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1. LO TEN _ A 155 43 a E 53 57 54 va B A a R2 RI V3 el MA 1 2 3 AS Y N VI 1 ANJE aii e JN E 55 gt RI 54 55 oan 7 a ssor sd Lo 54 55 58 2 v2 Alt SAI GAIL mall H Pp Valco Trap 1 Flush Top2 Control Control 50 51 52 56 52 53 54 Figure 7 10 Compressed Air Schematic of GasBench Il Actual Part No 111 4262 7 20 Finnigan GasBench Il Operating Manual Thermo ELECTRON CORPORATION Technical Information Finnigan GasBench Il Compressed Air Schematic es 9 3 73 71 1 2 69 70 78 21 8 50 52 70 478 33 8 2 20 25 amp D 218 n E LO LO 2 lt R m Xx o N tT tO N 00 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 7 21 Technical Information Compressed Air Schematic Finnigan GasBench Il es Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Index Index 017 1911 7 19 050 5260 7 16 052 0910 7 3 052 0940 7 3 052 1320 7 16 052 1860 7 16 052 3460 7 19 054 3380 7 2 7 19 056 6390 7 2 7 19 060 5470 7 19 064 4520 2 18 067 4570 7 2 067 4790 7 2 7 19 067 4910 7 2 7 19 067 49
2. CO He Figure 4 7 Basic Test for Sample Section Autosampler and Bottles Excluded Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Basic Operations Finnigan GasBench Il Starting an Automated Sequence 4 6 Starting an Automated Sequence Before Starting an Automated Sequence 1 Frequently check the sample needle flush needle and acid needle for remainders of the vial septa Small parts can be removed using a syringe tip Check the flow through the sample needle 0 5 0 8 ml min at the exhaust vent connection of the valco 8 port while a sample is connected 2 From time to time at least once a month heat out the GC column Set the temperature regulator to 140 C and keep this temperature constant for 12 hours 3 From time to time check whether the water background of the IRMS is within acceptable limits that is less than 3 V See Water on page 4 3 Preparing a Test Sample The basic principle of the GasBench II technique is the measurement of any gas e g CO from the headspace in a vial Therefore it is unimportant for the GasBench II measurement how the gas was produced and released into the headspace For a basic system check that is with no sample involved a gas mixture is ideal Prepare this gas into an exetainer by flushing the vials with a mixture of 0 3 0 5 CO in He The flow should be about 100 ml min Hold the tube upside down onto the flushing capillary for approximate
3. Finnigan GasBench Il Operating Manual Click on the arrow and choose Save as to optionally choose a new name and folder for the currently active single document e g method or sequence Notice that the particular folder is shown that contains the currently active method Choose the folder above the Example folder not the Example folder itself This ensures not to mix or even overwrite the predefined example method with your own method Give the method a significant name e g similar to the sequence it corresponds to Keep the extension met Confirm by Save Click onthe arrow and choose Save All to save all currently active Isodat 2 0 documents e g methods sequences result files Result Workshop files They will be stored without changing names and folders Thermo ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Different GasBench Il Methods 3 6 Different GasBench Il Methods Depending on the particular GasBench set chosen in the Configurator different configurations will result as was depicted in Creating a GasBench Configuration on page 3 4 Gas Bench Gas Bench A2005 Sampler lt gj _ Gas Bench Acid Pump Gas Bench Acid Pump A2005 Sampler lt agj _ Gas Bench Precon Gas Bench Precon A2005 Sampler lt qgj Figure 3 24 The GasBench Sets Chosen in the Configurator Finnigan GasBench
4. Note A syringe must be used to prevent the sample from contacting and exchanging with ambient air Thermo ELECTRON CORPORATION Allow 18 hours to equilibrate Finally the sample will be measured Finnigan GasBench Il Operating Manual 5 23 Measurement Procedures for Real Samples Breath Gas Analysis 5 24 Finnigan GasBench Il 5 4 Breath Gas Analysis Using the Autodiluter for Blanking The atmospheric mixture used here contains lots of nitrogen and oxygen that severely distort operation of the source when reaching the inlet To avoid this the autodiluter arrangement has been modified to guarantee extreme dilution The modification can be obtained by e loosening the two screws and moving fully upwards the small metal plate that limits the movement of the autodiluters pneumatic lever See arrows in Figure 5 15 Figure 5 15 Adjusting the Open Split for Blanking Additionally the capillary feeding the split with helium needs to be retracted into the inner glass tube See Figure 5 15 and Figure 5 16 When unlimited in movement the lever moves the capillary leading from the autodiluter to the IRMS into the inner tube of the autodiluter In this position the capillary samples almost entirely helium and the dilution factor is larger than 100 Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Breath Gas Analysis
5. frequently used ones Table 7 1 as Kit with Part No Position Quantity Part No 1 1 113 7030 2 1 113 7120 3 1 104 4110 4 1 104 0430 5 1 112 1170 6 5 104 0490 7 2 900 0342 8 1 104 0480 8 5 106 0170 9 5 067 4790 9 5 100 6490 10 5 056 6390 11 5 100 4850 12 5 100 4640 13 2 067 4910 14 1 104 5480 15 2 054 3380 16 1 100 2605 17 1 074 3390 18 1 104 1800 1 1 067 4570 19 1 104 1730 20 1 104 1860 21 400 116 8780 22 1 112 1070 Finnigan GasBench Il Operating Manual Spare Parts and Consumables for GasBench Il Available 113 6810 Designation acid needle needle holder complete reducing valve ZRU1 5J VICI t piece ZX 5J VICI bulkhead connection VICI ferrule ZF1V VICI ferrule Valco FS1 5 ferrule FS 5 VICI ferrule 1 16 GVF2 003 ferrule 1 8 1 16 TEF ferrule 1 16 GVF2 004 ferrule 1 16 GVF 005 ferrule 1 16 GVF 003 capillary 0 32 mm d fused silica capillary 0 10 mm i d fused silica capillary 0 075 mm i d fused silica capillary 0 05 mm i d fused silica water trap 1 Nafion tubing i d 0 3 mm pipette micropipette 100 pl outer glass tube at sample open split inner glass tube as guide unit for capillaries of sample open split 12 ml uncoated soda glass vial RB single use syringe 1 ml PK 100 Thermo ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Table 7 1 Position 23 24 25 26 27 28 29 30 31 T
6. IRMS IRMS IRMS 0 1 1500 0 1 1500 0 1 1500 actuator actuator actuator He He He 0 1 500 0 1 500 0 1 500 Water Trap 2 Water Trap 2 Water Trap 2 0 3 200 0 3 200 0 3 200 Figure 5 16 Principle of Blanking e leftside no dilution e middle normal dilution e right side maximum dilution Results of Blanking Pee Name U Veveguvidvodet ATA da Une War Verter Ir TIN of j tg mem E a If f Lo 20 mo 200 o Figure 5 17 Blanking Chromatogram Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 25 Measurement Procedures for Real Samples Breath Gas Analysis Finnigan GasBench Il CO2 error Extended Sequence Line Peak Nr Width Ampl 46 BGD 46 Area All 13C 5180 mY Vs e o vs VPDB vs VSMOW 65 551 2 ae r fiss feos re fersa foio ooa 3 ss 712 169 fosos 19 67769 ome 10 053 jar fei7 962 jise foso 153 67713 ooo ooo gez pera ies mem lise levers ooe jomi CAI CE ESO ON E EE CT E ECN EE 650 0 6540 228 13 425 17 256 gt ee e E 950 1 9547 96 6300 191 10877 17 375 33612 12 moo3 1m045l91 euro 193 9859 17 384 33503 13 i2a7 e i2si6je se 163 asss 17306 30665 Figure 5 18 Blanking Result Grid Breath Gas Analysis in Brief To perform breath gas analysis the sample loop of the valco valve must be replaced by a 10 ul volume Refer to How to Change the Loop Si
7. Programming JUMO itron 16 Temperature Controller for Sample Tray For programming JUMO itron 16 temperature controller for GC oven see Programming JUMO itron 16 Temperature Controller for GC Oven on page 2 32 For details refer to Jumo itron 16 temperature controller manual The temperature controller located externally allows controlling sample tray temperature Notice the three keys see arrows in Figure 2 12 e P key for programming the values will be accepted automatically after 2 s e Arrow Up key to increase a particular value e Arrow Down key to decrease a particular value Figure 2 12 JUMO itron 16 Temperature Controller for Sample Tray Step 1 of Programming e Press the P key and hold it for 2 s Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 11 Hardware Components Sample Trays 2 12 Finnigan GasBench Il Pass through the menu until Y 0 is displayed Again press the P key and hold it for 2 s Set C111 to 003 transducer type e g Pt 100 2 wire Set C112 to 1 number of decimal places and temperature unit e g 1 and C Set C113 to 33 controller type e g double setpoint Set C115 to 1 ramp function that is ramp function in C min Set C116 to 0 outputs on fault that is 0 minimum output limiting Y 2 is effective Set SPL to 0 lower setpoint limiting Set SPH to 80 upper setpoint limiting Set OFFS to 0 process value correction
8. Set HyS 1 to 0 differential 1 Set HyS 2 to 0 differential 2 Set KO to 0 working point in Set Y Z to 100 maximum output in Set 2 to 0 minimum output in Set d F to 6 5 filter time constant in s Set rA Sd to 0 ramp slope in C h or C min For details refer to Jumo itron 16 temperature controller manual Alternative Automatic Programming Let the temperature controller program itself automatically Thereby you don t need to specify all the parameters mentioned above on your own For details refer to Jumo itron 16 temperature controller manual Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 33 Hardware Components Open Splits Finnigan GasBench Il 2 11 Open Splits Reference Injection This chapter outlines the functioning of the reference section of GasBench II Three reference gases can be injected via a three port open split interface A He stream of 2 ml min permanently flushes the interface tube see also Figure 2 36 and Figure 2 37 A permanent flow of 0 25 ml min transports the content of the interface tube to the IRMS Figure 2 36 Reference Inlet Open Split Thermo 2 34 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Hardware Components Open Splits Ref2 Ref2 0 025 400 0 025 400 actuator actuator IRMS IRMS 0 05 1500 He IN 0 05 1500 He IN 0 1 500 0 1 500 Principle Principle Open Split Open Split 3 fold 3 fold
9. Step 2 of Programming Again press the P key and hold it for 2 s Press the Arrow Up Down key to change values Set Pb 1 to 2 8 proportional band 1 Set Pb 2 to 2 8 proportional band 2 Set d t to 35 derivative time in s Set rt to 135 reset time in s Set CY 1 to 2 cycle time 1 ins Set CY 2 to 2 cycle time 2 ins Set db to 0 contact spacing Set HyS 1 to 0 differential 1 Set HyS 2 to 0 differential 2 Set Y 0 to 0 working point in Set KJ to 100 maximum output in Set Y 2 to 0 minimum output in Set d F to 5 filter time constant in s Set rA Sd to 9 99 ramp slope in C h or C min Alternative Automatic Programming Let the temperature controller program itself automatically Thereby you don t need to specify all the parameters mentioned above on your own Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Gas Supply 2 4 Gas Supply Gases in Use For all applications helium is needed as carrier gas Its purity should be at least 99 999 He We recommend to use a second cylinder switchover to prevent pressure loss during overnight operation A standard 50 gas tank has a lifetime of half a year in continuous operation For all applications with CO as molecule of interest that is water equilibration DIC or carbonates CO having a purity of 99 995 CO is recommended as reference gas A 40 1 tank will last lo
10. a Carbonates saq jun Equilibration seq a Flush Fill seq a H2_zero seq a Zero seq File name Acquisilion 1 seq Save as type Sequence seq z Cancel Save All Command Thermo Isodat 2 0 Software Creating a New Sequence e Click the Save button to save a sequence created on your own e Click on the arrow and v choose Save as to optionally choose a new name and folder for the currently active sequence Select a suitable folder Create a new one if you want e g to separate predefined sequences from those created on your own Give the sequence a significant name e g similar to the method it corresponds to Keep the extension seq Press the Save button e Clickonthe arrow and choose Save All to save all currently active Isodat 2 0 documents e g methods sequences result files Result Workshop files They will be stored without changing names and folders ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 37 Isodat 2 0 Software Creating a New Sequence Finnigan GasBench Il Starting a Sequence SS e To start the sequence finally gt press the Start button Sert The window below appears AAA Xi Results Define full path for results Isodat Object storage gt TemplateDataSequenceHeader Export Define the format of p Results measurement data to be exported Folder Name Pre Post Jfaco Resuts Ss choose between None Excel Lotus T Auto Enum
11. gas sampling section 4 4 5 2 gas supply 2 13 gas tank 1 3 2 13 to 2 15 5 3 GasBench A200S autosampler method 3 19 3 31 GasBench acid pump A200S autosampler method 3 32 GasBench PreCon A200S autosampler method 3 32 GasBench II configuration 3 4 IV Finnigan GasBench II Operating Manual GasBench II connector 3 9 GasBench ll hardware component 3 11 GasBench II main module 2 26 GasBench Il method 3 18 to 3 19 3 31 GasBench II oven 4 4 GasBench II sequence 3 39 GasBench II set 3 5 3 31 GasBench II window 3 10 to 3 12 gasket 7 16 GC application 2 37 3 22 to 3 23 3 25 5 2 5 5 GC column 2 22 to 2 23 2 26 to 2 27 3 25 3 27 4 4 to 4 5 4 12 to 4 14 4 16 5 2 5 4 6 13 to 6 14 GC column flow 2 23 6 12 to 6 13 GC column temperature 2 26 to 2 27 GC GasBench Il 7 19 GC housing 4 5 GC injection 2 16 GC oven 2 26 to 2 27 GC oven isolation 2 28 GC PAL 2 6 3 42 GC PAL loader software 3 42 GC peak 6 12 to 6 13 GC peak shape 4 12 GC separation 5 2 geochemistry 5 4 geology 5 4 glass tube 2 21 global change research 5 2 glove box 2 18 gloves 5 16 5 20 GND 2 15 goggles 5 16 graphical object 3 12 Grootes P M 5 10 grounding cable 2 28 to 2 29 guard trap 2 21 2 26 guide unit 7 2 GVF 003 7 2 7 19 GVF 005 7 2 7 19 GVF2 003 7 2 7 19 GVF2 004 7 2 H H D 5 2 H D equilibration 1 3 3 39 5 33 H D measurement 2 13 5 4 5 34 5
12. three port open split interface 2 34 time adjustment 3 27 time delay 4 12 time difference 5 4 time events list 3 20 3 22 to 3 23 3 25 to 3 26 3 39 5 5 5 28 to 5 29 7 16 time events tab 3 19 3 21 to 3 23 3 33 timeshift 3 27 to 3 28 timeshift correction 3 28 timeshift suppression 3 27 timing 3 23 to 3 24 3 27 5 5 5 10 title bar 3 7 3 11 trace gas 5 2 transfer line length 4 12 transfer needle 2 16 transfer time 3 21 5 4 trap 2 14 3 5 to 3 6 3 12 3 21 5 2 6 9 6 12 to 6 13 trap 2 3 5 trap arrangement 6 8 trap connection 6 11 trapping system 6 12 tray 3 35 3 45 4 14 5 7 5 31 6 2 tray cover 6 2 tray holder 3 44 to 3 45 tray temperature 5 31 tray type 3 45 tree of hardware commands 3 47 to 3 48 trigger signal 3 23 triple collector 3 20 troubleshooting 3 9 tubing length 6 2 tubing nozzle 7 16 tune 5 10 U uncoated soda glass vial 7 2 uncorrected result 5 10 upper inlet port 2 15 user programmable autosampler 5 2 Thermo ELECTRON CORPORATION V vacuum chamber 5 4 valco ferrule 4 4 valco loop 2 16 2 21 4 14 valco port 5 2 6 8 6 12 to 6 13 valco valve 2 14 2 16 2 21 to 2 23 3 12 3 22 4 4 to 4 5 4 13 4 16 5 3 to 5 4 5 26 6 12 to 6 13 valco vent 2 24 valve action 4 14 valve system 2 14 vent 2 16 2 23 6 2 vent connection 4 13 vent exit 6 12 vial 2 24 3 21 3 45 3 50 4 13 to 4 14 4 16 5 5 5 7 to 5 8
13. 101 111 4360 needle GasBench Il 1 108 111 2870 column open split GasBench II 1 109 1116620 GC GasBench Il 1 112 037 0650 clamp 6 4 4 113 067 4651 coupling complete M5i M5i 1 115 0470070 disc 8 4 DIN 125 1 116 052 1950 blind plug M5 6 117 052 4070 reducer R1 8 M5 1 120 045 2450 threaded rod M6 MS 4 123 033 1250 flat connection 2 6 3 mm M4 2 124 033 0820 flat connection 5 126 112 1170 bulkhead connector VICI 2 130 067 4790 ferrule 1 8 1 16 TEF 4 134 048 0060 bolt 2 10 DIN 7 3 141 112 7680 fastener gas supply GBC 1 142 0171911 capillary FS Poraplot Q 25 m 1 200 112 1060 installation kit GasBench Il 1 Table 7 2 refers to Figure 7 1 Figure 7 2 and Figure 7 8 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 7 5 Technical Information Mechanical Parts Finnigan GasBench Il 3 a 3 PA gt ha oil E E ims gt goo er oye re SE le HR L E LH 151 s S
14. 204 asa121 075000 66758 60 006 0278 70s 0688370417 4 792 280 20 4158 012 676 908 97 124 67 019 60 424 705 0000000000 Troas maa raa arsar 7250197471 osaat 20 068 7050231000027 e iza roa 203 2807200 620 112 07803 eo 722 22 57 7712000700007 7 104 1044 203 002200 500 000 08221 06 53 20 508 721300000100 fe __ 228e 2397 190 007 007 50 124 05208 00708 10 082 7719000073102 fe 2762 285 2 100 071007 510302 95 03 00953 10708 7719225515207 ro _ s2ra ss27 109 5007505 078 318 0501006331 17 006 771 2050700402 m 2777 382 5 100 370060 24207105500 00 320 10 072 710006503541 2 eer2 20 100 2267 705 451 00 9540506209 16763 771720510000 Pa area 017 108 3111000 20200595200 6305 18950 7718717305801 a paez es 7 105 2000008357 70205222 08503 12 00 7720100750010 e 9700 2018 10 1 2700 20 333 128 05202 06 209 13201 7720000000479 Figure 5 33 Water Equilibration H D Result Grid Sample Amount Consideration for Both Water Equilibration Types In this section the sample amount needed for both types of water equilibration is estimated via an approximate calculation It helps to decide whether a mass balance calculation needs to be performed for a particular sample or not Thermo 5 38 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Water Equi
15. 5 10 open split lever 2 14 operation mode 5 31 optimal setting 5 37 optional hardware 3 5 O ring 6 2 6 5 to 6 6 OUT position 2 37 out signal 3 45 outer glass tube 7 2 overlapping peak 3 27 overnight operation 2 13 overpressure section 5 4 P packing material 2 27 paleoclimatology 5 2 PAL GASBENCH V2 33 021031 sss 3 42 3 49 Parafilm 5 17 parameter tree 3 44 parity 3 51 parts list 6 8 6 10 pass to gas configuration 5 34 passive tray 5 31 path 3 44 to 3 45 PDB 5 13 Thermo ELECTRON CORPORATION Finnigan GasBench Il Index peak amplitude 5 11 to 5 12 peak area 5 11 to 5 12 peak center 3 2 3 35 4 14 5 34 5 37 peak center cup 3 20 peak center cycle 3 20 peak center offset 3 3 peak center postdelay 3 20 peak center predelay 3 20 peak detection 3 26 peak detection parameter 3 26 peak detection tab 3 19 3 26 to 3 27 peak discrimination 3 28 peak height 3 28 4 10 5 10 5 22 peak min height 3 26 to 3 27 peak resolution 3 27 peak shape 3 28 4 12 6 7 to 6 8 peak shape distortion 5 36 peak shape scan 5 36 peak slope 3 26 peak start 3 25 peak stop 3 25 peak width 3 28 peripherals support table 1 2 phosphoric acid 5 5 to 5 8 5 16 6 2 6 5 phosphoric acid preparation 5 16 phosphorous pentoxide 5 16 to 5 17 pipette 5 30 7 2 pitfall 5 17 Platzner I T 5 3 plot column 4 4 plug amp measure device 3 9 plug and measure adapte
16. 5 30 5 33 6 2 virtual parameter 3 26 viscosity 5 10 Viv Cin Slv 1 3 50 Viv Cln Slv 2 3 50 Vogel J C 5 10 VPDB 5 13 5 16 VSMOW 5 31 VSMOW SLAP normalization 5 32 5 35 W wash station 3 45 washing bottle 5 5 water background 4 13 water equilibration 1 3 2 13 4 6 5 30 5 32 to 5 33 5 38 water gradient 2 21 water level 4 4 water peak 5 18 water phase 5 39 water removal 2 16 5 2 water sample 5 2 5 32 5 35 water standard 5 22 water trap 2 37 4 4 to 4 5 5 4 7 2 7 9 working area 2 14 working standard 5 12 to 5 13 5 16 6 2 Z zero enrichment test 3 18 4 6 4 16 5 6 zero met 3 19 3 40 4 6 zero seq 3 39 to 3 40 Finnigan GasBench II Operating Manual IX
17. 5 33 sample section 4 12 sample side 4 16 sample size 5 2 sample stream 2 21 2 37 sample transfer path 4 5 sample tray 2 4 2 7 to 2 8 5 13 5 26 5 31 6 2 sample tray layout 2 10 sample tray temperature control 5 31 sample tube 5 2 sample vial 4 12 5 2 5 5 5 7 5 18 5 26 5 39 6 2 7 3 sample volume 3 50 sample helium mixture 5 10 5 22 sampling capillary 2 37 sampling flow 6 13 sampling line 4 14 sampling loop 2 22 to 2 23 sampling needle 2 2 2 19 3 22 4 5 5 7 to 5 8 5 33 6 3 sampling needle connector 4 4 sampling technique 5 4 sampling time 3 50 script editing 3 20 search tab 3 16 security 3 22 sensitivity 4 12 5 37 septum 4 13 5 2 5 7 5 18 5 22 to 5 23 5 26 5 30 6 2 6 5 sequence editing 4 15 sequence grid 3 35 to 3 36 3 39 sequence line 4 14 sequence list 4 14 sequence script 3 38 sequences tab 3 14 3 39 service engineer 2 15 set path 3 15 side panel 2 29 signal height 2 13 3 21 5 10 signal intensity 5 37 signal source 3 23 signal to 5 value scale 5 10 VIII Finnigan GasBench II Operating Manual silicon tubing 7 16 simultaneous 180 and 13C determination 5 2 simultaneous measurement 5 6 single measurement 3 14 single needle holder 2 19 single result printout 4 6 single stroke 6 5 single trap application 6 7 6 12 single trap system 6 12 single use cannula 7 3 single use syringe 7 2 site requirement 1 2 six port
18. in the Examples folder are only example files They only show guidance through helpful default values but must never be used for measurements Never overwrite an example file with a sequence created on your own Depending on your software version these examples may not work properly Press the New button e To create a new sequence mark Sequence Confirm by OK Sequence Properties x Number ol Samples 8 y Esa e Specify the number of samples e g 96 e Confirm by OK Thermo 3 34 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Creating a New Sequence Note In case of carbonates 80 samples can be measured leading to 88 lines The first row can not be measured as it is not accessible by the acid needle without destroying the measurement needle The last row can not be measured as it is not accessible by the measurement needle without destroying the acid needle In case of equilibrations all 96 lines can be filled See Sample Trays on page 2 7 a S YX B EB Z te Insert t Options Auto Sort Reset Erro AS Method Prepatation Disabled Disabled Figure 3 27 Sequence Grid First 12 Lines The sequence grid contains all information about the individual samples bundled together in the sequence Line each line refers to an individual sample Peak Center markingit Y allows performing a peak center f procedure prior to measuring the par
19. s Result Workshop to select and display particular aspects of your acquisition data Refer to Result Workshop in ISODAT NT Operating Manual Upgrade to Version 2 0 Part No 115 4990 Results tab e Provides access to all previously acquired measurement results e Gives an overview of all results e Is empty prior to the first measurement Note To easily transfer and store data at your place of choice e g on a drive where data security is guaranteed change the result path by a right click and then select Set Path The basic path is automatically installed For reasons of data security we recommend you to frequently benefit from this feature Isodat Acquisition i j Attention System Path modification All Path related Actions are influenced 7 cea From now on all method sequence and result files will be stored at a different location ISL tab e Refer to ISODAT NT Operating Manual Upgrade to Version 2 0 Part No 115 4990 e In the GasBench folder you will find only one single acquisition script for GasBench II acquisition isl It is used for all possible configurations that can be selected in the Configurator see Creating a GasBench Configuration on page 3 4 It is not necessary to change it Thermo ELECTRON CORPORATION Finnigan GasBench II Operating Manual 3 15 Isodat 2 0 Software Accessories Bar 3 16 Finnigan GasBench Il Note All acquisition scripts are usually named
20. the latter only the number of acid drops has been reset to zero The sequence for HD equilibration Equilibration seq is also used for CO equilibration only the reference gas inlet must be changed and the reference gas be switched in the Time Events list Finnigan GasBench Il Operating Manual 3 39 Isodat 2 0 Software Creating a New Sequence Finnigan GasBench Il Method Sequence Correspondence Each predefined method corresponds lt gt to a predefined sequence and vice versa e Zero met lt gt Zero seq Flush Fill met lt gt Flush Fill seq e Acquisition 630s met lt gt Carbonates seq and Equilibration seq e Acquisition met lt gt Carbonates seq and Equilibration seq as an older method Acquisition met is no longer recommended e H2 zero met lt gt H2 zero seq Thermo 3 40 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Excel Export 3 8 Excel Export Figure 3 30 shows a simple Excel Export template created for GasBench II using the Excel Export Editor It can be used as an example for creating a customized export template In all cases the following columns should be exported El GasBench wke 7 Acquistion Mode I Included Sting F Gos Configuration Oe wp Se cas eli MEE a cee W Data Type Y Sequence Line IV Acquisition Message fF Molecule Della V Valuated Results Y Method Part Y Result Peak I Element Ratio Inte
21. 13 7 16 reference gas capillary 2 35 reference gas inlet 2 35 3 39 5 3 reference gas pulse 2 35 3 20 3 26 reference gas switch 3 21 reference gas tank 7 16 reference in 2 35 reference inlet 2 34 5 3 reference material 5 13 5 32 reference name 3 25 reference out value 3 20 3 26 reference port 2 15 3 12 3 21 5 3 5 5 reference pressure regulator 2 15 reference pulse 3 27 reference sample 5 12 5 31 reference section 2 34 reference signal height 5 34 request status 3 51 reservoir tubing 6 6 residual air 3 27 resistor 4 6 resistor value 3 2 result export 3 38 result file 3 16 3 30 3 37 result workshop 3 15 3 29 result workshop document 3 16 result workshop file 3 30 3 37 results tab 3 15 retention time 3 20 3 25 to 3 26 4 12 5 17 Finnigan GasBench Il Operating Manual VII Index Finnigan GasBench Il ribbed radiator 7 19 right needle 5 6 right side panel 2 26 to 2 29 rinsing agent 5 33 rinsing needle 5 30 5 33 S safety column 4 4 sample container 4 4 4 6 5 2 5 4 sample flow 2 21 to 2 23 2 37 6 8 6 12 sample gas 3 25 5 3 to 5 4 5 6 6 7 to 6 8 sample injection 2 36 sample inlet 2 36 sample line 4 12 sample loop 2 23 to 2 24 2 26 3 22 4 5 4 14 5 2 to 5 3 5 26 6 8 7 19 sample needle 3 50 4 13 7 19 sample open split 7 2 sample peak 4 6 4 14 sample peak voltage 3 21 sample preparation 3 36 5 2 5 4 5 7 5 31
22. 3 2 3 2 Creating a GasBench Configuration esessessesseessnennnennnnnennennnennnnsenneennennennnnnnenn essen 3 4 3 3 Acquisition Mode icceccosccnncinonsniodcondodacnndacuapoaneda a A EE E a A aaa a EE eE EES 3 7 3 4 Accessories Barinitas tt A ii 3 9 Troubleshooting Error Messages uunessesseenseennennnennneennennnnnnnnnnnnnnnennennenneennn ernennen 3 9 Changing Visibility of its Components uenesssesssesseeeneesnennennnnnnnneennennsennsennennennnnnnnn 3 11 The GasBefich Wind Weil nta aaa BR RN Pela taki HR areata 3 11 The Acid Pump Window fs gestae asi enlaces RR intends 3 12 AN A E 3 13 3 5 Creating a New Method ce cccccccccscesseesecesseeeceseceseeeseceseceseceseceneseeeceeeceesneeseeseesneesseeseengs 3 17 Predefined Methods as Examples cccccccsccsseesseessceseeeseceseeesecesecnseeeaecseecneeeeeeeeeeeseeeaees 3 18 Structure of GasBench Related Methods oooocciocnionnonoconoconononononononononononoonncno nono ccanncnnnos 3 19 Istria degen Sete sn 3 19 TimeByentsitabisesessunsssienehsegshnieun inusnsininneheinnkessrelsarin 3 22 Component Names tab ueesseessesssssnnsnennnennnennnennennnnnnnnennennensnnnnnneensnensesnsnnensnannn 3 24 Eyalu t ondab r uu aan a ca 3 25 Peak Detection taba O ta 3 26 PD a asia siete 3 29 Saving a Method tiara 3 29 3 6 Different GasBench II Methods oooooonocnnocinonononcnonconnconocononononononnnonn nono n corn cann cana rnn rro n rra nnrnnnnnss 3 31 The Ga
23. 38 Ho 1 3 2 13 to 2 15 3 21 3 27 3 39 5 3 to 5 4 5 34 5 37 H 4 5 1 3 Hp in He 2 13 H2_zero met 3 18 3 40 H2_zero seq 3 39 to 3 40 Hzfactor 5 34 Habfast K 5 3 HayeSep D GC column 2 26 to 2 27 He CO mixture 2 35 5 30 He CO mixture tank 5 30 He 5 36 He formation 5 36 to 5 37 headspace 2 16 3 50 4 13 5 2 5 4 to 5 6 5 39 headspace flushing 2 13 Thermo ELECTRON CORPORATION Finnigan GasBench Il Index headspace sampling 5 4 headspace sampling needle 5 3 heating unit 2 4 heavy isotope signal position 3 27 height width ratio 3 28 helium 4 6 1 3 helium 5 0 1 3 helium carrier gas 1 3 helium flow 2 16 2 21 2 26 to 2 27 2 34 to 2 35 5 7 7 16 helium inlet port 2 15 helium overpressure 5 3 helium pressure 2 22 2 26 to 2 27 6 13 to 6 14 helium tank 2 13 high capacity purifier 1 3 high pressure tank 2 15 hollow nut 6 2 7 3 host computer 2 6 hydrogen calibration 5 34 hydrogen equilibration 3 21 5 33 hydrogen isotopic ratio 5 4 hydrology 5 2 hyperterminal 3 51 I IAEA 3 25 5 12 to 5 13 7 14 IAEA Analytical Quality Control Services Reference Materials Catalogue 7 14 IAEA primary standard 7 14 IAEA TECDOC 825 7 14 ideal gas 5 39 ideal signal height 2 13 IN position 2 37 individual background 3 27 initial filling 6 5 injection head 2 4 injection mode 2 22 to 2 24 4 14 6 8 injection needle 7 19 inject
24. 4 3 074 3390 0 25m Nafion tubing i d 0 3 mm 4 0674930 4 nut SSNE 16 5 056 6390 3 ferrule 1 16 GVF 005 6 065 2190 2 O ring 6 07 mm 1 78 mm Viton 1 055 2180 2 O ring 6 07 mm 1 78 mm Viton 7 053 5930 2 spacer bolt M 4 25 8 045 1740 2 knurled head screw M 4 10 DIN 464 7 10 Finnigan GasBench Il Operating Manual The rmo Finnigan GasBench Il Thermo ELECTRON CORPORATION Technical Information Water Traps Table 7 3 Position 9 11 12 13 14 2 Parts List Referring to Water Trap Figure 7 4 Part No 100 2605 Part No 111 6830 034 2040 100 4850 046 0220 047 0040 100 4640 Quantity 2 0 09 m 1 2 2 0 82 m Description clamp shrinkable tubing 9 5 SW ferrule 1 16 GVF 003 nut M 4 DIN 934 washer 4 3 DIN 125 fused silica capillary i d 0 32 mm Finnigan GasBench II Operating Manual 7 11 Technical Information Reference Open Split Finnigan GasBench Il 7 6 Reference Open Split Figure 7 5 Reference Open Split Part No 109 6570 Table 7 4 Parts List Referring to Reference Open Split Figure 7 5 Part No 109 6570 Position PartNo Quantity Designation 6 067 4590 5 screw connection SSU 16 16 7 067 4930 5 nut SSNE 16 10 067 4580 3 lift cylinder 8 25 SMC 11 070 3780 3 tube nozzle 12 050 5260 3 gasket 8 5 17 1041800 1 pipette 1 0674570 1 micropipette 100 ul Thermo 7 12 Finnigan GasBench II Operating Manual ELEC
25. 4 4 42 Checking Column Blows eiii irn 4 5 4 3 Zero Enrichment Test Standard On Off Test ooonoocnncccconacoonncononcnonnconnncnnnanonnnconnnconnnccnnnconnncnnos 4 6 Testing Reference Gas Inlet Ports cccccccecssesssessecseeeseeeseceseeeeeeseeeseeeseceseeeseseseseseeeseennees 4 9 AA Eineantyalest au 2 Maneshdeus avucesast crates Ti AE 4 10 43 CONGIMON A RE 4 12 4 6 Starting an Automated Sequence ceecesseesseeseeeseeseeceseceseceseeeeeeeeseeeseeeseceseenseenseenseseseenaes 4 13 Before Starting an Automated Sequence cccceecsesseesecsseceseeeseceneesaeeseeseeeeeeeeneesseenes 4 13 Preparing a lest Sample iii il 4 13 4 7 Erequently Asked Questions u ns anna sates leases 4 16 Measurement Procedures for Real Samples cssesossssonssennssssnensnnnnnssnnsnnsnnsnsnnnnsnnnnnsnnnnnnnne 5 1 Dede Introduction le det tos tod 5 2 Gotieral REM rn dol to ns nes 5 2 Headspace Sampling ss A A dd dt 5 4 Cleaning Procedure for Sample Vials nsnesseesseesnesseennesnnennnennnennnennennennnnnnnnnanenn 5 5 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual iii Contents Finnigan GasBench Il 3 2 Carbon ates rien iii AA og Mena eas 5 6 Introduction NN 5 6 Double Needle Sui iia 5 6 Carbonates in Briefs nnne aa A A ang al oe aie ee eee en aes 5 7 LIS ar y COMEN seen des dotage AR arian ae ee ee 5 10 Referencing versus VPDB nipu E A A A A R es 5 13 Remark on the Strange
