IAEA Standard Operating Procedure for the Liquid
Contents
1. Two adjustable wrenches keys or one each 9 13 15 and 18 mm open end wrenches A stable table or bench top 180 cm x 80 cm works well to set up the instrument and autosampler A few hours time Note that the instrument should be installed in a room that has good temperature stability and away from areas where harsh chemicals such as acids or bases are used It should not be placed next to a window or in direct sunlight because temperature stability is important for getting good precision from the instrument The instrument should also not be installed in areas where strong vibrations from for example trains or automobile traffic occur PAL Autosampler Set Up The major components of the autosampler are labelled in Figure 12 below You should be familiar with the names before assembling the autosampler Page 20 Injection Sample fer line Septum housing Figure 12 Key components of the PAL autosampler 1 Carefully remove the autosampler parts from the box and place it in position on the table and remove the packing material from the parts 2 Taking the main body of the auto sampler move it to the edge of the table so that the front part of the arm overhangs from the edge You can also gently push the autosampler arm toward the edge so that the feet stay on the table This is necessary because the needle guide syringe carriage will need to be lowered below the top of the table for installation 3 Remove the2. 3 Clean the sample transfer line and filter assembly as described in subsection 2 below weekly unless high salinity samples are being run 2 Cleaning the transfer line and filter After 1 2 weeks of continuous use e g 2000 4000 injections the sample line and the attached 10 um filter should be cleaned to remove small pieces of septum and sample impurities that have been carried into the line 1 First run the laser shutdown procedure by depressing the Exit button Once the instrument has completed the shutdown routine turn off the power 2 Remove the line and filter assembly by unscrewing the Swagelock nut that is immediately adjacent to the instrument DO NOT unscrew the nut that connects the line to the filter Then immediately screw on the Swagelock cap that was supplied with the instrument to prevent dust from entering through the back of the instrument You can also unscrew the sample line from the autosampler at the bottom of the septum holder if this makes it easier for cleaning however removal of the line from the autosampler is not typically necessary 3 Unscrew the septum nut remove and dispose of the old septum Also remove the small black ferrule that sits underneath the septum in the threaded tube You can give a short puff of air through the filter and line see Figure 13 if the ferrule does not come out with the septum A can of air or your in house air system can be used to remove the ferrule and for the next ste
3. 5 THldr1 will appear then press enter to select it 6 press F1 to run check position The needle guide ring should be centered over the hole in the tray holder In addition the lower needle guide ring should extend down into the hole 7 adjust x y zZ using the keypad as necessary Usually no or very little adjustment is necessary See step 7 above which describes how to make adjustments 8 select F4 to go home when the position is correct 13 Now the only thing left is to install a syringe in the autosampler See sub procedure F Changing the autosampler syringe for directions on how to install a syringe Once the syringe is installed you can turn the laser and pump power switches on and begin making analyses I Maintenance Troubleshooting and Notes on Running Dirty and High Salinity Samples 1 Regular Maintenance 1 Adjust the Laser Offset if necessary as described in the Adjusting Laser Offset section in the LGR manual 2 Remove the syringe from the autoinjector and manually rinse with de ionized water to remove any salt build up or septum residue that has collected in the syringe Confirm that the syringe has some resistance when manually actuated If there is little to no resistance tighten the syringe nut slightly When inserting the syringe holder into the Autoinjector extra caution is required to assure that the syringe needle does not bend see section F for syringe change information Page 24
4. cable 2 to 4 metres long with surge suppression e g a circuit breaker or fuse to protect the autosampler and laser instrument from high voltage spikes such as from lightning Two adjustable wrenches preferable or a set of open ended SAE wrenches Note that metric 9 13 15 and 18 mm wrenches will also work Compressed clean dry air for cleaning sample transfer line and filter e g Envi Ro Tech Duster Techspray VWR catalogue 58542 430 3 cans note clean dry air from your laboratory in house system can also be used A small pair of wire cutters for cutting cable ties A set of elastic bands for the LC PAL autosampler injection head CTC PAL part numbers MZ 30 21 tension Cord 280mm and MZ 30 23 tension Cord 90 95mm Nearest supplier can be found at http www ctc ch f_contacts htm or order directly through CTC PAL in Switzerland Note it is possible to make your own if you can find a similar type of elastic band bungie cord locally Bands usually last at least a few years A set of IAEA Stable Isotope 8 H and 5 O V SMOW2 and SLAP2 Standards You will also need to acquire or prepare and characterize a few litres at least of three or more different in house standards see the IAEA Water Resources Programme guidance on standard preparation and storage H Initial Set Up of the PAL Autosampler and the Laser Isotope Instrument What you will need in addition to what is supplied in the boxes from instrument
5. ferrule that sits below the septum because it sometimes comes off with the nut Page 15 3 Use the supplied small metal hook or a tweezer pincette to pull out the septum The hook works best if you slide it around the side of the septum instead of trying to grab it from the hole in the center of the septum Gently clean the cavity of the housing with a lint free tissue 4 Slide the septum nut and new septum onto a blunt 22 gauge needle e g Hamilton AS tip style or similar The Teflon coated side of the septum should be facing away from the bottom of the septum nut see Figure 10 Teflon coated Side Figure 10 Arrangement for septum predrilling 5 Place the entire assembly over the injection tube and screw it down tightly see Figure 11 Then move the needle in and out of the septum about six times to make sure the septum is predrilled Take care not to push the needle in too deep because it could damage the plastic sample transfer line Remove the needle from the septum Page 16 Figure 11 Septum septum housing and needle in place for predrilling The needle should be moved in and out six times and then removed The needle only needs to pierce the septum make sure you do not puncture the transfer line at the bottom of the septum housing 6 Click the septum changed check mark on the instrument screen and the instrument will begin evacuating the instrument cavity After evacuation is finished you should see sept
6. on each side of this plate that need to be removed Once the plate is off install the new band by hooking the knotted ends into the appropriate spots Replace the plate and reinstall the injection head Note that it is possible to make your own bands if you can find a similar elastic band material as the original 7 Running Dirty muddy or cloudy samples You should not run samples with lots of particulates mud sediment etc on the instrument without filtering e g with a 0 45 um filter If particles clog the needle the syringe will be ruined You also want to avoid introducing particles into the transfer line Typical clean looking groundwater and surface water samples do not need to be filtered Activated charcoal can be used to remove organics e g from soil distillation samples The sample is then filtered and measured on the instrument The basic recommendation is when in doubt FILTER 8 Running High Salinity Samples One concern with these kinds of samples is that because the entire injected volume is evaporated all the salts in the water are introduced directly into the sample line However by following the suggestions below high salinity samples can be run They do require a bit more work and good maintenance is essential Samples such as sea water should not be too much problem However brines can be more difficult and you may need to develop a procedure to get good results for your samples There is enough salt in brines th
