不同体系痕量磷检测及其在磷价态转化中的应用

摘要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0.52~6.40 μmol/L，检测限为0.52 μmol/L，对水溶液中亚磷酸的检测范围为1.60~6.40 μmol/L，检测限为1.60 μmol/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%。

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	毕明洋
	黄国强

关键词：磷氧化载体聚合物痕量检测萃取

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%.

Keywords： phosphorus； oxidation； support； polymers； trace detection； extraction

Received 2019-09-23;

Fund:国家自然科学基金项目（21676197）。

Corresponding Authors: 黄国强,E-mail:hgq@tju.edu.cn。 Email: hgq@tju.edu.cn

About author: 毕明洋(1996-),男,硕士研究生,从事络合吸附除氯硅烷中痕量磷、硼杂质的研究工作。

引用本文:

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(6): 54-60

Bi Mingyang, Huang Guoqiang.Determination of Trace Phosphorus in Different Systems and Its Application in Valence Transformation of Phosphorus[J]. Chemcial Industry and Engineering, 2020,37(6): 54-60

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