Abstract：During the analysis of metal and alloy samples by X-ray fluorescence spectrometry (XRF), the sample preparation by fusion method was advantageous to obtain more accurate composition information. In order to avoid the corrosion of platinum-gold crucible by sample during fusion process, the sample was pre-oxidized by acid dissolution or alkali digestion before fusion. The metals were translated to the salts, realizing the safe and reliable fusion operation. In acid dissolution method, HBr was firstly added to avoid the passivation of sample. Then, excessive HNO3 was added for the further dissolution and the removal of Br-. The solution was evaporated to dryness followed by fusion. Some special samples such as aluminum products could be digested with alkali solution. The sample was dissolved with LiOH followed by acidification with HNO3. The solution was evaporated to dryness for fusion. The relatively accurate content information of major components could be obtained by quantitative analysis without standard sample. The parallel experiments of By1901-2 copper alloy sample (n=6) indicated that the relative standard deviation (RSD) of major components were less than 7%. Meanwhile, the study provided idea for the quantitative analysis of metals and alloys by XRF.
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LI Ke-ji. Acid or alkali pre-oxidization method for fusion sample preparation in X-ray fluorescence spectrometric determination of metals and alloys. , 2016, 36(4): 76-79.
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