7. see also Figure 1 e Table with sufficient working space e Fine point permanent marking pen e Autosampler vials e Autosampler caps with PTFE septa e ImL 1000 uL automatic pipette e Disposable pipette tips for 1 mL e Box of tissue papers e Your samples e Three bottles of in house standards two for calibration and one for a control their 5 O and 8H values should be well determined using an independent set of analyses such as from another couple of laboratories or a dual inlet instrument The calibration standards should preferably bracket the expected range of isotope values The control standard should have an intermediate isotope composition compared to the two calibration standards it is also good if it is similar to the expected values of the samples These in house standards are not typically IAEA standards but should be Page 3 calibrated to them Also remember to store the standards properly and protect them from evaporation b a Figure 1 Photo of Sample preparation table Procedure 1 Select the group of samples for analysis Using a permanent marker label empty vials with the name of the standard or the sample ID and place them in proper position on the autosampler tray positioning is described below and shown in Figure 2 Record this information in the instrument logbook Sample and standard positions for three standards should be determined as follows 1 position on the tray top le
8. standard 2 vials and so on then cap the vials Sample 4 Sample Sample Sample Sample 6 8 9 10 Sample 14 Sample Sample Sample Sample 16 18 19 20 Sample Sidi Sample 24 s 26 he Sample Sample 29 30 Dummy Oa Suggested batch size is 53 an Standards i Deionised water including standards Figure 2 Sample positions in the autosampler tray for a three standard arrangement D is the dummy sample position 1 the yellow purple and green spots are for standards DI is for post run cleaning of the syringe 3 Shake the samples to equilibrate and put on a fresh pipette tip Using the pipette and a fresh tip for every sample fill the remaining autosampler vials with the appropriate sample It is best to only fill five vials at a time then cap the filled vials finger tight and the open sample bottles This will help you keep track of what needs to be filled next and prevents evaporation of the samples Be careful to pipette the samples and standards into the correct Page 5 vials use_the logbook to help verify this The vial at position 53 should be filled with deionized water and is used to help clean the syringe after the run 3 When all the vials are filled and capped double check that the logbook matches what is in the tray by spot checking a few different locations 4 Place the tray on the autosampler Figure 3 and configure the run on the laser instrument Figure 3 Autosampler with vials ready for
9. 0 24 77 43 42 99297 0 0002875240 0 0019820500 0 40 0 08 Cal5 amp H Inj 211 258 m 43 99302 0 0002888040 0 0019841700 0 40 0 08 _ intercept 1021 0916082800 45 a 99302 0 0002884520 0 0019837200 0 40 0 08 X Variable 1 Slope 3325343 3765412300 46 45 99302 0 0002884590 _0 0019844400 0 40 R Calibration plots Calculations Checkplots Figure 7 Example of the calculations worksheet in the laser isotope Excel template Individual injection permil results are not shown in this figure but can be found to the right of column M in the worksheet 9 For the linear regression calibration equations column M intercepts slopes and R values will be calculated automatically for both 180 and 7H Calibrations are calculated for each set of five unknown samples using the standards immediately before and after the set of five unknowns You will need to clear the contents of any rows in columns F K if no real data are shown to get the regressions to calculate properly this occurs if you only ran part of a tray If you have deviated from the standard sample Vvial layout i e Figure 2 you may need to make sure that the cell references in the intercept slope and R equations match the range of standard values you have in the worksheet To do this click on the 5H intercept value in column M row 6 Edit the equation cell references so that the references for columns H and I match the rows where you have in house standard data Do this for all o
10. 000198231 32923607 0 00014 000198273 3 29239E 07 80808 1107 10382 95 29 0 00289137 4 28779E 16 1 53371E 13 0 000287586 1 622466 07 001 513855607 00014 000192 513855607 s0902 T107 1127576 29 402 000220605 4 26212E 16 203587E 13 0000287524 156547607 00019205 406946607 000014 00019021 __ 4 069465 07 090909 T108 11490 06 79 462 000175938 431866E 16 181721E 13 0 000286804 10147607 000198417 281213607 000014 5 00019842 2 61213E 07 00309 T108 1174389 2 00017798 427057E 16 257659F 13 0000288452 10636607 00019837 271801607 000014 001837 2716801607 00309 11 08 11997 71 29 4299 000105281 4067746916 9 91561E 12 0 000288459 1 69692E07 CODA 251624607 00W14 BS 0001844 251624607 090302 T1 00 12251 04 0 00303367 4 25726E 16 1 93704E 13 0 000200507 1 57709E 07 00019842 33477607 000014 79 00019042 3 354776 07 080803 T1 06 12504 92 29 42 000106527 397635E 16 1 45965E 13 0 000286256 110767607 000198353 249922607 000014 00019835 2 49922 07 CT 12758 72 z3 000205975 4195916916 1 15951E 13 0 000209523 1 22288607 u 20E 29555607 0 00014 0 0019837_ 2 B555E 07 0808 11 03 1301204 3 0 0013631 4 19114E 16 W SOSESE 13 000029105 1201607 00019719 318518607 0001972 318518607 gt Figure 5 Raw worksheet example from the laser isotope Excel template 7 Go to the worksheet named checkplots Figure 6 Here you will do the first evaluation of the overall quality of the run Be aware that you may need to rescale the Y axes The plots should be scaled to show fine sca
11. 019797800 Inj HOD H20 Value 3 2 dummy 0 0002831260 0 0019790600 0 40 0 08 __ Calt 8H Inj 1 66 4 3 dummy 0 0002836600 0 0019798800 0 40 0 08 Intercept 1020 1834994954 5 4 dummy 0 0002834550 0 0019799600 0 40 0 08 X Variable 1 Slope 3324166 29384 10300 6 5 dummy 0 0002838170 0 0019796500 0 40 0 08 EA dummy 0 0002835750 0 0019798700 15 Std9 0 000250455 0 00195301 189 10 24 77 8 7 Std11 0 0003063270 0 002000790008 16 Std9 _ 0 000250184 0 00195304 189 10 24 77 Ea 8 Std11 0 0003072340 0 0020016600 17 stad 0 000249908 0 00195307 189 10 24 77 10 9 Std11 0 0003071880 0 0020021800 18 Std9 0 000249829 _0 00195328 189 10 24 77 j 10 Std11 0 0003071690 0 0020022800 0 40 0 08 2 n Std11 0 0003072740 0 0020016000 0 40 0 08 13 12 Std11 0 0003071930 0 0020024800 0 40 0 08 Cal2 8H Inj 67 114 14 13 Stog 0 000252586890 0 0019539300 0 40 0 08 intercept 1022 00787 15659 15 14 Std9 0 0002506600 0 001953320008 63 0250168 0 0019533 189 10 24 77 X Variable 1 Slope 3330752 5019150700 16 15 Stog 0 0002504550 0 001953201008 64 189 10 24 77 7 16 Stog 0 0002501840 0 0019530400 65 189 10 24 77 18 17 Stog 0 0002499080 0 0019530700 66 I 189 10 24 77 19 18 Stag 0 0002498290 0 0019532800 0 40 0 08 2 19 Std6 0 0002872470 0 0019841700 0 40 0 08 2 2 Std6 0 0002883020 0 0019844300 0 40 0 08 a2 a Std6 0 0002882830 0 0019845900 0 40 0 08 23 22 Std 0 0002883360 0 0019845800 111 std9 0 000250172 _0 00195283 189 10 24 77
12. 02 0 002060 aj a BW 0 001386 99303 t 0 001019 s 99303 0 001475 AL UA a Ce gt ERENT Sine Catz pts Caledon kpin Is al Figure 6 Examples of the three checkplots 8 Next go to the standards checks worksheet Enter the previously determined values for the in house standards permil relative to V SMOW in the Standards Known Value cells Rows 36 38 columns B and C Then go to the calculations worksheet The known values for the standards that you entered into the standards checks worksheet should have been copied to columns J and K in the calculations worksheet automatically see Figure 7 If they were not just copy and paste the appropriate known values downward in columns J and K so that all rows of data for the in house standards red section of the worksheet labelled calibration data are associated with a known value Note that only data from the two calibration standards will appear in the red section not the control standard It is very important to have accurately determined the isotope values for the in house standards A B D E F G H 1 J K L M N ie HOD H 0 1 Calibration Plot no EH Known 2 1 dummy 0 0002825640 0 0