26. 5 E er cH 7 a x H i HEO o Eg ea coun H z z L HIH CB E Bu Sh 24 ET TZ aise H e n ZLL LLL ve 0LL ezL Pi Figure 7 1 GasBench Il Top View Part No 111 4260 Outdated Thermo 7 6 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Technical Information Finnigan GasBench Il Mechanical Parts 10 113 52 53 2 19 120 121 122 Figure 7 2 GasBench Il Side View Outdated Part No 111 4260 Thermo Finnigan GasBench II Operating Manual 7 7 ELECTRON CORPORATION Technical Information Plug and Measure Adapter Finnigan GasBench Il 7 3 Plug and Measure Adapter On the plug and measure adapter pnm adapter Part No 205 2660 two addresses have already been adjusted by Thermo Electron Bremen via the two coding switches See arrows in
27. 5 Isodat 2 0 Software Creating a GasBench Configuration Finnigan GasBench Il Contrary to former times Finnigan GasBench II now always contains a Flush Fill Finnigan GasBench II can be used either without a trap or with one trap or with two traps Traps are optional and provide additional opportunities Note In Isodat versions older than Isodat 2 0 occasionally software problems due to old scripts that is sct occurred when no trap was installed In Isodat 2 0 however new scripts that is isl are used eliminating this problem 4 Isodat Configuration iso IsoConfigurator File Edit View Options Interfaces Help E db B Wr GasBench II and A200S autosampler have been attached to Capillary port Ty GasBench amp 42005 Sampler EMS Delta Plus XP u MA e Close the Configurator Capillary All settings will be saved automatically Thermo 3 6 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Acquisition Mode 3 3 Acquisition Mode This section outlines Acquisition Mode For detailed information refer to e JISODAT NT Operating Manual Part No 109 2481 e JISODAT NT Operating Manual Upgrade to Version 2 0 Part No 115 49 90 e Start Isodat 2 0 by a double click e Start Acquisition Mode Acquisition You are now able to run any Continuous Flow application which gives you full control over the automated measurement
28. 50 fill stroke 3 50 Finnigan GasBench Il Operating Manual II Index Finnigan GasBench Il filling needle 5 7 5 30 filling volume 5 30 Finnigan DeltaPluSXP 1 2 Finnigan GasBench Il 1 2 3 6 3 31 to 3 32 5 2 7 16 Finnigan isotope ratio mass spectrometer 1 2 fire 2 14 first peak 5 10 fissure 5 18 flag 2 16 Fleischer M 5 4 flow control 7 9 flow meter 4 5 flow rate 4 14 5 10 flow restricting capillary 5 34 flow restriction 7 9 flush capillary 4 13 flush connection 2 15 5 30 flush fill 3 5 to 3 6 7 16 flush fill on column 7 16 flush fill valve 3 12 flush fill met 3 18 3 35 3 40 flush fill seq 3 39 to 3 40 flush gas 2 14 5 30 7 16 flush needle 2 18 to 2 19 4 5 4 13 to 4 14 5 7 5 30 7 19 flush sequence 5 7 5 30 5 33 flush valve 4 5 5 30 flushed vial 5 23 focusing trap 6 13 food authentification 5 2 foraminifera 6 2 fractionation 2 15 5 10 5 12 5 22 fractionation factor 5 4 Franklin J L 5 37 Friedman l 5 4 FS 5 7 2 FS 1 3 7 19 FS 1 5 7 2 7 19 fused silica capillary 2 16 6 7 to 6 8 6 12 fused silica column 2 26 fused silica trap 6 12 to 6 13 G gas bubble 2 14 gas component 5 4 gas configuration 3 10 3 17 3 19 to 3 20 3 39 5 34 gas configuration editor 3 3 4 6 gas connection 2 14 4 4 gas connection terminal 2 2 gas flow scheme 7 9 gas line 1 3 7 19 gas phase 5 4 5 39 gas requirements 1 3
29. 50 4 6 5 2 5 4 to 5 8 5 13 6 2 7 16 carbonate ion 5 6 carbonate kit 2 18 carbonate measurement 2 8 3 39 5 4 to 5 5 5 7 to 5 9 5 28 to 5 29 carbonate option 5 6 6 2 carbonates seq 3 39 to 3 40 carrier gas 1 3 2 13 carrier gas connection 2 15 center cup 3 20 center knob 3 44 central gas distribution t piece 7 9 checklist 4 16 chromatogram type 3 28 chromatographic peak 3 27 to 3 28 chromatographic system 3 28 chromium dioxide 5 17 CO 4 4 CO 2 13 2 15 to 2 16 2 18 2 21 to 2 22 2 26 2 35 3 10 3 17 3 19 3 21 3 25 to 3 27 4 4 4 6 4 13 to 4 14 5 2 to 5 4 5 6 5 18 5 28 5 30 5 34 5 39 CO 4 5 1 3 CO application 3 27 CO configuration 3 3 CO equilibration 3 27 3 39 CO in He mixture 2 13 4 12 CO peak 3 27 4 6 5 10 5 22 CO tank 5 10 CO water equilibration 2 13 CO 5 6 coding switch 7 8 column flow 4 5 column pressure 5 4 column type 2 24 COM 1 3 51 Combi PAL autosampler 2 6 2 16 3 42 4 14 5 2 Combi PAL autosampler method 4 14 to 4 15 command script 3 21 compatibility mode 3 50 component Names tab 3 19 component names tab 3 24 to 3 25 compressed air 1 3 2 14 to 2 15 compressed air distributor 1 3 7 16 compressed air schematic 7 15 to 7 16 7 20 compressed air supply 6 9 Thermo ELECTRON CORPORATION Finnigan GasBench Il Index configuration 3 3 to 3 4 3 9 to 3 12 3 15 3 17 3 31 configurator 3 2 3
30. 6 Refer to Nelson S T A simple practical methodology for routine VSMOW SLAP normalization of water samples analyzed by continuous flow methods Rapid Communications in Mass Spectrometry 14 1044 1046 2000 John Wiley amp Sons Ltd Results _Rpalibestion ct AN Aa AH AN LE LLL LLLLI BSD 44 860 45 mv mv a 9 201 9 953 E 0 04047 15422 0 0247573304 A A A E A eieiei A A peteti iti fe O E aranea ossa ma 171 EC E fs CA ann O somas E CA EI 7 ron 257 irasos 1700 15000 ears ooro 13022070205 250922007000 fe 200 7 25 1 roza o7a 10500 15008 eave ooro 1370700000 25 1197901708 fe 210 4 209 1320000 921 10205 15001 7300 ooroo _ 12000180171 251052200500 fro _ ppoal2a2 1200000 ose 11500 15305 7558 00120003 12010002000 25054110000 m aene v1oa a0 oo 11200 15 188 7102 00120103 _ 12078010406 250422751007 12 esa 292 1135373 0205 10505 15013 osoo_ oo1zooe 11514021328 250570538020 sa Jerso 2a2 1075507 0200 11000 12013 ose 000102 12927002000 250032008000 a Jeps2 202 1010200 0250 10908 13000 ome oor20005 12700751720 253001067725 Ls Jerao 204 005237 0 162 10501 13030 5201 oo120000 12008511347 230201001091 Figure 5 28 Water Equilibration 180 Result Grid Thermo 5 32 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Water E
31. 6 3 9 3 12 3 15 3 19 3 31 to 3 32 configurator window 3 2 to 3 4 ConFlo Ill 3 16 connection panel 2 15 connection terminal for sampling needle 2 2 consumable 7 2 container 4 12 contamination 5 5 continuous flow application 3 7 continuous flow method 5 32 5 continuous operation 2 13 control line 6 9 controller 5 31 correction 5 12 correction factor 5 12 Craig 3 25 critical parameter 3 44 cryo trap option 6 7 cryofocusing 5 2 to 5 3 cryofocusing trap 6 13 cryo option 6 7 cup 2 4 6 cylinder switchover 2 13 D 5 definition 5 15 to 5 16 5 value 3 25 3 27 5 10 to 5 13 5 15 to 5 16 5 39 51 C 4 6 5 13 6 2 51 C value 4 8 4 11 8180 4 6 5 13 6 2 data acquisition 3 16 to 3 17 3 20 3 22 to 3 23 4 14 5 13 data evaluation 3 25 data point triplet 3 20 data security 3 15 dead volume 2 16 debugging 3 20 decoupling 2 37 default autosampler configuration 3 42 default value 3 14 3 17 3 26 3 28 to 3 29 3 34 3 36 delay 2 8 3 20 3 26 to 3 27 Delta series 4 10 DeltaP us 4 10 DeltaPlUSAdvantage 2 3 DeltaPlUSXP 3 2 5 34 detection mass 3 26 detection trace 3 27 DIC measurement 5 4 to 5 5 diffusion 6 8 dilution 2 36 to 2 37 5 29 direction button 3 13 dissolved CO 5 4 dissolved inorganic carbon DIC 1 3 2 13 2 18 4 6 5 2 5 20 distilled water 5 5 dolomite 5 6 6 2 double needle flush sequence 5 7 5 30 double needle
32. A la AAN E PEE E IAN BEER EC ee ee ee EC NAAA E EA COM a CIN A A A 80 I u ee EC E ee CHINA AE eee ee Figure 5 12 Dissolved Inorganic Carbon DIC Measurement Time Events List Partly Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 21 Measurement Procedures for Real Samples Dissolved Inorganic Carbon DIC Finnigan GasBench Il Die Wome Ciber VIARIA Lerida id O of un Te hi Figure 5 13 Dissolved Inorganic Carbon DIC Measurement Chromatogram Peak E Width Ampl 44 Ampl 46 BGD 44 Area All 8 13C fl s mV mv EIER 41 8 7357 43 1 ere ee io lo a ET Tasse 290 sms loses ss sas IN CAT 5 395356 285 5464 7668 419 31 039 1127 27216 as ess xo fase rm sea ass fs fora 7 592 535 3 277 4684 Figure 5 14 Dissolved Inorganic Carbon DIC Measurement Result Grid e Almost no signal occurs on m z 46 between the CO peaks e Decreasing peak height indicates proper transport of sample He mixture Warning When filling a number of tubes from the same water standard do not fill from sealed vessel with septum A negative pressure will be created that could cause fractionation Ther 5 22 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Measurement Procedures for Real Samples Dissolved Inorganic Carbon DIC Warning When filling real samples use a new syringe for ea
33. AS200 autosampler 3 50 atmospheric concentration 5 28 auto dilution 3 21 auto square pulse recognition 3 27 automated sequence 4 13 automatic square peak detection 3 28 autosampler 2 6 2 19 3 11 3 21 3 31 3 35 3 42 3 48 3 50 to 3 51 4 12 5 5 5 7 to 5 8 5 30 autosampler display 2 6 3 43 autosampler hardware 2 4 autosampler memory 3 42 3 44 autosampler method 3 35 3 50 autosampler panel 3 42 to 3 44 autosampler power supply 2 6 autosampler programming 3 42 autosampler settings 3 42 autosampler tray 5 30 auxiliary gas 1 3 auxiliary unit 7 2 B background detection 3 26 background gas 4 3 background gas composition 4 2 to 4 3 background type 3 26 to 3 27 backup 3 42 backup file 3 35 bars tab 3 8 baseline 4 6 basic bar 3 8 basic function 3 19 3 39 basic measurement 3 14 4 1 basic path 3 15 basic system check 4 13 basic test 4 12 4 16 basis method 3 18 borosilicate glass 6 2 bottle connection 4 5 breath gas analysis 5 2 5 24 5 26 II Finnigan GasBench II Operating Manual browser tab 3 16 bubble flow meter 4 5 bulk sediment 6 2 bulk volume 3 32 bulkhead connection 2 16 4 5 6 2 6 6 7 2 bulkhead union 6 14 C CaCO 5 6 to 5 7 6 2 calcite 5 6 6 2 calibration 3 3 3 9 4 14 5 13 5 34 7 14 capillary feedthrough 2 15 capillary port 3 5 to 3 6 capillary tubing 7 17 7 19 carbon dioxide 5 10 carbonate 1 3 2 13 2 18 3 35 3
34. Figure 7 3 pnm ID First Device s2 0 Sl 8 Figure 7 3 Plug and Measure Adapter pnm Adapter Thermo 7 8 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Technical Information Finnigan GasBench Il Capillaries 7 4 Capillaries Finnigan GasBench II contains two groups of capillaries 1 Capillaries that connect two points in the gas flow scheme e usually of size i d 0 32 mm e length not important 2 Capillaries that control flows e all the capillaries that start from the central gas distribution t piece belong to this group There are Two capillaries 0 1 500 that support the open splits with 2 ml min of He each Two capillaries 0 1 250 4 ml min of He to water trap One capillary 0 075 1000 for 0 5 ml min to measurement needle An exception is the column itself It acts as its own flow restriction 1 5 ml min Thermo gt ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Technical Information Water Traps Finnigan GasBench Il 7 5 Water Traps 2 E lheit x MS 1 4 12 6 IN 7 N 8 iS gt IN MID o ies Pos 5 je 0 02 m et ee 1 oben und ten 7 gleiche L g 8 9 Gegen Schmutz u Beschaedigung geschuetzt 13 Figure 7 4 Schematic of Water Trap Part No 100 2605 Table 7 3 Parts List Referring to Water Trap Figure 7 4 Part No 100 2605 Position PartNo Quantity Description 1 1004651 1 glass tube 2 100 4620 2 t piece 1 16 1 16 1
35. Font amp Print Gad wki Export Y Excel Export ASCII Export cut Bd Copy A Pasta Choose Calculate Calculate Results Regression Slope Regression Offset Note The standard deviation of the e g ten sample peaks internal error must be less than 0 1 for 8 80 and 3 C Thermo 4 8 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Basic Operations Finnigan GasBench Il Zero Enrichment Test Standard On Off Test Testing Reference Gas Inlet Ports If the Zero Enrichment test was unsuccessful check reference gas inlet ports e Check the dimensions of your fused silica reference gas capillary as shown in Open Splits on page 2 34 e Check the distances of your reference gas capillaries as they should be set up in Open Splits on page 2 34 Use the GasBench window as a part of the Accessories window 1 The functionality of all three fused silica reference gas capillaries can be tested a No bending shall occur b Transfer of reference gas if installed must be possible c Mechanical and air pressure movements must be possible 2 If la or 1b is out of order the following checks can be performed Warning Be careful not to cut any of the capillaries inside GasBench II a Loosen the upper straight connector screw of the reference gas capillary so that the capillary can be moved with ease b Take out the capillary c Cut off approximately 1 cm from the capillary d
36. I can be used alone In this case choose e GasBench In most cases however Finnigan GasBench II is used together with an autosampler that is the A200S sampler Note GC PAL and Combi PAL must be treated as A200S Thus mostly choose between e GasBench A200S Sampler e GasBench Acid Pump A200S Sampler e GasBench Precon A200S Sampler Different configurations will lead in turn to different corresponding methods The particularities in the tabs of the various possible methods will be described one by one now The GasBench Method If you use Finnigan GasBench II alone and therefore chose the GasBench set in the Configurator see Figure 3 24 the corresponding GasBench method results showing no particularity See Creating a New Method on page 3 17 The GasBench A200S Sampler Method If you use Finnigan GasBench I together with an A200S autosampler and therefore chose the GasBench set in the Configurator see Figure 3 24 the corresponding GasBench method will result See Creating a New Method on page 3 17 Finnigan GasBench Il Operating Manual 3 31 Isodat 2 0 Software Different GasBench II Methods Finnigan GasBench Il The GasBench Acid Pump A200S Sampler Method If you use Finnigan GasBench II in combination with an acid pump plus an A200S autosampler and therefore chose the GasBench Acid Pump A200S Sampler set in the Configurator see Figure 3 24 the corresponding GasBench Acid Pump A200S aut
37. Il Operating Manual Hardware Components Autosampler Finnigan GasBench Il 2 2 Autosampler 1 display and controls 2 heating unit with JUMO itron 16 temperature controller syringe carrier injection head syringe Sy HE u position of measurement needles u 7 sample tray Figure 2 4 Schematic of Autosampler A200S and Sample Tray Figure 2 5 Autosampler A200S and Sample Tray Thermo 2 4 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Autosampler Installing the Autosampler Note The x axis is the long axis at the autosampler whereas the y axis is directed forward and the z axis downwards respectively 1 Unpack the box containing the autosampler s components 2 Screw the autosampler s feet onto the base plate Note The base plate is not packed into the autosampler box but into the box containing GasBench II The feet however are packed into the autosampler box 3 Place sample tray and heating block onto the base plate Therefore the base plate has prefabricated cut outs where the heating block is simply inserted Due to its heaviness the heating block must not be fixed by screws underside 4 Unpack the temperature controller for the heating block The lid of the heating block needs to be screwed sideways onto the heating block by two provided kurled head screws Note In case of carbonate option a cut out must
38. Readjust the capillary in the straight connector Warning Avoid any blockage of the capillary e Check for the correct distances of the capillaries inside the reference open split f Tighten the capillary carefully until no movement is possible by hand anymore Warning Do not overtighten Check la and 1b If either of them is out of order pass again through all steps 2a to 2f Thermo ELECTRON CORPORATION Finnigan GasBench II Operating Manual 4 9 Basic Operations Linearity Test Finnigan GasBench Il 4 4 Linearity Test The mass spectrometers normally used together with GasBench II that is Delta DeltaPlus MAT 253 are not ideally linear This means that the measured 6 value depends on the actual peak height With each IRMS a certain slope is guaranteed e g 0 05 o V for the Delta series To check for this effect and to ensure proper operation the following linearity test should be performed from time to time Run a sequence using the method zero met While the method is running vary the reference gas pressure to obtain different peak heights for the various pulses Plot peak height versus 6 value for 13C and 0 respectively Determine the slope uae rea jan B Figure 4 5 Linearity Test Chromatogram co2 Error Extended Sequence Line Ampl 44 BOD 44 BOD 45 BOD 45 Area All R 45C02 44C02 d 130 12C d 180 60 mv mv mv mv va per mil per mil
39. acid drops may be deposited on the septa If so acid can enter the measurement needle and travel towards the valco valve Warning This must be avoided under all circumstances Severe damage to water trap and valvo valve will result Therefore refer to Acid Pump Adjustment on page 6 5 Handling Septa Ensure that the sample vials are screwed down correctly in order to be really closed left will not be leaktight e middle fits correctly e right will develop fissures and tends to be cut by the needle Figure 5 10 Correct Handling of Septa Condensation of Water beneath the Septa During equilibration when tray temperature is only slightly above room temperature water vapor condenses benath the septa This effect is unavoidable and usually poses no problem Once the septa have been punctured by the needle these water droplets accumulate to one large drop If now this particular vial will be measured again there is a significant chance to pick up this drop This results in water travelling towards water trap and valco valve possibly clogging the system Warning Therefore never measure equilibrated samples twice Thermo 5 18 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Carbonates Neogloboquadrina Pachyderma Ehrenberg 1894 Left coiled specimen umbilical view scale bar 0 1 mm Right coiled dextral specimen umbil
40. and ASCII Name the export file ech Pre Post Acarssiton Excel xls VW Auto Enum Export Printout Format Excel xls Modity Template List Decide whether you want a printout Capon fae Hamo _Pre Post Export If so choose between one printout per sample or per sequence Printout Resutwokshop Templates C No 1 Printout Sequence Properties Yez 1 Printout Sample Type an arbitrary comment applied m Properties ur j to all result files in this sequence r Sequence Scripts Sequence Scripts Pre Script an Select an ISL script isl to be executed before and after the Post Script m sequence Cancel Finally confirm by OK Figure 3 28 Defining Parameters for Results Export Printout and Sequence Scripts e Ifan error message indicates low memory close other applications The measurement will be started Refer to Measurement Procedures for Real Samples on page 5 1 Thermo 3 38 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il FileBrowser Figure 3 29 File Browser lun Carbonates seq 2 Equitbration seq a Flush Fil seq Ze A H2_zero seq Thermo ELECTRON CORPORATION Isodat 2 0 Software Creating a New Sequence Predefined Sequences as Examples For the sake of simplicity predefined sequences can be selected via the File Browser Use them only as examples It would even be sufficient to deliver only one or at most two such
41. and a mixture of helium and CO as the sample gas passes to GasBench II Note The vials on the positions 1 9 are neither filled with carbonates nor with acid but they will be flushed with He These vials are used as dummies for the sampling needle while the acid needle is dosing the phosphoric acid in vials 9 to 16 The analysis pathway follows the positions 1 4 9 12 17 20 and so on This defines a reaction time four times as large as the acquisition time for a single sample Refer to Figure 5 2 Figure 5 6 Figure 2 15 and Creating a New Sequence on page 3 34 If everything operates successfully you should receive a result chromatogram for each sample that looks like the one shown in Figure 5 4 Formation of carbon dioxide from limestone When dropping water free phosphoric acid upon limestone i e calcite or aragonite phosphates of calcium carbon dioxide and water will be formed Possible reactions are 3 CaCO 2 H PO gt Caz PO4 3 H O 3 CO CaCO 2 H PO gt Ca H PO H20 CO CaCO H PO H O gt CaHPO 2 H 0 CO Notice that water is formed in each step Thermo 5 8 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Carbonates Results of a Carbonate Measurement te Name Ciinnigan isodat NT GloballWrer iGas Bench Resuts acgusition_09444 7 000 1 01 400 Time x Figure 5 4 Carbonate Measur
42. and filled into a He CO tank Open the He CO tank connected to the flush gas input Increase the pressure to result in a flow of the He CO mixture of approximately 100 ml min 150 ml min at the vent of the flush needle When using a new gas mixture wait for 10 15 min until all the lines are completely filled with this new mixture i e until it is ensured that the former gas mixture has been completely exchanged with the new one Note The flush needle is sometimes synonymously called flushing needle rinsing needle or filling needle Accordingly one speaks of flush valve and flush connection Ensure that the flush needle is properly mounted in the autosampler Depending on your hardware use the flush sequence or the double needle flush sequence to fill the vials automatically Refer to Creating a New Sequence on page 3 34 Close the He CO mixture tank when the flush sequence is finished Wait for approximately 18 h for proper equilibration Start measurement sequence See Creating a New Sequence on page 3 34 Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Water Equilibration 180 0 5 CO in He i screw cap 200 ul aqueous sample 2 SEDA sedan H d PA into the vial wh e fushieg inte the autosampler tray AN vials are automatically Bushed O transfer from He CO H O into CO i
43. as the retractable sampling capillary of the IRMS A third capillary protection capillary delivers a constant stream of dry helium which purges the exit volume of the open split at any time OUT position The gas from the protection capillary mixes with the sample flow The IRMS capillary sniffs the diluted sample stream IN position The IRMS capillary is moved to the bottom of the open split The IRMS capillary sniffs the sample stream eluted by the capillary that comes from the second water trap Note Notice a difference between GC applications and GasBench applications In case of GC applications the mass spectrometer capillary is completely decoupled from GC In case of GasBench applications however only partial decoupling occurs Finnigan GasBench Il Operating Manual 2 37 Hardware Components Open Splits Finnigan GasBench Il Thermo 2 38 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Thermo ELECTRON CORPORATION Chapter 3 Isodat 2 0 Software 3 1 Starting Isodat 2 0 3 2 Creating a GasBench Configuration 3 3 Acquisition Mode 3 4 Accessories Bar 3 5 Creating a New Method 3 6 Different GasBench II Methods 3 7 Creating a New Sequence 3 8 Excel Export 3 9 Autosampler Programming Finnigan GasBench Il Operating Manual 3 1 Isodat 2 0 Software Starting Isodat 2 0 Finnigan GasBench Il 3 1 Starting Isodat 2 0 e After installing Isodat 2 0 st
44. axially inside a glass tube This glass tube and therefore the outer surface of the Nafion tube is constantly kept dry by a He flow of approximately 8 ml min Due to the water gradient through the Nafion wall any water in the sample flow will move through the Nafion A dry He CO gas results which flows towards the Valco loop He H O He He flow 8 ml min e HO vr HA He f 2 A A A u ae a ee He CO COS H O H O_ Mo 2 Ho U l J 0 5 ml min glass tube Nafion Figure 2 21 Schematic Online Water Removal Thermo ELECTRON CORPORATION Finnigan GasBench II Operating Manual 2 21 Hardware Components Principle of Valco Eight Port Valve Finnigan GasBench Il 2 9 Principle of Valco Eight Port Valve 1 compressed air control 2 long shank allows to introduce the functional head into the oven as head and control are thermally separated by the distance 3 functional head consists of a mounting plate 3a a n port 3b and a chequered knob on top 3c The chequered knob must be unscrewed if you want to withdraw the rotor After inserting the rotor screw in the chequered knob again Figure 2 22 Valco Eight Port Valve Side View LOAD mode The Valco eight port valve is used in a six port setup LOOP Two ports are in standby for each injection mode OUT 1 Load Mode e Ports 1 and 8 are in standby e The sample flow He CO purges the sampling loop e g 100 ul
45. be rasped at the right rear edge of the lid The cut out will be used as feedthrough for the acid line of the acid reservoir Usually this is performed by a service engineer 5 Take out the z arm 6 Mount the x axis guidance upon the feet and fasten it there using a torx screwdriver Three torx screwdrivers are provided together with the autosampler 7 Unscrew the retaining screws out of the y arm 8 Attach the z arm at the y arm To fasten the z arm move the plunger entirely downward as this allows accessing the eyelets 9 Remove the protective faceplate from the z arm This allows to plunge in the syringe from the front side later on Note When the autosampler is switched off e g during installation here in most cases the plunger falls completely down and can then be moved freely However the plunger cannot be moved when the autosampler is switched on Torx Screwdrivers Provided with the Autosampler e 360 T 10 80 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 5 Hardware Components Autosampler Finnigan GasBench Il e 360 T 20 100 e 360 T 25 100 Connecting the Autosampler Warning Never unplug or connect any cables while the autosampler is switched on This may lead to damage of the autosampler Note for Service Engineer Part No of replacement fuse is 114 1420 1 Connect the serial cable of the autosampler to the serial port COM 1 of your computer 2 M
46. holder 2 18 to 2 19 6 2 to 6 3 7 19 double needle setup 5 6 5 8 drying chamber 5 5 3 5 35 Thermo ELECTRON CORPORATION drying stage 5 3 dual trap application 6 12 to 6 13 dual trap version 6 7 6 12 to 6 13 E electrical security 2 29 electron energy 5 36 to 5 37 electron energy control 5 36 to 5 37 electron impact 5 37 elemental analyzer 3 21 enable auto dilution 3 21 end slope 3 26 equilibration 2 13 3 35 3 50 5 2 5 4 5 30 equilibration measurement 3 9 3 39 equilibration sequence 5 26 equilibration technique 5 4 equilibration seq 3 39 to 3 40 5 26 error margin 2 13 error message 3 9 3 36 3 38 error tracking 3 20 ethanole 5 4 evaluation 3 27 evaluation tab 3 19 3 25 evaluation type 3 25 Excel export 3 15 3 41 excess gas 5 4 excess pressure 4 4 excess pressure section 4 4 exetainer 2 16 4 13 to 4 14 exetainer vial 4 14 5 30 exhaust capillary 4 5 exhaust connection 4 5 4 13 exit volume 2 37 explosion 2 14 export file 3 38 export tab 3 15 export template 3 15 external error 4 6 extra script 3 21 F f value 3 28 F1 3 43 to 3 45 F2 3 43 F3 3 43 to 3 45 F4 3 43 face mask 5 16 factor f 3 28 fake mode 3 9 fan 2 2 ferrule R 7 3 ferrule V 7 3 Field F H 5 37 file browser 3 10 3 13 to 3 14 3 18 3 39 4 14 5 28 file manager 3 16 file search 3 16 fill grid with data command 3 36 fill speed 3
47. i 8 o i 8 i f Figure 2 37 Principle of Reference Gas Introduction Principle of Reference Gas introduction e leftside reference gas on e rightside reference gas off To inject a reference gas the corresponding reference capillary moves to the bottom of the open split interface see Figure 2 37 The reference gas e g COs is then mixed with the 4 ml min He flow Now 0 25 ml min of this He CO mixture is transferred to the IRMS resulting in a rectangular shaped reference gas pulse The width of this pulse e g 20 s is defined by the time between injecting and removing the reference gas capillary Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 35 Hardware Components Open Splits Finnigan GasBench Il Sample Injection and Dilution vg Figure 2 38 Sample Inlet Open Split IRMS IRMS 0 1 1500 0 1 1500 actuator actuator He He 0 1 500 0 1 500 j y s A Water Trap 2 Water Trap 2 0 3 200 0 3 200 Figure 2 39 Sample Injection and Dilution Thermo 2 36 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Hardware Components Open Splits Principle of Active Open Split e left side no dilution e right side dilution active The transfer of the sample stream into the IRMS is achieved via the open split The capillary that leaves the second water trap enters the open split interface as well
48. including e g an autosampler an acid pump or a PreCon Finally basics of autosampler programming are discussed Chapter 4 Basic Operations describes several test routines e g leak check checking column flows zero enrichment test that is standard on off test linearity test and condition test The chapter ends pointing out how to start an automated sequence and summarizing Frequently Asked Questions FAQ Chapter 5 Measurement Procedures for Real Samples deals with carbonates Dissolved Inorganic Carbon DIC breath gas analysis CO in atmospheric concentrations and water equilibration 180 and H D respectively Chapter 6 Options describes carbonate option and cryo traps option Chapter 7 Technical Information outlines test instructions auxiliary parts and mechanical parts It provides technical information about the capillaries in use and compressed air supply as well Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual vii Read This First Changes to the Manual and Online Help Finnigan GasBench Il Changes to the Manual and Online Help To suggest changes to this manual or the online Help please send your comments to Thermo Electron Bremen GmbH Finnigan Advanced Mass Spectrometry Barkhausenstr 2 D 28197 Bremen Germany You are encouraged to report errors or omissions in the text or index Thank you Thermo viii Finnigan GasBench Il Operating Manual ELECTRON CORPORATION
49. intensity ratio of the three peaks is 1 2 4 e contains ions of m z 28 m z 32 and m z 40 e appears around magnet current values of approximately 7800 steps 8500 steps and 9700 steps respectively e maximum intensity for m z 40 is 30 mV e intensity ratio of the three peaks is 4 1 0 7 Thermo 4 3 ELECTRON CORPORATION Finnigan GasBench II Operating Manual Basic Operations Leak Check Finnigan GasBench Il 4 4 e contains ions of m z 28 CO and m z 44 CO e appears around magnet current values of approximately 7800 steps and 10300 steps respectively e intensity of m z 44 must be less than 50 mV e the CO portion can easily be confused with nitrogen from air If air appears in the spectrum check the IRMS for leaks e g by using argon from a tank In case of a too high water level heat out the IRMS using the source heaters for at least 12 hours When a high water level is present in the source usually some air is leaking into the mass spectrometer as well Once this check has been performed within the given limits open the inlet valve and repeat the mass scan If air appears in the spectrum again check all gas connections at GasBench II for air leaks Do not forget to check all connections under excess pressure as they may leak too The best way to find leaks in the excess pressure section is to use a standard soap solution e g SNOOP which is applied to the connectors Small bubbles appear when gas
