MICADAS manual

Make sure to finalize the flushing before the last run has finished (otherwise the system changes automatically into standby mode)

A: Change the EA flow (not needed if you use a separate MFC):

Choose tab 'Options' → Service → Parameters

Change flow to 105 mL/min

A: Fill out the EA sample sheet (copy and paste the output information from the 'LamaImport' file or follow the procedure as decribed hereinafter):

Fill out the sample and standard numbers (as created in LaMa) into the column 'Name'

Write an estimated mass value or any value different from zero in the column 'Weight'

Select the method 'Gary_new50s' in the column 'Method'

If a flush/cleaning run is desired between two sample runs, then insert an additional line each between two samples:

Write 'Pre' in the column 'Name'

Write any weight (e.g. 1) in the column 'Weight'

Select the method 'Blank_Gary' in the column 'Method'

If the name of the next sample is 'End', the LabVIEW will trigger the sleeping down of the EA, the LabVIEW measurement stops and the magazine position will be changed to home position.

Check that GIS is switched on

Check that Sunset is physically connected to GIS

Check that EA line is physically connected to GIS

Check if He capillary is correctly connected to GIS box

Check that capillary from GIS box to ion source is connected

Turn on GIS pump and check if the manual valve on top of the pump is opened

Open He-bottle for GIS completely (both valves)

Set pressure to ∼1.2 (by adjusting pressure reducer, see label)

Set pressure to <1 barg (optimum is 0.8 barg) by adjusting pressure reducer

G: Start LabVIEW, choose latest version ("BernGasIonSource1XX.vi")

Click on white arrow (top left)

Go to header 'Control panel' and click 'start program'

Select Sunset-ini-file ('131010_1858GIS-SUNSET.ini') in the pop-up window and click 'OK'

Select CHS-ini-File ('GIS-carbonate-120mm') in the pop-up window and click 'OK'

Select EA-ini-File in the pop-up window and click 'OK'

Select Cracker-ini-File in the pop-up window and click 'OK'

Go to header 'Communication'. Computer cards should all state 'DLN_RES_SUCCESS' (otherwise stop and restart the program)

Go back to header 'Control panel'. Make sure V3 is found (green) (if necessary by changing the method)

Check that the 'Automatic off' button is green

Switch V7 to 'ON' (has to be on as soon as temperature of ion source is above 115℃!)

Tick 'auto adjust' (recommended)

G: Go to header 'Control panel' (tab 'Sunset') and click 'Clean syringe'

G: Go to header 'Control panel' (tab 'Acid') and click 'Clean syringe'

G: Go to header 'Control panel' (tab 'Cracker') and click 'Clean syringe'

G: Go to header 'Control panel' (tab 'EA') and click 'Clean syringe'

Leak test the syringe (area where the O-ring is placed) while the helium in the syringe is pressurized

M/S: Open TightVNC (pw: helloc14) to see GIS-Screen (GIS-Computer=06)

M: Open TightVNC (pw: helloc14) to see GIS-Screen (GIS-Computer=06)

M: Restart the service:

Click '☰' and 'Restart Service'

Confirm the warning message by clicking 'Yes'

Reload the webpage several times to get connection again

Click on the user icon and choose 'Take control'

Go to the task list and click 'Start' to start the automatically created wake up task

Click '⋮' of the wake up task and choose 'Finalize' (the system should now be in state 'Ready')

M: Choose gas measurement conditions (V7 has to be ON!!)

Search for tuning settings from the last gas measurement

Click on '⋮', 'show' and 'apply'

M: Create task for gas measurement

Click on '+', 'Measurement' and 'Gas measurement'

Type magazine number (CYYMMDDiniG ('ini' are your initials)) and cycle time (10s), confirm by clicking 'OK'

Click 'Start' in task list

G: Go to header 'Communication'

Click button 'Auto-reconnect' (turns green)

Make sure that the right IP address (130.92.107.74) is written in the field 'Computer name (soproni)'

Click 'Establish connection'. Then click 'TCP test', write 'getstatus' in the field 'Send command to Squirrel' and click in the field 'Squirrel response log'. The answer should be 0/0. If this is fulfilled, unclick 'TCP test' (turns blue)

Check that the button 'Diolan State' is green

Check that there is no Error for the Omron Temperature controller (light should be off)

Check communication with the pressure sensors. The light of 'RS-converter: echo' should be on

G: Go to header 'General parameter' and check that the state machines are all in state 'release' or 'idle'.

