Determination of Antimony and 14 Trace Elements in Antimony Ores by X-ray Fluorescence Spectrometry with Fusion Sample Preparation

The analysis of antimony ores usually uses acid decomposition and an alkali fusion system, followed by the volumetric method after solvent extraction. Each component employs various analytical methods such as capacity, Atomic Absorption Spectrometry and Atomic Fluorescence Spectrometry. These methods not only have complicated operations with long time consuming, but also obtain low or become distorted due to incomplete digestion or serious interferences, which subsequently make it difficult to meet the needs of geological analysis. The glass fusion preparation technique and establishing the rapid analysis method by using wavelength dispersion X-ray Fluorescence Spectrometry (XRF) are discussed and presented in this paper to determine antimony and 14 kinds of trace and associated elements (Cu, Pb, Zn, As, Co, Ni, W, Ba, S, SiO₂, Al₂O₃, TFe, CaO and MgO) in antimony ores. The calibration cure was calibrated by using the national standard material and synthetic standard reference material, in order to study melting conditions. The sample and lithium teraborate-lithium metaborate-lithium fluoride were melted with dilution ratio of 1:20 with ammonium nitrate as oxidant and lithium carbonate as protective agent. The sample was preoxidated at 700℃, and was melted completely at 1050℃, which effectively prevented the volatilization of arsenic and sulfur to solve the problems of complex procedure, the inability to simultaneous determine elements and insufficient test elements by chemical methods. The method detection limits are lower than previous methods (Sb: 0.14%, Cu: 0.0027%, Pb: 0.0025%, Zn: 0.0046%, As: 0.0028% and S: 0.021%) and the method precision degree (RSD, n=12) is lower than 5.0%. Verified by synthetic standard material and the actual production of an antimony ore sample, the results show good consistency with the reference value obtained by the chemical method. Although the detection limits are higher than those for the powder pellet method, the operation if this method was simple, rapid and accurate making it applicable to lab analysis requirements of varied and batch antimony ores samples.