50. reference samples that is working standards by plotting the measured value for 80 and BC amp versus peak area or peak amplitude meas The correction factor ea must be evaluated from absolute standards IAEA For an explanation in detail see Referencing versus VPDB on page 5 13 To achieve proper results you need to include working standards in your sequence of measurements It is absolutely necessary to keep all possible sources of fractionation constant during the sequence The reference samples Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Carbonates that is working standards should be well distributed in the sample tray To get a proper estimate for the slope sample amount should vary Furthermore this procedure allows quality control during the entire data acquisition Referencing versus VPDB All carbonate 6 values must be referenced to the international standard VPDB Vienna Pee Dee Belemnite the successor of PDB as PDB is exhausted However VPDB with 513C 0 and 8130 0 as one would expect does not exist Instead standards exist which are related to this virtual that is unreal definition See Table 7 6 Note See Reference and intercomparison materials for stable isotopes of light elements In IAEA TECDOC 825 IAEA ed Vienna 1995 At present there are a couple of primary standards available from IAEA and NIST
51. respectively with given 6 values for 180 and C To determine the actual value of a sample relative to VPDB measure standard and sample under the same conditions and perform the following procedure e Determine the 6 value of your working standard e Calibrate versus known standards supplied by IAEA or NBS e Use a primary standard to determine the value of the reference gas e With x meaning working standard and z denoting VPDB the following equation is valid refer to Remark on the Strange Mathematics of Delta Values on page 5 15 x i y Ss 8 8 2 1000 y 2 and by 4 OF with X working standard y gas z absolute standard that is VPDB Thermo Ber ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il IAEA accepted vales measured cakubted IAEA accepted vales calculated BU 4130 1 136 03003 12673 12828 16825 24 357095 Dets SHK POB Dele SHK Ge Deta SHK PDB DAtSHK G3 SHK 1 70 1750 4 485 Delta Gas PDF Delta Gas S TF b DebG gt PDB HB daticassHR gt Ca 197309001 A 1903972041 THH MN 2828339314 NES 18 4 08 4268 302 2 9 15457 23 000423 0 03 0 067 NES 19 1 90 47 19 Figure 5 8 Calculation Example Figure 5 8 is an example for obtaining values specified against VPDB starting from measured and corrected 6 values 1 Determine absolute value of primary standard In this exam
52. setup 2 22 slot 6 3 SNOOP 4 4 soap sud 2 14 4 5 solid phase 5 2 source heater 4 4 source region 4 3 spare part 7 2 speaker 2 6 specific gravity 5 17 split in column 5 29 square peak 3 27 to 3 28 3 27 SSH 3 25 stainless steel capillary 6 7 to 6 8 stainless steel column 2 26 stainless steel ferrule 2 23 stainless steel micro packed column 2 27 stainless steel trap 6 12 to 6 13 standard 3 25 4 8 4 14 5 13 5 23 standard database 3 25 standard deviation 3 26 4 6 4 8 standard flow condition 3 22 standard gas tank 2 13 standard on off test 4 6 standard peak 3 25 standard setup 5 4 standard soap solution 4 4 standby mode 3 21 start slope 3 26 statistical error limit 5 12 status bar 3 8 to 3 10 3 20 stop bit 3 51 stroke 3 12 to 3 13 stroke button 3 13 subtree 3 44 supply line 1 3 supporting screw 2 19 swagelok type connector 1 3 switch method column 3 22 switch to column 3 21 sync signal 3 45 syringe 2 4 3 45 3 50 4 13 5 23 syringe carrier 2 4 2 6 syringe needle 2 19 T t piece 2 15 7 2 7 19 temperature control 5 31 Thermo ELECTRON CORPORATION Finnigan GasBench Il Index temperature drift 5 31 temperature regulator 4 13 temperature stability 5 3 5 31 test mixture 4 6 test protocol 3 3 test sample 4 13 to 4 14 test tube 5 16 7 3 thermal mass 5 31 thermocouple 2 26 7 19 thermodynamic mechanism 5 4 third reference inlet 7 16
53. step down further into the parameter tree To inspect the subtrees locate the highlighted bar above the menu entry using the dial and press the center knob on the dial e To access some more critical parameters press F3 and the center knob simultaneously e To locate all parameters of the object tray holders follow the path given below Thermo 3 44 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Autosampler Programming Menu FI Methods Utilities Logfile Info Setup F3 bh Ident Access Sounds Time SYSTEM SERVICE Objects Vials SYRINGES TRAY TYPES Tray Holders Trays Wash Stations Injectors VALVES AGITATORS POSITIONS PATHS Sync Signals Out Signals Events e ESC command leads you back to the previous menu Press it repeatedly to go back to the main menu e Home command directly leads you back to the main menu mostly F4 Finnigan GasBench Il Operating Manual 3 45 Isodat 2 0 Software Autosampler Programming Finnigan GasBench Il e Stop command stops the autosampler during operation E g when a sequence is being performed in Isodat 2 0 the autosampler is running and can only be stopped by the Stop command Note Enter is the center knob on the autosampler s dial If you press Enter alone that is without F3 you only get access to the entries that are not uppercase The add
54. stored RE a Flush Fal met 05 07 03 16 49 37 01 24 01 19 05 42 A E a H2_zero met 05 07 03 16 49 37 05 22 01 15 13 24 Do not mix them up A O A zero met 05 07 03 16 49 37 01 24 01 19 06 08 with the predefined a methods in the folder rl Examples e Double click on your example method of choice e g Acquisition met Figure 3 10 File Browser Displaying Predefined Methods for GasBench Il Instead of double clicking on the example method of choice drag and drop it to the Isodat Acquisition window right to the File Browser The example method will be displayed Proceed with Structure of GasBench Related Methods on page 3 19 Select between the following example methods e Acquisition 630s met considerably faster than Acquisition met requires the column to be pre heated to 70 C e Acquisition met lasts longer than 1400 s no longer recommended as it is an older version first basis method of GasBench used at ambient temperature e Flush Fill met for flushing the samples prior to measuring them that is during their preparation e H2 zero met for zero enrichment of hydrogen Thermo 3 18 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Isodat 2 0 Software Creating a New Method e Zero met to test the basic functions of the IRMS The reference gas is just switched on and off several times e g 10 or 100 pulses and one watches the obtained result The more pulses you apply th
55. the Low Voltage Directive Designed manufactured and tested in an ISO9001 registered facility this instrument has been shipped to you from our manufacturing facility in a safe condition Caution This instrument must be used as described in this manual Any use of this instrument in a manner other than described here may result in instrument damage and or operator injury Identifying Safety Information This reference manual contains precautionary statements that can prevent personal injury instrument damage and loss of data if properly followed All statements of this nature are called to your attention through the use of bold type and the following icons AAAAA Warning Cold Surface Hot Surface Strong High Voltage Magnetic Field Every instrument has specific hazards so be sure to read and comply with the following precautions They will help ensure the safe long term use of your system 1 Before plugging in any of the instrument modules or turning on the power always make sure that the voltage and fuses are set appropriately for your local line voltage 2 Only use fuses ofthe type and current rating specified Do not use repaired fuses and do not short circuit the fuse holder 3 The supplied power cord must be inserted into a power outlet with a protective earth contact ground When using an extension cord make sure that the cord also has an earth contact Finnigan GasBench Il Operating Manual a S
56. the tray To ensure proper closing of the tray cover a small cut must be made at the edge of the cover using a file Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Options Carbonate Option e Connect the acid needle tubing to the acid pump see Figure 6 4 and place the needle in the double needle holder on the right side See Figure 2 18 e Place the sampling needle in the left slot of the double needle holder Acid Pump Figure 6 1 shows the switches that have been deactivated by Thermo Electron Bremen in the modified version Direction and volume pumped per stroke are accessed externally via an additional device TO CHANGE PUMP RATE WITHIN RANGE TURN CONTROL RING CLOCKWISE FOR DECREASE COUNTERCLOCKWISE FOR INCREASE TO CHANGE PUMPING RANGE DISCONNECT POWER PLUG FROM OUTLET REMOVE COVER AND CHANGE BELT PULLEY ARRANGEMENT AS PER DRIVE PULLEY MODE DIAGRAM INSIDE CASE RESTORE COVER BEFORE REPLACING CORD INTO ELECTRICAL OUTLET TO PREVENT POSSIBLE ELECTRICAL SHOCK pase TY a Figure 6 1 Acid Pump Side View 1 control housing 2 adjusting screw important is used to adjust the volume pumped per stroke via its mark Refer to the calibrating instructions on top of the acid pump This volume pumped per stroke is then reported to Isodat 2 0 See also Instrument tab on page 3 19 3 head of pump within a polypropylene
57. two steps e The setting is precise enough if the jump finds 50 of peak intensity From now on the IRMS will always correctly jump to m z 2 and m z 3 Adjust Reference Signal Height e To achieve optimal performance it must be possible to set the reference signal height to 8 V Therefore it is necessary to cut the flow restricting capillary by 30 from its original length Note Ask your service engineer upon installation of GasBench II to do this Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Water Equilibration H D Referencing versus VSMOW When performing water equilibration with its larger error bars and accuracy requirements compared to carbonate measurements it is possible to use a simplified calculation scheme Note Refer to Nelson S T A simple practical methodology for routine VSMOW SLAP normalization of water samples analyzed by continuous flow methods Rapid Communications in Mass Spectrometry 14 1044 1046 2000 John Wiley amp Sons Ltd This eliminates the need to worry about the water to gas fractionation factor a as well as using the complicated 6 value equations explained in Remark on the Strange Mathematics of Delta Values on page 5 15 Assume you measured the following values for the two primary standards VSMOW and SLAP and one sample GISP measured value accepted value IAEA VSMOW 650 0 SLAP 757 4
58. 0 11 58 39 401 1 342 4 dummy sample 0 17 38 39 532 2 523 9 CaCO3 Merck 100 12 53 30 292 12 049 10 CaCO3 Merck 41 3 63 29 885 12 154 11 CaCO3 Merck 39 3 57 30 083 12 219 12 CaCO3 Merck 112 9 96 30 333 12 171 17 CaCO3 Merck 77 7 18 30 198 12 070 18 CaCO3 Merck 188 19 02 30 350 12 054 19 CaCO3 Merck 80 6 29 30 193 12 192 20 CaCO3 Merck 34 3 42 30 196 12 277 25 CaCO3 Merck 72 6 82 30 199 12 296 26 CaCO3 Merck 139 13 63 30 340 12 230 27 CaCO3 Merck 176 15 19 30 381 12 170 28 CaCO3 Merck 147 15 11 30 390 12 107 33 CaCO3 Merck 38 3 16 30 155 12 250 34 CaCO3 Merck 78 6 52 30 316 12 386 35 CaCO3 Merck 142 12 93 30 374 12 208 36 CaCO3 Merck 67 5 78 30 330 12 373 41 CaCO3 Merck 36 3 69 30 356 12 370 42 CaCO3 Merck 48 5 14 30 130 12 157 43 CaCO3 Merck 12 0 51 29 484 12 100 44 CaCO3 Merck 311 32 57 30 449 11 849 49 CaCO3 Merck 52 5 29 30 501 12 250 50 CaCO3 Merck 303 32 99 30 394 11 827 51 CaCO3 Merck 48 4 06 30 289 12 235 52 CaCO3 Merck 26 2 14 30 309 12 211 57 CaCO3 Merck 143 13 47 30 474 12 196 58 CaCO3 Merck 108 10 79 30 437 12 205 59 CaCO3 Merck 48 2 55 30 292 12 346 60 CaCO3 Merck 201 9 84 30 445 12 097 65 CaCO3 Merck 21 1 58 30 411 12 387 66 CaCO3 Merck 57 5 64 30 323 12 340 67 CaCO3 Merck 250 25 03 30 474 12 035 68 CaCO3 Merck 235 24 41 30 511 12 031 73 CaCO3 Merck 86 9 23 30 441 12 149 Figure 5 6 Raw Data Example to Illustrate Linearity Correction If you p
59. 0 5260 9 070 3780 6 10 Designation lift cylinder C85KN hub 250 mm reducer R1 8 M5 gasket 8 5 tubing nozzle Finnigan GasBench Il Operating Manual Finnigan GasBench Il Cryo Trap Option Version with One Trap Part No 112 1300 Quantity 1 2 10 8 Thermo ELECTRON CORPORATION Options Finnigan GasBench Il Cryo Traps Option Table 6 3 Parts List Referring to Figure 6 7 Part No 112 1300 Position PartNo Designation Quantity 10 049 3621 wire end sleeve for compressed air tubing AE 101 12 116 9570 installation kit for cryo trap option 1 19 106 8510 valve 5 2 way 1 20 052 1860 muffler M5 2 21 101 5830 silicon tubing 1 0 1 75NF 3 22 046 0560 nut M8 DIN 934 1 4301 1 23 047 0070 disc 8 4 DIN 125 1 24 045 1440 screw M5 10 DIN 963 9 25 047 0050 disc 5 3 DIN 125 1 4301 9 26 046 0590 nut M5 DIN 934 9 27 113 0741 screw M6 16 DIN 7991 4 28 047 0060 disc 6 4 DIN 125 4 29 046 0520 nut M6 DIN 934 4 42 045 4980 screw M3 10 DIN 963 2 Connecting Cryo Trap Sample In Sample In Figure 6 8 Fused Silica Trap Connection Thermo a ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Options Cryo Traps Option 6 12 Finnigan GasBench Il Notes for GasBench Il Trapping System Installation Note GasBench II can either be equipped with e a single trap system or with e adual trap system The single trap system serves as a cryoge
60. 28 GISP 697 189 73 Plot the measured 6 values versus the accepted values IAEA as given in the example below amp E g o y 3 9987x 2598 5 IAEA accepted value 3 Measured Value Determine a trend line that fits the two primary standards in this case Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 35 Measurement Procedures for Real Samples Water Equilibration H D Finnigan GasBench Il accepted value IAEA 3 99 measured value 2598 5 From this equation deduce the accepted values of the samples In this case GISP would yield a value of 188 59 which is fairly good compared to the accepted value given above Adjusting Electron Energy If the ionization energy electron energy is set to above 100 eV doubly charged He ions that is He are formed in the ion source Since they have a significant mass difference to H2 Am 0 5 their presence leads to peak shape distortion See Figure 5 30 Setting the electron energy below 100 eV considerably prevents He formation Peak Shape vs Electron Energy 6000 50 eV m z 2 eV mass 150eV mass2 50eV Amplitude mV 9 3 9 4 9 5 96 9 7 98 99 10 10 High Voltage kV Figure 5 30 Peak Shape Scan for m z 2 under Different Electron Energy Conditions 5 36 Finnigan GasBench Il Operating Manual Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Water Equilibratio
61. 30 7 19 069 1130 7 16 070 3780 7 16 074 3390 7 2 100 2605 7 2 100 4640 7 2 7 19 100 4850 7 2 7 19 100 6490 7 2 101 5830 7 16 104 0430 7 2 104 0480 7 2 104 0490 7 2 104 1730 7 2 104 1800 7 2 104 1860 7 2 104 4110 7 2 104 5480 7 2 7 19 104 8990 7 19 106 0170 7 2 7 19 106 1390 7 19 106 1410 7 19 106 8410 7 16 109 2481 3 7 to 3 8 3 10 3 15 3 17 4 14 to 4 15 5 34 111 2640 6 2 111 4260 7 15 7 17 111 4262 7 18 to 7 20 111 4290 7 19 111 4330 7 19 111 4340 7 19 111 4350 7 19 111 4360 7 19 111 6620 7 19 111 7410 7 19 111 9170 6 2 7 3 112 1070 7 2 112 1080 7 3 112 1170 7 2 112 3380 7 3 113 2471 6 2 113 6810 7 2 113 7020 7 3 7 19 113 7030 6 2 7 2 7 19 113 7070 6 2 Thermo ELECTRON CORPORATION 113 7080 2 19 6 2 7 3 113 7120 2 18 to 2 19 7 2 7 19 113 7301 6 2 113 7390 6 2 7 3 114 0790 1 3 114 1450 6 2 114 1460 6 2 114 7070 6 2 114 7090 6 2 115 49 90 3 7 115 4990 3 15 4 6 4 15 115 7620 6 2 116 8780 7 2 116 8790 6 2 7 3 13C 5 2 5 6 5 12 to 5 13 13c determination 5 2 180 1 3 5 2 5 6 5 12 to 5 13 5 32 189 determination 5 2 180 equilibration 5 31 205 2660 7 8 80 100 mesh 2 27 900 0342 7 2 7 19 A a factor 5 4 A200S autosampler 3 6 3 10 3 31 to 3 32 absolute standard 5 12 to 5 13 5 16 abundance 5 4 acceptance test 1 3 5 23 accessories bar 3 8 to 3 11 accurac
62. 6 3 180 160 1893 91 0 45 x 10e 6 7 55 50 6 V SMOW NBS 19 calcite 13C 12C 1 95 8 V PDB 180 160 2 20 8 V PDB 28 6 9 V SMOW intercomparison materials GISP water 2H 189 73 0 87 V SMOW 180 24 784 0 075 V SMOW NBS 18 calcite 13C 5 029 0 049 V PDB 180 23 035 0 172 V PDB IAEA CO 1 calcite 13C 2 48 0 025 V PDB 180 2 437 0 073 V PDB IAEA CO 8 calcite 13C 5 749 0 063 V PDB 180 22 667 0 187 V PDB IAEA CO 9 BaCO3 13C 47 119 0 149 V PDB 180 15 282 0 093 V PDB Calibrating versus international standards requires users to have their own speimens of Primary Standards Primary Standards are exclusively distributed by the IAEA via agencies in Europe and the US The reference list is taken from IAEA TECDOC 825 and the IAEA Analytical Quality Control Services Reference Materials Catalogue 2002 2003 Note Refer to e YAEA TECDOC 825 Reference and intercomparison materials for stable isotopes of light elements Proceedings of a consultants meeting held in Vienna 1 3 December 1993 International Atomic Energy Agency IAEA e Chapter 5 2 Environmental Level pp 55 in IAEA Analytical Quality Control Services Reference Materials Catalogue 2002 2003 First edition January 2002 Edited by Analytical Quality Control Services International Atomic Energy Agency P O Box 100 A 1400 Vienna u Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Technical Information Finnigan GasBenc
63. 7 3 Pligcand Measure Adapter dais 7 8 TAS Capillaries O EN 7 9 Tea E IS ia 7 10 7 0 Reference Open Planta ea obdlleeh aia a E eA 7 12 nk Sample Open Split emailen Eis nn EA Nieren 7 13 1 8 TAEA Primary Standards tx sis un Ru achicha ar an Rn BI an 7 14 1 9 lt Compressed Air Schematic ts sis sleet adic tates Ra ne IHR 7 15 The rmo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual V Contents vi Finnigan GasBench Il Operating Manual Finnigan GasBench Il Thermo ELECTRON CORPORATION Read This First Welcome to the Thermo Electron Finnigan GasBench I Operating Manual Finnigan GasBench II Operating Manual describes how to setup and use Finnigan GasBench II It includes the following chapters Chapter 1 Preinstallation Requirements summarizes requirements related to site power and the various gases in use before operating Finnigan GasBench II Chapter 2 Hardware Components treats autosampler installation sample tray and its temperature control gas supply measurement needle and flush needle water removal valco eight port valve GC oven and open splits Chapter 3 Isodat 2 0 Software describes how to start Isodat 2 0 and subsequently how to create a GasBench related configuration Then the chapter denotes how to create a new GasBench II method and a new GasBench II sequence in Isodat 2 0 s Acquisition Mode Various types of GasBench II methods are demonstrated as examples
64. 9 3190 right angle connection B 100 2 2 12 31 1068510 valve 5 2 way 1 32 108 3241 manifold standard 4 station 10 PO 2 39 1117410 ferrule FS1 3 Valco 2 50 106 8410 distributor for compressed air 1 9 fold M5 51 052 1320 tubing connection M5 3 52 050 5260 gasket 8 5 17 53 070 3780 tubing nozzle 11 54 049 3621 wire end sleeve AE 101 32 55 101 5830 silicon tubing 1 0 1 75 NF 3 56 069 1130 tubing 4 1 PU 4 5 57 052 1860 muffler M5 2 80 060 5470 capillary tube 1 16 0 8 mm 3 82 052 3460 t piece 1 16 B 100 3 3 84 900 0342 ferrule FS1 5 Valco 2 Thermo 7 4 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Technical Information Finnigan GasBench Il Mechanical Parts Table 7 2 Spare Parts for Gasbench Il Outdated Part No 111 4260 Position PartNo Designation Quantity 85 104 8990 capillary i d 0 10 mm fused silica 1 86 100 4640 capilllary i d 0 32 mm fused silica 2 64 m 87 056 6390 ferrule 1 16 GVF 005 10 88 106 0170 ferrule 1 16 GVF2 003 8 89 067 4910 capillary i d 0 10 mm fused silica 3 91 100 4850 ferrule 1 16 GVF 003 15 92 067 4930 nut SSNE 16 17 93 111 2650 soap bubble counter 10 ml 1 94 054 3380 capillary i d 0 05 mm fused silica 7 50 m 95 104 5480 capillary i d 0 075 mm fused silica 1 96 111 4290 line for gas supply GZG 4 98 111 4330 sample loop 50 ul Valco 1 99 111 4340 sample loop 100 ul Valco 1 100 111 4350 sample loop 250 ul Valco 1
65. Area All R 45C02 44C02 d 13C 12C d 180 180 E is mv mv mv mv vs per mil per mil vs VPDB vs VSMOW 0 0403999953 0 0083090401 z eas 20s 2501785750 3078 10051 95178 Joana _ Tammoo z s s oorrz7aa706 7 129 6 29 5 4822 312 6 768 3 051 0 050 95 06 0 0119849 0000000000 0 0000000000 fa 1005 205 243 200 6 703 2 108 10 121 04901 uormess onzos a2aso 010330557016 5 2305 205 asosora 6510 2 107 10 110 95104 0011938 oooasrezewo 00190322008 s_ 2002 203 22 250 6202 2208 10704 05000 00119925 00201343755 0 0967770605 sazss 0260 8217 10281 06 128 oorieeas 0 0003728079 o 0ar1ozozar 5207 10234 95001 o orisso oorososez20 ocaz02o0e76 ae25727 eco 9228 1020 05 170 001108 00005700020 00320800210 fears aeziaee 5000 9208 10250 05 132 00110048 _ 0000211615 0 05200050 Figure 4 4 Zero Enrichment Result Grid Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 4 7 Basic Operations Zero Enrichment Test Standard On Off Test Finnigan GasBench Il To obtain the standard deviation of all ten peaks e Click on the column header e g of the d 13C 12C per mil vs VPDB column It will be highlighted completely The same principle is valid for the d 180 160 per mil vs VSMOW column Qa Fill Grid with Data IM Columns ET Fit Cells to Grid e Right click on the column header Fit Cells to Text Tea U
66. C Column The GC column is now visible and consists of two parts e the functional part light yellow see 3 in Figure 2 34 It is the packed part of the column that is the plot part e the post column or pre column nearly transparent see 1 in Figure 2 34 The junction between both parts is established by a press fit and shown as 2 in Figure 2 34 Figure 2 32 Column Installed Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 29 Hardware Components GC Oven Finnigan GasBench Il Figure 2 33 Column with Blocked Ends Figure 2 33 shows the ends of the column which are blocked by silicon plugs e Cut the silicon plugs off using a capillary cutter Thereafter insert each end into its bulkhead connection at the left side of the oven see 1 and 2 in Figure 2 32 as follows e The bulkhead connection which is connected to the valco is intended for the inlet of the column It must be connected to the functional part of the column light yellow e As the outlet the post column must be connected to the bulkhead connection that is directed towards the water trap The water trap in turn leads to the diluter that is to the open active split The post column nearly transparent acts as a particle trap that is it prevents particles from reaching rear valves e Screw the Swagelok connection or valco connection on as follows e Insert the respective ferrule e Newly cut the capillary off
67. Finnigan GasBench Il Operating Manual Revision A 111 8342 Thermo ELECTRON CORPORATION F innigan is a trademark of the Thermo Electron Corporation Thermo Electron Bremen is part of the Thermo Electron Corporation Chrompack is a registered trademark of Varian Inc SNOOP is a registered trademark of the NUPRO Company Viton is a registered trademark of DuPont Dow Elastomers Teflon and Nafion are registered trademarks of the DuPont Company Swagelok is a registered trademark of the Crawford Fitting Company Valco is a trademark of VICI Valco Instruments Co Inc Microsoft Windows 95 Windows 98 Windows 2000 Windows NT and Windows XP are trademarks of Microsoft Corporation Technical information contained in this publication is for reference purposes only and is subject to change without notice Every effort has been made to supply complete and accurate information however Thermo Electron assumes no responsibility and will not be liable for any errors omissions damage or loss that might result from any use of this manual or the information contained therein even if this information is properly followed and problems still arise This publication is not part of the Agreement of Sale between Thermo Electron and the purchaser of a Thermo Electron system In the event of any conflict between the provisions of this document and those contained in Thermo Electron Terms and Conditions the provisions of
68. Finnigan GasBench Il Thermo ELECTRON CORPORATION Read This First Abbreviations Abbreviations The following abbreviations are used in this and other manuals and in the online Help A ampere ac alternating current ADC analog to digital converter AP acquisition processor APCI atmospheric pressure chemical ionization API atmospheric pressure ionization ASCH American Standard Code for Information Interchange b bit B byte 8 b baud rate data transmission speed in events per second C degrees Celsius CD compact disc CD ROM compact disc read only memory cfm cubic feet per minute CI chemical ionization CIP carriage and insurance paid to cm centimeter cm cubic centimeter CPU central processing unit of a computer CRC cyclic redundancy check CRM consecutive reaction monitoring lt Ctrl gt control key on the terminal keyboard d depth Da dalton DAC digital to analog converter dc direct current DDS direct digital synthesizer DEP direct exposure probe DS data system DSP digital signal processor Finnigan GasBench II Operating Manual ix Read This First Abbreviations Finnigan GasBench Il EI EMBL lt Enter gt ESD ESI eV f F Jasta file FOB ft FTP 8 G GC GC MS GND GPIB GUI HPLC HV Hz ICIS ICL ID IEC IEEE in VO k K KEGG kg electron ionization European Molecular Biology Laboratory enter key on the terminal keyboard electrostatic disc
69. LECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Read This First Typographical Conventions Typographical Conventions Typographical conventions have been established for Thermo Electron San Jose manuals for the following e Data input Boxed information e Topic headings Data Input Throughout this manual the following conventions indicate data input and output via the computer e Messages displayed on the screen are represented by capitalizing the initial letter of each word and by italicizing each word e Input that you enter by keyboard is represented in bold face letters Titles of topics chapters and manuals also appear in bold face letters For brevity expressions such as choose File gt Directories are used rather than pull down the File menu and choose Directories e Any command enclosed in angle brackets lt gt represents a single keystroke For example press lt F1 gt means press the key labeled F1 e Any command that requires pressing two or more keys simultaneously is shown with a plus sign connecting the keys For example press lt Shift gt lt F1 gt means press and hold the lt Shift gt key and then press the lt F1 gt key e Any button that you click on the screen is represented in bold face letters and a different font For example click on Close Finnigan GasBench Il Operating Manual xiii Read This First Typographical Co
70. Mathematics of Delta Values oonnooniccnnconoconocconnconnconcconnconononos 5 15 Phosphoric Acid Preparation sree e a a a e e a 5 16 Adding Phosphorous Pentoxide cassie nae a A R EE 5 17 Common Pta nie e a E E a a S ea E AET 5 17 Neogloboquadrina Pachyderma Ehrenberg 1894 cccccescssscesseesecsseeseeeseeetseeseeeseeees 5 19 5 3 Dissolved Inorganic Carbon DIC ccccecscesssesneeseeesceeseeesceeseeeseceseceseenaeseeceeeeeeeneeeeenseenas 5 20 Dissolved Inorganic Carbon DIC in Brief eeecccesseeseesseceeeeeseeeeeeseeeseesseeeeenseeaes 5 20 3 4 Breath Gas A SS A Ilka india ih me 5 24 Using the Autodiluter for Blanking eensnssennseenennennennnenennenene en 5 24 Results of Blanking 2 83 22 havea tvs ales deeds i eee en eee 5 25 Breath Gas Analysis in Brief ccccccccscesscssseesseesseeseeeseceseceseceeeaeeeseeeseenseeeseeeseeeseenseenaes 5 26 Results of Breath Gas Anal ysis c cccccccccssccsseesseeseeeseeesecesecsseceeeseeeseeeeeeseeeseeeseseseenseenaes 5 26 3 2 COs In Almosphenie Concentrallons an n ale 5 28 Editing a Method nc 5 28 Res llss A RON 5 29 5 6 Water Equilibration 180 RON 5 30 180 E uilibration im Briefe mnei a r aa 5 30 Sample Tray Temperature Control eesesssesseessnessnenneenneennennnnennennnennnnnneennennsnnnsennnann 5 31 Referencing versus VSMOW cccccccesssesscesssetseeseeesecesecnsecsecseecneecaeeeneeseeeeeeeeeeeeseenaes 5 31 Resol ii A cele Shat
71. Methods tab They cover all basic measurements Warning Take them only as a guideline but do not use them for measurements For measurements always create your own methods Sequences tab Refer to Creating a New Sequence on page 3 34 e Sequences contain the description of a sequence of single measurements methods Sequences can be programmed or changed by the user e Different sequences have been predefined covering all basic measurements in the Examples folder of the Sequences tab Warning Take them only as a guideline but do not use them for measurements For measurements always create your own sequences Warning You must create and save a new method and a new sequence on your own The predefined methods and sequences delivered by Thermo Electron Bremen in the Examples folders are only example files They only show guidance through helpful default values but must never be used for measurements Never overwrite an example file with a method or sequence created on your own Depending on your software version these examples may not work properly Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Accessories Bar Export tab e Edit voluminous amounts of GasBench II acquisition data for your own data systems using export templates cf LIMS e Refer to Excel Export in ISODAT NT Operating Manual Part No 109 2481 e Use ISODAT NT
72. Note It is recommended to check first whether the following toolbars that is dialog bars are activated Proceed as follows P Isodat Acquisition b File View Help The Acquisition window appears D m E e Right click on the title bar in its upper left New Open Save corner Accessories E amp Restore e Select Properties Nove Size Minimize 7 Maximize x Close AR F4 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 7 Isodat 2 0 Software Acquisition Mode Finnigan GasBench Il e Click on the Bars tab X Status Bar A 3 Tool Bars Mark the checkboxes of the bars you _ Script Bar want to be displayed X BasicBa en 3 Dialog Bars X Accessories lt q __ Information E Dialogs Help Dil amp Class Informations e Finally confirm by OK The bars will appear in the Acquisition Mode window Figure 3 3 Properties Box It is important to mark primarily the following bars e Status Bar e Basic Bar e Accessories Bar The individual bars mentioned in the box above are described in detail in the ISODAT NT Operating Manual Part No 109 2481 Thermo 3 8 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Accessories Bar 3 4 Accessories Bar To display the Accessories bar mark the corresponding checkbox in Figure 3 3 and confirm by OK e tis important that you have already created a Configurati
73. ORATION Isodat 2 0 Software Finnigan GasBench Il Different GasBench Il Methods Instrument Time Events Component Names Eyaluation CO2 Peak Detection C02 Printout C02 Experiment Continuous flow Configuration GasBench Il Precon 42005 Sampler Comment re Gasconfiguralion Acquisition Script PreCon Acquisition isl Furthermore notice the PreCon box on the Instrument tab PreCon Script 5 Script Variables Figure 3 26 Instrument tab PreCon Part The script that controls PreCon is integrated Specify its name and location The folder Finnigan Isodat NT Global ISL PreCon contains the following selection e Blank isl to perform blank measurements Precon test field isl used in our test field e Precon with autosampler isl to run PreCon in combination with the GC PAL belonging to Gasbench II e Precon isl to run PreCon in combination with GasBench II The Time Events tab additionally contains entries for all the components in PreCon e g valco valve and additional traps Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 33 Isodat 2 0 Software Creating a New Sequence Finnigan GasBench Il 3 7 Creating a New Sequence After creating and saving a method see Creating a New Method on page 3 17 a sequence must now be created as follows Warning As with methods you must create and save a new sequence on your own The predefined sequences delivered by Thermo Electron Bremen