13. 110 or 220 volts If it is not change it to the proper setting 2 Take the beige computer cable from SER1 on the autosampler and plug it into the place labelled to LC PAL on the back of the instrument 3 Take the green and black braided wire from the septum heater and connect it to the septum heater connection on the back of the instrument Be careful when cutting the wires loose from the cable ties Use a pair of wire cutters not a knife so that you don t damage the wires 4 Take the small clear tubing with the Swagelock fitting on the end from the bottom of the septum area on the autosampler and connect the swagelock to the to septum connection on the instrument using a wrench Do not overtighten the nut Be careful when cutting the tubing loose from the cable ties Use a pair of wire cutters not a knife so that you don t damage the tubing The autosampler should now be fully connected to the instrument However do not turn on the power The autosampler still needs to be configured and this step is covered later Next you will finish the pump and drierite column connections to the instrument 5 Take the vacuum pump and connect it to the To Ext Pump connection of the instrument using the short stiff white tubing Tighten the nuts with a wrench Hook the power cable to the pump and to the back of the instrument to the connection marked Ext Pump Power Page 22 6 Now you will hook up the Drieri
14. 539 4 24587E 07 000131849 425502E 16 1623 amp 13 000250665 20818607 00019537 4085607 000013 00019533 401845607 Bsus 0 00124697 4264316416 1 61058E 13 0 000250455 24852607 00019531 41553607 0 00013 0 001953 4 15253607 waT 2 OOS 4241586416 2183866 13 0000250184 199148607 00019534 47557607 00013 o 0001953 4755276 07 090909 T1 03 5 6 000191781 4721076E 16 173861E 13 0000249908 177445607 000195307 259241607 000012 00019531 259241E 07 T 70 _ OMNS65I83 4192576416 2OS6I7E 13 000M4 17466607 0001538 37WUE0 0012 000153 37W4E07 0000842843 431606E 16 207847E 13 00002872347 1352E07 000198417 3 MED 5 00019842 33486 07 000213255 423157616 1 52546E 13 0 000282 201512607 00019843 325316607 00144 325316607 000218574 4222046416 1 17785E 13 0 00028623 187057607 000138459 35107607 9 001846 35107607 000167176 41943E 16 193963E 13 0 000288306 168245607 000198458 276573607 00019846 276573E 07 000151777 398106E 16 25659 13 0000268181 196344607 000198485 402734607 00019849 402734607 00012032 4 205626 16 1 49396E 13 0 000288331 206495607 000138469 35777607 001847 35777607 6924 81 2 000159597 411129616 21916E 13 0000265663 255453607 000198201 262538607 000014 000198 262538607 7178 11 9 59 0 00118792 4 20673E 16 1 72029E 13 0 000205737 1 76429607 000199147 55455607 0 00014 0 01915 5 54055 07 7431 97 0 000836731 4 23172E 16 2566E 13 0 000205973 249761E 07 000199179 264008E 07 0 00014 1 2607 00019010 2 64000E 07 768577 2 0000770682 422058E 16 181254E 13 000026567
15. 8 191738607 000198175 3720ME07 000014 00019818 372002E07 00ST 05 7933 06 2359 O 00129047 4 19581E 16 1 30455E 13 0 000205682 214942607 000198195 355673607 0 00014 0001919 3 556736 07 090909 T1 05 8192 85 0 00120549 4 24822E 16 1 56556E 13 0 000265793 _ 1 77893E 07 _ 0 00198156 3 97879E 07 0 00014 89 00019816 __3 97879E 07 090909 T1 06 0446 66 0 00110474 4 30542E 16 1 759E 13 0 000287433 1 00262E 07 000198313 3 39205E 07 0 00014 00019831 3 39205 07 00309 T106 8699 96 29 5723 000316338 4 25854E 16 1 56515E 13 0000287177 186239607 000190274 4400607 000014 00019627 4 42609 07 30903 1105 9953 76 23 0 00351379 4 22487E 16 1 52209E 13 0 000287457 191E MIBI 52918607 00W14 9 OMNIS 5 2910607 030309 T1 06 9207 21 O 00147014 4 22829E 16 1 32082E 13 0 000267382 1 49681E07 000198255 43335607 000014 75 00019826 4 33435E 07 080309 T106 946103 2 000146071 4 20574E 16 1 53135E 13 0000267273 220397607 000190247 28054607 0004 00019625 263154E 07 20903 1105 9714 83 95357 00012574 4 O4493E 16 2 70276E 13 0000287119 163051607 O00 18341 SF OABIED 0 0014 82 00019834 _3 04951E 07 998 2 9 O 001S 38 4 30391E 16 1 4853E 13 0 00028773 1 656607 OCI 37382607 0 00014 OOO 3 738207 10222 O 00214026 4 17607E 16 1 80064E 13 0 000287183 1 56364E07 000198297 399523607 0 00014 0 001963 3 99623 07 10475 66 2 57 000154982 4 218 HE 16 1 14022E 13 0000267353 153001607 000192351 25364607 OOM 77 00019025 253554E6 07 10729 67 9 4859 0 00142 4215446416 1 14845E 13 0000287529 1 71267607
16. IAEA Standard Operating Procedure for the Liquid Water Stable Isotope Analyser 5 10 09 B Newman A Tanweer T Kurttas IAEA Water Resources Programme laser_procedure_rev12 doc Page 2 IAEA Standard Operating Procedure for the Liquid Water Stable Isotope Analyser This procedure is comprised of eight sub procedures and an equipment list for the Los Gatos Research DLT 100 analyzer for H and 0O Page Ax Sailipls Pre par atl onns ieseni tee a nevgheacsaseaeoo ages ae Raagbgevsans Medaheneaesegts 2 B Configuring the Run and Starting the Analysis cee eeesceceenceceseeeceeeeeceeeeeceteeecnteeeenaeees 6 Cs D ta Transferni os dest cae meee ee EE reeds a ws cepla pean ES ANE RS 7 D Data Post Process s e r oooh a a r ass seed cg a 8 E Changing the Autosampler Septum sesssesssssessessseesseresssessstessersseesseeesseessresseesseesseeesseee 14 F Changing the Autosampler Syringe and Recovering from an Aborted Run Becauseot a Bent Needle esse lic es aaa asec gece EAA ATA AAS EEEE T SaS 16 G Equipment ASt i etia E E E a EA erecta a 18 H Initial Set Up of the Laser Isotope instrument and the PAL Autosamplet 0 19 I Maintenance and Troubleshooting sssssssssesssesesseeesseesseessersseresseessseessersseesseeesseeesseesseesse 23 Please also be familiar with and refer to the LGR Liquid Water Isotope Analyzer manual and the LC PAL Auto sampler user manual A Sample Preparation What you will need
17. O range values in column Y If as above the values are over about 0 5 then you may have at least one bad injection Repeat the clean up procedure that you did for the standards by verifying bad injections and then deleting the bad ones If you have more than one bad injection out of four then you should flag the sample e g make a note next to the sample in the results worksheet and rerun it E Changing the Autosampler Septum The autosampler septum should be changed after every 325 injections Note that running a full tray of 53 vials results in 318 injections so you should change the septum before the next run When in doubt change the septum It only takes a few minutes and a leaky septum will ruin the run Warning Failure to properly follow this procedure could severely damage the instrument by letting air into the system 1 Before removing the old septum from the autosampler you must first prepare the instrument for a septum change To prepare the instrument choose setup with the mouse and click on change septum The screen will say initiate septum change Click on the green check with the arrow then click OK using the mouse The screen will first say venting cavity Wait until the system says ready for new septum before proceeding 2 Once the instrument has indicated it is ready unscrew the knurled nut from the autosampler It may be hot from the heater so use a tissue or glove Also be careful you do not loose the dark colored
18. __ Cal3 8H Inj 115 162 24 23 Std6 0 0002881810 0 0019848500 p stad 0 000250213 0 00195281 189 10 24 77 __ Intercept 1021 5808473482 25 24 Std6 0 0002883310 0 001984690008 113 std 0 000250404 0 00195278 189 10 24 77 X Variable 1 Slope 3326472 2247667900 2 25 99295 0 0002856830 0 001982010008 114 stag 0 000250011 0 00195276__ 189 10 24 77 i 7 2 99295 0 0002857370 0 0019814700 0 40 0 08 23 27 99295 0 0002859730 0 0019817900 0 40 0 08 23 28 99295 0 0002858780 0 0019817600 0 40 0 08 30 2 99295 0 0002856820 0 0019818500 0 40 0 08 31 30 99295 0 0002857930 0 0019815600 159 std9 196 189 10 24 77 32 31 99296 0 0002874330 0 0019831300 0 39 189 10 24 77 3 32 99296 0 0002871770 0 001982740008 161 std9 189 10 24 77 __ Cal4 8H Inj 163 210 34 33 99296 0 000286874570 0 0019829300 162 std z 189 10 24 77 _ Intercept 1021 2497760336 35 34 99296 0 0002873820 0 0019825500 0 40 0 08 X Variable 1 Slope 3324365 4266580700 3 35 99296 0 0002872730 0 0019824700 0 40 0 08 37 36 99296 0 0002871190 0 0019834100 0 40 0 08 38 37 99297 0 0002872360 0 0019829400 0 40 0 08 39 38 99297 0 0002871830 0 001982970008 207 std9 0 000250563 0 00195334 189 10 24 77 40 39 99297 0 0002873630 0 0019825100 25 s9 0 000250362 _0 0019533 189 10 24 77 99297 0 0002875290 0 0019823100 209 std9 0 000250227 __0 00195298 189 10 24 77 41 99297 0 0002875860 0 0019828000 20 st 0 000250117 0 00195296 189 1