G: Go to header 'Control panel'. Clean trap 1-2 times by clicking 'Clean trap' (tab 'Sunset')

G: Go to header 'Control panel'. Clean trap 1-2 times by clicking 'Clean trap' (tab 'Acid')

G: Go to header 'Control panel'. Clean trap 1-2 times by clicking 'Clean trap' (tab 'EA')

G: Click 'sample list import' and select the first sample in the drop down menu 'sample label'.

G: Click 'sample list import'.

G: Go to header 'General parameter' and copy the path in the field 'Measurement file path' to the field 'Sequence folder'

Check gases for Sunset (all of them need to be open). If one of the bottles runs low (<50 bar), someone should be informed to order a new one.

Oxygen (label indicates minimal pressure (∼1.3 bar). However, pressure is mostly higher due to back pressure)

Calibration Gas (5% methane in helium)

S: Click 'out of standby'

S: Choose the right valve table

Go to folder 'Sunset Software > OCECPAR'

Save the file 'valve_table_O2' as 'valve_table', (i.e. replace previous one)

S: Change 'Cal. Constant'

Go to folder 'Sunset Software > OCECPAR'

Save the file 'InstrumentParameters-online' as 'InstrumentParameters', (i.e. replace previous one)

Click button 'Reload Params' in Sunset-Software

S: Tick 'show valve value table' and click 'Auto Zero Flows - IDLE only' in the pop-up window

S: Put your name/initials in field 'Analyst'

S: Tick 'save NDIR data to File "NDIR_Data.txt"'

Put a blank filter in the oven

Switch black valve to the vent

S: Click header 'Action' and choose 'Clean Oven'

Flush the lines with helium (as soon as oven cleaning has finished)

Switch black valve to GIS

S: Type 'He flush' in field 'Sample ID #'

S: Choose '3600s He flush' as parameter file (in folder 'Sunset Software > Parameters')

S: Click 'Start Analysis'

Test for leaks while the system is flushed with helium

Measure bottle standards (once each) in order to check how the system behaves:

Measure bottle standards (3x oxaII & 2x blank):

G: Flush system with bottle standards (3 times):

G: Flush system with bottle standards (3 times (only 2 times if same standard is remeasured)):

Go header 'Control panel' and then choose the tap 'tuning' (confirm by clicking 'OK')

Select the corresponding gas in the dropdown menu 'Combo box' (Ref. gas 1 (oxII) or Ref. gas 2 (blank), resp.)

Correct for the pressure offset using the fields 'Cracker offset' and 'Syringe offset' in header 'General parameter' (pressure sensors should state '0')

Open screw of the corresponding standard gas bottle and close it again. Open then the valve in front of the bottle manually to fill the line with gas. Aimed pressure: ∼1200 mbar (be careful!)

Move syringe forward by clicking 'Fast forward' (pressure should not exceed 1600 mbar)

Move syringe 20 forward (set steps to 20) by clicking 'Fast forward', then click 'Fast backward' (repeat)

Click 'Home position'

Switch V0 a few times for- and backward

Set steps to 100. Click 'Fast Forward', then open immediately V1. Important: Set the steps back to 20 (cleaning) or 1 (loading)

Click 'Home position' and close V1

G: Open V1 and V2 to pump the lines

G: Close V1 and fill the line with standard gas. Make sure to have 1200-1300 mbar (by moving plunger stepwise)

M: Click '⁝' of gas measurement task, choose 'Measure manually'

M: Type target ID of the last measured bottle standard (19287 for oxaII & 1216 for blank, respectively) and click 'Create Next'

M: Set target position (start at 2 (!) for first measurement and increase by 1 for each run)

M: Click 'OK' to start the measurement

M: To show results click on '⁝' of the current task and choose 'Result'. Make sure 'Live' is ticked.