74. RATION Technical Information Compressed Air Schematic Spare Parts for GasBench Il Actual Part No 111 4262 Figure 7 9 Quantity Designation 3m capillary tube 1 16 0 8 mm 4 ferrule 1 8 1 16 3 t piece 1 16 2 ferrule FS 1 5 Valco 3 3 m capillary 0 32 mm fused silica 10 ferrule 1 16 GVF 005 8 ferrule 1 16 GVF2 003 3m capillary 0 10 mm fused silica 1m capillary 0 10 mm fused silica 15 ferrule 1 16 GVF 003 17 nut SSME 16 7 5m capillary 0 05 mm fused silica 2m capillary 0 075 mm fused silica 4 gas line GZG 2 ferrule FS 1 3 Valco 1 sample loop 50 ul Valco 1 sample loop 100 ul Valco 1 sample loop 250 ul Valco 1 injection needle 1 acid needle 1 sample needle flush needle 1 double needle holder complete 1 GC GasBench Il 1 column 1 16 Poraplot Q 1 thermocouple type K 1 ribbed radiator Finnigan GasBench II Operating Manual Part No 060 5470 067 4790 052 3460 900 0342 100 4640 056 6390 106 0170 067 4910 104 8990 100 4850 067 4930 054 3380 104 5480 111 4290 111 7410 111 4330 111 4340 111 4350 111 4360 113 7030 113 7020 113 7120 111 6620 017 1911 106 1390 106 1410 7 19 Technical Information Compressed Air Schematic Finnigan GasBench Il
75. TION Finnigan GasBench Il Operating Manual 2 7 Hardware Components Sample Trays Finnigan GasBench Il Figure 2 8 Non Thermostated Sample Tray Side View Part No 111 2780 Figure 2 9 Non Thermostated Sample Tray Top View Part No 111 2780 However if temperature control is required for your application the thermostated sample tray Part No 111 2800 is used See Figure 2 10 When using this sample tray take into account that e itis optimized for carbonate measurement refer to Carbonates on page 5 6 e the delay between acid dosing and measurement is 1 hour Thermo 2 8 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Sample Trays e the acid reservoir is thermostated two columns can not be used Figure 2 10 Thermostated Sample Tray Top View Part No 111 2800 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 9 Hardware Components Sample Trays Finnigan GasBench Il Figure 2 11 Sampling Positions as Defined in the Tray 01 Object in the Autosampler Memory and Crosslink to Sequence Lines within Sequence Examples Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Sample Trays a autosampler position in sequence b row number in sequence carbonates c row number in sequence equilibration d double needle flush e flush fill
76. TRON CORPORATION Technical Information Sample Open Split Finnigan GasBench Il Table 7 5 Position Part No 5 104 1730 6 067 4580 14 070 3780 15 050 5260 16 067 4590 17 067 4930 18 100 4850 21 104 1860 2 104 1880 1 067 4900 22 045 0710 23 047 0090 Thermo ELECTRON CORPORATION 7 7 Sample Open Split 4 zu 21 22 23 12 15 10 I 3 7 8 ATA Vy W 3 1500 er lalala olas di Figure 7 6 Sample Open Split Part No 104 1760 Description outer glass tube at sample open split lift cylinder 8 25 SMC tube nozzle gasket 8 5 screw connection SSU16 16 nut SSNE 16 ferrule 1 16 GVF 003 inner glass tube as guide unit for capillaries of sample open split pipette micropipette 20 ul screw M 2 6 DIN 84 disc 2 5 DIN 125 Finnigan GasBench Il Operating Manual Parts List Referring to Sample Open Split Figure 7 6 Part No 104 1760 Quantity 1 1 1 1 2 2 2 1 1 1 1 1 7 13 Technical Information IAEA Primary Standards Finnigan GasBench Il 7 8 IAEA Primary Standards Table 7 6 IAEA Primary Standards Name Nature Isotopic 5 o Reference ratio standard V SMOW water 2H 1H 155 761 0 05 x 10e 6 1 0 V SMOW 155 751 0 08 x 10e 6 2 155 601 0 12 x 10e 6 3 180 160 2005 20 0 45 x 10e 6 4 0 V SMOW 170 160 379 91 0 8 x 10e 6 5 0 V SMOW SLAP water 2H 1H 89 021 0 05 x 10e 6 1 428 0 6 V SMOW 89 12 0 07 x 10e 6 2 88 88 0 18 x 10e
77. Toxicology U Research Institute U Energy A University College Q Food Agriculture U Veterinary A Forensic Toxicology A Other Pharmaceutical U Research Education A Other Job Function Check one only Administration Lab Management Operator Other oOo a a Reader Survey Help us to improve the quality of our documentation by answering a few questions Finnigan GasBench Il Operating Manual e o Strongly Strongly Agree Agree Disagree Disagree The manual is well organized 1 2 3 4 The manual is clearly written 1 2 3 4 The manual contains all of the information need 1 2 3 4 The instructions are easy to follow 1 2 3 4 The instructions are complete 1 2 3 4 The technical information is easy to understand 1 2 3 4 The figures are helpful 1 2 3 4 Additional Comments Attach additional sheets if necessary Tear this sheet from the manual fold it closed stamp it and drop it in the mail From Thermo Electron Bremen GmbH Finnigan Advanced Mass Spectrometry Product Marketing Barkhausenstr 2 D 28197 Bremen Germany 4 fold Place Stamp Here _ fold bereinstimmungserkl rung gem EN 45014 declaration of conformity according to EN 45014 Dichiarazione di conformit alla EN 45014 Name des Herstellers manufacturers name F innigan MAT GmbH nome produttore Adresse des Herstellers Barkhausenstra e 2 manufacturers address 28197 Brem
78. acquisition isl no matter to which application they belong e g GasBench II or ConFlo III However they are stored in separate folders that is in a GasBench II folder or in a ConFlo III folder Search tab e Allows to find any result files of data acquisitions by pressing the File Search button e Like a file manager it displays the results of a file search and allows to move files Browser tab e Ifa Result Workshop document is open this tab shows the objects that can be imported e g methods sequences results e A file manager that allows to browse to an arbitrary directory of your choice even to a root of a harddisk drive e As with other file managers files and folders can be created moved or deleted Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Creating a New Method 3 5 Creating a New Method Isodat 2 0 s Acquisition mode allows fully automated isotope ratio determination All parameters relevant for data acquisition of a sample are stored in a method The following steps are needed to create anew method Note For an extensive description of the options of the method definition refer to ISODAT NT Operating Manual Part No 109 2481 In this section only the entries that are specific for operating GasBench II will be described Warning You must create and save a new method on your own The predefined methods delivered by Thermo El
79. afety and EMC Information Identifying Safety Information Finnigan GasBench Il Do not change the external or internal grounding connections Tampering with or disconnecting these connections could endanger you and or damage the system Caution The instrument is properly grounded in accordance with regulations when shipped You do not need to make any changes to the electrical connections or to the instrument s chassis to ensure safe operation Never run the system without the housing on Permanent damage can occur Do not turn the instrument on if you suspect that it has incurred any kind of electrical damage Instead disconnect the power cord and contact a Service Representative for a product evaluation Do not attempt to use the instrument until it has been evaluated Electrical damage may have occurred if the system shows visible signs of damage or has been transported under severe stress Damage can also result if the instrument is stored for prolonged periods under unfavorable conditions e g subjected to heat water etc Always disconnect the power cord before attempting any type of maintenance Never try to repair or replace any component of the system that is not described in this manual without the assistance of your service representative Warning Avoid any contact of the system with liquids Permanent damage can occur due to high voltage e g leaking liquids might get into contact with electronic comp
80. ak center cycle and start of data acquisition e g 5 s Reference Device I Use Soripts Relerence Pos ee y Figure 3 13 Instrument tab Reference Device Part a Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Creating a New Method e Select the Reference Port to connect the reference gas to e g Reference 1 Reference l Reference 2 Reference 3 Choose between Reference 1 Reference 2 and Reference 3 as equivalent ports Refer to Connection Panel of Gas Bench II on page 2 15 e Always only one reference gas is used mostly CO However in case of hydrogen equilibration H is required as reference gas instead of CO3 Some applications need N as reference gas instead of CO gt Contrary to e g Elemental Analyzer applications where two reference gases are necessary no reference gas switches occur during GasBench II applications Therefore the Switch To column in the Time Events tab is empty e Mark the Use Scripts checkbox 4 UseSeripts to start an ISL script Gas Bench Transfer Time s 60 Enable Auto Dilution I Activation Amplitude mV 10000 00 Extra Script J ra Figure 3 14 Instrument tab GasBench Part e Transfer Time s is the time the autosampler needs to run from standby position to the vial and pierce at least 15 s GasBench Il is in Standby Mode during this period Note If additional time is needed between p
81. aps 1 id 0 32 mm V 80 ul m 2 id 1 0 mm V 780 ul m General Notes e Before releasing ferrules in the valco valve slowly reduce the He pressure in GasBench II to zero Do not forget to close the needle valve leading into the ion source before reducing the He pressure e The dual trap system serves as a cryogenic pre concentration unit for flows in the range of the GC column flow 0 5 15 ml min including a eryogenic focusing trap in front of the GC column e The cryofocusing trap is a fused silica trap 0 32 mm fused silica tubing from valco port C to port D for very sharp GC peaks It also serves as a mediator between high sampling flows and low GC flows the sample is dissolved in other gases Here the fraction that can be frozen out is collected from a bigger gas amount To collect this fraction completely high througputs through the trap are used during a long period of time e The cryogenic pre concentration trap is a nickel filled stainless steel trap inner diameter 1 mm connected from valco port C to port D e An application for one trap is given in CO in Atmospheric Concentrations on page 5 28 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 6 13 Options Cryo Traps Option Finnigan GasBench Il e Before releasing the ferrule in the bulkhead union in front of the GC column slowly reduce the He pressure in GasBench II to zero Do not forget to close the needle valve leading into the ion s
82. art it by a double click ey e Open the Configurator by a double click Configurator The Configurator window will appear i gt Welcome to ISODAT NT e This box only appears when starting the system the very first time or after Reset of the IRMS Select the MS altached to this Computer Available Isotope MS Types Select your particular IRMS e g DeltaP S XP OK Cancel e Confirm by OK Cup Settings x Indicate the installed cups Look whether the cups are ren Installed or Not Installed Look at the Peak Center option of the cups a e Look at the Resistor values Q of the cups a i 21212 HE 4144414 e Look at the Resistor 2 values Q of the cups 1 Thermo 3 2 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Starting Isodat 2 0 Refer to the delivered test protocol and compare it with your order Gas Configuration Editor Add Delete See se oe et Rc ee oe Te pe gt o ww p 7 a a ETC E C E er trent UB P 110102 B co 1108 Inthe Gas Configuration Editor check for your particular Configuration e g CO2 whether the masses are assigned correctly to the cups e Check Calibration Ratio Groups magnet position and Peak Center Offset The default values for magnet position are averaged experience values that cannot be checked and edited here but later on during calibration procedure The number of requir
83. ate Focus Delta GasBench window See The GasBench Window on page 3 11 File Browser The Status Bar displays the actual Configuration GasBench ll amp A2005 Y lt p c02 e g GasBench II amp A200S and the actual nn E En OO Gas Configuration e g CO2 Figure 3 4 The Accessories Bar Together with the Status Bar For detailed information about the components of the Accessories bar refer to ISODAT NT Operating Manual Part No 109 2481 FEN on Ther Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Accessories Bar Changing Visibility of its Components Change visibility of individual components of the Accessories bar as follows e Right click on an arbitrary title bar e g GasBench or Focus Delta Administrate Panel Mark the Administrate Panels button Accessories xj Dialog visibility Mark the information to be displayed additionally on the Accessories bar e g Focus Delta Object Properties ISL Scripts File Browser e Unmark the information not to be displayed on the Accessories bar e g ISL Scripts e Finally confirm by OK The GasBench window Figure 3 5 ap pears with any configuration containing a GasBench no matter whether an au tosampler or an acid pump or a PreCon device are additionally attached to it The GasBench window allows direct control of all GasBench II hardwa
84. atio Mass Spectrometry 1997 p 11 82 John Wiley amp Sons Ltd In all types of measurements the isotopic composition of a sample gas is compared to the isotopic composition of a reference gas GasBench II consists of a reference inlet system that allows to use three different reference gases Reference or Reference 2 or Reference 3 only one of them per measurement Refer to Instrument tab Reference Device Part on page 3 20 Usually CO and H are choosen to cover all applications mentioned above Reference gases are expected to be clean and stable with respect to their isotopic compositions For a gas tank that contains a liquid phase like CO this means absolute temperature stability The sample gas is fed into GasBench II by a specially designed headspace sampling needle By a helium overpressure the gas will be transported through the capillaries into GasBench II where a drying stage removes water from the sample gas mixture Otherwise it tends to clog the valco switching valve or the mass spectrometer inlet valve A portion of the sample gas Thermo T ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Measurement Procedures for Real Samples Introduction Finnigan GasBench Il mixture is cut from the continuous stream by switching the valco valve to the inject position The portion is injected into the GC column where a separation in time between CO and other gas components takes place To decoup
85. bout 2 kg of phosphorous pentoxide to obtain the required final specific gravity of greater than 1 92 This quantity of PO is gradually added over a period of 2 3 hours while constantly stirring and heating to a temperature of around 80 C The powder forms gelatinous lumps initially but will gradually dissolve The complete process can take 4 5 hours A few crystals of chromium dioxide that is approximately 0 5 g are added at the final dissolution stage Heating and stirring continues until all phosphorous pentoxide has dissolved The stirrer hotplate is switched off allowing the acid to cool down to room temperature before checking specific gravity If it is less than 1 92 the acid must be reheated and more P205 needs to be added Finally the acid which should be about 3 after P205 addition is stored in bottles until required Use Parafilm to seal the screw cap Common Pitfalls Retention Times first injection Second injection v4 ra third injection Figure 5 9 Upon Retention Times Combining Chromatograms Thermo ELECTRON CORPORATION Finnigan GasBench II Operating Manual 5 17 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il 1 Air peak precedes CO See 1 in Figure 5 9 2 Water peak may follow CO but must not interfere with CO See 2 in Figure 5 9 3 Additional peaks e g due to solvents must not interfere with CO Wasting Acid Due to improper adjustment of the acid pump
86. ch sample When running standards for acceptance tests a single syringe is sufficient Care must be taken to allow any ocean water to remain on the inside of the septum Note Wipe the outside of the needle prior to puncturing the septum When filling the flushed vial with ocean water do not puncture the septum in the center but close to the edge If samples are stored for a longer period that is for several months only use large sample amounts above 100 ml This avoids isotopic fractionation due to evaporation Carefully close the bottles using parafilm Avoid headspaces filled with air and store them in a cooler at 4 C To maintain water as a working standard stable in isotopic composition over a longer time it has been proven useful to store them in large canisters Use at least a 50 stainless steel barrel and vent it using only dry inert gas e g Np It is not dissolved in the water and thus the CO content will not change l Fill some drops of 98 H3PO about 30 ul into an empty vial See Phosphoric Acid Preparation on page 5 16 for its preparation Close the vial and place it in the tray Exchange the headspace that is via the needle He streams in and replaces the gas in the vial which in turn streams out of it Inject the sample about 700 ul through the septum into the closed vial using a syringe CO will be released from these different origins and will then be mixed with the helium in the headspace
87. column or a PoraPlot Q fused silica cap column A JUMO itron 16 temperature controller and a type K thermocouple guarantee stable isothermal conditions The opened right side panel of GasBench II shows the GC oven with the column See Figure 2 28 and Figure 2 32 GC box inside view GC column PoraPlot Q or HayeSep D thermocouple Figure 2 28 GC Oven Open 2 26 The GC column separates the different gas compounds released from the sample loop e g N and CO The compounds eluting from the GC column are transferred through the Nafion guard trap and via open split into IRMS Type PoraPlot Q GC Column This column type is used in the current versions of GasBench II and part of your equipment Warning Avoid fast pressure variations along the column A p lt 0 5 psi s Table 2 1 Properties of PoraPlot Q GC Column type fused silica column length 25m inner diameter 0 32 mm helium pressure 10 12 psi helium flow approximately 2 ml min GC column temperature room temperature that is 24 C Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il GC Oven Type HayeSep D GC Column This column type has been used in prior versions of GasBench Table 2 2 Properties of HayeSep D GC Column type 1 16 stainless steel micro packed column length 2m inner diameter 0 76 mm packing material polymer HayeSep D 80 100 mesh helium
88. d pumping the viscous concentrated phosphoric acid Follow the instructions on the acid pump housing Adjust the pumping volume until you obtain one drop of acid by every 10 pump strokes Use the manual switch at the pump to force a single stroke Wait between single strokes for at least 30 s These settings are a precondition for retracting the acid from the needle tip This also avoids spoiling the acid to the septum Note It may be useful to set a larger pumping volume during the initial filling of pump and tubing Warning Never use solvents to test the pump as the rubber made O rings might be destroyed For details about how to communicate this acid pump adjustment to Isodat 2 0 refer to Figure 3 6 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 6 5 Options Carbonate Option Finnigan GasBench Il Connecting the Acid Needle safety holder Figure 6 4 shows proper arrangement of O rings in the bulkhead connec tors to get a leaktight connection for acid nee 3 dle and reservoir tubing ee 4 y eel I En O i on ee gt a amy metal 7 Figure 6 4 Connecting the Acid Needle Thermo 6 6 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Options Cryo Traps Option 6 2 Cryo Traps Option Introduction The basic problem to deal with is that a very small sample has to be analyzed from a relative big gas volum
89. e Comment optional add an arbitrary comment concerning the particular sample Preparation optional add an arbitrary comment concerning sample preparation Method important the IRMS method edited in Creating a New Method on page 3 17 can be selected here from the pulldown list By selecting it here you determine the particular IRMS method to be used indeed during measurement Without a selection from the pulldown list no measurement will take place Instead the error message No valid method found in sequence grid will occur Note After you typed data in only one cell of the sequence grid easily fill each of its columns right click the column and choose the Fill Grid with Data command Ly Fill Grid with Data Saving a Sequence As done with a method see Saving a Method on page 3 29 after defining the new sequence you must save it before it will start Proceed as follows Warning The predefined sequences in the Examples folder are only example files They only show guidance through helpful default values but must never be used for measurements Never overwrite a sequence example file with a sequence you created Depending on your software version these examples may not work properly Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Save Command Save Save As Command E Save Pr Save All CT T E C FINNIGAN ISODAT NT GloballUser Gas Bench Example
90. e The Finnigan cryo option now renders this possible using the so called GasBench II cryo option Two different types of the cryo option can be delivered e single trap version comprising only one trap double trap version comprising two traps Within the single trap version either a stainless steel capillary or a fused silica capillary is used depending on gas flow and sample amount Both types of capillaries are used within the double trap version namely the fused silica capillary follows the stainless steel capillary The general idea of the cryo option is to obtain higher peak shapes by analyzing small samples in bigger gas volumes The cryo traps option contains an automated lever used to move a sample loop in and out of a dewar filled with a cooling agent to be supplied by the customer By filling the dewar with liquid nitrogen substances like carbon dioxide water methane or nitrous oxides can be frozen out trapped Via the proper timing it is possible to collect these substances in the trap and yield high amplitudes from low concentrations Principle of Operation A sample loop is formed from a portion of a3 m long piece of fused silica tubing The rest of the full length is used to connect the trap setup to the valco switching valve The complete scheme replaces the standard sample loop that comes with GasBench II According to the Time Event list of the method the trap is moved into liquid nitrogen LN2 at regular i
91. e acquisition Timing Considerations When setting up the Time Events list keep in mind the different transition times through the various components of GasBench II When moving a reference capillary into the reference split the gas travelling towards the IRMS almost instantaneously changes its composition However it takes about 5 s for the mixture to arrive in the source This is the time the gas needs to travel the capillary length When injecting a sample to the GC via the valco valve several factors influence the travel time of the gas to the IRMS Finnigan GasBench II Operating Manual 3 23 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il e First of all the flow velocity of the gas through the length of the GC capillary determines the required time The flow velocity in turn is determined by the helium pressure at the central helium control of GasBench II e Additionally the material of the actively separating part of the GC column causes different gases to travel at different velocities retention e Finally column oven temperature biases this time difference 10 00 9 000 8 000 j 7 000 f N 6 000 j f i 44 M 5 000 3000 4 4 000 y 2 000 4 1 000 4 0 000 ju UW Uv JW IN JU Ma r T time s 100 200 300 400 500 600 delay due to gas transport through inlet capillary Y 1 26 51 76 10 delay due to gas tran
92. e aragonite that is mainly CaCO3 or dolomite that is MgCO3 will be covered The latter is subject to a lot of discussion and results should be discussed carefully The idea is to react the carbonate species with phosphoric acid to yield CO that carries an image of the isotopic value of the carbonate ion CO3 Double Needle Setup Sampling Acid Dosing Sampling Acid Dosing Figure 5 2 Defining the Sequence Double Needle Setup The double needle setup allows acid dosing to one sample while measuring another one refer to Figure 5 2 Figure 5 6 and Flush Needle on page 2 18 While the right needle transports acid to a bottle filled with He the left needle takes sample gas from the headspace Thermo 5 6 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Carbonates Carbonates in Brief Place carbonate in oa Close vial and an open exetainer flush with He 3 i 4 Inject acid ld and equilibrate Run acquisition Figure 5 3 Sample Preparation for Carbonate Measurement Heat the tray to 72 C This will speed up the reaction between the carbonates that is mainly CaCO3 and phosphoric acid that is H3PO and shortens the time required to reach isotopic equlibrium Place 50 600 ug of solid carbonate containing sample e g dolomite calcite foram
93. e Introduce the capillary e Carefully tighten the ferrule until the capillary can no longer be pulled back Do not tighten the ferrules connections too strong Thermo 2 30 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il GC Oven Warning If you want to tighten the ferrule further it is absolutely necessary to perform a leak check first Only tighten it further if gas is still coming in after the leak test has been performed Act extremely carefully while opening and closing connections Do not tighten any Swagelok connection around the column too strong as this causes demolition Only connections made up by metal ferrules can be tightened strongly Normally the only connections to be touched by users are those of the column the loop and for installing a flush needle or a sample needle respectively Note For detailed information about Installation of the column in the GC Conditioning Storage and Description refer to Capillary Column Test Report by Chrompack It is part of your Chrompack capillary column Figure 2 34 Junction between Both Parts of the Column Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 31 Hardware Components GC Oven Finnigan GasBench Il Programming JUMO itron 16 Temperature Controller for GC Oven Figure 2 35 2 32 Jumo itron 16 Temperature Controller The temperature controller located at the s
94. e more exact the result Structure of GasBench Related Methods The following method is a GasBench Autosampler A200S method It corresponds to the GasBench Autosampler A200S configuration which results if you have selected the GasBench Autosampler 42008 set in the Configurator before Other GasBench related methods will be described in Different GasBench II Methods on page 3 31 All GasBench methods are organized by the following tab pages e Instrument tab Time Events tab e Component Names tab e Evaluation tab e Peak Detection tab e Printout tab In these tabs the currently active gas configuration is indicated e g Evaluation CO2 alludes to CO2 whereas Evaluation N2 alludes to N2 Instrument tab Instrument Time Events Component Names Evaluation C02 Peak Detection C02 Printout C02 Experiment Configuration Comment Gasconfiguralion an Seat Per default this field is empty Continuous How You can type in comments GasBench Il 42005 Sampler Method for fast 180 160 and 1 analysis of carbonates Main Scnpt C Finnigan User GasBench S cripts acquisition carbonates sct Time Events C Finnigan User GasBench Scnpts GB Carbonates Events lst tev Figure 3 11 Instrument tab Experiment Part Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 19 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il At Comment you can type in genera
95. e ten sample peaks of one sample It should be less than 0 05 o for all measurements This result is called internal error The external error is the standard deviation of the mean values of all measurements It should be less than 0 08 o for 5 8O and less than 0 06 o for 513C If this is obtained you are ready to measure carbonates see Carbonates on page 5 6 DIC see Dissolved Inorganic Carbon DIC on page 5 20 or water equilibration see Water Equilibration 80 on page 5 30 and Water Equilibration H D on page 5 33 Run a sequence using the standard on off method that is zero met Note The amplitude of m z 44 must be between 4 V and 5 V This refers to the cup having a resistor of 3 10 Q that is usually Cup 2 where m z 44 is measured under standard conditions All necessary information is given in the Gas Configuration Editor See Creating a GasBench Configuration on page 3 4 and ISODAT NT Operation Manual Upgrade to Version 2 0 Part No 115 4990 Thermo 4 6 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Basic Operations Finnigan GasBench Il Zero Enrichment Test Standard On Off Test File Name Meresgerviteodet TRETEN Berria O Or OF of Figure 4 3 Zero Enrichment Chromatogram Note If the capillaries got entangled the reference gas peaks shown in Figure 4 3 begin to differ in peak height Error Extended Sequence Line Rt Width Ampl 44 BGD 44 BGD 45 BOD 46
96. e the flow which should be between 1 and 1 5 ml min for normal operation During the removal of the capillary be careful when you tighten the ferrule Excessive force may lead to destruction of the ferrule or even the bulkhead connector at the GC housing Finnigan GasBench Il Operating Manual 4 5 Basic Operations Zero Enrichment Test Standard On Off Test Finnigan GasBench Il 4 3 Zero Enrichment Test Standard On Off Test Provided that GasBench II has no leak see Leak Check on page 4 2 the Zero Enrichment test and Linearity test see Linearity Test on page 4 10 can be performed using the standard acquisition scripts The final test for the overall performance of GasBench II and IRMS is the Zero Enrichment test also called Standard On Off test To perform it fill an arbitrary number of sample bottles with a test mixture of 0 3 CO in He and start an acquisition Use the acquisition method and printout templates supplied during installation of Isodat 2 0 A single result printout should look as shown below Check for each chromatogram whether the ratio baseline is flat Large peaks in the baseline of 44 46 just in front of each sample CO peak point towards air contaminating the sample Check whether the sample bottle was properly closed If in the intensity plot a peak larger than 100 mV appears just in front of the CO peak the result must be discarded In all other cases calculate the standard deviation o O gt of th
