钼蓝分光光度法测定铅锭中硅的条件优化设计
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摘要
采用钼蓝分光光度法测定铅锭中硅含量,研究了溶样试剂、显色酸度、钼酸铵加入量、还原液加入量以及基体效应等因素的影响,确定了最佳实验条件。对实际样品中硅含量测定的相对标准偏差(RSD, n=10)在2%左右,测得加标回收率在96.5%～104.8%之间。该方法操作简单,分析流程短,具有较高的精密度和准确度,能够满足铅锭中硅的测定。
Molybdenum blue spectrophotometry was adopted for determination of silicon content in lead ingot; the following items were researched, such as the digestion reagent, color developing acidity, the addition amount of ammonium molybdate, the addition amount of reducing agent, the effect of matrix effect and so on, therefore the optimal experimental conditions were confirmed. The relative standard deviation(RSD, n=10) of silicon content determination in practical sample is about 2%, the detected adding standard recovery rate is in the range of 96.5%～104.8%. The method is simple to operate, short analysis flow, which has higher precision degree and accuracy degree, it is suitable for measurement of silicon in lead ingot.
Molybdenum blue spectrophotometry was adopted for determination of silicon content in lead ingot; the following items were researched, such as the digestion reagent, color developing acidity, the addition amount of ammonium molybdate, the addition amount of reducing agent, the effect of matrix effect and so on, therefore the optimal experimental conditions were confirmed. The relative standard deviation(RSD, n=10) of silicon content determination in practical sample is about 2%, the detected adding standard recovery rate is in the range of 96.5%～104.8%. The method is simple to operate, short analysis flow, which has higher precision degree and accuracy degree, it is suitable for measurement of silicon in lead ingot.
引文
[1]中华人民共和国工业和信息化部. YS/T319-2013,铅精矿[S].北京:中国标准出版社,2013.
[2]国家质量监督检验检疫总局. GB/T 469-2013,铅锭[S].北京:中国标准出版社,2013.
[3]曹海峰.钼蓝分光光度法测定铅精矿中二氧化硅[J].中国无机分析化学,2016,6(4):41-45.
[4]于长珍.电感耦合等离子体发射光谱法测定镍铜合金中高含量硅[J].分析测试技术与仪器,2010,16(3):198-201.
[5]刘霞,尤瑜生,柳洪超,等.硅钼蓝光度法测定碳化硅中二氧化硅的含量[J].化学分析计量,2012,21(6):26-28.
[6]冯先进.微波等离子体原子发射光谱法直接测定金属铜中微量硅[J].矿冶,2013,22(4):121-123.
[7]霍红英.微波消解-电感耦合等离子体原子发射光谱法测定钒铁中7种杂质元素[J].冶金分析,2018,38(2):65-70.
[2]国家质量监督检验检疫总局. GB/T 469-2013,铅锭[S].北京:中国标准出版社,2013.
[3]曹海峰.钼蓝分光光度法测定铅精矿中二氧化硅[J].中国无机分析化学,2016,6(4):41-45.
[4]于长珍.电感耦合等离子体发射光谱法测定镍铜合金中高含量硅[J].分析测试技术与仪器,2010,16(3):198-201.
[5]刘霞,尤瑜生,柳洪超,等.硅钼蓝光度法测定碳化硅中二氧化硅的含量[J].化学分析计量,2012,21(6):26-28.
[6]冯先进.微波等离子体原子发射光谱法直接测定金属铜中微量硅[J].矿冶,2013,22(4):121-123.
[7]霍红英.微波消解-电感耦合等离子体原子发射光谱法测定钒铁中7种杂质元素[J].冶金分析,2018,38(2):65-70.