Determination of antimony in lead concentrate containing antimony by filter paper reduction-cerium sulfate titration
ZHAO Xiurong, WANG Heng, QIN Lijun, ZHUANG Mei, SHI Hui
Lianyungang Customs, Lianyungang 222042, China
摘要：建立滤纸还原-硫酸铈滴定法测定含锑铅精矿中锑含量的方法。采用硫酸、硝酸溶解样品，以滤纸作还原剂，在盐酸介质中，用磷酸掩蔽高价铁，以甲基橙和亚甲基蓝为指示剂，于80～90℃下，用硫酸铈标准溶液滴定至溶液突变至亮蓝色( 铁含量高时为黄绿色) 为终点。在实验条件下对3 个含锑铅精矿样品进行分析，测定结果的相对标准偏差为0.7%～2.2%(n=8)，加标回收率为95%～106%。分别采用该方法和锑矿石中锑的国家标准分析方法GB/T 15925-2010 对含锑铅精矿样品进行测定，两种方法的测定值基本一致，相对误差为1.4%～4.5%。该方法准确度高，精密度好，成本低，适用于铅精矿中锑含量的测定。
Abstract：A method for determination of antimony in lead concentrate containing antimony by filter paper reduction
cerium sulfate titration was established. The sample was dissovled in sulfuric acid and nitric acid with quantitative filter
paper as reducing agent. In hydrochloric acid medium, phosphoric acid was used to mask high valent iron. Methyl orange
and methylene blue were used as indicators, and at 80-90℃, cerium sulfate standard solution was used to titrate until the
solution suddenly changed to bright blue (yellow green when iron content was high) as the end point. Three samples of
lead concentrate containing antimony were determined under experimental conditions, the relative standard deviation of
determination results was 0.7%-2.2%(n=8), and the recovery was 95%-106%. This method and GB/T 15925-2010 were
used to determine the samples of lead concentrate containing antimony. The determination results of the two methods were
basically the same, with the relative error of 1.4%-4.5%. The method has the advantages of high accuracy, high precision
and low cost. It is suitable for the determination of antimony in lead concentrate.
Keywords：titration; lead concentrate containing antimony; antimony; cerium sulfate
赵秀荣，王恒，秦立俊，等. 滤纸还原- 硫酸铈滴定法测定含锑铅精矿中锑[J]. 化学分析计量，2020，29(2)：54-58.
ZHAO X R，WANG H，QIN L J，et al. Determination of antimony in lead concentrate containing antimony by filter paper reduction-cerium sulfate titration[J]. Chemical analysis and meterage，2020，29(2)：54-58.