19. analysis Notes Warning Do the sample preparation very carefully Mixing samples up can create many problems It may take around two hours or more to prepare a tray with 25 to 50 samples If you want to do a rerun of the same sample just replace the cap with septa you don t need to re pipette it You can do this once If you need to rerun a third time it is best to prepare a new vial After 12 injections 2 runs from the same sample vial with 6 injections the sample precision will start to decrease Do not reuse the autosampler vial caps septa Sample vials are also disposable so use new ones If it is necessary to reuse vials make sure they are well cleaned rinsed and oven dried before using Again never reuse caps septa Page 6 B Configuring the Run and Starting the Analysis 1 Examine the logbook and determine if it is time to replace the autosampler septum at 325 injections or sooner Analysis of a tray with 53 vials requires 318 injections If a new septum is required follow the replacing the septum procedure later in this document Warning improper changing of the septum can severely damage the instrument follow the procedure 2 Examine that there is sufficient active Drierite in the column at least 2 5 cm of blue is left if not refill or replace the column Drierite can also be regenerated following the manufacturers directions 3 Check the spectrum on the laser see example in Figure 4 by selecting
20. at the transfer line can become clogged after only a few samples Do some testing before running brines The following is based on suggestions from Los Gatos and our experience here at the AEA for running saline samples 1 Manually rinse the syringe daily with distilled water to remove any salt buildup in the syringe 2 Place at least one vial of DI water after every saline sample to help rinse the syringe Don t be afraid to run lots of DI water in between samples especially brines 3 Remove salt deposits from the transfer line every 1 2 days This can be readily done by using compressed air as described in the maintenance discussion above Some users rinse the entire assembly filter and transfer line with DI water and then Page 27 thoroughly dry it before reattaching it to the instrument Alternatively the transfer line can be replaced We have found that with brines rinsing is required The black ferrule underneath the septum should also be cleaned with air and or rinsed because salts will precipitate there as well 4 Thoroughly clean replace the transfer line every 20 30 days or when excessive salt build up can no longer be blown out 5 Use a larger syringe The instrument uses a 1 2 microliter syringe however a 5 microliter syringe can also be placed in the syringe holder A few software settings can then be altered e g smaller injected volume sec syringe hold 69 sec post withdrawal delay to allow for the lar
21. controller bar Use the long thumbscrew to install the side of the guard with the controller bar The controller bar should be screwed on at the same time as the guard Warning the safety guard is fragile do not lean your arms on the safety guard when working on the autosampler 8 Place the keypad on the bar by sliding the tab on the rectangular metal support into the back of the keypad The top of the keypad will be held in place by a magnet 9 Take the white coiled cord and plug it into SER3 and the back of the keypad 10 Take the black cable with the round ends and plug one end into the back of the PAL transformer box this is a separate rectangular box marked PAL and the other end into the connection marked Power on the back of the autosampler 11 Plug the power cord to the back of the PAL transformer box and plug the other end into the electrical extension cord surge suppressor Do not turn the autosampler on yet You will finish making the rest of the autosampler connections later now it is time to set up the laser isotope instrument Isotope Instrument Setup 1 Open the laser box and with one or two helpers carefully remove the instrument and place it on the table next to the autosampler Remove any packing material from the instrument and other parts Warning check that the red voltage indicator on the back of the laser machine near the on off switch is set to the power system that you will be using e g
22. eds to be finger tight 8 Press the enter button on the control panel continue to complete installation 9 Verify that the needle is centered on the septum hole by running the septum referencing check as follows note that it is ok to have a needle in place for this just do not run the tray referencing procedure 1 on the control panel press F1 to get into menu 2 rotate the big silver knob until setup is highlighted then press enter center button in the silver knob 3 rotate the knob to highlight objects then hit the enter button 4 rotate the knob to highlight injectors then hit the enter button 5 LC V1v1 will appear then press enter to select it 6 press F1 to start check pos the arm will start moving and then stop over the septum 7 Lift the needle guide up gently without moving the syringe needle and check that the needle is centered over the septum hole you may want to use a flashlight and a magnifier to assure it is well centered If it is not adjust x and y as necessary using the keypad To make adjustments use the knob to highlight x or y and hit enter You can then use the knob to change the values and the arm will move You should only have to make very small adjustments or none at all because this position is set at the factory When it is correct hit enter and proceed to the next dimension if necessary You shouldn t need to adjust the needle depth z Page 18 8 s
23. ee part of it through the syringe window The short band is in the rear of the injection head and is difficult to see without removing the head For replacement perform the syringe change procedure sub procedure F but just remove the syringe After the syringe is removed you need to get access to the bands It may be easier to remove the injection head for this task just reverse the injection head installation steps in sub procedure H for the PAL autosampler setup Remember you will need to move the autosampler to the edge of the table and gently let the needle guide drop down fully over the edge to access the three screws To access the long band remove the top plate from the injection head there is one screw in the top rear of the injection head The top of the long band is attached to a hook that is built into the top plate Unhook the old band and then lower the needle guide and you can unhook the lower part of the band Take a new band it should be about 29 cm long and attach it to the top hook it is held in place by a knot in the band Slide the band into the injection head and place the top plate back on Then using a long wire hook the bottom of the band and pull it out of the bottom of the injection head and hook the knotted end into the clip notch Replace the retaining screw that holds the top plate If you need to replace the rear short band you will need to remove the black plate on the rear of the injection head There are screws
24. elect F4 to go home when if the position is correct Warning do not turn off the power switch to the autosampler when a syringe is installed The syringe will drop rapidly and this will likely bend the needle and will ruin the syringe If you need to power off follow the procedure as described in this subsection and remove the syringe Then you can support the needle guide with one hand and turn off the power with the other Gently lower the needle guide downward do not let it drop rapidly 10 To recover from the aborted run you need to start over on the instrument Click Configure keyboard symbol then delete everything from the run list except for the one file you can t delete 11 Reload all the files back into the run list delete the old file and start the instrument run procedure G Equipment and Consumables List This list includes consumables and items not typically supplied with the instrument or the autosampler Autosampler vials screw thread 1 5 mL glass 32x11 6 mm disposable VWR catalogue 548 0018 1000 pack From Los Gatos Research use cat 908 0008 9005 100 pack You should have at least 1000 vials to start with Note that the VWR and Los Gatos vials are not interchangeable Caps and Teflon coated septa for autosampler vials disposable VWR catalogue 548 0022 1000 pack From Los Gatos Research use cat 908 0008 9006 100 pack You should have at least 1500 caps and septa to start with Note that t