97. e to thermodynamic mechanisms The abundance of this isotopic dilution effect is described by a number usually denoted as a factor Note The a factor for HD is 4 00 and about 1 04 for CO from dissolved CO Refer to Friedman I and O Neill J R Compilation of stable isotope fractionation factors of geochemical interest Chapter KK in Fleischer M ed Data of geochemistry 6th ed 1977 U S Geological Survey Professional Paper 440 In equilibration techniques the gas to be measured is added to the headspace This requires the air in the headspace to be exchanged with He or a mixture of He and the gas to be analyzed It is assumed that after some time an isotopic equilibrium is reached between the gas in the headspace and the molecules in the liquid Only then the gas mixture can be analyzed In carbonate analysis the gas to be measured is released from the carbonate material by adding Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Introduction phosphoric acid A similiar idea leads to DIC measurements In both cases the air in the headspace must be replaced prior to the reaction by He which is inert and thus will not influence GC analysis Measurement timing must take into consideration the times reqired for the reactions mentioned above as well as the times the autosampler needs to perform its
98. echnical Information Spare Parts and Consumables for GasBench II Spare Parts and Consumables for GasBench Il Available as Kit with Part No 113 6810 Quantity Part No 1 2 N N N A A N gt 112 1080 112 3380 113 7020 052 0910 052 0940 113 7390 113 7080 111 9170 116 8790 Designation single use cannula PK 100 test tube rack for 72 samples measurement needle ferrule V 1 16 stainless steel ferrule R 1 16 stainless steel hollow nut with hole 1 16 needle holder knurled nut M8 sample vial washed Finnigan GasBench Il Operating Manual 7 3 Technical Information Mechanical Parts Finnigan GasBench Il 7 2 Mechanical Parts Table 7 1 summarizes important spare parts of the outdated version of GasBench II Part No 111 4260 Table 7 8 however lists important spare parts of the actual version of GasBench II Part No 111 4262 Table 7 2 Spare Parts for Gasbench Il Outdated Part No 111 4260 Position PartNo Designation Quantity 13 100 2605 water trap GC C III 2 14 111 3290 8 port Valco valve VICI 1 15 109 6570 reference open split 1 16 104 1760 sample open split 1 17 003 0960 fan 8550N Papst 1 18 003 1100 protective grating for fan 2 19 056 7350 coupling 1 16 B 100 61 5 20 067 4552 JUMO itron 16 temperature controller 1 21 028 1310 relay S0302 A210 1 22 052 4391 manometer 1 8 0 2 5 bar 4 23 074 3360 coupling 1 8 Rcx3M0 7 B 4 24 067 4880 pressure reducer 4 25 04
99. ectron Bremen in the Examples folder are only example files They only show guidance through helpful default values but must never be used for measurements Never overwrite an example file with a method created on your own Depending on your software version these examples may not work properly ER Open the Acquisition mode Acquisition e Select a Configuration for GasBench Il GesBench i amp A2005 Y applications e g GasBench IT amp A200S co 5 e Select the appropriate Gas Configuration lt p for the intended measurement type e g CO2 D Press the New button New Penn o S Sequence To create a new method mark Method DataExport A2005 Trace la le A AS2000 Peripheralvi ISL x Coma e Confirm by OK Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 17 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il The new method is organized in tab pages Proceed with Structure of GasBench Related Methods on page 3 19 where they are described in detail Predefined Methods as Examples For the sake of simplicity predefined methods can be selected via the File Browser Use them only as examples It would even be sufficient to deliver only one or at most two such predefined methods to cover all kinds of measurements File Browser e Click on File Browser s Methods tab e Select the location where your own GasBench II methods are to be
100. ed cups e g 3 is displayed together with the corresponding masses e g m z 44 m z 45 m z 46 below the grid e Finally press the Save amp Close button Save amp Close e The Configurator window will then appear Thermo u T ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Isodat 2 0 Software Creating a GasBench Configuration Finnigan GasBench Il 3 2 Creating a GasBench Configuration Isodat Contiguration iso IsoConligurator A B0ual Inlet HDevice E Boual Inet HDevice A2005 Sampler 2 EHDual Inlet Multiport Reference Refill If Dual Inlet Multiport Microvolume EB B Bua Inlet Multiport Multiport Ext Dual Inlet Multiport Multiport Ext Reference Refill EBOual Indet Multiport Multiport Ext MicroVolune A Oval Indet MicroVolume E Bdual Inlet Carbonate Device Reference Refill LT oual Inlet EQ Unit Reference Refil O Gas 3 f le Devices El sc Figure 3 1 Configurator Window e Isodat 2 0 automatically creates a new Configuration named My Configuration by default To give it a significant name right click on it and choose Rename e Type a significant name e g GasBench amp A200S Sampler File Edt View Options Interfaces Help E Boual Inlet Multiport Multiport Ext Reference Refill E BOual indst Multiport Multipart Ext MicroVolume g Dual Inlet MicroVobume o A E Oval Inlet Carbonate Device Reference Ref
101. ed to the respective connector for detailed explanation refer to Measurement Procedures for Real Samples on page 5 1 Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Gas Supply Warning When installing CO reference gas tanks keep in mind that standard high pressure tanks for CO contain a liquid phase that is subject to fractionation when temperature changes These tanks must be stored at constant temperature to obtain stable isotope values for your reference gas When using hydrogen H3 as reference gas it is necessary to shorten the internal flow restricting capillary that is the capillary leading from the reference pressure regulator to the open split 3 fold to approximately 50 of its original length This ensures that enough hydrogen enters the mass spectrometer s reference port Refer to Figure 7 8 Figure 7 9 and Table 7 8 Use the quick release connection to connect the blue compressed air cable to the compressed air connectors of the IRMS See Figure 7 10 As the IRMS has four connectors four screws wing unions for compressed air quick release connections are provided either with GasBench II or with the IRMS itself 4 5 1 3 connections for reference gases 1 4 capillary feedthrough to IRMS 5 connection for compressed air 2 6 He carrier gas connection 7 flush connection 3 8 GND ground 7 8 Figure 2 14 Connection Panel of Gas Bench I
102. ement Chromatogram co2 Error Extended Sequence Line D i Width Ampl 44 BGD 46 Area All d 130 12C d 180 60 s mv mv vs i 3 0 225 248 168 3635 123 1 50 505 0 204 feo ars aoe 106 2005 _ 1258 0002 oos foo fs er vas pas froe Jose us Jon ome orz e mofa ver wo amo os sore om fo The arrow shows the e120 1600 ses 128 100031270 s0822 sans 80085 overranged peak 7 Tposafzor2 21a2 108 s12 101 10302 927 Tore No fe__ 2ssa 2072 2000 108 770 1257 17208 0309 15301 0 era see os Figure 5 5 Carbonate Measurement Result Grid Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 9 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il e The first peak may be overranged Due to the open split action the subsequent peaks are in range e Almost no signal occurs on m z 46 between the CO peaks e Decreasing peak height indicates proper transport of the sample He mixture Note We use the term chromatogram even though it may not be a chromatogram in a narrower sense However one obtains ten or less repetitions of the same sample i e ofthe same small chromatogram Linearity Correction The system GasBench II IRMS with its different gas flows and slightly varying temperatures is never perfectly linear To achieve the best possible result with respect to both accuracy and stability either
103. en indirizzo produttore Germany erkl rt da das Produkt declares that the following product dichiara che il seguente prodotto GASBENCH mit den folgenden Produktspezifikationen bereinstimmt complies with the following product specifications rispetta le seguenti specifiche del prodotto EMV St remissionen EMC emissions EN 50081 1 EN 55011 EMC emissioni EMV St rfestigkeit EMC immunity EN 50082 2 EN 61000 4 2 3 4 6 EN 50204 EMC immunit Elektrische Sicherheit electrical safety EN 61010 1 sicurezza elettrica Erg nzende Informationen complementary information informazioni complementari Dieses Produkt erf llt die EMV Richtlinie 89 336 EWG und Niederspannungsrichtlinie 73 23 EWG This product complies with the EMC directive 89 336 EEC and the Low Voltage Directive 73 23 EEC Questo produtto rispetta la direttiva 89 336 EEC e la direttiva 73 23 EEC Bremen Germany 7 July 1998 Der Entwicklungsleiter Head of Engineering Responsabile construzione SBrreter bereinstimmungserkl rung gem EN 45014 declaration of conformity according to EN 45014 Dichiarazione di conformit alla EN 45014 Name des Herstellers manufacturers name F innigan MAT GmbH nome produttore Adresse des Herstellers Barkhausenstra e 2 manufacturers address 28197 Bremen indirizzo produttore Germany erkl rt da das Produkt declares that the following produet dichiara che il segu
104. ente prodotto GASBENCH mit Option Heizbarer Probentr ger mit den folgenden Produktspezifikationen bereinstimmt complies with the following product specifications rispetta le seguenti specifiche del prodotto EMV St remissionen EMC emissions EN 50081 1 EN 55011 EMC emissioni EMV St rfestigkeit EMC immunity EN 50082 2 EN 61000 4 2 3 4 6 EN 50204 EMC immunita Elektrische Sicherheit electrical safety EN 61010 1 sicurezza elettrica Erg nzende Informationen complementary information informazioni complementari Dieses Produkt erf llt die EMV Richtlinie 89 336 EWG und Niederspannungsrichtlinie 73 23 EWG This product complies with the EMC directive 89 336 EEC and the Low Voltage Directive 73 23 EEC Questo produtto rispetta la direttiva 89 336 EEC e la direttiva 73 23 EEC Bremen Germany 2 November 1998 Der Entwicklungsleiter Head of Engineering Responsabile construzione L Brook Thermo ELECTRON CORPORATION Notice on the Proper Use of Thermo Electron Bremen Instruments In compliance with international regulations If this instrument is used in a manner not specified by Thermo Electron Bremen the protection provided by the instrument could be impaired Thermo ELECTRON CORPORATION Safety and EMC Information In accordance with our commitment to customer service and safety these instruments have satisfied the requirements for the European CE Mark including
105. er 2 7 Mounting Syringe Needles into Autosampler Figure 2 18 outlines the mounting of needles into the autosampler s needle holder Notice that the relative positions between two needles are fixed when inserted into the holder See Carbonate Option Part No 113 2471 Components on page 6 2 for the part numbers any needle from flushing measuring or acid supporting screw Refer to needle holder Part No 113 7080 nut single needle holder or double needle holder complete Part No 113 7120 2 W 30 Figure 2 18 Mounting Sampling or Flush Needles into Needle Holder Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 19 Hardware Components Mounting Syringe Needles into Autosampler Finnigan GasBench Il Figure 2 20 Inserting Double Needle Holder into Autosampler Thermo 2 20 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il On Line Water Removal 2 8 On Line Water Removal GasBench II is equipped with two on line water removals One of them is positioned in front of the Valco eight port valve whereas the other one is used as a guard trap in front of the open split interface to the IRMS See Figure 2 21 Principle of On Line Water Removal Water is removed from the transfer sample stream by a gastight but hygroscopic Nafion tubing The sample flow He CO H20 0 5 ml min passes through the Nafion tubing which is mounted co
106. erating Manual Part No 109 2481 In this section only the entries that are specific for operating GasBench II will be described Method definition The main visible procedure is e perform a peak center before the acquisition e define CO as a reference five times duration 20 s and take the fifth as standard Ten loop switches for ten sample peaks on GC column 1 100s sampling line and valco are rinsed with sample He 200 s first injection of the loop onto the GC column Inject Mode 230s loop is in Load Mode again 230 270 s valco loop is filled with sample He 270s second injection of the loop onto the GC column Inject Mode Each line of the sequence list refers to a specific analysis It combines the position of the specific sample 1 with the Combi PAL method 9 a preprocess file or any valve actions before data acquisition and the respective acquisition method Thermo 4 14 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Basic Operations Finnigan GasBench Il Starting an Automated Sequence Note For detailed information about sequence editing and Combi PAL methods refer to the ISODAT NT Operating Manual Part No 109 2481 the ISODAT NT Operating Manual Upgrade to Version 2 0 Part No 115 4990 and the Combi PAL Manual Note When the sequence is finished calculate all the averaged results for all vials The standard deviation of these newly obtained results must be less
107. erating Manual 4 11 Basic Operations Condition Test Finnigan GasBench Il 4 12 4 5 Condition Test A simple way to check the condition of GasBench II alone that is without a set of individual sample vials is to gently flush the sample line with a 0 3 0 5 CO in He mixture The check should be performed using a filled container of a larger volume e g 500 ml The following parameters can be optimized by this check temperature and flow of GC column PoraPlot O GC temperature changes separation between peaks belonging to the same sample injection aliquot GC column flow shifts all GC peaks in time higher flow means shorter retention time and vice versa retention time and GC peak shapes Atp NyCO Retention time depends on column type Peak shapes tend to be tailed ifthe column is heavily used and needs recovering Refer to GC Oven on page 2 26 time delay between METHOD PROCESS At loop injections Use this type of condition test when changing the timing to control the results of manipulations to the Time Events list loop size 10 250 ml sensitivity vs peak shape Different loop sizes require different times for loading and injecting the loop Calculate load times from loop volume and sample needle flow Calculate inject times from loop volume and GC column flow Allow extra times for safety IRMS sensitivity length of transfer line Frequently check the sensitivity ofthe whole apparatus by this test
108. erred through the water removal 1 see Principle of On Line Water Removal on page 2 21 and the valco loop for GC injection The He flow should be at approximately 0 4 0 5 ml min measured at the vent of the valco valve see Figure 2 25 Thermo 2 16 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Measurement Needle He He y He flow ca 0 5 ml min 4 fy Hert CO AR co Figure 2 16 Connection of Measurement Needle Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 17 Hardware Components Flush Needle Finnigan GasBench Il 2 6 Flush Needle How to Connect the Flush Needle e Flushing with He 100 ml min during nen 4 6 min in case of carbonates and DIC e Filling with a gas mixture of 0 3 0 4 CO in He and a flow of of 50 ml min 4 He makes the use of glove bags and glove boxes unnecessary Figure 2 17 Connection of Flush Needle Note It is possible to connect two flush needles and operate them simultaneously by using our double needle holder Part No 113 7120 Refer to Pos 2 and Pos 4 in Figure 2 18 The double needle holder is part ofthe Carbonate Kit Part No 064 4520 Refer to Table 6 1 2 18 Finnigan GasBench Il Operating Manual Thermo ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Mounting Syringe Needles into Autosampl
109. esurement sequence See Creating a New Sequence on page 3 34 Thermo Ea ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Measurement Procedures for Real Samples Water Equilibration H D 5 34 Finnigan GasBench Il Preparing an H D Measurement Preparing an H D Method When preparing a method for H D equilibration choose Low pass filtered background In case of H D equilibration this background algorithm yields better results than the Individual background algorithm recommended for CO measurements H3 Factor For H factor determination in detail refer to ISODAT NT Operating Manual Part No 109 2481 Due to timing considerations the H factor needs to be corrected Experience shows that correcting the Hz factor by 0 5 units is sufficient in most cases Determine the exact value by reevaluating whole sequences with the goal to minimize internal errors Adjust Hydrogen Calibration We provide no special procedure to adjust the mass scale for H D measurements Instead you must set the calibration manually by following the procedure given below e Switch the reference H on e Set DeltaPl S XP to approximately 1000 magnet steps e Press the right mouse button on the magnet steps value e Select Pass to Gas Configuration Force the IRMS to jump to m z 2 for instance by changing the Gas Configuration to CO2 and back to H2 e Carefully adjust the magnet steps value to hit the peak center and repeat the last
110. eter supplied with GasBench II can be used to check various flows throughout the system Fill the small rubber ball with some soap solution and press it until bubbles appear in the inlet region Connect the inlet tube to the capillary under test The bubbles should then be transported along the tube by the gas flow under inspection By measuring the time needed to fill a certain volume the flow at the inlet tube can be calculated The flow through the sampling needle should be checked regularly before each run using a flow meter Measure at the exhaust capillary at the valco switching valve which is connected to port 7 Measure while a closed bottle is attached to the measurement needle and while the valco is in LOAD mode For normal operation the flow should be in the range between 0 5 and 0 8 ml min Measuring at the exhaust of the loop allows checking the complete sample transfer path To check the flow through the flushing needle a bottle must be connected and the flush valve be open This flow is measured at the open exhaust capillary at the bottle connection of the flushing needle and should be in the range between 100 and 150 ml min for normal operation Checking the flow in the GC column is more difficult Since the GC column itself is the restriction for the gas flow the flow can only be measured behind the column The best point is the exit of the GC column Carefully remove the capillary that leads to the second water trap and measur
111. h Il Compressed Air Schematic 7 9 Compressed Air Schematic V1 v2 Figure 7 7 Compressed Air Schematic of GasBench Il Outdated until 2002 Part No 111 4260 Note Pos 5 is not shown above Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 7 15 Technical Information Compressed Air Schematic Finnigan GasBench Il Table 7 7 Spare Parts Referring to Compressed Air Schematic Outdated Figure 7 7 Position Quantity Designation Part No 1 1 compressed air distributor 9 fold M5 106 8410 2 1 connection 052 1320 3 9 gasket 8 5 050 5260 4 3m silicon tubing 1 0 1 75 NF 101 5830 5 5m tubing 4 1 069 1130 6 2 muffler M 5 052 1860 7 11 tubing nozzle over silicon tubing 070 3780 Note Finnigan GasBench II now allows using the third reference inlet for reference gases see Instrument tab Reference Device Part on page 3 20 No more pressure regulator is required to adjust Flush Fill Instead use the pressure reducer of the reference gas tank cf Optional Hardware Flush Fill Trap and Trap 2 on page 3 5 As no additional pressure regulator is available when flushing with helium e g when preparing carbonates control the flush gas amount by timing Therefore in the method s Time Events list use the Flush Fill On column to switch helium flow on and off see Time Events tab Time Events List on page 3 22 The flush gas amount recommended is 500 ml This means to switch on Flu
112. harge electrospray ionization electron volt femto 10 degrees Fahrenheit extension ofa SEQUEST search database file free on board foot file transfer protocol gram giga 10 gas chromatograph gas chromatography gas chromatograph mass spectrometer electrical ground general purpose interface bus graphical user interface hour height high performance liquid chromatograph high voltage hertz cycles per second Interactive Chemical Information System Instrument Control Language inside diameter International Electrotechnical Commission Institute of Electrical and Electronics Engineers inch input output kilo 10 1000 kilo 2 1024 Kyoto Encyclopedia of Genes and Genomes kilogram Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Read This First Abbreviations LC IRMS LC MS LED 5 min ml MS MS MS MS MS m z NCBI NIST OD Pa PCB PID P N length liter local area network pound liquid chromatograph liquid chromatography liquid chromatography isotope ratio mass spectrometer liquid chromatograph mass spectrometer light emitting diode micro 10 meter milli 10 mega 10 molecular ion Megabyte 1048576 bytes protonated molecular ion minute milliliter millimeter mass spectrometer mass spectrometry MS power where n 1 MS power where n 2 MS
113. he stainless steel capillary a better peak shape is achieved N N UF QU OF Figure 6 5 Trap Arrangement Part No 114 1260 Table 6 2 Parts List for Trap Arrangement Figure 6 5 Part No 114 1260 Position PartNo Designation Quantity 1 114 1140 curved sheet metal 1 2 106 8330 trap subassembly 1 3 106 8600 bulkhead connection 1 16 SGE 2 4 067 4930 nut SSNE 16 4 5 067 4800 ferrule 1 16 GVF 16 2 6 056 6390 ferrule 1 16 GVF 005 2 7 100 4640 capillary i d 0 32 mm fused silica 5 Trap subassembly comprises outer capillary tube 1 16 0 8mm stainless steel 600 mm Part No 060 5470 and nickel wire d 0 125 mm 600 mm Part No 104 4070 Ed Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Options Finnigan GasBench Il Cryo Traps Option Trap 1 Trap 2 control 1 control 2 compressed air supply 4 bar compressed air supply 4 bar Figure 6 6 Compressed Air Schematic for Double Trap Arrangement For connecting compressed air supply and control lines refer to Figure 7 7 and Figure 7 8 The compressed air supply should always be set to approximately 4 bar Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 6 9 Options Cryo Traps Option Isoliergefaess 05428 30 gehoert ins Kit 1169570 Parts List Referring to Figure 6 7 Part No 112 1300 Figure 6 7 Table 6 3 Position Part No 5 111 6760 7 052 4070 8 05
114. housing shows the metric screw connections for the stainless steel pipes 3a and 3b Usually the outlet 3b is on the right and the inlet 3a on the left For the layout of these metric screw connections refer to Figure 6 4 Finnigan GasBench II Operating Manual 6 3 Options Carbonate Option Finnigan GasBench Il 4 power cable 5 cable with a push button at its end Pushing the button triggers a single stroke at the pump manually Figure 6 2 Acid Pump Top View Open The acid pump can be operated at three drive levels i e at different rotational speeds which are described inside the control housing See 1 in Figure 6 1 Figure 6 3 Acid Pump Side View Open Operate the acid pump at slow rotational speed This means the rubber ring should be mounted on top as shown in Figure 6 3 usual adjustment sometimes ex factory also in the middle Thermo 6 4 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Options Finnigan GasBench Il Carbonate Option Note If the tension of the rubber ring is not sufficient open the two screws shown in Figure 6 2 Then pull the motor in one direction so that the tension of the rubber ring increases Warning Always pull the plug out of the socket before opening the control housing Acid Pump Adjustment For proper function the acid pump needs to be adjusted prior to operation Set the pump to minimal pumping volume This allows exact dosing of the acid an
115. ical view Left coiled sinistral specimen umbilical view Neogloboquadrina Pachyderma is the most abundant planktonic foraminifer of high latitudes As any planktonic foraminifer it avoids low salinity and shallow waters The left coiled morphotype prevails at lowest temperatures and occurs throughout the Arctic Ocean Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 19 Measurement Procedures for Real Samples Dissolved Inorganic Carbon DIC Finnigan GasBench Il 5 3 Dissolved Inorganic Carbon DIC Dissolved Inorganic Carbon DIC in Brief 1 2 He air Fill with acid Flush with He 3 4 Inject sample Run acquisition Figure 5 11 Sample Preparation for Dissolved Inorganic Carbon DIC Measurement When real samples are collected they must be poisoned using a saturated HgCl solution to stop all biological activity Warning Strictly avoid any exposure to the severely toxic HgCl Always wear protective gloves Refer to your supplier s Material Safety Data Sheet MSDS for proper handling Thermo 5 20 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Dissolved Inorganic Carbon DIC Instrument Time Events Evaluation CO2 Peak Detection 002 Printouwt C02 AAA Man CN RE IS CZ E EEE DEREN a EN a Y ltz E l jo S Lo o C o AA ES pa ES ds ie
116. ide panel of GasBench II allows to control the temperature of the GC oven Notice the three keys Pkey for programming values will be accepted automatically after 2 s Arrow Up key for increasing a particular value Arrow Down key for decreasing a particular value Programming Step 1 Press the P key and hold it for 2 s Pass through the menu until Y 0 is displayed Again press the P key and hold it for 2 s Set C111 to 043 transducer type e g NiCr Ni K Set C112 to 1 number of decimal places and temperature unit e g 1 and C Set C113 to 33 controller type e g double setpoint Set C115 to 0 ramp function that is ramp function off Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il GC Oven Set C116 to 0 outputs on fault that is 0 minimum output limiting 2 is effective Set SPL to 0 lower setpoint limiting Set SPH to 200 upper setpoint limiting Set OFFS to 0 process value correction For details refer to Jumo itron 16 temperature controller manual Programming Step 2 e Again press the P key and hold it for 2 s e Press the Arrow Up Down key to change values Set Pb 1 to 9 1 proportional band 1 Set Pb 2 to 0 9 proportional band 2 Set d t to 61 derivative time in s Set r t to 243 reset time in s Set CY 1 to 50 4 cycle time 1 in s Set CY 2 to 50 4 cycle time 2 in s Set db to 0 contact spacing
117. idth 900 mm depth Finnigan GasBench II will be supplied by the IRMS line distributor Therefore the total IRMS power consumption will increase by 0 5 kW Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Preinstallation Requirements Finnigan GasBench Il Gas Requirements 1 2 Gas Requirements a He 5 0 that is 99 999 4 bar as carrier gas o He 4 6 with 0 3 CO 4 5 4 bar for acceptance tests For Water Equilibration a e 10 He 4 6 with 0 3 1 CO 4 5 4 bar as auxiliary gas CO 4 5 that is 99 995 4 bar as reference gas e HD He 4 6 with 2 H 4 bar as auxiliary gas H 4 5 that is 99 995 4 bar as reference gas For Carbonates a CO 4 5 that is 99 995 4 bar as reference gas For DIC Dissolved Inorganic Carbon a CO 4 5 that is 99 995 4 bar as reference gas Warning All gas lines should be oil free and preferably flame dried The a gas lines or gas tanks respectively should be at a distance of 1 1 5 m to the instrument Warning All regulators should be oil and fat free and be specified for a gases of high purity The supply lines should terminate with 1 8 male Swagelok type a connectors Compressed air will be supplied by the compressed air distributor of the a IRMS and should be between 40 psi and 70 psi Note Sometimes it may be necessary to check the unit for leaks Therefore a use an argon tank Note Thermo Electron Bremen recommends to install a high capaci
118. iercing the vial and starting the measurement transfer time should be increased e Enable Auto Dilution enables the action of the open split The signal amplitude needed to activate the auto dilution is set at the Activation Amplitude window in mV Whenever a sample peak voltage exceeds this limit the split will be activated Extra Script refers to additional hardware of GasBench II e g to traps which include the command scripts Select an appropriate Extra Script by a click on the C button To edit the Extra Script press the button Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 21 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il Time Events tab The Time Events list controls all operations during data acquisition Instrument Teme Events Evaluston C02 Peak Detection CO2 Pintou C02 643 E59 amp xB Figure 3 15 Time Events tab Time Events List e While editing the time events keep in mind that it takes some time to flush the capillary from the sampling needle to the valco valve approximately 70 s In the above sample this time has elapsed during the subsequent acid dosing e Under standard flow conditions the time required to inject the whole gas sample into the GC should not be less than 15 s loop 100 u flow gt 1 ml min plus security Allow at least 25 s for loading a 100 ul loop using a flow of 0 5 ml min e As no switch of gases occurs the Sw
119. ill DA EME Dual Inlet EQ Unit Reference Refil Expand the tree of the new Configuration by clicking the g Y signs T Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Creating a GasBench Configuration e Press the GasBench Sets tab O Gas Bench Sets The different GasBench Sets are shown in the right pane as shown below Isodat Confiquration iso IsoConfigurator Fie Edt View Options Interfaces Help noil BS OR lt 8 ENa Configurabons Isodat Configuration izo EY GasBench ll amp A200S Sampler MS Deka Plus XP lt Source Capillary Gas Bench Precon A2005 Sampler Your selection should look similar to this example Mark your particular GasBench Set on the right pane e g GasBench A200S Sampler For details refer to Different GasBench IH Methods on page 3 31 Drag and drop it to Capillary port in the left pane File Edi View Options Interfaces Help 92 Gas Bench Deal bel Isodat Configuration iso Sas Bench 42005 Sample E E GasBench amp A200 Sampler 7 Acid Pump MS Delta Plus XP 2 Bas Acid Pump A2005 Sampler Gas Bench Precon A2005 Sampler Optional Hardware xj e Select or deselect optional hardware that is Flush Fill Trap or Trap 2 e Confirm by OK Figure 3 2 Optional Hardware Flush Fill Trap and Trap 2 Finnigan GasBench II Operating Manual 3
120. in dopant BIT aes Adee ea Nay agin a 5 32 5 7 Water Equilibration H D 0202eeeeseenseensennnennnennnnneennennennenne nor nennen 5 33 HD Equilibration in Brie fontit tiene eien a e a a a 5 33 Preparing an H D Measurement ucenesssenssenssensesnnennnennennnennnnennnennnensnenn nennen 5 34 Referencing versus VSMOW cccccscesssesscessceseeeeenseenseceseceseceeeceaecseeeeseeseeeseeeeeeseenaes 5 35 Adjusting Electron Energy NR Reina Paiste 5 36 Determining the Optimal Setting of the Electron Energy 5 37 Re stain lesen ee TEILE 5 37 Sample Amount Consideration for Both Water Equilibration Types un 5 38 A A TTE A E OEE 6 1 Thermo iv Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Contents OA Carbonate Option nan genen Sigg MER ce RL ean eel oes 6 2 COMPONEMIS erein Tears SOR Leah eet 6 2 Acid PUMP tit 6 3 Connecting the Acid Needle iii ER eden A de RR EES 6 6 6 2 OS 6 7 Introduction nn rs a a E NN 6 7 Principle of Operation Gata A AS 6 7 Procedure ace tane tirane eie ado ada 6 7 Connecting Cryo Tap insista oia 6 11 Notes for GasBench II Trapping System ccccccsccesceeseeseeseeeseeeseeeneceseeeseeneenseeeseensees 6 12 Trapping of Na I Cita a da a io 6 14 Technical Information 2 it 7 1 7 1 Spare Parts and Consumables for GasBench I ussessesseeeneeeneennnennnnnee nn ennnne 7 2 7 21 Mechanical Parts oi ia Ra 7 4
