServer Internal Std T Use iA with Air erie Ultts has ISDP Acey i RE di iti iiil FY EI iH L enman E lr iti haz Dry Fi ige dcr y I Use Unity with Flow Control Module ie Mo ISDP or Unity DP Accy i Operate Direct Mode with HP7694 Figure 18 UNITY Options menu displaying selection to operate direct mode with HP 7694 QUI 1043 V1 2 _ a Jan 2011 14 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a a D 4 A O
4. allow full leak testing Use the UNITY Leak test dialogue to pressurise the system and test for leaks 4 Software Instructions Prior to installing software the Headspace system should be connected via a LAN cable to the network and a spare IP address should be available Using the HSS menu function Check LAN settings Sub net mask must be the same as on the operating PC This can be checked on the PC by doing the following Click on Run from the Start menu Type CMD in the box When command prompt is launched type in ipconfig al The subnet mask will be displayed ia Installing s w Load CD and copy folder to Program directory on PC Open executable file Agilent G1888 exe This will open the HSS operating software Connecting to HS Select TCP IP from the remote menu This will open a TCP IP Connection window Insert the IP address that you will be running the HSS from Click connect The TCP status should change from yellow to green and state online Setting up UNITY for operation with G1888 HS system Select the Unity opt file in the UNITY program folder Open this file using notepad In this text file change the following lines Direct off should be changed to Direct on Syncstatdisplay Probe in should be changed to Syncstatdisplay start sampling Save the changes to this file close and restart UNITY QUI 1043 V1 2 _ _ Jan 2011 13 a a D 7 A
5. into the PTFE collar 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 a a D 4 O O QUI 1043 V1 2 6 Jan 2011 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Figure 6 Fit the perspex cover supplied Connect the 1 16 inch stainless 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 by loosening the two screws and lifting off the cover figure 8 QUI 1043 V1 2 ads Jan 2011 a a D A O O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Figure 8 Removing the HS valve cover Unscrew the screw and remove the black cover over the headspace needle to expose the silcosteel union figure 9 E HEGRZRT 0602 a E Figure 9 Removing the black needle cover Remove the silcosteel tubing from the union as shown figure 10 QUI 1043 V1 2 8 Jan 2011 Markes Internat
6. TD 1229 Also insert the three screws supplied p n SERZ M416PPSS into the PTFE block as shown in figure 1 PTFE Collar Aluminium tube inserted inside PTFE collar Figure 1 PTFE collar with aluminium tube inserted QUI 1043 V1 2 4 Jan 2011 a a D 4 O O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International 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 collar as shown figure 3 UNITY Link tube Brass sleeve Zero dead volume union Figure 2 UNITY HS link tube assembly UNITY Link tube PTFE collar r Zero dead volume union Figure 3 Link tube inserted into PTFE collar Insert the link tube into UNITY with the PTFE collar to the back of the system but do not seal the link tube into place Connect the HS transfer line into the union as shown figure 4 a a D A O QUI 1043 V1 2 lt 5 Jan 2011 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Figure 4 Connecting the HS transfer line to the inert zero dead volume union Now secure the transfer line into the PTFE collar using the three screws as Shown figure 5 Figure 5 Secure the transfer line
7. e be used with single needle headspace systems Sampling parameters Prepurge Prepurge pressurises the sample vessel and cleans out the sampling lines thus helping prevent carryover from previous runs and sweeps any air out of the flow path However as there is no overall flow in the sampling vessel prepurge does not flush the vessel Prepurge therefore defines the time for which gas Sweeps through the sample lines and into UNITY through the flow path bypassing the trap and out through the split at the flow rate set on the split needle valve Pressurisation time When set to zero UNITY runs in dynamic direct sampling mode When set to any non zero value UNITY will run in pulsed rather than dynamic direct sampling mode When in pulsed sampling mode this defines the time for which carrier gas is Supplied to the sample vessel to build up pressure prior to releasing that pressure through the cold trap Sampling time Defines the amount of time for which the solenoid valve downstream of the cold trap is opened so that sample is transferred from the sample vessel to the cold trap The pressure drops as soon as sampling begins until it eventually reaches atmospheric pressure QUI 1043 V1 2 _ 2 Jan 2011 17 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a a D A O HS TD Gi888 User Manual Markes International Equilibration time Governs the amount of tim
