Quick Reference Guide OPTIC 3 - PTV on
Contents
1. Quick Reference Guide OPTIC 3 PTV on Shimadzu GC 2010 Gas Chromatograph ATAS GL International B V De Run 4441 5503 LS Veldhoven The Netherlands Tel 31 40 254 9531 Fax 31 40 2549779 e mail info atasgl com Author M Kurano Quality Control ATAS GL International Doc ID SM 052 Quick Reference Guide OPTIC 3 PTV on Shimadzu GC 2010 OS O Date 06 06 2008 Quick Reference Guide OPTIC 3 PTV on GC 2010 This Quick Reference Guide is an addendum to the OPTIC 3 PTV Installation Guide onto Shimadzu GC 2010 OEM Doc ID SM 042 Please read both documents attentively before installing the system This guide is made to understand 1 How to operate GC MS Solutions and Evolution Workstation software with OPTIC 3 PTV Injection system installed on Shimadzu GC MS QP2010 How to use GC 2010 AFC unit for carrier gas control with OPTIC 3 PTV injector How to configure dummy injector on GC MS QP2010 system in case no Shimadzu injector is installed 4 How to create independent method using Evolution Workstation software in order to make temperature program and set the control parameters for venting process if using Large Volume Injection mode 5 In case if OPTIC 3 PTV is combined with LINEX and CDC options these options must be controlled by CTC Analytics CycleComposer software running outside GC MS Solution 1 Installation of OPTIC 3 PTV 1 1 GC MS QP2010 system If OPTIC 3 PTV is the only injection port2. The only solution is then upgrading the OPTIC 3 PTV to OPTIC 3 S version This version contains a dedicated Electronic Gas Control designed to work with LINEX and CDC Station p no H400062 Upgrade kit OPTIC 3 PTV to OPTIC 3 S 4 Connecting LINEX Head to GC 2010 AFC To install OPTIC 3 PTV with LINEX option perform the following steps 1 Cut the ends of the PEEK lines connected to the LINEX Head as it is shown in Fig 15 2 Connect the carrier line blue marker to AFC carrier line using the 1 8 union and the 1 8 to1 16 reducing ferule 3 Connect the second line to the AFC purge flow line using the 1 8 union and 1 8 to 1 16 reducing flow Please contact ATAS GL International BV if you have any questions info atasgl com http www atasgl com ATAS GL International Page 11 of 11
3. ua 200 De Data File Name R Time 27 756 min 10 018 103 means split valve closed 103 means split valve opened 5 0 25 Figure 6 GC Temperature Program Large Volume Injection requires eliminating solvent before injector is heated up This process should programmed as a pre running process see example of the OPTIC 3 LVI method programmed within Evolution Workstation in Fig 7 However GC 2010 does not allow this kind of pre run programs LVI is simple cold injection with solvent vent Injector temp Column flow Split flow Solvent vent ATAS GL Figure 7 Example of LVI method within Evolution Workstation ATAS GL International Page 5 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 The LVI method for OPTIC 3 PTV should be made as a Split method within GC Solutions because the split valve must be opened during the solvent eliminating During the method run after solvent is vented OPTIC 3 sends start signal to GC 2010 the split valve is closed and GC program is started NOTE _ If this method is cancelled during the GC run the split valve cannot be initialized In this case the split valve should be opened manually from the GC keypad 2 2 LINEX Method LINEX method is very complex because the injector pressure must be released before opening the LINEX head This is needed in order to avoid jumping up the liner out of injector Also solid material powder like pack
4. 100 ml min in order to flush the interior of the injector after the LINEX head is closed The flush time should be set through the Evolution Workstation using LINEX TD or LINEX DMI method Initial Septum Purge Flow should be set to ZERO because GC 2010 gives an error status if the LINEX head is opened for long time Since it is very difficult to control ZERO Septum Purge Flow its control parameters should be optimized see Section 3 When LINEX head is closed and the GC method is started the injector pressure should be built up to required pressure immediately Purge Flow should also be built up to a value of 3 ml min or so For this Pressure program and Purge Flow program created be created according to the required analytical parameters see example in Fig 9 EM GCMS Real Time Analysis Admin Acquisition Method_test01 qgm confirmation qgd Line1 20080519 qgt ai File Edit View Method Instrument Acquisition Data Tools Window Help pejal S ala RTI ml 2 wise Ly olele tis Det _1 40 k set lo Gc e ms Inj Port SPL1 Inj Heat Port INJ1 Column Oven Temp 50 0 CT mL min Injection Temp 30 0 40 Injection Mode Split eer ee Pee i SE eee Sampling lime fi 00 min m Carrier Gas He Prim Press 500 900 j Purge Flow PEE Flow Control Mode Pressure ied Pressure 12 0 kPa Holds E Total Flow fi 46 1 mL min 15 00 000 0 0 0 00 Sta