121. inifera into a clean sample vial Close the vial with a new cap and a new septum Place the vials within the tray Ensure that the rinsing filling needle is properly mounted in the autosampler Depending on your flushing needle setup either choose the flush or double needle flush sequence Select the appropriate line numbers and start the sequence By default the sequence is set up to flush each vial with a helium stream of 100 ml for 5 min Ensure that the sampling needle is properly mounted in the autosampler Finnigan GasBench Il Operating Manual 5 7 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il Note It is strongly recommended to choose a double needle setup that is measurement needle plus acid needle for fully automated measurement of carbonates This ensures proper timing of the measurement Mount the sampling needle on the left side of the autosampler s double needle holder e Start the analysis sequence with a double needle setup refer to Double Needle Setup on page 5 6 Use the Carbonates sequence Select the appropriate lines The method used in connection with this sequence ensures that the following steps will take place 1 Dosage of H3PO using our automatic device Reaction between carbonate containing sample and H3PO begins CO will be released into the headspace 2 Waiting about 1 hour for equilibration of the CO3 3 During measurement helium enters the system
122. initely be prevented Warning A leak in the hydrogen H2 supply may cause fire or an explosion Before starting the system a leak check must be performed outside the working area 1 After mounting the reducing valve to the gas tank both valves should be open that is the on off valve and the reducing valve see Figure 2 13 2 Open the main valve for two or three seconds to let the gas purge the whole valve system see Figure 2 13 3 Close the on off valve Then close the main valve 4 Mark the manometer positions of on off valve and main valve and wait for 10 15 min 5 Ifthe manometer positions have changed a leak may be present 6 To detect the leak brush all valves and connections carefully with soap sud A possible leak is indicated by gas bubbles Gas Connections To operate GasBench II and the IRMS several gases are needed either from gas tanks or from the laboratory s main gas supply e g compressed air Refer to Figure 2 14 to locate the following numbers To operate the open split levers the valco valve and eventually the traps compressed air of 4 bar is required 40 70 psi see also Pos 5 in Figure 2 14 It can be provided by the pressure regulator of the IRMS Two capillaries leading the gas flow to the mass spectrometer input valve must be installed see Pos 4 in Figure 2 14 The connections 1 to 3 are used for the reference gases used in the various applications Flush gases must be connect
123. injections Nevertheless one can use only one acquisition script for all analysis types If you take care of the reference gas settings in the method that is the reference port setting in the Instrument tab and the reference port switching in the Time Events list you can use the same method and sequence for all GasBench II standard work It is comprehensible that acqisition script method and sequence must satisfy the most complicated of all measurements i e carbonate analysis Cleaning Procedure for Sample Vials The sample vials used for carbonate measurements should be free of organic and inorganic contaminations before they are loaded with carbonate To clean them perform the four steps described below 1 Fill up the vials with warm diluted phosphoric acid i e phosphoric acid plus warm distilled water and leave them for eight hours 2 Rinse the vials repeatedly with distilled water using a washing bottle 3 Rinse the vials with acetone using a washing bottle too This helps to dry the vials faster 4 Dry the vials in a drying chamber at 72 C for 2 5 hours Cover them with aluminum foil to protect them against contamination Finnigan GasBench Il Operating Manual 5 5 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il 5 2 Carbonates Introduction In order to measure carbonates you need the carbonate option In this chapter simultaneous measurement of C and 80 isotopic ratios in calcit
124. intout tab the use of printout templates is controlled e Single selects a print template from the Result Workshop for an individual printout per sample e Sequence selects a print template from the Result Workshop for a reduced printout per sample within a sequence summary Saving a Method Warning You must create and save anew method and a new sequence on your own The predefined methods and sequences delivered by Thermo Electron Bremen in the Examples folders are only example files They only show guidance through helpful default values but must never be used for measurements Never overwrite an example file with a method or sequence created on your own Depending on your software version these examples may not work properly After you met all your decisions throughout the method s tabs you must save it Proceed as follows Save command e Click on the Save button to save a i method or sequence previously Save created on your own Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 29 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il Save As command Bw Save Pr Save All Save in E Example E e Ed A Acquisition630s Mod for Air met A Acquisition 6305 met AlAcquisition met Flush Fil met H2_zero met Zero met Fene int Save as ype Method me we Cancel 3 30 Save All command Ole Save Pr Save All Save s
125. ion 5 10 mathematics 5 15 max peak width 3 27 maximum intensity 4 3 measure of precaution 3 27 measured 6 value 4 10 5 10 5 12 measured to real 5 value scale 5 10 measurement needle 2 4 2 16 to 2 17 2 24 4 5 5 8 6 7 7 3 7 9 mechanical parts 7 4 memory content 3 42 memory free sampling 2 16 methane 5 2 method Internal No 1 3 35 method Internal No 7 3 35 to 3 36 method Internal No 8 3 36 method Internal No 9 3 35 to 3 36 methods tab 3 14 3 18 4 14 5 28 method sequence correspondence 3 40 MgCO3 5 6 micropipette 7 2 minimal pumping volume 6 5 Mook W G 5 10 MS state 3 10 muffler 7 16 multiple analysis 5 2 VI Finnigan GasBench Il Operating Manual N No 2 26 3 19 3 21 5 2 5 4 N20 3 27 Nafion 2 21 2 26 Nafion tubing 2 21 7 2 NBS 5 13 needle holder 2 19 7 3 needle holder complete 7 2 needle set 5 33 needle tip 2 16 6 5 needle type 5 33 needle valve 6 13 to 6 14 negative pressure 3 32 5 22 Nelson S T 5 32 5 35 new method 3 14 3 17 3 29 to 3 30 new script 3 6 new sequence 3 14 3 29 3 34 3 36 nickel 6 12 to 6 13 NIST 5 13 NO 3 27 nut 2 19 2 24 7 19 O O Neill J R 5 4 Oo 5 4 objects submenu 3 48 ocean water 5 2 5 23 old script 3 6 on off valve 2 13 to 2 14 online interface 5 2 online water removal 2 21 open split 2 15 2 21 2 26 2 34 to 2 37 3 12 3 21 3 27 5 2 5 4 7 9 open split action
126. ion position 5 4 injection speed 3 50 injector 3 45 inlet region 4 5 inlet tube 4 5 inlet valve 2 14 4 2 4 4 5 3 inner glass tube 7 2 Instrument tab 3 19 instrument tab 3 19 to 3 21 3 32 to 3 33 5 5 integration time 3 20 intensity plot 4 6 intensity ratio 4 3 intercomparison material 5 13 5 32 7 14 interface 1 2 6 interface 2 2 6 interface tube 2 34 interference 3 27 internal error 4 6 internal flow restricting capillary 2 15 internal method 3 35 international standard 5 13 7 14 ion correction 3 25 ion source 3 27 5 36 6 13 to 6 14 Thermo ELECTRON CORPORATION ionization energy 5 36 IRMS capillary 2 37 IRMS method 3 36 IRMS sensitivity 4 12 ISL script 3 21 3 38 ISL tab 3 15 Isodat 2 0 3 2 3 4 3 6 to 3 7 3 12 3 17 3 25 3 30 3 37 3 51 5 28 6 5 Isodat 2 0 database 3 13 ISODAT NT Operating Manual 3 7 to 3 8 3 10 3 15 3 17 4 14 to 4 15 5 34 ISODAT NT Operating Manual Upgrade to Version 2 0 3 7 3 15 4 6 4 15 isothermal condition 2 26 isothermal gas chromatograph 5 2 isotope effect 3 27 isotope ratio 5 6 isotope ratio determination 3 17 5 2 isotope ratio mass spectrometry 5 3 isotope value 2 15 5 4 5 6 5 39 isotopic abundance 5 4 isotopic characterization 5 2 isotopic composition 5 3 isotopic dilution effect 5 4 isotopic equilibrium 5 4 isotopic equlibrium 5 7 isotopic fractionation 5 10 J JUMO it
127. ioning is not discussed here but it can be performed in the same way as GasBench tray holder Go to Gas Bench tray holder Example for Adjusting GasBench Tray Holder 1 Go to the positioning variables x y z 2 To prevent the sample tower from crushing into the tray set the positioning variables x y z to zero 3 Determine the dimensions of the tray relative to the zero position of the autosampler Again readjust only if the dimensions are false or if a different tray is in use 4 Each position that is x y or z can be configured by turning the wheel to the correct dimensions Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 49 Isodat 2 0 Software Autosampler Programming 3 50 Finnigan GasBench Il Using Autosampler Method We use the autosampler s compatibility mode where the autosampler emulates the behavior of an AS200 autosampler Therefore only ten different methods can be used and they must be named A200S 0 to A200S 9 Initially the autosampler uses three methods for GasBench II e A200S 7 is used for flushing e A200S 8 is used for carbonates and e A200S 9 is used for equilibration Their main difference is the duration during which the sample needle will stay injected in the headspace of the vial This time is given by the method parameters Fill strokes and Pullup delay according to the formula Time for one sample Fill strokes 1 x Pullup delay The settings in
128. is leaking Warning The connection between plot column and safety column located in the GasBench II oven is critical Warning Be careful when tightening the connectors Do not use excessive force Tighten only if you are absolutely sure that the connection is leaking If the water level is too high after the leak check heat out the GC column at 140 C overnight The GC column accumulates water by and by and releases it when heated The water level only decreases after prolonged heating and continues to fall for some time even after heating is switched off provided that there are no leaks Leak testing is especially laborious in the gas sampling section A leak in this section has no continuous connection to the mass spectrometer Instead the valco 8 port valve needs to be switched to introduce a portion of the gas stream into the IRMS Warning When checking this section comprising sample bottle sampling needle connectors water trap and the appropriate connectors at the valco valve be extremely careful not to overtighten the connections When replacing ferrules in this section be sure to use only the listed valco ferrules Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Basic Operations Checking Column Flows 4 2 Checking Column Flows For optimal operation certain flows in GasBench II must be within a specific range The bubble flow m
129. itch Method column is currently not used in GasBench operation that is it stays empty on Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION 3 Isodat 2 0 Software Finnigan GasBench Il Creating a New Method e The display of the Time Events List can be Instrument Time Events Eos enlarged pressing the Big Edit View oh amp BS 6 2x button G gt Time fs Reference 1 On Reference 2 On Insert lines using the right mouse button or click on 4 Edit the Time s at which the event will happen e Double click on the field of a valve or use the space bar to set toggle its status to active or inactive a Acquistion Stat immedatey y Acquistion End Time s 450 a by GC immediately by Enter Ke Figure 3 16 Time Events tab Acquisition Start and Acquisition End Time Thermo ELECTRON CORPORATION Select the Acquisition Start The acquisition start defines the signal source to trigger the start of data acquisition Choose between Immediately by GC or by Enter Key In the vast majority of cases Immediately is used By GC refers to a trigger signal from GC whereas the user gives the trigger signal via keyboard at by Enter Key Edit the Acquisition End Time The Acquisition End Time is the end time of data acquisition After the Acquisition End Time no further actions will be executed from the Time Events list Allow some time to finish the last event before ending th
130. itional entries which are UPPERCASE can not be accessed directly when passing through the autosampler s menus Press the F3 key once at the position of the arrow shown above followed by Return at the autosampler to access them Thereby sensitive entries that lead to large scale changes are protected against clumsy access This principle is valid for the entire tree of commands shown above at any position within the tree F3 leads to additional commands The autosampler commands can be classified into several groups e tray related commands e tray holder related commands e g the tray holders which are used dimensions that is the number of rows and columns e positioning of the autosampler in order to adjust sample positions e adjustment of the needle holder or Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Autosampler Programming Hs J amp ei H in The layout depends on the hardware configuration for each indivedual PAL System The standard software does not include all Objects as shown in the Overview Revision C Firmware 2 3 1 November 2000 Bie El EHE i pnih fpu lis ios Firmware Overview Other selectable Cycle os Figure 3 33 Adjustment Possibilities of Autosampler Tree of Hardware Commands Main Menu Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 47 Isodat 2 0 Soft
131. k 4 2 Checking Column Flows 4 3 Zero Enrichment Test Standard On Off Test 4 4 Linearity Test 4 5 Condition Test 4 6 Starting an Automated Sequence 4 7 Frequently Asked Questions Finnigan GasBench II Operating Manual 4 1 Basic Operations Leak Check Finnigan GasBench Il 4 1 Leak Check To check whether the IRMS is ready to operate close the inlet valve and run a mass scan from 3000 magnet steps to 12000 magnet steps It should look more or less like Figure 4 1 or Figure 4 2 respectively 7 E s 2 H gt E gt 2 E 4000 5000 6000 7000 8000 9000 10000 11000 1200C MagnetCurrent Steps Figure 4 1 Mass Spectrum of Background Gas Composition for Finnigan DeltaPl S XP Thermo 4 2 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Basic Operations Finnigan GasBench Il Leak Check IF BockgroundScan GB_background scn E z 900 2 2 lt 4000 0000 8000 10000 12000 MagnetCunent Steps Figure 4 2 Mass Spectrum of Background Gas Composition for Finnigan MAT 253 The mass scan shows the composition of the background gas in the source region and informs about the amount of gases present Try to identify the following patterns and compare them with the maximum values below Water e contains ions of m z 16 m z 17 and m z 18 e appears at magnet current values approximately between 5300 steps and 6000 steps e peak intensity should be maximal 1 V e
132. k Using the same program the memory contents of the autosampler can be restored via a backup file Thus these backup files contain the autosampler settings needed for the different applications Some exemplary backup files are provided by Thermo Electron Bremen as PAL GASBENCH V2 33 021031 sss Using GC PAL Loader Software 1 For any GC PAL a loader software is provided which needs to be installed on your computer It is necessary for adjusting the autosampler settings As a stand alone software it can be installed independently of Isodat 2 0 2 Start the loader software Communication between computer and autosampler is now possible via COM Port 3 Default installation location is Program Files gt PAL gt Loader Notice the two subfolders Backup and Update Save the PAL GASBENCH V2 33 021031 sss file in the subfolder Update 4 Open GC PAL loader software via Start gt Programs gt PAL System gt PALLoader 5 Perform a backup of the default autosampler configuration 6 Wait until backup is complete 7 On the Isodat 2 0 CD look for the GC PAL folder It contains two files with autosampler settings adjusted ex factory PAL GASBENCH V2 33 021031 sss one for Combi PAL and one for GC PAL The latest version is available also on CIS that is in our Customer Information System 8 Copy these two files to the GC loader s update folder 9 Press Update and select the file PAL GASBENCH V2 33 021031 sss Perform the
133. king standard R R R R R R 5 2 1 1000 y ee e eer R R R R R R R Z y Z Rx 241424 11 1000 RAR R R z Ry Zz i pas R R R This equation has been used above special case working standard x absolute standard z that is VPDB See Referencing versus VPDB on page 5 13 Phosphoric Acid Preparation Phosphoric acid H PO is prepared from Puranal grade orthophosphoric acid gt 85 and Puriss grade phosphorous pentoxide or trade names of equivalent purity Inside a fume cupboard one Winchester that is a 2 5 1 package of phosphoric acid is poured into a 5 1 beaker that stands on a magnetic stirrer s hotplate Use a magnetic stir bar PTFE Warning Gloves and a face mask must be worn whenever handling P O Goggles are not sufficient Note A useful thermometer or stirring rod can be obtained by enclosing the thermometer in a large piece of heavy walled Pyrex tubing with its bottom sealed off that is shaped like a test tube Warning Between the additions and during the final cooling stage the beaker is kept covered with cling film Thermo 5 16 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Carbonates Adding Phosphorous Pentoxide Warning Take care during the initial stage of adding P205 the reaction can be vigorous as the powder contacts the relatively wet acid It normally takes a
134. l It is intended to connect only one equilibration gas to the flush port Ex factory the helium inlet port is connected to a t piece which feeds the flush port with helium The service engineer will connect helium at the upper inlet port and the reqired flush gas at the lower inlet port Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 15 Hardware Components Measurement Needle Finnigan GasBench Il 2 5 Measurement Needle CO He 4 transfer needle A rubber septum El He output gt yl 4 y el PE 12mm exetainer Figure 2 15 Measurement Needle Note The measurement needle is sometimes synonymously called transfer needle The measurement needle is located in the Combi Pal autosampler The correct connection is important to guarantee high GC performance Refer to How to Connect the Measurement Needle on page 2 16 How to Connect the Measurement Needle Connect the measurement needle as outlined in Figure 2 16 The measurement needle should direct the He flow through the side hole and take up the sample through the needle tip This ensures dead volume free and therefore memory free sampling The CO He carrying capillary and the corresponding bulkhead connector should be marked by a flag see Figure 2 16 Now helium gently moves CO from the exetainer s headspace into the fused silica capillary within the needle tip From here the sample is transf
135. l notes about Method Acquisition Script Time Events etc e At Gas Configuration select the appropriate one e g CO2 Usually the default entry can be accepted Refer to the Status Bar in Accessories Bar on page 3 9 e Select an appropriate Acquisition Script by a click on the LJ button Acquisition isl is the default entry and can usually be accepted It controls the acquisition cycle To edit the script press the 24 button Warning It should only be edited by users trained on script editing debugging and error tracking Otherwise potential errors within scripts which are due to editing maybe difficult to be discovered afterwards Isotope MS Integration Time 0 200 s Peak Center Predelay s 5 Peak Center Cup Cup 3 v Peak Center Postdelay s o Figure 3 12 Instrument tab Isotope MS Part Integration time is the time integrated to form a data point triplet e g 0 200 s e Select the Peak Center Cup e g Cup 3 as narrow center cup in a triple collector e Peak Center Predelay is the time the system waits between activation of reference gas and start of peak center cycle e g 20 s Note The retention time should be set to the Reference Out value of the respective reference gas pulse in the Time Events list This accomodates for the delay of 7 10 s associated with the gas passage through the capillary to the IRMS e Peak Center Postdelay is the time the system waits between end of pe
136. le the overpressure section of GasBench II from the mass spectrometer s vacuum chamber the gas mixture passes a second water trap and enters the open split arrangement While a fixed amount of the gas mixture travels to the mass spectrometer the excess gas leaves the split to the surrounding atmosphere The different gases contained in the original mixture arrive at the mass spectrometer source separated by polarity Using a Poraplot Q no time difference can be detected for O Nz Hz and He Their travel time along the column is approximately 120 s depending on column pressure and temperature CO needs about 20 s longer while more polar compounds like water or ethanole may travel 300 to 500 s or get stuck on the column and bleed off only when the column is heated Headspace Sampling In standard setup that is used for equilibration DIC and carbonate analysis the sample gas is taken from the headspace of a sample bottle In all of these cases the gas to be measured is not identic with the substance whose isotopic value should be determined This leads to numerous complications in sample preparation sampling technique and results interpretation First of all the isotopic abundances in the liquid phases are different from those in the gas phase This effect is most striking when measuring hydrogen isotopic ratios here the abundance of the heavier isotope in the gas phase is approximately four times lower than in the liquid phase du
137. less measurement The signal of residual air together with CO acts as an interference The column has to separate these two components because residual air produces NO and N O in the ion source which can only hardly be pumped off Additionally a peak on m z 46 occurs which could coincide with a CO peak and thus would lead to considerable shifts of the 6 value Also during the ten repetitions one runs the risk of coincidence with the CO peak if the timing is wrong This would also result in a massive shift of the value Note Therefore clearly separated peaks are a crucial measure of precaution to be taken e Max Peak Width s broader signals will not be recognized as peaks e Background Type it has been proven experimentally that the background type is important for GasBench measurements HD equilibration and CO equilibration require different background types Mostly especially for all CO applications Individual Background yields the best results whereas H evaluates best with Low Pass Filtered Background Pertorm Timeshift iv A Auto Square Pulse Recognition Timeshift Supression Enable Be Factor 0 55 rArea Pk Width Pk Height Figure 3 22 Peak Detection Tab Auto Square Pulse Recognition Timeshift Suppression As chromatographic peaks emanate from a GC column an isotope effect is noticed during their detection a slight delay of heavy isotopes signal positions occurs compared to those
138. libration H D Depending on how much gas of a particular 6 value has been filled into the headspace and how much water has been added to the sample 6 value unknown a final 8 value between these two original 6 values will result Remember that 1 mol of water equals 18 ml and 1 mol of an ideal gas commensurates to 22 4 1 One sample vial contains 12 ml that is 12 22400 mol 5 357 10 mol of an ideal gas We do not use pure CO but 0 5 CO in He and consider this mixture to be an ideal gas Therefore one sample vial contains 12 22400 0 005 mol CO 2 679 10 mol CO Let us return to the water 1 ml of water equals 1 18 mol of water Using 1 ml of sample in the sample vial yields 10000 times more oxygen atoms in the water phase compared to the gas phase As a good estimation we can therefore assume the isotope value of the gas to be equal to the initial isotope value of the sample This means the isotope value will not shift but the gas will indeed take the original value of the sample Thus using ml or 500 ul or 200 ul of sample no mass balance calculation is required Finnigan GasBench Il Operating Manual 5 39 Measurement Procedures for Real Samples Water Equilibration H D Finnigan GasBench Il Thermo 5 40 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Chapter 6 Options 6 1 Carbonate Option 6 2 Cryo Traps Option Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Man
139. lot the value versus the peak area or the peak amplitude which is strictly proportional to it a graph like the one shown in Figure 5 7 will be obtained Thermo ELECTRON CORPORATION Finnigan GasBench II Operating Manual 5 11 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il 26 000 27 000 11 400 10 15 20 25 30 35 40 11 600 in y 0 013x 12 273 11 800 28 000 29 000 813C T 12 000 T 12 200 30 000 31 000 12 400 T 12 600 513C E 8180 32 000 33 000 T 12 800 linear 5180 13 000 Peak Area Figure 5 7 Measured Value versus Peak Area for a Set of Measurements Same Sample but Different Sample Amounts Experience teaches that the functional dependence between 6 value and peak area or peak amplitude always is a linear one Thus within the statistical error limits all results are distributed along a line with a small slope The slope is small 0 013 o Vs for 180 and 0 o Vs for 1 C in the example above but depends on all of the the factors mentioned above Therefore the following correction procedure is recommended The correction can be approximated by a linear function Seas A mxA meas real meas denotes the measured 6 value rea the real one A describes the peak area Determine the correction factor m i e the slope from
140. ly 20 s and close the tube immediately after flushing See Figure 4 8 1 2 in exetainer vial co flushing Capillary 0 3 0 5 CO in He Figure 4 8 Flushing an Empty Exetainer for Preparation of a Test Sample Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 4 13 Basic Operations Starting an Automated Sequence Finnigan GasBench Il A more convenient way to fill the He CO mixture into an exetainer vial is to use the flushing needle refer to Flush Needle on page 2 18 together with the Combi PAL autosampler To fill the exetainer properly each tube is rinsed for approximately 5 min with He CO at a flow rate of 100 ml min Note To guarantee high performance the exetainer should be washed prior to using it refer to Cleaning Procedure for Sample Vials on page 5 5 After preparation of the test sample there are two possibilities to proceed e A predefined sequence can be used for a measurement Make sure that the IRMS is calibrated e Make sure that the vials are prepared and placed in the tray e Select an appropriate line in the sequence e Press the Start button e The user must define a method for a measurement The chapter The File Browser on page 3 13 gave an overview about what can be defined and seen by using the Method tab within the File Browser Note For an extensive description of the options of the method definition refer to the ISODAT NT Op
141. n H D Determining the Optimal Setting of the Electron Energy The following procedure should be performed to achieve the optimal setting e Perform a peak center with reference On Switch the reference Off e Record the signal intensity on mass 2 versus the electron energy see Figure 5 31 The optimal setting is just below the appearance of the He signal where the sensitivity for H is optimal 60 80 100 120 140 160 Electron Y 11 814x 1294 7 Energy Figure 5 31 Signal Intensity on m z 2 vs Electron Energy Note For further information refer to Field F H and Franklin J L Electron Impact Phenomena pp 244 1957 Academic Press Results AS Sample AS Method Identifier 1 Identifier 2 Comment Method 0 ee gt Internal No Q H2_Equilibration empty vial HDBroenst 200ul Thermo Eur ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Measurement Procedures for Real Samples Water Equilibration H D Finnigan GasBench Il le Mara CAFineiganlisodat NICOLAS Wei Gas BenchiRessistHD Equlitrierung ct 1 LU Y A hk LT Figure 5 32 Water Equilibration H D Chromatogram H2 Error Extended Sequence Line Stat Rt Width Ampl 2 Ampl 3 8602 B603 Area All d 2H 1H fs s fs mv mv vs 46 15 9 20 1 4163 104 878 829 94 704 88 291 59 664 704 6292876581 2 pas aoa 201 4500 75 o70 9 8 00 253 00 205 00 400 7051174245027 a saa ora
142. n the headspace Analysis ii f Equilibre alo for 20 h Start the swunse aro Figure 5 26 Sample Preparation for 180 Equilibration Sample Tray Temperature Control For high precision 180 equilibration the temperature of the sample tray needs to be stabilized Two operation modes are available e Passive Tray at room temperature that is 24 C The thermal mass of the cast aluminum tray and its isolation allow to keep the temperature control of the tray deactivated Only long term drifts in tray temperature will occur within a certain time interval Placing reference samples allows correcting for possible temperature drifts e g one reference sample for six unknown samples e Active temperature control at 32 C Ensure that room temperature is approximately 5 C below the set tray temperature Check the temperature stability over several hours The controller read out may not alter by more than 0 1 C Referencing versus VSMOW Referencing can be performed either using the complete and precise mathematical pathway outlined in Carbonates on page 5 6 or using the simplified scheme given in Water Equilibration H D on page 5 33 Finnigan GasBench Il Operating Manual 5 31 Measurement Procedures for Real Samples Water Equilibration 120 Finnigan GasBench Il Note Refer to Reference and intercomparison materials for stable isotopes of light elements In IAEA TECDOC 825 IAEA ed Vienna 1995 See also Table 7
143. nger than one year in continuous operation In case of CO water equilibration additionally a mixture of CO in He is needed for headspace flushing The purities are recommended to be as stated above for He and CO respectively A CO content of 0 3 leads to an ideal signal height of 9 V In case of H D measurements H is needed as reference gas Its purity should be 99 996 Hp In case of headspace flushing a mixture of 2 H in He should result in a signal height of 9 V which is optimal with regard to error margins Warning The pressure of new gas tanks is up to 200 bar helium tank The pressure must be adjusted to approximately 4 bar using the pressure regulator mounted at the gas tank 123 45 BOTH H dh dy 1 Main valve 2 Manometer 200 bar He for pre pressure GAS 3 Line pressure regulator 4 Manometer 4 bar He 5 on off valve 6 High pressure gas tank Figure 2 13 Gas Tank Installing the Gas Tanks 1 Connect the reference gases 2 Connect the measurement gases Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 13 Hardware Components Gas Supply Finnigan GasBench Il 2 14 3 Connect the equilibration gases that is flush gases Either CO He or H He are used as equilibration gases 0 5 CO in He because of 50 V dynamic range Working with the Gas Tanks Warning It is strongly recommended to install the gas tanks firmly Tumbling must def