G: Switch V0 to AMS as soon as ACS states 'Measuring' and 2-3 cycles have been measured

Finish run when enough cycles were measured:

M: Click '⁝' on the gas measurement task and choose 'Duplicate' (confirm by clicking 'OK')

M: Click '⁝' again on the current task and choose 'Finalize'

G: Change to header 'Sunset' (in order to have a helium flow for cleaning process) and click 'Clean syringe' (only needed after first bottle standard; restart with flushing precedure for second bottle standard as soon as cleaning syringe has finished)

G: Change to header 'Cracker' (in order to have a helium flow for cleaning process) and click 'Clean syringe' (only needed before switching to other bottle standard; restart with flushing precedure for second bottle standard as soon as cleaning syringe has finished)

G: Change to header 'Acid' (in order to have a helium flow for cleaning process) and click 'Clean syringe' (only needed after first bottle standard; restart with flushing precedure for second bottle standard as soon as cleaning syringe has finished)

Prepare Sunset (during last bottle standard measurement):

S: Click 'Cancel Run' if he flushing has not finished yet

Do a TC dummy run (to circumvent the different calibration peak of the first run)

Switch manual valve (black) to vent

S: Choose path of 'parameter file' (in folder 'Sunset Software > Parameters'): 'TC_withTempOffsets_xxxxxxxx.txt'

Click 'Start Analysis'

Place standard in oven as soon as dummy TC run has finished

S: Choose path of 'parameter file' (in folder 'Sunset Software > Parameters')

For TC/EC: 'TC_withTempOffsets_xxxxxxxx.txt'

For OC: 'Swiss3S_OCremoval_withTempOffsets_xxxxxxxx.txt'

S: Choose path for 'Output Raw Data file' and set name for the file

Switch manual valve (black) to GIS

S: Choose 'Punch Area' of filter (for standards choose '1 sq cm')

Open TightVNC (pw: helloc14) to see CHS-Screen (CHS-Computer=13)

C: Click 'Go Home' and leave the syringe in position 'up'

C: Click 'autosampler on' (has to be off). Then click 'Stop program' and close LabVIEW.

Physically change the USB connection of the autosampler from CHS to GIS.

G: Go to header 'Communication' and click 'Autosampler on' (the light next to 'PAL COM state' should turn green)

G: Go to header 'Control panel'. Enter '42' in the field 'Set position' and click 'Autosampler move'. Go to header 'Settings' and click 'down'.

Physically connect the line from CHS to GIS using the valves in the preparation lab (U115).

Leak test all connections between CHS and GIS.

If you want to install a separate mass flow controller (MFC) (no need to do this):

Place the MFC in line just before the GIS inlet.

Turn the MFC on and connect the serial cable to the GIS-computer.

G: Go to header 'Communication'. Choose the right com port for the MFC and click 'Start' (the state button should turn green).

G: Set the Setpoint to 210 mL/mL (is later controlled by the method).

Leak test all connections between EA and GIS.

G: Establish connection between EA and GIS.

Go to header 'Communication' and select 'szidat-07.dcb.unibe.ch' from the dropdown menu 'Computer name'.

Click 'TCP test' (top right corner). EA response log should then state 'STS READY'. Unclick 'TCP test'.

G: Go to header 'Settings' and click 'up'. Change to header 'Control panel' and click 'Go Home'.