5. 19 qgd Linel abi File Edit View Method Instrument Acquisition Data Tools Window Help Dieta Sle ala mE mel 2 sa se ty oleo x k GC a ms 1 Inj Port SPL1 Inj Heat Port INJ1 Top Column Oven Temp 50 0 CTC A Injection Temp i in Injection M e wizard Sampling lime 1 00 0 0 5 0 10 0 BPA mp i im 500 Column Oven Temperature IE yy 2 Carrier Gas He Prim Press 500 900 Pran Calan en TAAA pee eee Flow Control Mode Linear Velocity Sii Rate _ Final Temperature Hold Time Pressure 14 3 kPa o 500 gt 00 E s Total Flow fi 54 5 mL min 1 25 00 325 0 2 00 0 00 0 0 0 00 Standby Column Flow fi 50 mL min Lo iD Pelee hia noi ea Total Program Time 15 00 min ae Purge Flow 3 0 mL min Column ar Split Ratio fi 00 0 Name InertCap5MS Sil Thickness 0 25 um Length 30 0 m Diameter 0 32 mm Stop Detail of Injection Port Peano High Press Injection Carrier Gas Sayer i ji aN Method Detail Spliter Flo plea ce lt u a oo ee Figure 5 Setting up LVI Method ATAS GL International Page 4 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 Create a GC time program as it is shown in Fig 6 x Prerun Program __ Time Device _ _ AEVENT Yaha 0 00 0 00 4 _ This time must be the same Time Program EVENT EVENT die Device EVENT EEIN Pi 0 00 Wer
6. 60 Temperature Control Keep Until Erd Solvent Yenting Threshold Went Time sec 30 Solvent Monitor Level 2 10 Solvent Monitor Threshold 25 solvent Monitor Level 3 Solvent Monitor Threshold Using solvent monitor Figure 12 Example of LINEX DMI Method Using Fixed Vent Time 3 Optimizing control parameters for purge flow The optimization settings mentioned here only for the reference purposes Please consult the service manual of the GC 2010 gas chromatograph or contact Shimadzu service department In case the septum purge flow should be set to zero offset in the list the control parameters for Purge Pressure should be optimized see Fig 13 ATAS GL International Page 9 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 Figure 13 Offset Optimization lf the value of the purge flow should be set to some value 3 ml min for example gain in the list the control parameters for Purge Pressure should be optimized see Fig 14 Figure 13 Gain Optimization ATAS GL International Page 10 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 Even with above described optimization of the offset and gain the error message can be delayed for a maximum of 2 minutes For this reason in order to avoid the error message the time between opening and closing the LINEX head must be shorter then 2 minutes In some cases 2 minutes is not long enough to perform all the required manipulation with the sample
7. ing material or sample introduced into liner for the direct thermal desorption can pusher out of the liner if pressure is not released Fig 8 below shows an exampled of the LINEX method FA GCMS Real Time Analysis Admin Acquisition Method_test01 qgm confirmation ggd Line1 70060515 qgt abe File Edit wiew Method Instrument Acquisition Data Tools Window Help Dsm Sa eel mE ma 2 aE ty oee Det 1 40 k Set cd GC Ms Inj Fort SPL1 Ini Heat Fort INJ e on oo S a Injection Temp joo 0 JE l f ae z E Injection Mode i ee wae a oe Sampling Time rnin 0 0 25 5 0 7 5 10 0 Carrier Gas He Prim Press 500 900 Flow Control Mode Pressure Total Flow Colunn Flow Pre aaa Total Program Time 12 46 min Purge Flow Column Split Ratio Mame test Thickness 0 25 um Length 60 0 m Diameter 0 25 mm Detail of Injection Port Peace High Press Injection amen las Saver araa Splitter Hald Earn GE Program a Split Ratio Program Eren Progam Time Program i Figure 8 Example of LINEX method within GC Solutions ATAS GL International Page 6 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 For the reasons mentioned above Injection Mode should be set to Split Flow Control Mode should be set to Pressure and the initial pressure should be set to a minimum possible value 12 kPa for instance At the same time Total Flow should be set to a high value more then