25. etimes fix this problem in the calculations worksheet First note which injections are problems in the standards checks worksheet and then go to the calculations worksheet Scroll over to the right side of the calculations worksheet and look at columns N through Y Scroll down until you can find the injection number for the suspect standard analysis Look at the range column Y for this sample standard The range of the 5 O values for the last four injections should generally be less than about 0 5 permil If it is not then there is likely a bad injection or more than one bad injection You can usually identify the particular injection because it will be lighter or heavier than the rest Once you have noted the suspect bad injection s you need to verify there was a problem by examining the checkplots worksheet Check the injection by clicking on the data point for the particular injection in amount of water plot third plot Excel will pop up the information on each data point and tell you Page 14 which injection you have clicked on If the injection is on a spike higher water amount or a large dip then you have a bad injection Alternatively you can consult your previously prepared list of potential bad injections so you don t have to go back and forth to the checkplot so much If the amount of water is ok then check the temperature data upper and middle plots Occasionally there will be a temperature shift that may cause a poor
26. f the intercept slope and R equations in column M 10 Look at the R values they should be higher than 0 99 Otherwise the wrong data were used in the regression i e your cell references in the equations are wrong or there was a problem with the run If the values are lower than 0 99 then go back and check the intercept slope and R equations and make sure they reference the proper cells for the in house standards 11 The values in column M are the slope x variable and intercept that describe an equation of a line y slope x intercept that is used for the calibration equations 12 Delta values permil V SMOW for each injection and reportable values permil V SMOW and standard deviations for each sample are calculated automatically in columns Q R S and V W X The reportable value is based on the average of the last four injections of a particular sample the first two are prone to be bad so they are not used The results Page 12 worksheet Figure 8 has a simple formatted version of the sample reportable values and their standard deviations and is set up for easy printing Columns T and Y in the calculations worksheet contains the range maximum minimum for the last four injections of each sample This value is useful for fixing problems and evaluating the quality of a particular sample value or the run as a whole use of the range values is discussed later in this sub procedure SH Standard Deviat
27. ff the laser power switch 3 Perform any necessary actions including changing the septum cleaning the transfer line and or cleaning the syringe 4 Turn on the instrument power 5 Reconfigure the run and start over 5 Autosampler arm moves to the back rail and makes grinding or strange noise The control panel reads limit switch not found motor y reference fault or something similar This can especially happen during installation of the autosampler injection head Turn off the autosampler and reach around underneath the back of the arm and make sure the ribbon cable is free and has some slack Try turning the autosampler on again If it still has the problem turn the autosampler off remove the injection head unhook the ribbon cable and reinstall the injection head as described in subproceedure H If the ribbon cable binds inside the arm it can cause the limit switch error make sure it is free to move 6 Autosampler lifts sample vials out of the sample tray or the needle guide lacks tension In other words a sample vial is still stuck on the needle after injection or the needle guide no Page 26 longer has the tension to operate properly This may occur after many uses of the autosampler e g often a year or more or use The dark colored elastic bands inside the injection head need replacement or one may have come loose There are two bands in the injection head The long one is on the left side of the injection head and you can s
28. from the blue plate 4 Insert a new syringe into the blue plate by inserting the flange finger grip of the syringe into the upper slot Make sure that one of the flat sides of the syringe flange faces the back of the blue plate and close the black lock over the new syringe 5 Carefully put the blue plate back into the injection head and do not bend the needle on the lower black needle guide rings It helps greatly if you lift the black needle guide carriage the part that has the round rings upward with your left hand the carriage will move up to the injection head housing With your right hand you can take the blue plate near the top and gently tilt it to insert the needle through the rings at an angle Then keep moving the blue plate into the housing until the two small pins on the bottom back of the plate line up with the lower holes in the injection head housing and the blue plate clicks into place It helps if you look over the top of the blue plate and move it so that the bottom two pins line up with the bottom two holes on the injection head The magnets will then pull the top of the plate into position When it is right it often makes a click noise when the magnets pull the blue plate in place 6 Double check that the needle is properly centered in the lower black ring If not the syringe or blue plate is not installed properly 7 Retighten the red nut immediately above the plunger by rotating it to the left It only ne
29. ft corner should be a dummy sample because this analysis is usually not a good one and the results will be discarded The dummy can be any clean water e g tap water it doesn t have to be a standard or even a sample with a known isotope value on position should be for the light isotope calibration standard 3 position should be for the heavy isotope calibration standard 4 position should be for the third standard the control standard Note that putting the dummy sample and calibration and control standards in this order is important if you want to use the IAEA spreadsheet for post processing of the instrument data The next five positions 5 9 are for the first five samples Page 4 Positions 10 through 12 should be for the same three in house standards And so on just remember to put three standards after every five samples including a last set of standards at the end of the tray run Suggested maximum number of samples is 52 including standards even though the autosampler will hold many more A deionized DI water sample can also be placed in position 53 to clean the syringe after the run 2 Place a disposable pipette tip on the pipette Shake the standards to equilibrate and dispense 1 mL into the appropriate vials on the autosampler tray you only have to change the pipette tip when you change standards or between samples e g fill all the standard 1 vials with one pipette tip then put a new tip on and fill all the