G: Go to header 'Settings'

Set 'Pre trapping' to 130s

Set 'Pre trapping' to 0s

Set 'Trap sampling time' to 240s (TC/EC) or 335s (OC)

Set 'Trap sampling time' to 180s

Set 'Squirrel next target' to 4

Set 'Squirrel next target' to 7 (or to the next one after having measured standards and blanks)

Set 'Squirrel last target' to 40 (if magazine is completely filled with targets)

Set 'target home' to 1

Set 'flow temp' to 45/50

Set 'flow temp' to 60

Set 'preP temp' to 1250

Set '# Cycle limits' to an appropriate number (e.g. 70)

Set 'C flow temp' and 'Aimed C flow' to 1.1

Set 'Aimed C flow' to 1.4-1.5

Set 'Minimum sample mass' to 10μg

Set 'max ¹⁴C' to 2E6 (can remain mostly unchanged)

Set 'Trap syringe pressure' to 0.44

Set 'EA constant' to 48

Under 'measure mass' choose the option EA area

Set 'Normal inflow' to 210 (if MFC is active)

Set 'Trapping flow' to 80 (if MFC is active)

Click 'No Pre' (turns into 'Pre')

G: Go to header 'General paramter' and check the 'row to update' and 'file row' (consecutive number on control panel in the sample list: position # minus 1 is the row to update). Note that the 'File row' may extend the value of 8, e.g. cracker position 4 of the second cracker magazine has the file row 12.

G: Check again all settings. Then go to header 'Control panel', choose tap 'SUNSET' and click 'Start Method'.

Put samples in Cracker magazine/tube. Make sure they are in the right order (1-8).

G: Go to tab 'Cracker' and click 'open cracker magazine'. To unlock the magazine there is a small lever.

G: Flush the system twice with He by clicking 'Flush Cracker'

G: Check again all settings. Then go to header 'Control panel', choose tap 'Cracker' and click 'Start Method'.

Open TightVNC (pw: helloc14) to see LICOR-Screen (LICOR-Computer=17)

L: Start recording data:

Open the program 'LI-COR LI-8x0_v.1.0.2' (can be found on the desktop)

Click 'Connect'. Then choose 'Connect to: 0 - COM5 LI-850', untick 'Manual port', set 'Data rate' to 0.5 and confirm by clicking 'Connect' again.

Click the button 'Setup Login' and choose the following logging settings:

Click 'Select file' and choose a file name (YYYY-MM-DD_HH_MM_Description) in the pop-up window (files should be saved locally in the folder 'Documents')

For 'File headings' and 'Log values' leave all options ticked

Choose 'Tab' as 'Field delimiter'

Set 'Log rate (seconds)' to 0.5 and close the window by clicking 'Close'

Click the button 'Start Logging' (make sure that the 'Cell Temperature' has reached 51.5℃)

G: Check again all settings. Then go to header 'Control panel', choose tap 'Acid' and click 'Start Method'.

G: Check again all settings. Then go to header 'Control panel', choose tap 'EA' and click 'Start Method'.

As soon as Sunset is ready, indicated by 'Save to put a new sample' (green window), the next sample can be placed in the oven.

S: Type sample name in field 'sample ID #' and change path of parameter file if necessary.

When status of LabVIEW says 'Sunset burning can be started NOW', click 'Start Analysis' in Sunset Software and then immediately 'Start Analysis' in LabVIEW.

Check that the ampoules are correctly cracked.

Recommended: sample mass should be taken from 'p gauge' (header 'Settings') and not from the Excel-file.

If the ampoule is not cracked, a message will pop up and the measurement will not be continued:

Pop up message: Sample mass does not match the excepted mass

If there is a pressure reading >0 but different from the excepted mass and the sample mass is uncertain → click 'continue'

If pressure = 0 (ampoule not cracked or empty) → click 'correct'

Try to crack ampoule by manually pressing and releasing 'Crack' several times.

If it works the pressure rises. If you are confident in your own sample mass (excel file), write that value and click 'SET'. The procedure will continue as usually. If you are not confident about your m_c, read the pressure and write down the mass as m = 0.44×pressure, click 'SET'

If it does not work, you need to scratch the ampoule again. To do so, click 'open', remove the cracker, and scratch the ampoule again. Put the cracker back, press 'open' again and manually flush the cracker with He 3 times. With syringe in home position, pump the line until V8 (closed), correct pressure offsets of both sensors and then close the pump and V2. Press and release 'Crack', and if it works, proceed as described in the previous bullet point.

