WSEL ICP Instrument Operating Procedure

 

 

1)      Turn the chiller on, if it isn’t already on

 

2)      Check the Argon cylinder pressure.

 

3)      Turn on the computer and monitor

 

4)      Click on the WINLAB32 icon on the desktop.

 

5)      A diagnostic window comes up with the System Status of “Spectrophotometer is in standby mode”

 

6)      Click on the Spectrophotometer tab and click on Initialize. Warm up begins in 2 minutes and goes for another 75 minutes.

 

7)      Replace peristaltic pump tubing on the sample nebulizer assembly. Use red-red clear tubing for the waste line and black-black solvflex tubing for the sample line. Gradually stretch the tubing first before attaching the tubing to the peristaltic pump to avoid uneven sections in the tubing when it is stretched across the peristaltic pump rollers.

 

8)      Click Winlab32 Offline icon to create a sample identification file while the spectrophotometer is still warming up.

 

9)      Click on the file, then open sample info and select a previous similar file or template. Modify the file with new sample ID’s, etc., and save the file as a new file with the project name and date of analysis. Ex. LTER_042505.

 

 

10)  Exit Winlab32 offline, and place the samples and standards in the autosampler tray, according to the sample info file.

 

 

11)   After warmup is complete, click on Plasma Control . Check the line pressure, and if the pressure is less than 800kpa, slowly open the pressure builder.

 

12)  Click on Plasma On to ignite the plasma. Shortly after the plasma lights, the peristaltic sample pump will start to rotate.

 

13)  Stretch the pump tubing over the mounting brackets. Adjust the peristaltic line pressure clamps to ˝ to 1 full turn from the end.

 

14)  Observe the nebulizer spray chamber, looking for a uniform and steady sample  mist. The plasma should also appear steady without flickers or pulses.

 

15)  Click on tools, spectrophotometer control, and then Hg align. After the Hg wavelength alignment procedure is completed, write the intensity count in the logbook.

 

16)   Place the sample probe in a 1 ppm Mn solution. Click align view and radial, to align the torch position. After the torch has been aligned radially, click on axial to align the torch along its axis, and write down the intensity in the logbook.

 

17)  Click on file, open and method to select the method to be used. Choose the LTER method that corresponds to the set of standards that are being run.

 

18)  Select the sample information file (that was just created offline) in the same manner as step 17.

 

19)  In the sample information popup window, input the sample result file – usually the analysis date.

 

20)  Click on Auto Shutdown and select At the end of analysis, place the spectrophotometer on standby and turn the sample pump and plasma off after a 5 minute rinse.

 

21)  After the sample pump and plasma are on for over an hour, the system is stable enough to start the analysis.

 

22)  In the automated analysis window select Run Standards to have the instrument stop after calibration. Run Samples must then be selected to start sample analysis. Select Run All to run the samples automatically after running the standards regardless of the quality of the calibration.

 

23)  When the analysis is done, cap the samples and standards as soon as possible to avoid evaporation loss.

 

24)  Turn the water cooler off and close the argon tank pressure builder valve.\

 

25)  Release the sample pump tubing and clean the area, replacing printer paper and ink cartridges as necessary.

 

26)  Enter the number of hours of ICP use (Argon use) in the logbook. 

 

(updated 5/11/2005 jat)