30. ge nut and reinsert the syringe You will likely examine the checkplots again when you are checking specific sample or standard results this is discussed later A B I c D G CS a Jeeg T M N o F 1 Inf Sample name Temp_Celsius Stdv_Celsius 2 1 dummy 29 6305 0 001306 Temp_Celsius SIA dummy 0 001909 man dummy 0 002035 2 i 5 4 dummy 0 001280 am 6 5 dummy 0 000912 29 60 7 6 dummy 0 000601 lie S11 0 002881 2940 3 8 Stani 0 002120 29 20 10 9 Sid 0 002292 i 10 Stitt 0 002716 23 00 12 W Std 0 01241 13 12 Sidi 0 001053 so 14 13 Sid 0 003039 20 60 16 14 S18 0 001318 0 0 100 150 200 250 00 350 16 15 Ste 0 001246 17 16 S18 0 002648 Bg on etn 19 S105 0 000843 2 a S165 0 002133 2 2 S16 0 002186 B 2 St 0 001672 aj 3 S105 0 001518 Bl u S105 0 001203 5 5 925 0 001596 t rid rt 325 0 001168 E 3 7 99295 0 000839 EE eT eer Rares Bl 2 5 0 00771 EECA DP PE PETT V tel x 3 m5 0 001220 STRAIT TAN Ta 31 E 99295 0 001205 Z a 20206 0 001185 o s0 10 150 20 250 300 3 g 2 9926 0 003163 3l 3 926 003514 xu 93296 0 001470 3 s 99796 0001461 w S 99296 0 001257 46E 16 x x R27 0 001335 456916 99297 0 002140 LEW 99297 000550 43E 16 aj a 99297 0 01423 426916 4 42 a cra 0 002891 41E916 a a 99297 0 002206 40E 6 uj s S8002 0 001759 396916 45 44 3302 0 001760 38E 16 45 a5 9x02 0 001063 37E 16 w 99302 0 003034 36E 16 wj n 99302 0 001088 c 5 s 983
31. ger bore syringe to be used This helps to prevent syringe breakage despite the build up of salt deposits 6 Typically sample impurities will precipitate out at the point of injection and remain in the transfer line or filter assembly Thus the instrument is usually safe from contamination However to prevent precipitation problems beyond the filter assembly the line should be cleaned on a regular basis especially when running saline samples
32. he VWR and Los Gatos caps are not interchangeable Autosampler Septa Los Gatos Catalogue number 908 0008 9004 pkg of 50 is 45 you should have at least 500 of these since you will replace them almost daily Septum Inlet Filter 10 um Los Gatos Catalogue number 908 0008 9007 25 ea you only need two or three of these because you can clean them see procedure below They are metal and last for years You may need a few more if you run lots of brines Drierite have one extra column or a jar of Drierite for refilling Prefilled column cat KH 07193 Cole Parmer Microsyringe for autosampler Hamilton 1 2 microliter syringe PN203185 01 Model 7701 2N These can be purchased through VWR and most other chemical suppliers Syringes last typically 2 3 weeks of daily running You should initially have at least 30 of these about 120 and reorder when down to four Needles for predrilling autosampler septa blunt 22 ga e g Hamilton AS tip style or similar three needles You can recycle old needles from bad syringes for this Pipettor An automatic pipettor e g an Eppendorf type with 1000 uL capacity for transferring samples and standards to the autosampler vials Example Cole Parmer Adjustible Volume Pippettor Cat KH 21600 18 Page 19 Pipettor tips disposable 1000 uL to fit the above pipettor Example Cole Parmer Cat KH 25711 50 200 1300 uL packs of 1000 Suggest at least 5 packs Multi port electrical extension
33. ion 03 03 2005 O permil 10 ee 12 10 8 6 4 2 210 2 4 30 E w az r 50 amp gr Sas wo 2 BRIW pai 93318 B54 O48 10 15 om 0303 2009 2 24 21 39747 76 21 025 1112 O14 03 03 2009 80 S 2 E 360 Of 1065 013 505 A068 aC 3 Eze n O21 EA Giz GENA Fi L 4 9750 51 12 043 1223 os 03 03 2005 Sample values vs the global meteoric water ine 2 3 39751 7601 048 ns 006 03 09 2009 s 7462 063 102 on 08 2008 Mw D 7 99753 7888 O32 1120 016 03 03 2003 5 s ET 2 39754 7874 03 1172 008 03 08 2008 15 110 EJE mia 231 0 063 O12 03 03 2009 s 5 mid 244 oF D4 013 pE 34 35 Berges os oI Pree ons as EJ Moar nD Resuats A G E E Checipots AE ix a Figure 8 Example of the Results Worksheet 13 It is important to evaluate the quality of the run and the individual sample values and this can be done starting with the standards checks worksheet Figure 9 Here you can assess the accuracy of analyses calibration by examining the big delta values for the two calibration standards and the control standard The red columns E and H contain the big delta values which should automatically calculate for you They represent the difference between the measured sample value and its real known value Big delta values should be less than 2 permil for SH and 0 3 permil for 5 O Note that the big delta values are only a guide ab
34. le variations in temperature and amount of water injected into the cavity in order to see potential problems Examine these three plots There shouldn t be any large changes in temperature this is the internal gas temperature in the cavity and the curve should look pretty smooth The internal gas temperature variation should be less than 0 3 C per hour upper plot The standard deviation of individual injections should be less than 0 01 C and typically around 0 002 C or less middle plot If the temperature variations are too large then better control of the laboratory temperature may need to be implemented It is recommended that the ambient laboratory room temperature should not vary by more than 3 C per hour The amount of water injected plot bottom plot shows molecules of water cm N cm3 It is an important one and should typically be about 2 to 4 x10 and should not vary by more than 3 rms fluctuation over the run Note that the dummy injections may be outliers and this is ok You can often identify a bad injection with this plot by a spike or large dip It may be helpful to list the injection numbers of any bad injections which can speed up the data clean up process that you will do later A consistent amount of water is critical and if it is not in the acceptable range higher uncertainties will result If many of the values are not acceptable Page 10 you may need to replace the septum remove and retighten the syrin
35. m your memory stick to the appropriate directory folder on the computer 2 Open Excel and then from Excel open the txt data file note you may need to select show all to see the file to load it then select delimited and click next 3 Click comma delimited then click finish 4 Choose save as and save the file as an Excel xls file to the appropriate directory This is basically the raw data file but in Excel format 5 Open the Laser Isotope Excel template and choose Save As and provide a new file name to store the results Do not use the same filename as the template because you do not want to over write it note that you can also create your own template or program for processing 6 Go back to the first Excel data file you created from the laser txt file and highlight all the data starting in row 2 not the column headings through the last row of data e g row 313 for a full tray of 52 vials then select copy Don t copy the diagnostic information below the data i e the information that that starts in Column A with ADVANCED SETTINGS Then go to the second excel file you created from the laser isotope template and use paste special values to paste it into row 2 column A of the raw worksheet The raw worksheet should Page 9 look like Figure 5 below except with your data in it Then save the file Other worksheets tabs in the file will be automatically updated with your new data and you will l
36. number However over 90 of the time the problem will be an inconsistent amount of water If you find a bad point go back to calculations and cut out the bad injection individual injection values in columns Q and V and paste it to the side The reportable value standard deviation and range will automatically recalculate For analysis of a standard it should now be closer to the known value If there is a problem with an injection of one of the two calibration standards then you must also go to the calibration data columns H and or I and clear the bad injection data from the appropriate cell This will improve your calibration and all the reportable values in the spreadsheet will update including those in the results worksheet Repeat this procedure for any suspect standards in the standards checks worksheet for both 8 O and 5 H you will find many more problems with the 5 O results so start with it You will occasionally find a bad injection that produces an unacceptable value for 5 0 but not 8 H In this case you can just remove the bad 5 O information and leave the SH alone Remember that for the calibration standards if you cut out an injection value you must also delete it from the calibration data 15 Once the standards and calibrations are cleaned up you should go to the calculations worksheet columns N through Y and review the 5 O and H data for the individual samples unknowns Pay close attention to the 5