Prepare the next cracker magazine before the first magazine reaches position 8. Make sure that there are no glass particles anymore in the tubes (Dust off spray)

After cracking and loading sample 8, a message will pop up, that the last position is reched. FIRST, take the measured magazine out and put the new magazine, THEN confirm the message.

For large samples (>threshold (85μg C)), the GIS software might dilute the sample too much. You may have to load these samples manually (same as for std/bk).

For all samples: check that current can go high enough (∼12). Adjust syringe pressure and C flow accordingly.

For last sample: click 'stop after next sample'. GIS will stop automatically and you do not have to restart the program before measuring std/bk.

Measure Std and Bk after the samples:

G: When reaching the last sample, click 'stop after next/this sample'.

M: Click '⁝' on the gas measurement task and choose 'Duplicate'

M: When the last sample has been measured, click '⁝' again on the current task and choose 'Finalize'

G: After the measurement has finished, you will have to wait a few minutes, before the GIS is stopped properly. If this does not work, you will have to restart LabVIEW again:

G: Click 'Stop program'. If this does not work, force the program to stop (red button top left).

G: Start LabVIEW again as in the start-up procedure. You may have to restart the program twice. Make sure, that you stop LabVIEW without force stop the second time.

G: Go to header 'Communication'. Click 'establish connection'. Then click 'TCP test' and write 'getstatus' in the field next to it. The answer should be 0/0. If this is fulfilled, unclick 'TCP test' (turns blue). If this does not work, restart the ACS service and try again.

Measure Std and Bk (usually 1 Std and 2 Bk). For procedure see above.

If the current drops before the desired number of cycles is reached even though there is still sample left, click 'Stop and Next' in LabVIEW and confirm (or change to another target if you would like to continuing with the measurement of the current sample).

Put a blank filter in the oven

Switch black valve of Sunset to the vent

S: Click header 'Action' and choose 'Clean Oven'

S: Fill in the measurement in the logbook (file on desktop) as soon as cleaning oven has finsihed

S: Click on 'Standby'

L: Click 'Stop' to stop the logging and close the LICOR program

M: Click '⁝' next to the gas measurement task and choose 'Finalize'

M: Move magazine to position 1:

Choose 'Sample Changer' on the Menu panel

Type '1' (as position) and press enter

M: Reduce Cs temperature to 115℃.

Insert new magazine if one has already been prepared:.

M: Choose 'Sample Changer' on Menu panel

M: Click 'OUT & VENT'

Physically change the magazine

M: Click on '+', 'System' and 'Sleep' to create the task. Then click on 'Start' in the task list to start the task.

M: If there is a measurement planned for the next day: Create task to wake up the system the next morning

Click '+', choose 'System' and then 'Wake up' and set time for wake up on day of measurement (60' before start of measurement)

Set stabilization time to 5 min and confirm by clicking 'OK'

Click 'Start' in the task list to start the task

A: Change the EA flow back to conditions for graphitization:

Choose tab 'Options' → Service → Parameters

Change flow to 180 mL/min

As soon as the Cs temperature reached 115℃ (or lower):

G: Stop the LabVIEW program by clicking on button 'stop program' (if this does not work, click the red button to force the program to stop). Close the program.

Turn off the GIS-pump

Close He-bottle for GIS (bottle valve and regulator valve)

M/S: Close TightVNC

Close He-bottle of CHS (make sure nobody else is using it, i.e. EA and AGE are turned off!)

Unplug USB-connection of autosampler.

Flush and clean syringe and cannulas.

Open program 'Calc426' (on Desktop)

Choose your Output Raw Data file

Click 'Calculate all Samples' (Excel file is created and saved to same folder as the Output Raw Data file)