Abstract：Accurate content of antimony was an important index to the trade settlement of antimony ore, so the accurate determination of antimony and other elements in antimony ore was pretty important to mineral comprehensive evaluation and utilization. Mixed reagent of Li2B4O7 and LiBO2 (m∶m=67∶33) was used for sample fusion at 1 050 ℃ and 0.20 mL of 60 mg/mL LiBr solution was used as release agent. Thus, simultaneous determination of twelve components such as Sb2O3, Al2O3, SiO2, CaO, TiO2, MnO, MgO, Fe2O3, Cu, Zn, Na2O and K2O in antimony ores was realized by wavelength dispersive X-ray fluorescence spectrometry. The corrosion problems of Pt-Au alloy crucibles by antimony sulfide ore containing high content of sulfur was solved by pre-oxidizing the sample with LiNO3 at low-temperature. The calibration curve which could satisfy the quantitative determination requirements of each component was established with eight antimony certified reference materials (CRMs) and calibration samples synthesized with CRMs. Besides, theoretical α coefficient method was adopted to correct matrix effect. After precision test, the relative standard deviation (RSD, n=12) of the determination of the components in antimony ore samples was between 0.1%-9.7%. The accuracy of CRMs and synthesized samples was validated, and the analytical results were consistent with the certified value or reference value.