37. ook at these next el Laser_Caiculations Laser Calndatens Temptate os OS0809 T101 85405 000130602 372588E 16 612565E 13 0000262564 000197978 370068607 000014 00019798 oww T 0 1107 56 0 001903235 3 634E 16 226045E6 13 0 000231 200077E0 0 00197906 470E0 0 00014 ear 0 019791 AMEY 080803 T1 01 1358 83 9 002035 416751E 16 1 81996E 13 000028365 25544607 000197388 364618607 000014 1 3607 00019799 3 64518E 07 090909 T1 01 161201 BES 000177991 A010G7E 16 1969E 13 00002383455 15724607 000197996 414601607 000014 79608 00018 4145476 07 50903 1101 1856 16 B27 0000912337 40331E 16 1 06991E 13 0 00028317 1 938607 001975 8648522607 000014 9760 OODISTS7 484512607 30803 151 O OOUSOI763 4112296416 151546413 0000283575 180045607 00019737 SBE 000014 SEW 007V 3 SSOUSEO OWS 4258316416 200712613 0003637 261060 OWAWYS 6PSE07 00WIS 13607 OUM 6 7607 000211974 4 23674E 16 1 49929E 13 0000307234 196319607 000200166 540553E07 000015 98E08 00020017 5 405536 07 000279194 414967E 16 198387E 13 0 000307169 756915607 000200718 45381607 000015 13607 00020077 45W0E 07 57 3 000271582 40017E 16 121441E 13 0 000307169 2054607 OWA 4107607 00W55 1607 OMNI 4 107607 3378 07 96793 000124143 4167376916 1 39077E 13 0 000307274 18837607 0006 4960 00005 34606 00M6 43689807 Dy 000105256 _ 4 13497E 16_ 1 76786E 13 0 000307199 2 48256 07 000200243 31232607 000015 172607 00020235 3 12637E 07 000303932 436821E 16 1 65138E 13 0 0002525869 16833607 000195393 424587E07 0 00013 00019
38. out the accuracy of the analyses and are not equivalent to the analytical precision The mean and standard deviation of each standard are calculated in columns C and F If the standard deviation is too high the spreadsheet will flag the analysis with check in columns D and G otherwise it says ok Typically the 5 O results are the most prone to high values If there are problems you may be able to resolve them as described in the next step 8H Big Delta 0 62 0 64 0 43 0 08 0 01 0 02 0 13 0 11 24 74 2 a 0 03 sto 189 35 189 10 188 65 189 10 5 24 88 24 77 0 11 188 89 189 10 0 21 24 70 24 77 0 07 0 00 0 02 Std 18949 18910 i eee 188 47 18810 _ Average 24 78 Std Deviation 0 01 0a 0 06 0 00 0 01 0 01 Std Deviation Big Delta Max limit Standard 5 Known 8H permil 8180 permil Please fill in this table with Values the known values of your odo 008 standards 61 870 40 Standards used by 41 IAEA Isotope Hydrology Laboratory Known 2H permil 5180 eae Values 4 gt h QUST Standards checks Calibration plots _ Calculations lt gt Figure 9 Example of the standards checks worksheet in the laser isotope Excel spreadsheet 14 If the standards checks worksheet says check for one or more standards you can som
39. ps as long as the air source is clean and dry 4 Next repeatedly pulse air through the filter assembly and transfer line as shown in Figure 13 to remove all visible septa pieces they will exit out of the septum tube This action will also back flush the filter 5 Blow any pieces that have collected in the well of the septum tube out the area where the black ferrule normally sits then replace the black ferrule in the septum tube and install a new septum remember the white side of the septum is down when the septum nut is screwed onto the tube 6 Remove the cap from the port on the back of the instrument and immediately reconnect the filter assembly and line to the instrument Tighten the nut firmly 7 Install a new septum according to the procedure and then turn on the instrument and let it warm up for analyses Page 25 Figure 13 Photo of compressed air setup for cleaning the filter and line The line is open at the septum end not shown Remember to blow out any septum pieces from the septum tube well area as well 3 Bent needle on syringe see subprocedure F for replacing a syringe 4 Laser locks up or freezes during a run The laser quits at some point in the run list and abort does not work 1 Turn off the laser power switch wait a few seconds then turn it back on Once the laser has fully come back up immediately shut it down by selecting Exit to assure that the cavity has been vented 2 Turn o
40. roubleshooting procedure in section I 5 If everything is ok then check the septum reference position using the keypad by 1 press F1 to get into the menu 2 rotate the big silver knob until setup is highlighted then press enter center button in the silver knob 3 rotate the knob to highlight objects then hit the enter button Page 23 4 rotate the knob to highlight injectors then hit the enter button 5 LC Viv1 will appear then press enter to select it 6 press F1 to start check pos the arm will start moving and then stop over the septum 7 The needle guide rings should be centered x y on the septum port and about 0 1 mm above the port z Adjust x y z as necessary using the keypad To make adjustments use the knob to highlight x y or z and hit enter You can then use the knob to change the values and the arm will move You should only have to make very small adjustments or none at all because this position is set at the factory 8 select F4 to go home if the position is correct 12b Check the tray holder reference position using the keypad by Note no syringe should be installed and all the sample vial trays should be removed from the autosampler before starting 1 select F1 to enter the menu 2 rotate the knob to highlight setup and press enter 3 rotate the knob to highlight objects and press enter 4 rotate the knob to highlight tray holders and press enter
41. spectrum This spectrum is from the last analysis that is stored in the system s memory note there will be no spectrum the first time you turn on the machine Examine the absorption peak and make sure it is within the shaded area on the plot If the peak is out of alignment to the right by at least Y division 0 25 GHz and the curve extends outside the right side of the shaded area follow the laser offset adjustment procedure in the LGR manual The adjustment should only be required every three to five days but always check it before starting a run Volts Transmitted Intensity hro Figure 4 Spectrum Check 4 Make sure the old data runs have been saved to another computer then select configure on the instrument screen and remove the old data from the run list Use the lt key to remove the files and click OK with the left mouse button The system will not allow you to remove the last file so there will always be one old one remaining Page 7 5 Check and set if necessary the number of injections to 6 this means 6 per vial 6 Go to the sample list and hit delete to remove the old listings It will also not allow you to remove the last one 7 Enter the new information into the sample list by first putting the mouse arrow on the left column and then click OK with the left mouse button Then click the arrow on row 1 column 1 name and type in the sample or standard name using the keyboard on the instrument The firs
42. t sample will be the dummy sample Then click insert on the screen or hit enter using the keyboard To add more samples to the list hit insert then move the arrow over the null cell and type in the new sample ID Enter samples in the same order as they are on the autosampler tray Repeat until all the samples and standards have been entered Delete any extra null rows that may be at the bottom of the list Be careful when entering the sample information It is easy to make a mistake so you should double check that the information is entered properly 8 Highlight a sample on the sample list and click select all 9 Then move the sample list to the run list side by clicking on the gt key only once otherwise you will get duplicate sample lists in the run list and it will run everything twice 10 Get rid of the remaining old sample file on the run list at this point by clicking it with the mouse arrow and then click on the lt key to delete it Check that the first sample is listed as tray 1 position 1 11 Click on run the syringe icon and you should see the run screen with all 6 injections labelled Then hit the right pointing arrow key on the screen The system will ask if it is OK to start acquisition and if so click on OK the check mark on the screen The system should say that it is flushing the cavity on the lower right of the screen 12 Watch the autosampler for the first sample to make sure it is opera