8. e for which the sample 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 Purge Defines the time for which carrier gas is purged through the cold trap in the sampling direction This procedure purges the trap of any oxygen prior to heating and under certain conditions allows selective purge of unwanted volatiles such as water or ethanol GC Cycle The GC cycle time should be set to 0 1 for all HS TD operations a a D A O QUI 1043 V1 2 _ _ Jan 2011 18 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com
9. ional Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com a a D 4 O O HS TD Gi888 User Manual Markes International Figure 10 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 11 Removing the silcosteel tubing from the 6 port valve Connect the 170 mm length of 1 16 inch silcosteel tubing supplied p n SERZ 0679 to the headspace needle and feed through as shown in figure 12 QUI 1043 V1 2 9 Jan 2011 a a D 4 O O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Figure 12 Connecting 1 16 inch silcosteel tubing Remove the HS fitting which connects the 6 port valve to the HS transfer line and position the sample outlet line in a vertical position as shown figure 13 Figure 13 Position sample outlet line vertically Connect 100 mm length of 1 16 inch silcosteel tubing supplied p n SERZ 0679 to the zero dead volume connector p n SERZ 0691 and connect this union to the sample outlet line as shown figure 14 QUI 1043 V1 2 _ _ Jan 2011 10 a a D 4 O O Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Marke
10. let line 11 Figure 15 Connecting up the Valco T piece 11 e Figure 16 Connect the UNITY line into the T piece 12 Figure 17 Gas line protruding from HS system 12 Figure 18 UNITY Options menu displaying selection to operate direct mode with with HP 7694 14 Figure 19 UNITY operating software displaying status of HS system 15 z Figure 20 Method parameter window for controlling HS sampler 16 A o A e QUI 1043 v1 2 _3 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International 1 Introduction Markes International s HS TD system brings together two of the most powerful GC introduction techniques equilibrium 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 Packing List Remove the contents from the shipping box inspect and check each item against the Packing List included with the order Retain the instrument packaging and reuse if ever the system is to be shipped using conventional Carriers 3 Installing UNITY e onto G1888 headspace system Take the aluminium tube p n SERUTD 1384 and insert into the PTFE collar p n SERU
11. oop fill time Not used in HS TD operation Loop equilibration Not used in HS TD operation Injection time Sets the time for which the HS needle is inserted into the vial to allow sampling This is calculated from the UNITY method conditions and is the total of all purge times and direct sampling times Note if multiple extractions are being carried out it is important to calculate the correct total time for direct sampling a a D 7 A O Vial Parameters Sets the sequence of vials to be sampled QUI 1043 V1 2 Jan 2011 16 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International 5 2 UNITY settings Note Dynamic direct sampling involves a continuous flow of carrier gas through or from the sample vessel sweeping the headspace vapours into the UNITY cold trap for a defined period of time and is not compatible with single needle headspace systems 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 Pulsed direct sampling is thus compatible with a single inlet outlet point and can therefor
12. s International Figure 14 Connecting the sample outlet line Connect both the lengths of 1 16 inch silcosteel tubing connected above into the silcosteel zero dead volume Valco T piece p n SERZ 0699 as shown in figure 15 Figure 15 Connecting up the Valco T piece Connect the 1 16 inch stainless steel tubing from the UNITY link tube into the Silcosteel T piece as shown figure 16 a a D 4 O O QUI 1043 V1 2 11 Jan 2011 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International Figure 16 Connect the UNITY line into the T piece Replace the black needle cover over the Headspace needle connection and 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 and carefully shut the headspace cover taking care to ensure that the cover does not crimp the gas line figure 19 Figure 17 Gas line protruting from HS system a a D 4 O O QUI 1043 V1 2 _ E Jan 2011 12 Markes International Ltd T 44 0 1443 230935 F 44 0 1443 231531 E enquiries markes com HS TD Gi888 User Manual Markes International This completes all the flow path connections To leak test the system place an empty headspace vial into position 1 in the G1888 and set to Inject with a long sampling time sufficient to
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