Dear researchers and fellows,
could any of you suggest the recipe of sample preparation for ICP-OES measurement, to those without experience with it?
Here is some information about the samples: Ni + Fe co-sputtered thin film on the 1x1 cm^2 Ti-substrate, thickness around ~50 nm.
Your question is a little vague at the moment. If you could elaborate on:
- the material you are wanting to analyse (e.g. purifed metal ingots, dust samples, plant tissue, animal organs, paper, pharmaceuticals)
- the sample mass you are dealing with (mg = tiny, or kg = massive)
- the elements you wish to quantify, and
- any potentially interfering elements present in the matrix (eg sodium from seawater, gold from ingots),
then someone might be able to help you.
A similar question was posed some time ago specifically for plant analysis: https://www.researchgate.net/post/Can_anyone_give_protocol_of_soil_and_Plant_Sample_preparation_For_ICP-MS.
Hi,
as already mentioned by Matthew: there exists no general/generic answer to your question. The digestion procedure is dependent on your sample type and also on the elements which you want to measure with ICP. Normally, the vendors of digestion systems provide application notes and have also experienced application chemists available which can help to define customer specific applications.
We have here a microwave digestion system and use it normally for solid samples. Most liquid samples (from 25% NaCl to organic solvents) are measured directly via ICP-OES and/or -MS.
Generally you have to be very carful that you use the right sample amount (especially for "reactive" samples) with the right vessels. Additionally, you have to inform you which type of matrix should not be digested with acids (methanol for example), because it will lead to significant safety issues.
I suggest that you contact the instrument vendor and discuss the samples which you plan to digest.
Dear Matthew Wheal and Kerstin Vogel
Thanks a lot for your quick answers!
I am very sorry for the lack of information. I had no idea what you might need.😅
I would like to measure the amount of Ni and Fe of NiFe-oxide thin film. The substrate is Ti, and all the procedures (except the substrate cleaning step) were done in UHV. So I would not much of dirts, but Ti will exist mostly.
However, how can I tell the sample mass, if I don't know the exact amount of deposited materials?
So you are dealing with fairly small quantities per individual item, but possibly many of these pieces (presumably you can always produce more). That means you only get a small sample mass each time, which will determine the volume or concentration you can reasonably achieve with sample prep.
Solid surface analysis is not my forte, but in terms of quantification, maybe you can calculate per mm2 or similar? Perhaps you should be considering Laser Abalation mass spectrometry? That uses a laser to vaporize the surface of your sample which is introduced into the instrument.
There are a number of older texts that deal with metal dissolution that are apparently quite useful:
- Lord and Demorest Metallurgical Analysis, 5th Edition, McGraw-Hill, New York, 1924 is one,
- Thomas R. Dulski, Manual for the Chemical Analysis of Metals, ASTM series is another.
I would also suggest looking up "metal dissolution" in the Plasmachem-L archives. https://listserv.syr.edu/scripts/wa.exe?A0=PLASMACHEM-L
In terms of interference during the analysis, Ti is your issue here. You will want to choose wavelengths of Fe and Ni that are not overwhelmed by the signals from the Ti matrix. Perhaps there is an acid mixture that you can find which will dissolve the surface layer and be less aggressive with the Ti.
Maybe ask your local librarian to run a literature search for "elemental analysis of surface layers" or something similar, and see what they can find for you. Don't reinvent the wheel, someone is quite likely to have tried something similar before.
Also, speak to your laboratory technician and see what they can suggest is possible with the equipment available at your facility. Some acids and digestion procedures are quite good at dissolving solid metals, but are extremely hazardous to health and safety so are not available or require specific equipment etc.
Best of luck.
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