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摘 要:本文对溴酸钾法测定锑矿石中锑的条件进行改进,用酒石酸、柠檬酸代替盐酸来“稳定”锑离子,抑制锑的水解,消除了盐酸对环境、对操作者的危害。研究了络合剂种类、用量,试剂加入顺序,硫酸浓度,指示剂种类,滴定温度等因素对硫酸锑溶液稳定性和测定准确度的影响。结果表明:硫酸-酒石酸-溴酸钾法测定锑的适宜条件为:温度控制在90℃,加入酒石酸的质量为1g;(1+1)硫酸的体积为10ml;以0.1%的甲基橙作为指示剂时测定锑的结果与传统的盐酸-硫酸-溴酸钾法的相接近。结果还表明,硫酸-柠檬酸-溴酸钾法也是可行的,同样也表明了硫酸-酒石酸-高锰酸钾滴定法对测定锑的稳定性较差,不宜使用。 关键词:溴酸钾;酒石酸;三氧化二锑;硫酸
ABSTRACT:In this paper, the potassium bromate for the determination content of antimony in the ore was improved. Addition of tartaric acid, citric acid instead of hydrochloric acid in the sample solution to keep antimony ion stable , to restrain antimony hydrolysis, to eliminates hydrochloric acid for the environment and the dangers of operator, Effect of several conditions above to solution stability and the accuracy was studied. It was indicated that the suitable conditions of determination of content antimony by KBrO3 method was follow: at 90℃ of the solution, addition of 1g tartaric acid, 10mL H2SO4(1+1) and titration of antimony ions in the solution with standard solution of KBrO3 with methyl orange to indicate end point of the reaction. It was shown that results obtained from class and improved KBrO3 methods is rather nearly. The new method is right. Keywords: Potassium bromated; tartaric acid; antimony trioxide; sulfuric acid |