Abstract:The content of micro elements in common binders (including amylum, methylcellulose, boric acid and stearic acid) was determined by qualitative and semi-quantitative analysis software IQ+. The sample was prepared by grinding and powder pressed method using boric acid and stearic acid as mixed binder. The content of iron, aluminum, calcium, manganese, nickel, titanium, copper, phosphorus, magnesium, chromium and vanadium in industrial silicon was determined by X-ray fluorescence spectrometry (XRF). The block-type industrial silicon samples were treated using iron crucible. The particles with size of 1-3 mm passing through the screen were used as samples for grinding. The optimal ratio of sample and binder was obtained by experiments, i.e., 15 g of industrial silicon sample was mixed with 3.0 g of boric acid and 0.20 g of stearic acid. The conditional tests showed that the granularity effect was obviously reduced when the grinding time was more than 120 s. The surface for analysis after sample preparation was firm and smooth. The calibration curve was prepared using the series certified reference materials of industrial silicon and then corrected by empirical coefficient method. The spectral overlapping between coexisting elements was corrected. The root mean square deviation (RMS) of calibration curve obtained by analytical software was less than the RMS value required. The precision test results indicated that the relative standard deviations (RSD, n=11) of iron, aluminum, calcium, manganese, phosphorus, nickel, vanadium, titanium and magnesium in industrial silicon sample were about 5%. The RSD of chromium was highest, which was also less than 9%. The proposed method was applied to the analysis of industrial silicon standard samples, and the found results were consistent with the certified values. The determination results of unknown samples had no significant difference with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
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