The elemental characterization which used as little powder as possible is preferable.
In some paper about fluoridated hydroxyapatite, I saw authors dissolve very little amount of powders in a suitable solvent. Then characterize elements of the solution by ICP-OES and calculate how much fluoride substituted in hydroxyapatite. But there is a problem, no one can confirm how much of the detected fluoride relates to the fluoride which substituted in hydroxyapatite and how much of the rest didn't substituted in hydroxyapatite and produced some byproduct in the powder producing step.
One suggest to me to use EDX (in SEM). You can select some area (at least 3 area) on your specimen under SEM and take a complete map of Si, Ca, and P distribution. According to the data, you can demonstrate how much silicon substituted in the hydroxyapatite (I think if you see some place of over-dosage of Si (abnormally), you could find that part of Si didn't substituted in HA).
Unfortunately, this suggestion come to me very late and I didn't have enough time to do it. I hope you can use it.
Hi, thank you. I have actually done ICP-OES and EDS. But still I'm not really confident. I want to do XRF but it require a lot of powders. The problem is I don't have that much powders!
Hi. Could I know what was the problem of EDS method that can't confident you? I want to know for my proceed researches.
EDS is semi-quantitative. One can not know the actual beam reaction volume and as such you can not really calculate the actual ratios of elements present. The only way to do have a quantitative method is to have a known chemical standard with a known volume present in the beam. Then you can generate the appropriate correction factors for the unknown sample. Additionally, EDS is, at best, a measure of parts per 100,000 resolution whereas ICP is in the parts per trillion. One may try XPS-Auger methods.
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