电感耦合等离子体原子发射光谱法测定云南某矿山锑矿选矿流程样品中锑

锑在现代工业体系中占有重要地位,快速准确测定锑矿中锑含量对锑矿的采选具有重要指导意义。云南某矿山锑矿以萤石为主要伴生矿,现有的盐酸、硝酸、氢氟酸和高氯酸混酸体系无法彻底分解样品,而采用碱熔处理流程长且引入大量基体,均无法满足准确快速测定的要求。选择硫酸-氢氟酸混酸体系分解样品,再用酒石酸-盐酸混合溶液加热浸取,锑完全溶解于溶液中,选择Sb 206.833{463}nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锑。结果表明,锑的质量浓度在5.0～80 μg/mL范围内与其发射强度呈良好的线性关系,校准曲线线性相关系数r=0.999 8;方法的检出限为0.012 μg/mL。按照实验方法对锑矿石成分分析标准物质和锑矿选矿流程样品中锑进行测定,结果的相对标准偏差(RSD,n=5)为0.71%～5.7%;标准物质的认定值和测定值相一致;锑矿选矿流程样品中锑的加标回收率为97%～102%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。

Determination of antimony in antimony ores from the beneficiation process in Yunnan by inductively coupled plasma atomic emission spectrometry

Antimony plays an important role in modern industrial system. The rapid and accurate determination of antimony content in antimony ore has important guiding significance for the mining and beneficiation of antimony ores. Fluorite is the main associated ore of antimony ore in a mine in Yunnan Province. The existing mixed acid system containing hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid cannot completely decompose the samples. The process of alkali fusion treatment is long and a large amount of matrix is introduced, which cannot meet the requirements of accurate and rapid determination. The samples were decomposed with mixed acid of hydrofluoric acid and sulfuric acid followed by heating extraction with tartaric acid and hydrochloric acid mixed solution. The antimony in sample could be completely dissolved in the solution. The content of antimony was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using Sb 206.833{463} nm as the analytical line. The results showed that the mass concentration of antimony in range of 5.0-80 μg/mL had a good linear relationship to the emission intensity. The linear correlation coefficient of calibration curve was r=0.999 8. The limit of detection of the method was 0.012 μg/mL. The contents of antimony in certified reference materials of antimony ore and actual antimony ores from the beneficiation process were determined according to the experimental method. The relative standard deviations (RSD, n=5) of the measured values were between 0.71% and 5.7%. The found results of certified reference materials were consistent with the certified values. The spiked recoveries of antimony for actual sample from the beneficiation process were between 97% and 102%, which could meet the requirements of the national geological and mineral industry standard DZ/T 0130-2006.