144. nic pre concentration unit for flows in the range of the GC column flow that is 0 5 5 ml min Depending on the GC performance needed a fused silica trap 0 32 mm fused silica tubing from valco port A to port B for very sharp GC peaks or a nickel filled stainless steel trap inner diameter i d 1 mm resulting in broad GC peaks can be used In case of the stainless steel trap the sample flow can also be increased up to 15 ml min Note A longer fused silica capillary needs to be installed in the vent exit Y of the valco valve to avoid freezing of ambient air into the trap See Figure 6 9 single trap application and Figure 6 10 dual trap application ze Vent GasBench E Autosampler A Injector Loop In B Injector Loop Out GB Single z X Change He in and Sa out at the Valco Trap Trap 1 SS Nickel filled Cryo Con centration Y Vent capillary needs to be prolonged Z Depending on the Sa flow Trap 2 may be SS Nickel filled or fused silica Figure 6 9 Single Trap Application Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Options Finnigan GasBench Il Cryo Traps Option to IRMS Hen gt Vent GasBench Autosampler A Injector Loop In Au B Injector Dual Trap Trap 1 SS Nickel filled Cryo Con D Trap 2 to centration GC column C Injector to Trap 2 Figure 6 10 Dual Trap Application Volumes of the Tr
145. nical seal 2 socket head screw is used after fixing the internal rotor by the che quered screw The socket head screw allows to ad just the pressure acting from above upon the cone By increasing this pressure the inter nal rotor is tighted against the side walls Figure 2 25 Valco Valve with Loop Top View 1 Switch the Valco to Load Mode 2 Open the nuts on Port 3 and Port 6 Refer to Figure 2 25 3 Replace the loop Use loop sizes less than 250 ml for the two column types 4 Tighten the nuts 5 Inject the measurement needle into a helium filled vial and purge the loop before switching to Inject Mode 6 At the Valco vent Port 7 check for a purge flow of 0 3 0 5 ml Figure 2 26 1mlLoop EN Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Principle of Valco Eight Port Valve Figure 2 27 2mlLoop Figure 2 26 and Figure 2 27 are shown above as examples Loops of 100 ul 250 ul and 1 ml are already part of your equipment provided by Thermo Electron Bremen If necessary loops of even bigger volumes are available The 1 ml loop and the 100 ul loop are very similar Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 2 25 Hardware Components GC Oven Finnigan GasBench Il in out heater assembly manometer 2 10 GC Oven The GC oven is either equipped with a HayeSep D micro packed stainless steel
146. nsity W Gas Configuration i Raw Ratio W Element Deta MW Environment Y Evaluation Part Molecule Ratio IF Atom V Mass Relevant Custom Idenkdier Sequence Information i Sequence Infomation Sequence Information Sequence Infomation Sequence Information Sequence Part Sampler Sequence Information FieHeader Sequence Information TimeDbject Sequence Information TimeDbject Sequence Information Es Result Data Information Grid Result Data Enot Grd E Resut Dala Erot Gnd Rena Dota Eno Gnd Rest Dala Enor Grd ES Result Data Enor Grd ES Rena Data Sequence Past 3 Enor Grid Sequence Part Enor Gnd Sequence Patt Enor Grid Sequence Part bse Eno Gnd Sequence Part Enor Gnd Figure 3 30 Excel Export Module Illustrating Basic GasBench Il Output Parameters Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 41 Isodat 2 0 Software Autosampler Programming 3 42 Finnigan GasBench Il 3 9 Autosampler Programming GC PAL Loader Software All autosampler settings positions and methods that include timing are entered directly into the autosampler s memory via the autosampler s panel All changes of autosampler programming are effective immediately To save a copy of the autosampler s memory contents use the PAL loader software provided with your Combi PAL or GC PAL This software package allows to read the autosampler s memory and to save its contents to a backup file on your hard dis
147. ntervals to achieve accumulation of CO in the cold spot of the sample loop When released from the dewar the trap heats up without significant time delay and the CO starts to travel towards the GC of GasBench II Due to cryo focusing the peak shape is extraordinary sharp The grade of CO enrichment can be determined by varying the time during that the loop stays in liquid nitrogen accumulation time Procedure This section will outline the cryo option s double trap version 1 Ina first step the sample gas is carried through the measurement needle into the nickel filled stainless steel capillary by a gas flow of approximately 5 15 ml min There the sample is frozen Load Mode In Finnigan GasBench Il Operating Manual 6 7 Options Cryo Traps Option Finnigan GasBench Il this case the big surface of the stainless steel capillary plays an essential role as the entire sample can be frozen on a short distance The stainless steel capillary is introduced into the sample gas flow instead of the loop of the valco port that has been within the sample gas flow so far For exchanging the loop see How to Change the Loop Size on page 2 23 2 After switching valco from Load Mode to Inject Mode the entire sample is carried over into the fused silica capillary and frozen a second time 3 Inject the sample gas into the IRMS by a continuous flow of less than 3 ml min Due to the lower diffusion in the fused silica capillary compared to t
148. ntrations use Acquisition 630s mod for air met that has been delivered as a particular predefined method Note It differs only with respect to the Time Events List from Acquisition 630s met used for carbonate measurements Select it from the File Browser s Methods tab Then double click or drag and drop it into Isodat 2 0 s Acquisition window Refer to Predefined Methods as Examples on page 3 18 and Creating a New Method on page 3 17 Time Events Instrument Time Events Evaluation CO2 Peak Detection C02 Piintou C02 43 Xx Reference 1 Referance 2 Reference 3 Split in Valeo Load Trap Up Trap 2 Up Flush Fill On Switch Method On Figure 5 22 CO in Atmospheric Concentrations Time Events tab Time Events List Partly Thermo 5 28 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il CO in Atmospheric Concentrations Note Note the differences compared with the Time Events List of Acquisition 630s met used for carbonate measurements Whenever you expect an air peak in the chromatogram it must be masked out This is achieved by setting the split to dilution position i e off in the Split In column during these time intervals The split will thus move upwards that is it is pulled out causing dilution Setting the split on amp in Split In column will stop dilution The split will be pushed in again This ensures tha
149. nventions Finnigan GasBench Il Boxed Information Information that is important but not part ofthe main flow of text is displayed in a box such as the one below Note Boxes such as this are used to display information Boxed information can be of the following types e Note information that can affect the quality of your data In addition notes often contain information that you might need if you are having trouble e Caution information necessary to protect your instrument from damage Warning hazards to human beings Each Warning is accompanied by a Warning symbol Thermo xiv Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Read This First Finnigan GasBench Il Typographical Conventions Topic Headings The following headings are used to show the organization of topics within a Chapter 1 Chapter Name 1 2 Second Level Topics Third Level Topics Fourth Level Topics Fifth Level Topics Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual XV Read This First Reply Cards Finnigan GasBench Il xvi Reply Cards Thermo Electron San Jose manuals contain one or two reply cards All manuals contain a Customer Registration Reader Survey card and some contain a Change of Location card These cards are located at the front of each manual The Customer Registration Reader Survey card has two functions First when you return the card you are placed
150. o 111 4260 91 z Technical Information Compressed Air Schematic Finnigan GasBench Il u gg y i I EL ro ip HG N if H H rut rin HSM LSL NIUSNI4 Figure 7 9 Tubing Scheme of GasBench Il Actual Part No 111 4262 Thermo 7 18 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Table 7 8 Position 0 SS O o A OO N a 11 12 13 14 15 16 17 18 19 20 21 22 23 Thermo ELECTRON CORPO
151. o Connect the Measurement Needle uusesseeseeeseesseesneennennneenneennnnenne nennen 2 16 2 6 Flush Needle 22 08 82 at A tn edna ioe 2 18 How to Connect the Flush Needle cccccccccccesecsceeseeeseeeseceeeeseeeseeseeeseeeseeeeeeeeeeeeaeens 2 18 2 7 Mounting Syringe Needles into Autosampler ccccccccesscesseeseeeseeeeceseeesecseeseseseaeseseeneeeseees 2 19 2 8 On Eme Water Removal u a en es an arms ann 2 21 Principle of On Line Water Removal uuensesssesseessenneennennnennnennnennennnnnenne nennen 2 21 2 9 Principle of Valco Eight Port Valve ccccccesscssseesseeseceeeeseesseeseeceeceeeseeeaeensecnsesesesnsesesesaeees 2 22 How to Change the Loop Size cccccccccsscssseesseesscsseceeeesecesecssecesecenecaeceeeeneecseeeseesseeeeeess 2 23 The rmo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual i Contents Finnigan GasBench Il 2 10 GC Oven A a N N aa 2 26 Type PoraPlot Q GC Colums danna a a a a n e 2 26 Typ HayeSep D GC Column u a aa EAA R a 2 27 Step 1 Accessing the GC Column eia n pa e E A A E E EG 2 27 Step 2 Changing the GC Column seisena aor ei iei 2 29 Programming JUMO itron 16 Temperature Controller for GC Oven ce 2 32 2 11 Open pls ti A alba 2 34 Reference Injection iii a 2 34 Sample Injection and Dilution uesseessesnessenneenneenneennennnnnnsennnennennennennenneenan nen 2 36 Isodat 2 0 Softwar cein dl 3 1 3 1 Starting Isodat 2 A
152. odulo 3 e ES 08038 Barcelona e 34 093 223 0918 Sweden Pyramidbacken 3 e S 141 75 Kungens Kurva Stockholm e 46 08 556 468 00 United Kingdom Stafford House e 1 Boundary Park e Boundary Way e Hemel Hempstead e Hertfordshire HP2 7GE e 44 01442 233 555 U S A 355 River Oaks Parkway e San Jose CA 95134 1991 e 1 408 965 6000 Notes The country code is enclosed in square brackets The city code or area code is enclosed in parenthesis For countries other than the U S A when you are dialing from within the specified country dial the 0 of the city code For countries other than Italy when you are dialing from outside the country do not dial the 0 of the city code Published by Product Marketing Thermo Electron Corporation Bremen Germany Copyright 2004 Thermo Electron Corporation All rights reserved Printed in Germany Thermo Electron Bremen GmbH Barkhausenstr 2 ermo D 28197 Bremen ELECTRON CORPORATION uhren Internet www thermo bremen com Reparatur Begleitkarte Repair Covering Letter Bitte vollst ndig ausf llen Please fill in completely Absender Ger te Type Service Nr Dispatcher Instrument Type Service No Sie erhalten zur Reparatur unter unserer Bestell Nr You receive for repair under our Order No rms DOA Teil wurde nicht benutzt part not used Teil wurde nur f r Testzwecke verwendet used for test purposes only Festgestellte M ngel oder deren Auswirkung Established Defect
153. of lighter ones When integrating chromatographic peaks this needs to be compensated by a timeshift detection trace is fixed the other traces are time adjusted to the detection trace Reference pulses however lead to square peaks Here no timeshift is necessary because they simply are fed into the open split and do not emanate from a GC column On square peaks one does not want to perform a timeshift whereas on chromatographic peaks one wants to do Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 27 Isodat 2 0 Software Creating a New Method 3 28 Finnigan GasBench Il The shape of a chromatographic peak or a square peak can be characterized by its height width ratio The factor f is dimensionless and defined as with Anw raw area of the chromatographic or square peak in Vs h peak height in V W peak width in s As square peaks and gaussian chromatographic peaks are considerably different with respect to f this factor can be used for peak discrimination It ranges between 0 and 1 A high f value alludes to square peaks a low one to chromatographic peaks Its default value 0 55 should be satisfactory for most chromatogram types In any chromatographic system however chromatographic peaks may sometimes occur which are of quite similar shape as are square peaks Thus although a peak is no square peak 1t might wrongly be identified as such In this case 1t is recommended to change
154. on that contains GasBench II e g GasBench II amp A200S Sampler refer to Creating a GasBench Configuration on page 3 4 e Select this Configuration at the Status Bar as shown below see also bottom of Figure 3 4 GesBenchil amp A200S lt x c02 x As defined in the Configurator the selected configuration GasBench II amp A200S will appear together its configured features Troubleshooting Error Messages If an error message appears at the Status bar check whether the configuration has been set up correctly The most common error messages are e Plug amp Measure devices could not been found Plug Measure Devices not found Isotope MS It typically appears when the GasBench II connector has not been plugged into the IRMS e A configuration containing the acid pump has been selected although the acid pump is not in use If you want to use this configuration anyhow you must calibrate the acid pump This is possible only in Fake Mode After this calibration a configuration containing the acid pump can even be used for equilibration measurements Thermo ar ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Isodat 2 0 Software Accessories Bar Finnigan GasBench Il 4 Isodat Acquisition File View Help D a B New ia ee Print Options The Accessories bar contains information about the TOEN MS 0 6 0 High Vokage KV y Magnet Steps IRMS 2951 A 10461 50 60 mv m MS St
155. on the Thermo Electron San Jose mailing list As a member of this list you receive application reports and technical reports in your area of interest and you are notified of events of interest such as user meetings Second it allows you to tell us what you like and do not like about the manual The Change of Location card allows us to track the whereabouts of the instrument Fill out and return the card if you move the instrument to another site within your company or if you sell the instrument Occasionally we need to notify owners of our products about safety or other issues Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Chapter 1 Preinstallation Requirements 1 1 Site and Power Requirements 1 2 Gas Requirements Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 1 1 Preinstallation Requirements Site and Power Requirements Finnigan GasBench Il 1 1 Site and Power Requirements Note Check all items mentioned below by O and confirm them by M Then send back this form to your Thermo Electron Customer Support Organization Finnigan GasBench II is attached to Finnigan isotope ratio mass spectrometers e g Finnigan DeltaP sXP and will be placed either on top of the IRMS or on a peripherals support table Gas Bench Main Module DeltaPlus XP _ Autosampler Sample Tray Figure 1 1 Site Requirements of GasBench Il Note The space required is 900 mm w
156. onents and cause a short circuit Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Contents Contents Preinstall tion Requirements aaa ae 1 1 1 1 Site and Power Requirements rennene a a a a a e a as 1 2 1 2 Gas ReQuirements aesir ona A a E R ER dhs E a EA AE 1 3 For Water Equilibrati on aiii A E avis Leeda RT 1 3 FOF Carbonales ds 1 3 For DIC Dissolved Inorganic Carbon c cccccesceesseesseeseeeseeeseceseeesecsseceeeceeeeesecseeeneeeeees 1 3 Hardware Components cscsiesisisccsciscccossssocssieesscsecssionssstetsssesasnssesnssssousssteieconsteconssetuatesdeovesecousbces 2 1 2 11 GasBench Layout rennen En A 2 2 2 2 AMOS MPa EAS RARA ANA A AAA 2 4 Installing the Autos mpler coastal dina tors hid eteuses a EES 2 5 Connecting the Autosampler ccccccccscesseeeseesseeseeeseceseceseceseeesecnseensecesecnseceseeeseseeeeseeessees 2 6 2 3 gt Sampler TAY Si ol 2 7 Layout satte ae ante i Ne needs nee eA 2 7 Programming JUMO itron 16 Temperature Controller for Sample Tray 2 11 2 44 EAS Supply A A A A A 2 13 Gases Usa A E AAA ai Pata ala heeled 2 13 Installing the Gas Tanks osin usinou a E E A an heumua 2 13 Working with the Gas Tanks euuussseesneesneenneenneennenneennennnennnennennnnnennennennnnnneennn nenn 2 14 Gas Eonnections nr ua sn ida A E 2 14 2 3 gt Measurement Needle nr ek Rai Aide tee des be ees 2 16 How t
157. ons e Select a Ref Name from your standard database e g Haus2 or edit the related values In the latter case User Defined will be shown at Ref Name More standards can be added using the right mouse button Enter the retention time in s that is Ref Time e g 90 00 of the standard peak s defined in the Time Events list which are used for calculating the corresponding 6 value s See Figure 3 15 e Ifthe assigned time for standard peak detection falls in between the Peak Start and Peak Stop marks of a peak this peak will be used for value calculation Finnigan GasBench Il Operating Manual 3 25 Isodat 2 0 Software Creating a New Method Finnigan GasBench Il Note The retention time should be based on the Reference Out time of the respective reference gas pulse in Time Events list This accomodates for the delay of 7 10 s associated with gas passage through the capillary to the IRMS Peak Detection tab Instrument Time Events Component Names Evaluation CO02 Peak Detection C02 Printout C02 Perform Peak Detection IV Perform Background Detection IV Detection on Mass 44 Figure 3 20 Peak Detection Tab Peak Detection and Background Detection e Mark the respective checkboxes if you want to perform a peak detection or background detection respectively e Type in the corresponding detection mass e g m z 44 in case of CO3 e Itis recommended to keep the defaults Detection Parameter
158. or its Effect Bitte detaillierte Angaben machen Please specify in Detail Ein Austauschteil haben wir erhalten unter Kommissions Nr An Exchange Part already received with Commission No Ja Yes Nein No Die Anlage ist au er Funktion The System is out of Function Ja Yes Nein No Durch die nachfolgende Unterschrift best tige n By signing this Document am we are certifying ich wir da die o g Teile frei von gesundheits that the a m Parts are free from hazardous sch dlichen Stoffen sind bzw vor Ihrer Einsen materials In case the parts have been used for dung an Thermo Electron Bremen dekontami the analysis of hazardous substances I we niert wurden falls die Teile mit giftigen Stoffenin attest that the parts have been decontaminated Verbindung gekommen sind before sending them to Thermo Electron Bremen Datum Date Unterschrift Signature Thermo ELECTRON CORPORATION Customer Registration Register now and receive all the privileges associated with being a Thermo Electron Finnigan product user including application reports and technical reports Name Title Company Address City State Postal Code Country Telephone Ext Tell us more Let us know more about how you use this product My Organization Is Check one only My Primary Application Is Check one only Q Commercial for profit lab A Analytical U Government lab Q Biomedical Q Hospital Clinic a Clinical
159. osampler method will result For basic information refer to Creating a New Method on page 3 17 Acid Pump Drop Count Forward E Delay s 05 Drop Count Backwards E Figure 3 25 Instrument tab Acid Pump Part As a particularity on the Instrument tab note the Acid Pump box The following parameters for acid pump control can be adjusted e Drop Count Forward number of drops pumped while the pump is in forward position that is releasing acid from the acid needle Drop Count Backwards number of drops pumped while the pump is in backwards position that is retracting acid Delay fs waiting time between two strokes To ensure that no drop remains sticking acid is first pumped in before the acid pump is switched over in order to draw it back again Due to the negative pressure a drop sticking at the tip should thus be drawn backwards into the bulk volume The GasBench PreCon A200S Sampler Method If you use Finnigan GasBench II in combination with a PreCon plus an A200S autosampler and therefore chose the GasBench Precon A200S Sampler set in the Configurator see Figure 3 24 the corresponding GasBench Precon A200S autosampler method will result For basic information refer to Creating a New Method on page 3 17 As a particularity on the Instrument tab note that the acquisition script acquisition isl is stored in a special PreCon folder Thermo 3 32 Finnigan GasBench II Operating Manual ELECTRON CORP
160. ount the autosampler display on the most convenient side of the autosampler Connect the autosampler display to the rear panel of the autosampler by the serial cable See 8 that is serial 3 in Figure 2 6 3 Connect the autosampler power supply to the mains supply and the autosampler Auxiliary 1 Combi PAL only Auxiliary 2 Combi PAL only 1 2 3 4 5 6 7 8 9 10 Interface 1 Combi PAL only 4 Interface 2 Combi PAL only 5 main power connect to autosampler power supply LED 6 7 speaker buzzer 8 Ser 3 to autosampler display 9 Ser 2 10 Ser 1 to host computer Figure 2 6 Syringe Carrier Rear Panel GC PAL or Combi PAL Thermo 2 6 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Sample Trays 2 3 Sample Trays m pa lt O c gt O0O00O O000O O00O J000 C200 0000 rra tor PA PP I 2 dh rro PA Lid o OOOO 0000 0000 0000 0000 0000 0000 0000 gt 0000 0000 no dropping no measurement Figure 2 7 Schematic of Autosampler Movement across the Trays Ex Factory The trays contain 96 holes e spacing of the holes is 26 mm 26 mm e diameter of the holes is 16 mm e depth of the holes is 85 mm Per default Finnigan GasBench Il is delivered with a non thermostated sample tray Part No 111 2780 suitable for equilibrium work or breath gas analysis See Figure 2 8 and Figure 2 9 ELECTRON CORPORA
161. ource before reducing the He pressure Trapping of N at 196 C Liquid nitrogen can be adsorbed on silica gel or nickel surfaces at about 196 C Thus it is possible to collect and cryofocus nitrogen for analysis by using a trap operating with liquid nitrogen The trap used with GasBench II is equipped with a nickel wire to perform N trapping Note When applying this kind of trap keep in mind that other air compounds like CO or water will also be collected therein Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Thermo ELECTRON CORPORATION Chapter 7 Technical Information Note This section is intended for use by trained Thermo Electron Bremen personnel only Thermo Electron Bremen discourages use by and denies liability for the consequences of use by other than Thermo Electron Bremen personnel 7 1 Spare Parts and Consumables for GasBench II 7 2 Mechanical Parts 7 3 Plug and Measure Adapter 7 4 Capillaries 7 5 Water Traps 7 6 Reference Open Split 7 7 Sample Open Split 7 8 IAEA Primary Standards 7 9 Compressed Air Schematic Finnigan GasBench Il Operating Manual 7 1 Technical Information Spare Parts and Consumables for GasBench II 7 2 Finnigan GasBench Il 7 1 GasBench Il Spare Parts and Consumables for Table 7 1 lists the spare parts and consumables for Finnigan GasBench II available as kit with Part No 113 6810 facilitating the selection of
162. ple SE 1 750 2 Invert the measured value for primary standard versus gas used Bon 1 908 Thus Bere 1 903 3 Determine absolute 6 value of gas used today with the aid of the equation 5 8 x _ ty zZ 5 9 2 1000 y Thus Sn 0 157 4 Use this value and any measured sample 6 vs Ref Gas to calculate value of sample vs PDB with the aid of Thermo 5 14 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Measurement Procedures for Real Samples Carbonates vw amp Sl L Zo 8 1000 y z Thus Sbp ee In this case the result is incorrect Remark on the Strange Mathematics of Delta Values The 6 definition with 9 5 value of x against y R raw ratio of x that is A 3 Aj gt can be rearranged As x and y are only arbitrary notations and thus can be interchanged an analogous equation for 5 can be written R Se R 1000 Considering reciprocity R __ 1 R RR combination of both equations yields the relationship between 5 and 5 we were aiming at 01 i 1000 5 1 1000 This shows indeed y y Finnigan GasBench Il Operating Manual 5 15 Measurement Procedures for Real Samples Carbonates Finnigan GasBench Il The 6 definition results in the following rule when calculating a 6 value with an intermediate result which is always the case when referencing to a gas or a wor
163. power where n 1 through 10 mass to charge ratio nano 10 National Center for Biotechnology Information USA National Institute of Standards and Technology USA outside diameter ohm pico 10 pascal printed circuit board proportional integral differential part number Finnigan GasBench II Operating Manual xi Read This First Abbreviations Finnigan GasBench Il xii P P ppm psig RAM RF RMS ROM RS 232 s SIM solids probe SRM ss SSQ TCP IP TIC Torr TSQ u URL peak to peak voltage parts per million pounds per square inch gauge random access memory radio frequency root mean square read only memory industry standard for serial communications second selected ion monitoring direct insertion probe selected reaction monitoring stainless steel single stage quadrupole transmission control protocol Internet protocol total ion current torr triple stage quadrupole atomic mass unit uniform resource locator volt volts alternating current volts direct current volume width watt World Wide Web Note Exponents are written as superscripts In the corresponding online Help exponents are sometimes written with a caret or with e notation because of design constraints in the online Help For example MS in this manual Ms n in the online Help 10 in this manual 1075 in the online Help Finnigan GasBench Il Operating Manual Thermo E
164. predefined sequences to cover all kinds of measurements 05 07 03 16 49 38 05 07 03 16 49 37 05 07 03 16 49 37 05 07 03 16 49 37 05 07 03 16 49 37 05 23 01 14 20 48 05 23 01 14 22 06 01 25 01 15 39 40 05 22 01 14 58 40 01 25 01 14 32 48 Click on File Browser s Sequences tab Select the location where your own GasBench Il sequences are to be stored Do not mix them up with the predefined sequences in the folder Examples e Double click on your example sequence of choice e g Carbonates seq File Browser Displaying Predefined Sequences for GasBench Il Instead of double clicking on the example sequence of choice drag and drop it to the Isodat Acquisition window right to the File Browser The sequence grid will be displayed Select between the following example sequences e Carbonates seq for all carbonate measurements e Equilibration seq for all equilibration measurements e Flush Fill seq for flushing the samples prior to measuring them that is during their preparation H2 zero seq as Zero seq but uses H2 as gas configuration to test the basic functions of the IRMS The reference gas is just switched on and off several times e g 10 or 100 pulses and one watches the obtained result The more pulses you apply the more exact is the result e Zero seq The sequence for carbonate measurements Carbonates seq differs just slightly from the one for equilibration measurements Equilibration seq in
165. pressure 10 15 psi helium flow 3 4 ml min GC column temperature 50 60 C Step 1 Accessing the GC Column Currently the GC column is a static part of GasBench II as it nearly never needs to be exchanged Only maintenance is necessary from time to time The GC oven is located at the right side of GasBench II front view When inserting the GC column for the first time or when exchanging it first remove the cover ofthe GC oven that is right side panel of GasBench II Therefore unscrew all seven screws using an allen wrench See Figure 2 29 Figure 2 29 GasBench Il Right Side Panel Being Opened Thermo Dr ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Hardware Components GC Oven Finnigan GasBench Il Figure 2 30 GasBench Il Right Side Panel Removed Afterwards only remove the two screws marked by arrows in Figure 2 30 Note Leave the remaining four screws that are marked by white circles untouched as they hold the isolation of the GC oven Figure 2 31 Grounding Cable of Right Side Panel Thermo 2 28 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il GC Oven Each side panel has a grounding cable of its own to guarantee electrical security Each grounding cable must be connected as shown in Figure 2 31 as an example for the right side panel Furthermore the top side and the oven housing are grounded as well Step 2 Changing the G
166. quilibration H D 5 7 Water Equilibration H D H D Equilibration in Brief n ar screw Cap JL aD 200 pl aqueous In S sample Mos AY m Ps u m Pic Pues 206 i of ma sangpu w Auld Mon pistenen stern Pere of sample vich a a De viel wine Burt wie the name Voy gt Chase me meer AD cial mo atmet sby Menton He He H 1H transfer from gt r z H O into H In the headspace i am um Analysis m AN Y EEE EEE S bun me 1equercs gr Don Figure 5 29 Sample Preparation for H D Equilibration In case of any hydrogen equilibration perform the following steps keeping the tray at room temperature see Sample Tray Temperature Control on page 5 31 e Insert the sample into the vials and insert the catalytic platinum sticks e Flush all samples with 2 H in He Run a flushing sequence See Creating a New Sequence on page 3 34 The equilibration is finished within 40 min It is not necessary to wait additional time Exchange the rinsing needle with the sampling needle There are various needle sets using the same needle type one set of needles exists for flushing that is rinsing needle and another one for measuring that is sampling needle The rinsing needle is used to rinse the vials the recurrent capillary must be broken off at 20 cm to let the rinsing agent pass into ambient air In case of the sampling needle the recurrent capillary leads into GasBench II Runa m
167. r 7 8 polarity 5 4 PoraPlot Q GC column 2 26 4 12 5 4 7 19 power consumption 1 2 Pre Cln Slv 1 3 50 Pre Cln Slv 2 3 50 Pre Cln Spl 3 50 Pre Inj Del 3 50 PreCon 3 11 3 32 to 3 33 pre concentration trap 6 13 pre concentration unit 6 12 to 6 13 predefined method 3 14 3 17 to 3 18 3 29 to 3 30 3 40 predefined sequenc 3 29 predefined sequence 3 14 3 34 3 36 to 3 37 3 39 to 3 40 pre pressure 2 13 preprocess file 4 14 pressure gauge 2 2 pressure loss 2 13 pressure reducer 7 16 pressure regulator 2 2 2 13 to 2 14 7 16 pressure variation 2 26 primary standard 5 13 7 14 print template 3 29 printout 3 38 printout per sample 3 38 printout per sequence 3 38 printout tab 3 19 3 29 printout template 3 29 4 6 protection capillary 2 37 Pst Cln Slv 1 3 50 Thermo ELECTRON CORPORATION Pst Cln Slv 2 3 50 Pst Inj Del 3 50 Pullup Del 3 50 pullup delay 3 50 pump head 6 2 pump stroke 6 5 pumping volume 6 5 Puranal 5 16 purge 2 2 2 14 purity 2 13 Pyrex 5 16 Q quality control 5 13 quick release connection 2 15 R ratio baseline 4 6 ratio group 3 3 raw area 3 28 raw data 5 10 to 5 11 raw ratio 5 15 reaction time 5 8 real 5 value 5 10 5 12 rear panel 2 6 recurrent capillary 5 33 reducing valve 2 14 7 2 ref time 3 25 reference capillary 2 35 reference gas 1 3 2 13 to 2 15 2 34 to 2 35 3 19 to 3 21 3 39 5 3 5 5 5 10 5
