
You need to submit your sample in a small vial that is clearly labeled with a sample code. You must also fill out an "Elemental Analysis Request Form". You can find blank forms in the box outside of room 2524. Or, if you are not in the Chemistry department, you can print out and use the blank form found on this website.
Please provide as much information as possible about your sample, and what type of analysis you would like done to it. It is essential that you provide your name, phone number, e-mail address, your advisor's name, and a valid shortcode account number for billing purposes.
You should provide a bare minimum of 4 milligrams for CHN analysis. This will be enough material for a duplicate analysis. If you can spare extra material, 8 mg would be better in case there are problems and the sample needs to be re-run. You will need to provide an additional 5 mg if you need ICP-OES analysis in addition to CHN. In cases where you have very little sample available, it is possible to do one CHN run with as little as 1 mg.
CHN and ICP-OES results are normally completed within 3 working days, but this can vary depending upon sample load and instrument problems.
If you have a mailbox in the Chemistry department, the results will be placed in your mailbox. If you are outside of the Chemistry department, you will be phoned or e-mailed to let you know that you can pick up the results. Alternatively, if you are out of the department and you do not want to reclaim the residual chemical sample, the results can simply be e-mailed to you.
CHN weight percentages should be accurate and reproducible to within + or 0.3%, provided that the sample is very pure.
The sample must have the correct structure and must also be very pure. If there are any solvents or moisture trapped in the sample, this will affect the accuracy of the results. This usually happens with samples that are oils. Also, if the sample is not homogeneous, duplicate runs will not agree to within 0.3%.
If a sample is extremely volatile, it may loose mass due to evaporation after it has been weighed out, even if it is crimp-sealed in a special volatile sample pan. This can also cause the results to be inaccurate.
Some compounds are inherently difficult to combust completely. Incomplete combustion can also cause inaccurate results. In this case, the sample could be re-run under different conditions, with an added oxygen boost, or with the addition of chemical combustion aid such as powdered tin.
Please let Carol know if you have any concerns about the results. She is willing to re-run a sample under different conditions if it doesn't work out the first time.
Yes, air or moisture sensitive samples can be analyzed by handling them in the dry nitrogen atmosphere of the glove box. For CHN, the procedure would be to first weigh the tin sample pans. Then the sample pans and sample are brought into the glove box. The sample is then placed into the tin pans, and the pans are crimp-sealed while inside of the glove box. Then they are brought out of the glove box and weighed again. The weight of the pan is then subtracted from the weight of the sample plus pan, in order to give the net weight due to the sample.
Yes, if the ICP-OES is configured with a different injector, and different tubing, then metals can be analyzed in organic solvent solutions.
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