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为了准确检测三氯氢硅相似体系中痕量磷,提出了一种测定水溶液中和有机溶液中不同价态磷的紫外-可见光分光光度法,采用高纯水萃取分离有机溶剂中的磷,该方法可应用于正己烷溶液中PCl3氧化效果的测定。此方法对水溶液中磷酸的检测范围为0.52～6.40μmol/L,检测限为0.52μmol/L,对水溶液中亚磷酸的检测范围为1.60～6.40μmol/L,检测限为1.60μmol/L;不同体积比下正己烷与水,萃取率与起始浓度的拟合曲线的调整决定系数Adj.R2在0.95以上;测定聚合物负载三氧化铬在固定床温度95℃下30 min对PCl3的氧化率可达到26.5%。
Abstract：In order to detect trace phosphorus in a similar system of trichlorosilane,a UV-visible spectrophotometric method was proposed for the determination of phosphorus in different valences in aqueous and organic solutions.Phosphorus was extracted and separated from organic solvents with high purity water.The proposed method was used to determine the oxidation effect of PCl3 in n-hexane.The detection range of phosphoric acid in aqueous solution is 0.52—6.40 μmol/L,and the detection limit is 0.52 μmol/L,while the detection range of phosphorous acid in aqueous solution is 1.60—6.40 μmol/L,and the detection limit is 1.60 μmol/L.At different volume ratios of n-hexane to water,the adjusted coefficient of determination of the fitting curve between the extraction rate and the initial concentration is above 0.95.It was determined that the oxidation rate of chromium( Ⅵ)-supported polymer to PCl3 at a fixed bed temperature of 95 ℃ for 30 minutes could reach 26.5%.
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基本信息:
DOI：10.13353/j.issn.1004.9533.20191912
中图分类号:O657.32;TQ127.2
引用信息:
[1]毕明洋,黄国强.不同体系痕量磷检测及其在磷价态转化中的应用[J].化学工业与工程,2020,37(06):54-60.DOI:10.13353/j.issn.1004.9533.20191912.
基金信息:
国家自然科学基金项目(21676197)