168. re components Set or reset hardware com ponents at any time even during an ac quisition Figure 3 5 The GasBench Window Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 11 Isodat 2 0 Software Accessories Bar Finnigan GasBench Il Click on a graphical object to operate the specific devices as there are e flush fill valve e valco valve e open split e reference ports or traps The Acid Pump Window Note If GasBench II is used with an acid pump the corresponding configuration containing the acid pump must be selected in the configurator first Beneath the GasBench window the Acid Pump window will appear Figure 3 6 Acid Pump r Direction FEEL Fore A e Figure 3 6 The Acid Pump Window The number of acid drops per stroke needs first to be adjusted at the acid pump itself see Acid Pump Adjustment on page 6 5 Then this number must be communicated to Isodat 2 0 Therefore right click somewhere into the Acid Pump window Click on the appearing Calibrate button Calibrate Acid Pump Strokes pet Drop fio e Type in the number of acid drops per stroke adjusted at the acid pump default is 10 and confirm by OK Thermo 3 12 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Accessories Bar Figure 3 7 The Stroke Button Stroke j Stroke When you press the S
169. ron 16 temperature controller 2 2 2 4 K Kiel Carbonate device 2 3 knurled nut 6 2 7 3 L leak 1 3 2 14 4 4 4 6 leak check 2 14 4 2 4 4 leaktight 5 18 leaktight connection 6 6 LED 2 6 left needle 5 6 lifetime 2 13 light isotope signal position 3 27 LIMS 3 15 line distributor 1 2 line pressure regulator 2 13 linearity correction 5 10 to 5 11 linearity test 5 6 liquid nitrogen 5 3 liquid nitrogen trap 5 3 liquid phase 2 15 5 2 to 5 4 5 10 load mode 2 22 to 2 24 4 5 4 14 5 3 6 7 to 6 8 long term drift 5 31 loop injection 4 12 5 2 loop size 2 23 to 2 24 4 12 loop switch 4 14 low memory 3 38 Finnigan GasBench II Operating Manual V Index Finnigan GasBench Il low pass filtered background 3 27 lower inlet port 2 15 M m z 16 4 3 m z 17 4 3 m z 18 4 3 m z 2 5 34 5 36 to 5 37 m z 28 4 3 to 4 4 m z 3 5 34 m z 32 4 3 m z 40 4 3 m z 44 4 4 4 6 m z 46 5 10 5 22 magnet current value 4 3 to 4 4 magnet position 3 3 magnet step 4 2 5 34 main fuse 2 2 main gas supply 2 14 main power 2 6 main power plug 2 2 main power switch 2 2 main valve 2 13 to 2 14 maintenance 2 27 manometer 2 13 manometer position 2 14 manual switch 6 5 masking out 5 29 mass balance calculation 5 38 to 5 39 mass difference 5 36 mass scale 5 34 mass scan 4 2 to 4 4 MAT 253 4 10 Material Safety Data Sheet 5 20 mathematical correct
170. sBench Method aia daros 3 31 The GasBench A200S Sampler Method suesseeeseenseessensnnnnnennnnnneennee nennen 3 31 The GasBench Acid Pump A200S Sampler Method ooooocionnnonnnononononnnononononnnononons 3 32 The GasBench PreCon A200S Sampler Method u220sseenseenseeneenneennn nen 3 32 Thermo ii Finnigan GasBench II Operating Manual ELECTRON CORPORATION Contents Finnigan GasBench Il 3 7 Creating a New Seguite soria AA EA 3 34 Daving a Seqlence uun1ennn sd Brennen BT 3 36 Sara a OUEN leia 3 38 Predefined Sequences as Examples cccccccecsessessseesseeseeeseceeeeseeeseeeeeeseseseeeseenseenseesseenes 3 39 308 EXCEL EXP OM nina ld ca 3 41 3 9 Autosampler Programming usesensesssesssensnennennnnnnennennnnnnnnensensennsnnseensesnsensensnonsnnen 3 42 GOPAL Loader Software sr Rinne nme 3 42 First Touch a EN sie RAN Geil E aetna paar R 3 43 Adjusting Autosampler Tray Position ccccccsccsssesseeseceseeeseeeeceseeeseeeseeseeeneeeseeeseeseeens 3 49 Using Autosampler Method 220susessessnsensnsennsensennennnnsensennennennnnennsennnnnnnn 3 50 Testing the Autosampler lirio orense 3 51 Basic Operations A dia 4 1 4 1 SEeakECheck ran len eyes a ren near ehe este l ge dee een 4 2 Water Narnia dhe bei Went he es tao eas 4 3 PTI seca ELLE IR SEELE EREERS SURCTERTER ANA AIG Li sR he Net Pate 4 3 SS Oe eR EN EE ELT Re ses yes Ren TVR ner Te
171. sh Fill for 300 s if the flow is 100 ml min Adjust the time to smaller values if the flow is higher or to higher values if the flow is lower For details refer to Figure 7 5 and to Figure 7 6 Thermo 7 16 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il F L JF i E HE I WW i H Hop Figure 7 8 Thermo ELECTRON CORPORATION ya NI ey J Technical Information Compressed Air Schematic aa i ee o O o E Finnigan GasBench Il Operating Manual Tubing Scheme of GasBench Il until Year 2002 Outdated Part N
172. sport through GC column and inlet capillaries A and due to separation processes on GC column retention time v 1 50 100 150 200 250 300 350 400 450 Figure 3 17 Timing Considerations Component Names tab Instrument Time Events Component Names Evaluation CO2 Peak Detection C02 Printout C02 c43 xE Figure 3 18 Component Names tab Thermo 3 24 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Creating a New Method e Hitherto it is of no importance for GasBench applications because only one sample gas is investigated e The Component Names tab is mostly important for GC measurements as many different substances having retention times of their own can be eluted from the GC column If the system is sufficiently stable each retention time can be assigned to its corresponding component that is substance Isodat 2 0 is supposed to find and designate each substance in the chromatogram Evaluation tab Instrument Time Events Component Names Evaluation C02 Peak Detection C02 Printoutt Evaluation Type CO2_SSH y gt 41301120 vs 4180 1060 vs 30 260 VPDB 25 540 vsmow Figure 3 19 Evaluation tab e At Evaluation Type select an appropriate ion correction for CO data evaluation from the list that is None SSH Craig or IAEA e Press the gt button to add own scripts for ion correcti
173. t is possible to introduce traps for cryofocusing methane and other trace gases in air mixtures or to determine 13C concentrations in breath gas The abilities in equilibration of oxygen and hydrogen isotopes can widely be used in food authentification The GasBench II system consists of e auser programmable autosampler e a gas sampling system e a maintenance free water removal system e a loop injection system e an isothermal gas chromatograph GC e an active open split interface Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Introduction e areference gas injection system with three reference ports e an optional LN2 trap for cryofocusing e an optional acid dosing system Water Removal 1 H O Reference Injection T 3 Ref Gases He Water Removal 2 Active H O Open Split Tr He H O He Autosampler 96 Vials Column 100 pl Loop Figure 5 1 Schematic of GasBench II Components LN2 is an abbreviation for liquid nitrogen Gas flow of GasBench II in Load Mode The sample loop is filled with the analytic mixture refer to Principle of Valco Eight Port Valve on page 2 22 Note For a description of the basic principles of Continuous Flow see Habfast K Advanced Isotope Ratio Mass Spectrometry I Magnetic Isotope Ratio Mass Spectrometers Chapter 3 in Platzner I T ed Modern Isotope R
174. t most ofthe sample can be measured Overall this change between on and off positions takes place ten times Acquistion Start immense I Acquistion End Times en H Figure 5 23 CO in Atmospheric Concentrations Time Events tab Acquisition Results Fe Mana Y Merrad Dina Bard E Oparsing Mirad Er ctra cf 4 2 Ema EA fee ta far eet tea 3 s6 m2 189 149 67 769 00 u jar fair 062 186 eso 153 67713 ooo ooo wer is fae Je me Jever Tan abr e hez ame ing piz jara 1900 fiese 3a aos face oe emo fas ir rior ses 504 2 9202 248 15 087 17 109 33 565 9 esoo esto os ess me asima mee 0 78 as a3 les 208 12137 17210 30574 m Is a47 96 eam CONEA E faen 12 1100 3 1104 5 gt 19 3 17 384 sa 13 1247 8 1251 6 18 3 17 208 Figure 5 25 CO in Atmospheric Concentrations Result Grid Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 29 Measurement Procedures for Real Samples Water Equilibration 120 5 30 Finnigan GasBench Il 5 6 Water Equilibration 190 180 Equilibration in Brief Fill the sample into the clean open exetainer vial 10 ml by using an adjustable pipette with disposable pipette tips It is not necessary to pierce the septum using the needle The filling volume should be 0 5 ml Close the vial and place it into the autosampler tray The flushing gas is a mixture of He and CO that usually has already been properly mixed
175. than 0 1 o for both 8 1 C and 6 180 Thermo re ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Basic Operations Frequently Asked Questions Finnigan GasBench Il 4 7 Frequently Asked Questions Note From time to time take a look at the checklist shown below It outlines the performance achievable by the system GasBench II plus IRMS Check all mentioned items 1 A basic test must be performed that is testing the IRMS alone 2 Perform a zero enrichment test outlined in Zero Enrichment Test Standard On Off Test on page 4 6 3 Carry out a linearity test as described in Linearity Test on page 4 10 4 Ensure that also the sample side that is valco valve GC column operates properly by performing the Condition test as described in Condition Test on page 4 12 5 Carry out a Zero Enrichment test with vial The filling can be done manually or automatically 6 Only if all the previous items are performed to specifications carry out the measurement Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Chapter 5 Measurement Procedures for Real Samples 5 1 Introduction 5 2 Carbonates 5 3 Dissolved Inorganic Carbon DIC 5 4 Breath Gas Analysis 5 5 CO in Atmospheric Concentrations 5 6 Water Equilibration 0 5 7 Water Equilibration H D Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 1 Measurement Procedures for Real Samples Introd
176. the Terms and Conditions shall govern Reference to System Configurations and Specifications supersede all previous information and are subject to change without notice Printing History Revision A printed in 9 28 04 Thermo ELECTRON CORPORATION The products of Thermo Electron Bremen are produced under ISO 9001 accredited quality management systems Australia P O Box 239 Rydalmere e Unit 14 38 46 South Street e Rydalmere N S W 2116 e 61 02 9898 9000 Austria Wehlistrasse 27b e A 1200 Wien e 43 01 333 50 34 0 Belgium Technologiestraat 47 e B 1082 Brussels e 32 02 482 30 30 Canada 5716 Coopers Avenue Unit 1 e Mississauga Ontario e L4Z 2E8 e 1 905 712 2258 France 16 Avenue du Qu bec e Silic 765 e Z A de Courtaboeuf e F 91963 Les Ulis C dex e 33 01 60 92 48 00 Germany Im Steingrund 4 6 e D 63303 Dreieich e 49 06103 408 O Italy Strada Rivoltana e I 20090 Rodano Milano e 39 02 95059 226 Japan C 2F e 3 9 Moriya cho Kanagawa ku e Yokohama Kanagawa e 221 0022 e 81 45 453 9100 Japan Esaka Grand Building e 2 3 1 Esaka cho Suita City e Osaka 564 0063 e 81 06 6387 6681 Netherlands Takkebijsters 1 e 4817 BL Breda e 31 076 5878 722 P R China Room 901 Ping an Mansion e No 23 Jin Rong Street e Xi Cheng District e Beijing 100032 e 86 010 6621 0839 Spain Sepulveda 7 A e ES 28108 Alcobendas Madrid e 34 091 657 4930 Spain Acer 30 32 e Edificio Sertram Planta 2 M
177. the default value of f e Mark the Enable checkbox to automatically 1 detect square peaks and 2 suppress the timeshift correction of square peaks e Ifyou unmark Enable and simultaneously mark Perform Timeshift timeshift correction will be enabled for all peaks As default Enable is unmarked because old chromatograms might have been calculated without automatic square peak detection In case of recalculating them Enable can be marked to include now automatic detection If Perform Timeshift is unmarked no timeshift correction will be performed on any peak Decide whether you additionally want automatic square peak detection suppression of timeshift correction to be performed or not As an example you can perform a timeshift and additionally let the square peaks be automatically detected If you do not want to detect them automatically you can define ranges instead where a timeshift will be performed or not e g in case of many different peak shapes one single factor f might not be sufficient Marking Enable is only useful if you simultaneously also mark Perform Timeshift Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Creating a New Method Printout tab Instrument Time Events Component Names Evalustion C02 Peak Detection C02 Printowt C02 m Printout Templates Single Default Result ew g Sequence Tg Figure 3 23 Printout tab e In Pr
178. the following example which is taken from A200S 8 method result in a sampling time of 682 s Cycle Syringe Sample Volume Air Volume Pre Cln Slv 1 Pre Cln Slv 2 Pre Cln Spl Fill Soeed Fill Strokes Pullup Del Inject to Inject Speed Pre Inj Del Pst Inj Del Pst Cln Slv 1 Pst Cln Slv 2 Viv Clin Siv 1 Viv Cln Slv 2 Finnigan GasBench Il Operating Manual LC Inj 10 ul 1 0 ul Onl 0 0 0 5 0 l s 10 62s NONE 50 ul s Oms Oms oO Oo O Thermo ELECTRON CORPORATION Finnigan GasBench Il Thermo ELECTRON CORPORATION Isodat 2 0 Software Autosampler Programming Testing the Autosampler For a convienient test of the autosampler s communication independently of Isodat 2 0 perform as follows l A Hyperterminal can be found in the Start Menu under Start gt Programs gt Accessories gt Communications gt Hyperterminal Use the following settings COM 1 9600 baud 1 stop bit no parity Type in the following command 010000 request status The autosampler should respond with 010001 STANDBY or 01w002 READY BUSY if w gt 0 Finally order the sampler to Execute method M on Sample NNN in TRAYOI 99MNNN Finnigan GasBench Il Operating Manual 3 51 Isodat 2 0 Software Autosampler Programming Finnigan GasBench Il Thermo 3 52 Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Thermo ELECTRON CORPORATION Chapter 4 Basic Operations 4 1 Leak Chec
179. ticular sample a This ensures the peak to be in the middle of the cup As this standard procedure is time consuming save a lot of time by omitting some peak centers The device is sufficiently stable to operate during a certain time period without a peak center AS Sample position of the sample to be measured The number between 1 and 96 corresponds to the sample s position in the tray See Sample Trays on page 2 7 Figure 2 7 and Figure 2 11 AS Method Autosampler method can be selected from the pulldown list In most cases only the internal methods that is Internal No 1 to Internal No 9 are in use Usually even only two or three ofthem are applied After setting up the autosampler with the corresponding backup file Autosampler method Internal No 7 corresponds to Flush Fill met Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 35 Isodat 2 0 Software Creating a New Sequence 3 36 Finnigan GasBench Il Autosampler method Internal No 9 corresponds to Acquisition 630s met Autosampler method Internal No 8 corresponds to Acquisition met old method no longer recommended Thus in a sequence used for flushing always select method Internal No 7 in each line In a sequence used for all kinds of measurements always select method Internal No 9 in each line or method Internal No 8 in each line but no longer recommended Identifierl 2 optional mostly used to identify the particular sampl
180. troke button a single stroke of the acid pump will be carried out The Stroke button usually grey changes its color to green for the duration of the stroke and returns to grey afterwards r Direction Direction Fore Back Figure 3 8 Positions of the Direction Button You can switch between the positions Fore and Back by pressing Direction button Both buttons are used to directly control the acid pump When you try them for the first time check via Direction button whether the acid pump rotates forward by switching to Fore Stroke button controls rotation of the acid pump A specific number of rotations is needed to produce one drop of acid This number must be determined by the user and then saved in the Isodat 2 0 database using the Calibrate button It appears after right click on the acid pump window The File Browser File Browser 05 07 03 17 49 37 06 26 03 12 15 47 C Time Event List 05 07 03 17 49 37 05 07 03 17 49 37 h v un z o 4 op 2 ra Figure 3 9 File Browser Finnigan GasBench Il Operating Manual 3 13 Isodat 2 0 Software Accessories Bar Finnigan GasBench Il 3 14 The File Browser also called File Browser bar comprises six tabs Methods tab Refer to Creating a New Method on page 3 17 e Methods provide the complete description of a single measurement e Methods can be programmed or changed by the user Different methods have been predefined in the Examples folder of the
181. tune your instrument to optimal conditions in every run or apply a mathematical correction for the effects The effects that influence fractionation of masses by the system include temperature first of all Temperature variations change the viscosity of He and thereby affect flow speeds They also change the 6 value of your reference gas if you use a pressurized CO tank with a liquid phase inside Note Refer to Grootes P M Mook W G and Vogel J C Isotopic fractionation between gaseous and condensed carbon dioxide Zeitschrift fiir Physik 221 257 273 1969 Experiment to experiment variations of fractionation occur if you tune the source or change the timing of the acquisition More reasons for applying corrections to the signal to 6 value scale and to the measured to real 6 value scale can easily be found This section Linearity Correction covers the relationship between measured 6 value and signal height The relationship between measured 6 value and real 6 value will be covered in section Referencing versus VPDB on page 5 13 Figure 5 6 shows an uncorrected result that is raw data from a series of measurements of the same sample Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Carbonates Position Bottle Number Weight Average Area ee 8 0 1 dummy sample 0 11 40 39 332 5 838 2 dummy sample 0 16 46 39 662 0 380 3 dummy sample
182. ty u purifier Part No 114 0790 to ensure constant and affordable high quality of the helium carrier gas Thermo 1 3 ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Chapter 2 Hardware Components 2 1 GasBench II Layout 2 2 Autosampler 2 3 Sample Trays 2 4 Gas Supply 2 5 Measurement Needle 2 6 Flush Needle 2 7 Mounting Syringe Needles into Autosampler 2 8 On Line Water Removal 2 9 Principle of Valco Eight Port Valve 2 10 GC Oven 2 11 Open Splits Thermo a ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Hardware Components GasBench II Layout Finnigan GasBench Il 2 1 GasBench Il Layout 1111 1212 front panel 345 6 7 8 9 10 Figure 2 1 GasBench Il Unit Front and Left Side View pressure regulator e g reference gas 1 pressure gauge e g reference gas 1 main fuse main power plug main power switch on off JUMO itron 16 temperature controller cable for connection to IRMS gas connection terminal refer to Figure 2 14 SOS A NA A oa fan connection terminals for sampling needles 11 sample purge 12 purge Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il GasBench Il Layout Figure 2 2 GasBench Il with Kiel Carbonate Device and DeltaP S Advantage Front View Figure 2 3 GasBench Il General Survey Open Thermo Se ELECTRON CORPORATION Finnigan GasBench
183. ual 6 1 Options Carbonate Option Table 6 1 Quantity 1 1 1 1 500 g 1 1 1 1 1 package 1 sample 1 2 2 6 2 Finnigan GasBench Il 6 1 Carbonate Option Components The carbonate option Part No 113 2471 is used to measure C and 80 values simultaneously from carbonates It allows for fully automated measurements of calcite dolomite foraminifera or bulk sediments and contains the following components Carbonate Option Part No 113 2471 Components Designation Part No Acid pump with connections 113 7301 Pump head for acid pump 115 7620 Acid needle 113 7030 Phosphoric acid PK500GR 111 2640 Acid reservoir with tubing 113 7070 Double needle holder for autosampler complete 113 7080 Knurled nut M8 111 9170 Hollow nut with drilled hole 1 16 113 7390 Sample vials borosilicate glass washed 116 8790 CaCO as working standard 114 7090 Bulkhead connection SERTO 2 mm 114 1450 O ring 1 5 1 5 114 1460 O ring 2 1 5 114 7070 A package sample vials made of borosilicate glass washed consists of 100 sample vials and 400 septa to hermetically close the vials Placement of the Components e Place the acid reservoir in the rightmost row of the sample tray and the acid pump behind the tray Connect them using the tubing supplied with the reservoir e Do not cut the tubing length The small diameter tubing is for venting the reservoir Place it beneath the cover of
184. uction 5 2 Finnigan GasBench Il 5 1 Introduction General Remarks Finnigan GasBench Il is an universal on line interface which allows automated isotope ratio determination of small gas samples isotopic characterizations of CO or N between 200 nmol and 20 mmol of total sample size The gas i e CO can either e be part of the original gas sample e g breathed air or e be released from liquid or solid phase into the headspace of the sample vial by different sample preparation methods for DIC carbonates or e be added to the original water sample equilibration Using a gentle stream of helium the CO in the headspace of a sample container continuously passes through a Valco sampling port Multiple analysis is achieved by switching the contents of the sample loop into a GC column every 90 seconds Each switch corresponds to starting GC separation of the sample coming from the loop GasBench II is supported by a Combi PAL autosampler for fully automated transfer of the gas samples which are contained in a sample tube with a septum top GasBench II covers a large variety of application areas The same device can be used in e Hydrology determination of 180 and D H from water samples e Global Change Research 13C determination of dissolved inorganic carbon DIC from ocean water or fresh water or e Paleoclimatology simultaneous 180 and 3C determination from carbonates of various sources Furthermore i
185. update The autosampler related file PAL GASBENCH V2 33 021031 sss will be installed automatically This may last some minutes Thermo Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Autosampler Programming First Touch e The autosampler s display shows four function keys F1 F2 F3 and F4 See Figure 3 31 e Pressing a function key leads to a specific submenu where F1 F2 F3 and F4 may have completely different meanings e Thereby a wide branched system of commands is accessible Figure 3 31 Autosampler Display General Menu Title Figure 3 32 shows the Job Cursor bars highlight meaning of the four an item in a Ist function keys in the Start Menu Function Key Definitions e F1 Menu Function K F2 Add Job F3 Delete Job F4 Start Press STOP to abort operation __ Press the inner knob to select an item highlighted by the cursor bars Press again to ENTER the selection Rotate the outer knob to move the cursor bars Press ESCape to return to the previous menu Figure 3 32 Autosampler Display Start Menu Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 3 43 Isodat 2 0 Software Autosampler Programming Finnigan GasBench Il e To find an individual parameter within the autosampler s memory press the Menu button FT on the autosampler s panel e You will see a menu on the panel that allows to
186. via ports213161 7 e The GC column is directly connected to the LOOP IN He pressure via ports 5 4 VENT Figure 2 23 Valco Eight Port Valve Load Mode Thermo 2 22 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Hardware Components Finnigan GasBench Il Principle of Valco Eight Port Valve INJECT mode LOOP 2 Inject Mode IN CO e The gas content of the sampling loop is He directly transferred onto the 3 GC column by the GC flow e g 2 ml min via ports 516 314 VENT e The sample flow is directly connected to Vent via ports 2 1 Y y X LOOP OUT Figure 2 24 Valco Eight Port Valve Injection Mode How to Change the Loop Size Note Refer to the valco documentation that is Valco Instruments Co Inc VICI Technical Note 201 Operation Notes and Cleaning Instructions It is part of your equipment Warning Make sure the Valco is in Load Mode Changing the loop in Inject Mode will interrupt the GC column flow This will cause damage to the GC column Warning Always use Valco stainless steel ferrules for mounting the loop Thermo 5234 ELECTRON CORPORATION Finnigan GasBench Il Operating Manual Hardware Components Principle of Valco Eight Port Valve Finnigan GasBench Il The arrows in Figure 2 25 show the two screws which fasten the loop 1 chequered screw is used to fix the internal rotor which is flexibly fitted within in the stator by a co
187. vs VPDB vs VSMOW 330 476 6 385 7680 9 220 6 333 0 0119856 0 0525950587 0 4434196816 0 m al DN 18 362 s lo j gt 01198 10000000 0 0000000 25 267 0 0119852 0 0363528147 0 1012398761 708 059 Sje ola 00 663 908 2190 3 E 3 7 329 8 9 10 11 P sza 87 02008020952 13 248 79 126 0 0119847 0 0050016053 0 3098256787 oonga 0 2 4021 943 114933 0 633 11 442 14 048 0 0119846 00085581097 0 370876399 11 10 058 00053447480 0 4006704781 az 11310 09265860027 0200177208 8 Figure 4 6 Linearity Test Result Grid Thermo 4 10 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Finnigan GasBench Il Ay Fill Grid with Data M Columns Ex Fit Cells to Grid Fit Cells to Text o TA Font amp Print Gad wki Export Y Excel Export ASCH Export Cut BD Copy A Pasta Calculate Results Regression Slope Regression Offset Thermo ELECTRON CORPORATION 0 008 0 008 0 027 0 008 042 Basic Operations Linearity Test To obtain the slope of all ten peaks e Click on the column header e g of the d 13C 12C per mil vs VPDB column It will be highlighted completely The same principle is valid for the d 180 160 per mil vs VSMOW column e Right click on the column header e Choose Calculate d 130 120 FET Note The slope should be less than 0 05 o V Finnigan GasBench Il Op
188. ware Autosampler Programming Finnigan GasBench Il mn a R EBLE iid al fa ll dbl el gt Pulse Time sight 5 BHT The standard softwere does not ndude all Objects as shown in the Overview The layout depends on the hardwere configuration for each individual PAL System Revision C Firmware 2 3 1 November 2000 Figure 3 34 Adjustment Possibilities of Autosampler Tree of Hardware Commands Objects Submenu 3 48 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Autosampler Programming Figure 3 33 and Figure 3 34 have been taken from CTC Analytics PAL SYSTEM User Manual Adjusting Autosampler Tray Position Note This is to readjust the GasBench tray In general the trays are predefined and preinstalled using the file PAL GASBENCH V2 33 021031 sss under Isodat 2 0 See GC PAL Loader Software on page 3 42 If preinstallation and configuration have already been performed redirect into the autosampler s menu via ESC See First Touch on page 3 43 e Remove the needles to avoid damaging them e Click Home gt Manual Setup gt F3 gt Object Trays gt Tray 01 e Click Home gt Manual Setup gt F3 gt Object Trays gt Holder Two tray holders will appear Gas Bench tray holder without numerical designation and Gas Bench tray holder 2 E g GasBench tray holder 2 is for a 96 sample tray setup with a specific sample positioning This posit
189. y 5 10 acetone 5 5 acid dosing 2 8 3 22 5 3 5 6 6 5 acid drop 3 12 3 39 acid needle 4 13 5 8 6 2 6 6 7 2 7 19 acid needle tubing 6 3 acid pump 3 9 3 11 to 3 13 3 32 6 2 to 6 3 6 5 acid pump adjustment 6 5 acid pump box 3 32 acid pump control 3 32 acid pump housing 6 5 acid pump window 3 12 to 3 13 acid reservoir 2 9 6 2 acid wasting 5 18 acqisition script 5 5 acquisition 3 11 3 23 4 6 4 14 5 10 5 29 acquisition 630s mod for air met 5 28 acquisition 630s met 3 18 3 36 3 40 5 28 to 5 29 acquisition cycle 3 20 acquisition data 3 15 acquisition end time 3 23 acquisition method 4 6 4 14 acquisition mode 3 7 3 17 acquisition script 3 15 to 3 16 3 20 3 32 4 6 5 5 acquisition start 3 23 acquisition time 5 8 acquisition window 3 7 to 3 8 3 18 3 39 5 28 acquisition isl 3 15 to 3 16 3 20 3 32 Finnigan GasBench II Operating Manual Index Finnigan GasBench Il acquisition met 3 18 3 36 3 40 activation amplitude window 3 21 active open split 2 37 active temperature control 5 31 additional hardware 3 21 agitator 3 45 air 4 4 5 4 to 5 5 air contamination 4 6 air leak 4 4 air mixture 5 2 air peak 5 18 5 29 air volume 3 50 allen wrench 2 27 aluminum foil 5 5 ambient air 5 33 6 12 ambient temperature 3 18 amplitude 4 6 Analytical Quality Control Services 7 14 aragonite 5 6 Araw 3 28 argon 4 4 argon tank 1 3
190. y Background Parameter Start Slope mVs 2 Background Type ravieuteco z End Siope mVis 24 History s is Peak Min Height mv fo Peak Resolution a x Max Peak With 2 iso Perform Timeshift Vv Figure 3 21 Peak Detection tab Peak Detection Parameters Notice the peak detection parameters that is virtual parameters used in peak detection Default values for Start Slope End Slope Peak Min Height and Background Type are shown above and can usually be accepted e Start slope mV s and End slope mV s are used to control the portion of the peak that is included in the integration Lower values will result in capturing more of the peak slopes Note Higher start slopes that is 1 2 mV s instead of 0 2 mV s for other applications and end slopes that is 2 4 mV s instead of 0 4 mV s for other applications have experimentally proven to yield a slightly smaller standard deviation in the final result over the ten repetitions performed in every chromatogram This is valid for systems running stable for a longer time Thermo 3 26 Finnigan GasBench II Operating Manual ELECTRON CORPORATION Isodat 2 0 Software Finnigan GasBench Il Creating a New Method Peak Min Height mV limits the number of reported peaks as it allows to exclude small ones from evaluation Peak Resolution overlapping peaks may not occur in GasBench applications Overlapping peaks would indicate a gross error leading to a worth
191. ze on page 2 23 and proceed as follows e Fill empty sample vials with breath using a straw e Close them with fresh cap and septum Place them in the sample tray e Perhaps you should modify the method as with CO in Atmospheric Concentrations on page 5 28 e A sequence of its own is not necessary Instead use the Equilibration sequence Equilibration seq to perform a measurement Results of Breath Gas Analysis Pie Name F ara Der Dench Operating Manus ohne blanking cf Figure 5 19 5 26 Chromatogram of Plain Analysis without Blanking Ther Finnigan GasBench Il Operating Manual ELECTRON CORPORATION Measurement Procedures for Real Samples Finnigan GasBench Il Breath Gas Analysis bee mn 6 Aner denon I Operating Meran LA et rg ot Vet mr Figure 5 20 Chromatogram of Analysis with Blanking Activated BGD 44 BGD 45 BGD 46 Area All 5 13C mV mv mV 0 5 36 Ja 218 25 085 3 489 124 2132 8 141 8 291 1357 34 s8 210 14849 Figure 5 21 Result Grid of Analysis with Blanking Activated Note Take into account the different ordinate scales when comparing Figure 5 19 and Figure 5 20 Thermo ELECTRON CORPORATION Finnigan GasBench Il Operating Manual 5 27 Measurement Procedures for Real Samples CO in Atmospheric Concentrations Finnigan GasBench Il 5 5 CQO in Atmospheric Concentrations Editing a Method To measure CO in atmospheric conce

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