43. te column Warning be careful not to loosen the large nut which is inside the column if it falls off you will have a big problem First unscrew the blue plastic plug from the lower nipple on the column using a wrench remember make sure the big nut inside doesn t fall off The lower nipple will be left open You only need to close it if you are not going to be using the instrument for a long time If you do put the plug back in make sure that a sign or visible note is posted on the instrument so that users are aware that the plug must be removed before the instrument is run 7 Unscrew the top cap from the upper port on the Drierite column using a wrench remember make sure the nut inside doesn t fall off or loosen 8 Screw on the small white hose onto the upper port of the column using two wrenches Connect the other end of the hose to the dry gas inlet connection on the back of the instrument using the 15 mm wrench 9 Hook the instrument power cable to the back of the instrument and plug it into the electrical extension cable surge suppressor main power However leave the power switch on the back of the laser instrument off at this point 10 Double check that all the instrument autosampler pump and Drierite connections have been made and are in the right spots The system should now be fully connected except for syringe installation and the power cord for the instrument can be plugged in 11 Unscrew the housing of
44. the autosampler septum and verify that a septum is in place It is a small red rubber septum with light colored Teflon on one side If it is still in the housing you should see the light colored white Teflon side when you look into the housing If it is still on the tube the light side will face downward and you will see the red side facing up There is also a dark colored cone shaped ferrule that sometimes comes out with the housing If this is the case put the ferrule back into the injection tube and you should be able to see the light colored side of the septum in the housing If there is no septum please put one in There is almost always a septum already in place Once you have verified that there is a septum screw the housing back on snugly and proceed to the next step 12 Prior to running the instrument and installing the syringe you must configure and test the autosampler Be aware that the directions that come with the instrument have some errors for this step Please follow the instructions below 12a Configuring and testing the Autosampler Do these steps without a syringe installed Turn on the autosampler power using the switch on the front of the transformer box It will take a minute to for the sampler to warm up you should see the intro screen on the keypad controller when it is ready If the injection head moves all the way to the back rail and makes an unpleasant grinding noise turn the power off and follow the t
45. three mounting screws on the front of the arm using the supplied screw driver 4 Take the injection head and hold it vertically and let the needle guide carriage the part with the small black rings gently drop out of the bottom of the injection head It will not fall all the way out but you need to let it lower to its full extent Hook the ribbon cable up between the arm and the top rear of the injection head 5 Place the injection head over the two mounting pins on the front of the arm and then replace the three mounting screws so that the injection head is attached to the arm It is easier if you put the screw on the supplied screwdriver and then insert the screw into the hole This is tricky because you have to stick the screws through the door in the injection head You can carefully pull the ribbon cable aside for better access 6 Once the injection head is screwed on check that the ribbon cable is not bound or pinched by checking it through the injection head door and by reaching beneath the rear bottom of the arm and seeing that there is some slack there You can now move the sampler back fully onto Page 21 the table by lifting the needle guide up and letting it rest gently on the table top or leg of the autosampler 7 Take the safety guard and install it around the front of the autosampler along with the keypad controller The notches in the guard should face up Use the small supplied thumb screw for the side without the keypad
46. ting properly takes about 4 5 minutes The syringe will move up and down three or four times before it actually injects the sample Also check the amount of water data and spectrum on the laser after the first injection has been measured Amount of water should be in the e 16 range and the spectrum should be a smooth curve If you see individual large markers on the spectrum or low water amounts anything less than 16 the syringe likely needs replacement Abort the run and follow the syringe change procedure sub procedure F This approach is a good way of detecting problems early before an entire run is wasted 13 Once the run is completed the screen will say run complete You can then transfer the run results to a memory stick for archiving and post processing see the data transfer procedure below Notes You do not need to use the standard scripts part of the software C Data Transfer 1 Choose file transfer with the mouse arrow 2 When prompted insert a memory stick into the USB port on the back left corner of the instrument and then click ok Page 8 3 At the please wait until prompted to remove the memory device message left click the mouse to say ok 4 See the directory of file listings and click on date modified at the top right hand to make sure the files are sorted There will be four files for each run txt txt igr text spectrum bz2 and __LIMS csv 4 Highlight the desired file e g
47. txt with the mouse arrow by clicking on the filename then click on the right pointing arrow on the screen and the file will be transferred to the memory stick Repeat this for the next file txt lgr You do not need to transfer the text spectrum bz2 unless you need to send it to Los Gatos for troubleshooting If you are using the Laboratory Information Management System for light stable isotopes LIMS see http isotopes usgs gov Research 20Highlights 20Pages LIMS htm you will need to transfer the _LIMS csv file 5 Click on exit then when you get the safe to remove message click the green check mark then click ok You can then pull out the memory stick 6 Proceed to a computer and backup the files in your laboratory data base or archive system so that you have at least two copies of the data files Always have two copies on separate computers or storage devices so that you do not loose data D Data Post Processing Currently the instrument does not output results as 5 values on the V SMOW scale it provides absolute abundance data This conversion must be done as a post processing step on a personal computer using MS Excel Note that in order for the IAEA laser spreadsheet template to function properly you should verify that the Windows control panel regional and language properties are set to English U S mode and that the Excel calculation mode is set to automatic go to tools options calculations 1 Copy the results files fro
48. um change complete on the screen Click on OK and then click the green check to complete the procedure Click on the green check again to return to the normal screen 7 Allow the system to warm up for at least 5 minutes This will soften the septum and prevent bent needles 8 Always watch the first injection after replacing the septum to assure that needle does not bend If it bends select abort black square on the instrument and wait for the instrument to complete the abort cycle it may take a few minutes and for the auto sampler arm to return to its normal spot You should see run aborted on the lower right side of the instrument screen 9 Proceed to the next subprocedure F to change the syringe and recover from the aborted run F Changing the Autosampler Syringe and Recovering from an Aborted Run Because of a Bent Needle Warning syringes are expensive do this step carefully to prevent damage to the needle or syringe 1 On the autosampler control select F1 change syringe hit the enter button press the button in the center of the round knob You should see replace syringe on the screen 2 Slide door over the syringe upward and loosen the red nut immediately above the syringe plunger Page 17 3 Grasp the near the top of the blue metal plate that holds the syringe and carefully pull the entire plate out The blue plate is held in place by a magnet 3 Flip the black plastic lock to the left and remove the old syringe
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