碱熔-氟硅酸钾容量法测定硅锰合金中硅含量

Determination of Silicon Content in Silicon Manganese Alloy by Potassium Hydroxide Decomposition-potassium Fluosilicate Volumetric Method

对氟硅酸钾容量法测定硅锰合金中硅的条件进行研究,建立一种测定硅锰合金中硅含量的简单方法。通过氢氧化钾熔融分解,在硝酸介质中,沉淀硅酸根离子,经过过滤,洗涤,中和残余酸,水解,用氢氧化钠标准溶液滴定生成的氢氟酸,计算出硅的含量。方法应用于硅锰合金标准物质中硅的测定,测定值与标准值一致。对样品进行精密度试验,三种硅锰合金标准物质中硅含量测定结果的标准偏差(RSD)均不大于0. 6%(n=8)。

The determination of silicon in silicon-manganese alloy by potassium fluosilicate volumetric method was studied. A simple method for determining silicon content in silicon-manganese alloys was established. Through the melting decomposition of potassium hydroxide,silicate ion was precipitated in nitric acid medium. After filtration,washing,neutralization of residual acids and hydrolysis,hydrofluoric acid was produced by titration with sodium hydroxide standard solution,and the content of silicon was calculated. The method was applied to the determination of silicon in silicon manganese alloy certified reference material. The measured values were consistent with the standard values. The samples were tested for precision,and the standard deviation( RSD) of the determination results of silicon content in three kinds of silicon-manganese alloy reference materials was not greater than 0. 6%( n = 8).