摘要
针对钨矿石中的微量元素磷,采用混合酸快速微波消解结合磷钼蓝分光光度法进行测定.经选择优化样品的微波消解和实验测定条件,结果表明：HCl＋ HNO3＋HF的混合酸微波消解后的样品,在硫酸介质中,有钼酸铵存在时,用抗坏血酸将磷还原成磷钼蓝络合物,在825 nm处比色测定.方法的加标回收率为98.9％～101.6％,结果准确可靠.硅在熔样过程中挥发除去不会干扰测定,砷会干扰实验,可在酸介质中加入碘化钾,使砷还原至低价而不干扰磷的测定.
A method for the determination of trace phosphorus（P） in tungsten ore samples by phosphorus molybdenum blue spectrophotometry was established. The sample was pretreated by microwave digestion with mixed acid. Analytical conditions were optimized as follows： the sample was digested by mixed acids HCI＋HNOs ＋ HF as digestion agent. The results showed that Beer＇s law was compiled in sulfuric acid medium with adsorption wave length of 825 nm. The recovery was 98.9%~ 101.6%. Silicon did not interfere in the determination of P by volatilization during the melting of tungsten ore samples, and the influence of arsenic（As） could be eliminated by adding potassium iodide in the acid medium to reduce As into low valent state.
出处
《中国无机分析化学》
CAS
2015年第1期24-27,共4页
Chinese Journal of Inorganic Analytical Chemistry
基金
广西科学研究与技术开发计划项目(桂科能14123006-14)资助
关键词
微波消解
钨矿石
磷钼蓝
分光光度法
磷
microwave digestion
tungsten ore
molybdenum blue
spectrophotometric measurement
phosphorus
