自动电位滴定测定锰矿石中锰的方法研究  

Determination of Total Manganese in Manganese Ores with an Automatic Potentiometric Titration Method

作　　者：马德起[1] 谷松海[1] 张国胜[1] 吴瑶[2] 韩娟[1] 

机构地区：[1]天津出入境检验检疫局,天津300456 [2]中国民航大学理学院,天津300300

出　　处：《岩矿测试》2013年第4期595-599,共5页Rock and Mineral Analysis

基　　金：中国民航大学理学院基金资助项目(07kys04)

摘　　要：多批次的锰矿石锰含量滴定分析消耗大量人工,随着自动化电位滴定仪的普及,利用仪器完成容量滴定成为可能,而将手工滴定向自动电位滴定移植是当前需要解决的课题。本文建立了一套自动电位滴定仪测定锰矿石中锰含量的方法,确定了相关滴定参数和等当点识别标准。锰矿石样品采用盐酸、磷酸分解,硝酸去除碳和有机物,高氯酸氧化,形成样品溶液。自动电位滴定仪先用硫酸亚铁铵标准溶液对预先移取的重铬酸钾标准溶液和标定空白溶液分别进行氧化还原滴定,用铂复合电极指示,计算得到硫酸亚铁铵标准溶液浓度,再对样品空白溶液和样品溶液进行氧化还原滴定,得到样品锰含量,方法检测范围为5%～60%。采用本法分析国家一级标准物质,测定结果的准确度和精密度高;分析多个产地不同水平的锰矿石样品,测定结果与手工方法进行对照,经t检验无显著性差异。建立的滴定方法自动化程度高、方法稳健,适用于冶炼企业、港口商检等行业,具有推广价值。In the batch analysis of manganese content in manganese ore with artificial titration method, it consumes a large amount of manual labor. With the popularity of automatic potentiometric titrator, it is possible to complete the volumetric titration using the instrumental equipment. The manual titration is conversed to the automatic potentiometric titration is the urgent study subject to be solved. In the paper, a method for the determination of manganese content in manganese ores with automatic potentiometric titration was established. The related titration parameters and the equivalence point identification standards is identified. Manganese ore sample was decomposed with hydrochloric acid and phosphoric acid, the carbon and organic matters in the sample were removed with nitric acid, then the sample solution was prepared with perchloric acid. In the experiment, at first, the platinum composite electrode was indicator electrode, the oxidation and reduction titration was made for the pre-pipette potassium dichromate standard solution and the blank solution with ferrous ammonium sulfate standard solution, the concentration of ammonium ferrous sulfate standard solution was calculated. Then, the oxidation and reduction titration was made for the sample blank solution and sample solution, the content of manganese was calculated. The detection range of the method for manganese is 5%-60%. The method was used to the determination of national standard reference materials, the accuracy and precision were high. A plurality of ore samples with different level of manganese from different mine area were determined using this automatic titration method, the analytical results had no significant difference with manual method by t-test. Titration method and high degree of automation, methods of robust, suitable for smelting enterprises, the port inspection and other industries, has the value of popularization. The automatic titration is robust, and is suitable for ore analysis in smelting enterprises and port inspection.

关 键 词：锰矿石 锰 自动电位滴定 氧化还原滴定 

分 类 号：P578.1[天文地球—矿物学] O614.711[天文地球—地质学]