ICP-OES
This manual is meant to complement your training and is not intended to replace on-the-job training.
WPC Activities Associated
MF-0005; Strong Acids Handling
Training Contact
Tracy Mattox
tmmattox@lbl.gov
67-4111
x2649
Last Updated
04/30/2015
OPERATING PROCEDURE
1. Turn on argon
Pressure in cylinder must be >500psi
YOU MUST CHANGE THE CYLINDER if the level drops below 500psi
Delivery pressure is just over 100psi
Open cylinder at the tank
Open the flow valve using the small knob on the regulator
2. Turn on chiller (press button on upper left corner of unit)
3. Turn on Autosampler
Wait for arm of Autosampler to stop moving before continuing
4. Open “ICP Expert II software” located on the desktop
The 20min timer for Peltier cooling starts at this point (details will follow)
5. Press the “Worksheet” button
6. Create a “New” Worksheet (or open an existing sheet)
7. Name the data set you will be running:
Select the C: drive Select “ICPOES data” Select your folder Enter the name of the data set you will be running
8. Under the “Method” tab select “Edit Method”
9. In the “Method Editor” window select the elements for which you have prepared standards
In the “Add Analysis Line” window, choose three wavelengths, ideally with differing intensities.
Be mindful that other elements within the sample may interfere with the element of interest and try to select wavelengths that will not conflict with other elements in your sample.
To add the wavelengths to the spread sheet:
Select each wavelength one at a time and then press “Apply” and then “Close” when finished
OR
Press “Ctrl” to select multiple wavelengths and then “OK”
10. In the “Standards” tab, enter the information of the standards you have prepared:
Input the number of standards
Select the correct units of measure
Enter standard concentrations from low to high values
DO NOT include the blank as a standard
Only include multiple values in a column if you have multiple standards within each tube of standard solution (example has one element per tube of standard).
11. Select File then Save (or Ctrl S) to save your standards.
12. Exit the “Method Editor” by clicking the red “X” in the upper right corner (or select File -> Exit)
13. Under the “Sequence” tab select “Sequence Editor”
Uncheck “Recalibrate every.” (It’s not necessary to re-run standards unless you are running >50 samples.)
Enter the number of samples you will analyze under “Sample Count” (NOT including the standards or blank)
14. Press OK to exit the “Sequence Editor” page
15. Under the “Sequence” tab select “Autosampler Setup”
You have the option to right click on the small racks on the top and bottom of the Autosampler set up. Right click on the rack, select “Rack Type” and then “Not Fitted.”
Though not required unless you have more than 12 standards, most people prefer to do this so that they can load standards and samples on the same tray.
Press “OK” to exit this window
16. Inspect all tubing, ensuring there are no cracks or flat spots. Replace any tubing necessary with the back-up supplies in the drawer below the Autosampler.
17. Set up tubing
On the Autosampler: Lift the grey tab up and secure in back slot. Set white cover against tubing, then secure with white covered pin.
On the ICP: Pull blue tab and secure it in the back slot. Pull the white tab and secure in the front slot. Lift black bars up and secure by pulling down the upper brackets (they will snap into place).
18. Place feed tube into 2% nitric acid washing solution
If you run low on washing solution after your run it is YOUR RESPONSIBILITY to refill it for the next user.
19. Ensure that the waste collection bottle has enough space for your wash solution. If the solvent will reach the level of the black mark in the photo below, you need to change out the bottle. Instructions on handling the waste are on the printout next to the instrument.
20. Fill all of the tubing with the washing solution (2% nitric acid in water)
Select the hammer icon then select the “Autosampler” tab
Press “Rinse” to start pulling solvent through the Autosampler
Press the “Pump Fast” icon to start pulling solvent into the nebulizer
21. Ensure that the washing solution is flowing properly through all of the tubing
Take great care to note a constant flow of liquid exiting the bottom of the nebulizer.
If the liquid does not flow as depicted by the red arrows in the image below then you have connected your tubing backwards!
DO NOT continue unless you confirm that liquid is flowing through the system!
21. Once you have confirmed liquid is flowing well through the system, turn off the rinse by pressing “stop-rinse” and the “stop pump” button, as shown below:
23. Once the pumping has stopped, select the “Status” tab
Ensure that the Peltier is at -35°C.
This temperature is only reached if the software has been on and the argon has been flowing for 20 minutes!
24. If (AND ONLY IF) the Peltier is at -35°C and all tubing is full of washing solution, it is safe to turn on the plasma torch by pressing the light torch icon. From this point on the washing solution must never run empty!
25. Gas flow will increase and eventually you will hear the click of the plasma igniting.
26. Allow the plasma torch to stabilize for 5-10 minutes before you run your samples.
27. Load samples in rack, ensuring that a blank is in position one. Secure rack in the Autosampler.
28. Once samples are loaded, select the analysis tab. If standards and samples are highlighted in yellow press the green arrow to begin running your samples. (Sometimes the standards do not highlight in yellow. If that is the case, just click on the first tube 1:1 and proceed as normal with the green arrow.)
29. It takes roughly two minutes per standard/sample to run. Feel free to leave the room and come return as the last samples are being analyzed.
30. Once your run has completed, turn off the plasma by pressing
and allow the system to continue flowing argon with the torch off for at least 10 minutes.
31. Remove tubing from washing solution and fast pump/rinse to dry out the tubing. (This is a repeat of steps 21 and 22 but without the 2% nitric acid wash.) Ensure both pumps have stopped moving before exiting the software!
32. If your results are values in black, skip to step 34.
33. If your results say "uncal" then you need to limit the concentration range of the standards:
Click on the “/” symbol to see the calibration information. If the error is less than 5% the green calibration line will automatically be drawn. Double click on the wavelength you wish to work with next. If your error is >5%, you need to tell the system which standard points you want to use in your calibration line. Right click on the black calibration screen and select “Adjust Calibration.”
In the “Method Editor”, ensure that you are working with the appropriate wavelength and adjust either the “Min. Conc.” or “Max. Conc.”, then save (File --> Save or Ctrl S).
If a calibration line forms and your sample values are visible then you are finished with that wavelength.
If a calibration line forms but your sample values are listed as a red number then your sample lies under the minimum concentration in your calibration line, so you need to go back and adjust the max instead of the min!
If your calibration line does not form and your %Error is <10% then you can change the “Max. % error” and save so that your calibration line forms.
If your concentration reads as “---x” then the actual value lies above the highest point in the calibration line. If your concentration reads as a red number then the actual value lies below the lowest point in your calibration line (or the actual value is zero). Double clicking the black screen allows you to toggle and view either all of the calibration wavelengths and the individual wavelengths with the error values listed. 34. To save your data you can print as a PDF.
35. To export your data there are two steps:
Select File --> Export Settings, enter what data you want to export, then click “Browse” to select your folder. This tells the system what and where to save, but does not actually save the data! Select Export to save the data 36. Exit the software, release the tubing, turn off the chiller, and close the gas cylinder (both at the tank and on the regulator).
37. Sign the log book, tidy up, and take your “stuff” away with you!