US Long-Term Ecological Research Network

Startup NOTE: skip to step 7 if machine is already on 1. Press the switch from OFF to RESET on the power strip beneath the NITROX unit. 2. Wait approx. 45 minutes for the NITROX unit to warm up. It is ready when the amber-colored OPERATING light slowly alternates between being lit and not lit. 3. Open the valve to the left of the NITROX unit, labeled GENERATOR. This kind of valve is open when the black handle is perpendicular to the wall and is closed when the handle is parallel to the wall. 4. Open the valve on the regulator that is just to the right of the Shimadzu analyzer (ProStar knobs). The correct knob is located towards the left and is the smaller of the two. 5. VERY SLOWLY open the air supply valve located to the left of the Astoria Pacific autoanalyzer and is connected to the blue hose. Open valve in a fluid motion and don?t be alarmed when hissing occurs. The hissing shouldn?t last longer than one minute. If it does, turn the air supply off and contact a supervisor. 6. Check the pressure gauge attached to the red receiving tank. It should display 75 psi. Check the outlet pressure of the regulator located to the right of the Shimadzu analyzer. It should read 400 kPa. (Check with a lab manager if these readings are not correct) 7. Create an entry in the Shimadzu log book. Note the following: start date, start time, # of samples (not including STD?s and BLK?s), operator, and the name of the project. 8. Startup the Shimadzu TOC Analyzer by creating a sample table and connecting to the instrument via the software: a. Click on the TOC Control V icon b. Turn on the instrument (lower right hand corner) c. Click on Sample Table Editor and Click OK when asked for user name d. Click File, New. A pop-up window will show several icons. Click on Sample Run and select the appropriate system (ex: LTER) and click OK. e. Click on Save, File and name the file without using spaces or slashes (ex: LTERdate.t32) f. Click Instrument, Connect, Use Settings on PC then click OK (make sure Shimadzu autosampler cover is closed) 9. Purge air through the system by accessing the Instrument section of the menu bar, followed by the Maintenance subsection, and ending with Mechanical Check. Click the Sparge button under the Syringe Pump section. Click the Open button for Sparge Gas under the Solenoid Valves section. Open the front door of the Shimadzu and verify air flow through the glass syringe. Let the system purge for several minutes. Click Close to stop. Click OK to exit mechanical check. 10. Verify a stable baseline by accessing the Instrument section of the menu bar and then selecting Background Monitor. Click the x50 button to zoom in, and then wait a couple minutes to verify a stable baseline. NOTE : skip step 11 if using an old curve and verify step 12 is correct 11. Create the calibration method: a. Click on File, New, and select Calibration Curve, which brings up the calibration wizard, Page 1. Choose the appropriate system (ex: LTER) and fill in comments like analyst, project, etc. (if desired). Click Next. b. Page 2. Select Dilution from standard solution to have the instrument dilute standards from the highest standard or stock solution. Edit Calibration Points Manually should be selected. Click Next. c. Page 3. For analysis, select IC first (if you plan on running IC and NPOC). Also select Zero Shift and Multiple Injections. The calculation method should be Linear Regression. d. In the Enter File Name field, click ? (to browse). Find the correct folder and enter a file name (ex: IC/ Click Next. e. Page 4. Entries for this page don?t change: mg/l units, number of injections 2/3, and the number of washes 2, SD max = 0.1000, CV max = 2. Click Next. f. Injection volume should equal 50. i.      Click Add. i-1.      Conc = highest standard i-2.      Conc dil = 1 if the highest standard is not a dilution (repeat for different dilution levels if desired) ii.      Click Add ii-1.      Conc = enter the next highest standard and the appropriate dilutions. ii-2.      When all standards are added, enter the blank, conc = 0 and dilution factor = 1. Click Next. g. Page 6. Select default. Click Next. h. Page 7. Don?t enable History log, just click Finish. 11. Click File, Open, choose Method Files from drop down list, LTER folder, select appropriate method, Open. (verify only if using old standards) 12. Generating the sample table order: a. Highlight line 1 on the sample table, select Insert, Autogenerate. b. Page 1. Select the appropriate method by clicking ? under Method and choose LTER, IC Method, (use one without extension if running an old curve) first (if planning to run IC and NPOC). Click Next. c. Page 2. No. of samples = 5 blanks to ensure baseline stability. Start vial = 1, sample name = MQ - , index start (check it) = 1. Click Next 3 times until the sparging/acid addition popup window appears and click OK. d. Highlight line 6. Select Insert, Calibration Curve. Select the Calibration File that was just created for the method. Enter vial position for the STDs and STD blank (usually at the end of the wheel and enter them in the STD notebook). Use arrow keys to move within the window that shows sample vial positions on the wheel. If you hit return, the program will scroll to the top of the sample list. Click OK. e. Highlight line 7. Select Insert, Autogenerate. Enter the method again (do this every time you use autogenerate). Click OK. (When removing rows, you must use CUT, NOT DELETE.) 13. The number of samples should not exceed 80 ? 85. The max number of positions on the autosampler is 93, but some space needs to be reserved for standards, blanks, etc. 14. Repeat for NPOC. (When copying rows of sample IDs, copy and paste selecting ?Paste Cells.?) 15. Save the file. 16. Before starting the run: a. Allow the combustion furnace to warm up to 680 degrees C (1 to 1.5 hours) b. Check the level of the rinse reservoir (replenish) and the waste container (empty if over half full) Replace the Milli-Q water in the diluent reservoir. c. Check level of the humidifier and add Milli-Q to maintain the level between lines d. Make sure bottle in the back of the Shimadzu is filled to the side arm. e. Select Instrument, Maintenance, Mechanical Check. Select Replace Flowline Content. f. Also, under Mechanical Check, select Open Acid Valve and pump for over 5 seconds then Close the valve. 17. Press Start (traffic light) to start run. Select Standby to leave the instrument running after your analysis is complete or Shutdown. . Shutdown 1. After the analysis is complete, shutdown the Shimadzu. Once the command is given, the instrument no longer requires carrier gas. This can be verified by watching the float in the flow meter that is visible through the front panel fall to zero. 2. Close the valve that supplies compressed air to the system. It is located to the left of the Astoria Pacific autoanalyzer, and is connected to the blue hose. 3. Close the open valve to the left of the NITROX unit labeled GENERATOR. This kind of valve is closed when the handle is parallel to the wall. 4. Open the valve on the regulator that is just to the right of the Shimadzu analyzer. The correct knob is located to the left and is the smaller of the two.

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