8. installed on the system a dummy SPL injector should be installed using a dummy connector for GC 2010 Injector Heater port This dummy connector is a part of the Shimadzu 223 57164 91 AFC addition kit for GC 2010 The dummy SPL Injector should be configured as it is shown in the example screens of GC 2010 in Fig 1 Pe Ie o Og at a pai j DI i th ATH N EIEEE p Ar r ere 1 nnn tet OH MUI DAA AT UTAT Figure 1 Configuration dummy SPL injector ATAS GL International Page 2 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 GC MS Solutions Configuration 1 1 1 Instrument System Configuration This configuration is similar to standard SPL injector since SPL is used as dummy injector for OPTIC 3 PTV see Fig 2 System Configuration x Available Modules Modules Used for Analysis gh gt Tesh Instrument E aT SPL Others bes SR Additional Heater ae Pe Additional Flow Properties Panicle se Cancel Print Help Figure 2 Instrument configuration 1 1 2 Instrument Parameters Set the parameters as it is shown in Fig 3 EM GCMS Real Time Analysis Admin Acquisition Method_test02 qgm 30_60 mesh glass beads pesticides grob19 qgd Line1 20080 a File Edit view Method Instrument Acquisition Data Tools Window Help Dizm an alx TES ml el ale ty olele w Gc e ms Inj Port SPL1 Inj Heat Por
9. n Workstation OPTIC Method Method5 LINEX TO File Edit View Method Sequence Configuration Window Help H a amp B eA D0 g E General Ee Ea 2 Method Hame Equilibration Time sec End Time sec TD Splitless Injector Temperature Initial Temperature C Ramp Rate C zec Final Temperature C Hold Time sec Temperature Control El Solvent Yenting MeathodS 5 B00 Mo 35 5 0 200 480 Keep Until Erd BO Figure 11 Example of LINEX TD Method ATAS GL International Page 8 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 Please note that Sample Sweep Time is the time needed to flush the injector after the LINEX head is closed When Sample Sweep Time is elapsed injector and GC programs are started 2 4 Settings for OPTIC 3 LINEX DMI Method In generally DMI method is used for liquid injections and requires solvent elimination similar to Large Volume Injection method The solvent elimination time should include the injector flush time see description for LINEX TD method above An example of the LINEX DMI method is shown in Fig 12 KJ ATAS Evolution Workstation OPTIC Method Methods File Edit view Method Sequence Configuration windo D U amp ba 4 General Method Name Methodb Equilibration Time zec z End Time sec B00 DMI Splitless Ho Injector Temperature Initial Temperature C 35 Ramp Rate Cser FO Final Temperature C 200 Hold Time sec 4
10. ndb y Column Flow 0 27 mL min 0 00 00 0 00 xj pee ee ue PS Total Program Time 15 01 min stat Purge Flow o o mL min Column i ar Split Ratio 544 3 Name test Thickness 0 25 um Length 60 0 m Diameter 0 25 mm Set Stop r Detail of Injection Port en A High Press Injection Warner Gas Saver Pi Splitter Hold Fan Method Detail mp yatta GE Program Split Ratio Program Prerun Program Time Program Figure 9 Example of a GC method In case of Splitless method the split valve must be closed immediately by GC program started at the same moment as the Large Volume Injection method Example of the program is shown in Fig 10 ATAS GL International Page 7 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 GC Program Prerun Program Time Device EVENT Vaka 0 00 a This time must be same as Time Program E z l eha mea d Mean of sampling time aif oo Ne EVENT deee EVENT Ea Data File Name R Time 27 756 min 10 012 Max Intensity O 75 103 means split valve closed 103 means split valve opened Figure 10 Example of GC Time Program NOTE _ If this method is cancelled during the GC run the split valve cannot be initialized In this case the split valve should be opened manually from the GC keypad 2 3 Settings for OPTIC 3 LINEX TD Method Example of the LINEX TD method is shown in Fig 11 ka 4745 Evolutio
11. t INJ1 Top Column Oven Temp x 50 0 C kPa a Injection Temp 3 ir j Injecti 1 E e wizard fico 00 me Carrier Gas He F Flow Control Mode Program Presswe H Pressue F Sample Login Pressure 100 0 kPa Total Flow 75 mL min 3 5 0 00 Standby Column Flow 4 55 mL min H gt Linear Velocity 77A cm sec eE OOO min Purge Flow 20 mL min Column Start Split Ratio 5 o Name InertCap5MS Sil Thickness 0 25 um Length 30 0 m Diameter 0 32 mm Set Stop Detail of Injection Pott Fest Chea g High Press Injection Carrier Gas Save 7 or Method Detail Splitter Hold Far GC Program A Split Ratio Program Prerun Brogan Time Program Figure 3 Instrument Parameters Window ATAS GL International Page 3 of 11 Quick Reference Guide OPTIC 3 PTV on GC 2010 In order to avoid the temperature ready check for dummy injector SPL1 SPL1 check box in the Ready Check dialog window should be unchecked Fig 4 x Heat Unit Injection Flow SPL1 Carrier Help APL Flow DetectorlFTD Detector APC Flow Baseline Drift T External wait Equilibriurn Time E min Figure 4 Ready Check Dialog 2 Setting up OPTIC 3 PTV methods 2 1 Large Volume Injection Method Set the parameters as it is shown in Fig 5 EM GCMS Real Time Analysis Admin Acquisition Method_test02 qgm 30_60 mesh glass beads pesticides grob
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