Determination of major and minor component in copper concentrate by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation
Abstract：The sulfur content was high in fusion sample preparation of copper concentrate. To solve this problem, lithium tetraborate-lithium metaborate (m∶m=12∶22) was used as flux, and sodium carbonate, silicon dioxide and lithium nitrate were used as auxiliary. The simultaneous determination method of major and minor components (copper, sulfur, iron, zinc, aluminum, magnesium, calcium, lead and manganese) in copper concentrate by wavelength dispersive X-ray fluorescence spectrometry after fusion sample preparation was established. The effects of oxidizer, auxiliary formula, fusion temperature and time on sulfur fixation and sample preparation efficiency were investigated. The experimental conditions were as follows: 0.1g of sample, 6.9g of lithium tetraborate-lithium metaborate (m∶m=12∶22), 1.06g of sodium carbonate, 0.38g of silicon dioxide, and 1.38g of lithium nitrate. The temperature was increased from room temperature to 600℃ followed by pre-oxidization for 15min. The sample was prepared by fusion at 960℃ for 5-8min and then determined by gravimetric method and X-ray fluorescence spectrometry. The recovery of sulfur was higher than 99%. The calibration samples with proper content gradient were prepared using certified reference material and high-purity copper oxide. The linearity of calibration curves was good with correlation coefficient (R2) reach 0.999. The standard substance verification and method comparison indicated that the relative deviation between determination values and certified values was 0.43%-6.9%. The determination results of same sample were basically consistent with those obtained by conventional method. The proposed method could meet the rapid detection requirements of copper concentrate samples.
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