高氯酸脱水重量法测定锰硅合金中硅

Determination of silicon in manganese-silicon alloy by perchloric acid dehydration gravimetry

锰硅合金中硅含量对炼钢过程用料配比具有重要指导作用,也是交易计价的重要指标之一,因此,快速准确地测定锰硅合金中硅显得尤为重要。采用盐酸、硝酸分开加入的模式分解样品,通过冒两次高氯酸烟使样品中碳炭化,再加入过氧化氢可得到清澈溶液利于过滤及灼烧。试验结果表明,滤液中二氧化硅含量与二氧化硅沉淀中杂质含量相当,由此引入的系统误差可相互抵消,实际工作中可不予校正。按照实验方法测定4个锰硅合金标准物质中硅,结果的相对标准偏差(RSD)为0.47%~0.69%,测定值与认定值相符。

The content of silicon in manganese silicon alloy has important guiding significance to the ratio of the materials in steel-making process.Moreover,it is also one of important indexes for the valuation in trade.Therefore,it is critical to rapidly and accurately determine the silicon content in manganese-silicon alloy.The sample was decomposed by adding hydrochloric acid and nitric acid separately.The carbon in samples was carbonized through perchloric acid fuming for twice.Then hydrogen peroxide was added to obtain clear solution,which was advantageous to filtration and calcinations.The experimental results showed that the content of silicon dioxide in filtrate was equivalent to the impurity content in silicon dioxide precipitation.Therefore,the introduced system error could be cancelled out,and the correction was not necessary in practical test.The content of silicon in four certified reference materials of manganese-silicon alloy was determined according to the experimental method.The relative standard deviations（RSD）ranged from 0.47% to 0.69%.The found results were consistent with the certified values.