不同酸溶解-硅钼酸盐光度法测定碳钢中硅含量的探讨

发布时间：2018-02-24 00:50

本文关键词： 碳钢硅分光光度法酸溶法硅钼酸盐　出处：《冶金分析》2015年12期 　论文类型：期刊论文

【摘要】：通过硫酸溶解法和硝酸溶解法处理碳钢,采用还原型硅钼酸盐光度法对碳钢中的硅含量进行了测定。对硫酸溶解法、硝酸溶解法显色反应的条件进行优化,发现不论选择硫酸溶解法还是硝酸溶解法溶解试样,均选择测定波长810nm,硅钼蓝显色时间5min,50g/L钼酸铵溶液用量5mL,50g/L草酸溶液用量9mL,60g/L硫酸亚铁铵溶液用量5mL,但用硫酸溶解法处理试样的硅钼黄显色时间为25min,用硝酸溶解法处理试样的硅钼黄显色时间为30min。按实验方法对标准溶液系列进行基体匹配并进行测定,结果表明,硅的质量浓度在0~1μg/mL之间与其吸光度呈线性关系,硫酸(1+17)溶解试样的线性回归方程为ρ=1.333 A+0.004,相关系数r=0.999,方法检出限为0.013%;硝酸(1+3)溶解试样的线性回归方程为ρ=1.277 A+0.006 8,相关系数r=0.999,方法检出限为0.014%。在优化条件下分别用硫酸溶解法、硝酸溶解法处理3个碳钢标准样品,按实验方法进行硅含量的测定,测定值与认定值一致,相对标准偏差(RSD,n=10)在0.26%~1.1%之间。
[Abstract]:Carbon steel was treated by sulfuric acid dissolution and nitric acid dissolution. The content of silicon in carbon steel was determined by reducing silicomolybdate photometry. The conditions of chromogenic reaction of sulfuric acid dissolution and nitric acid dissolution were optimized. It is found that no matter the method of sulfuric acid or nitric acid is chosen to dissolve the sample, The wavelength of determination was 810 nm, the reaction time of silicomolybdate blue was 5 min, the amount of 50 g / L ammonium molybdate solution was 5 mL / L, the dosage of oxalic acid solution was 9 mL / L, the amount of ferrous ammonium sulfate solution was 5 mL / L, but the color reaction time of silicon-molybdenum yellow was 25 min by sulfuric acid dissolution method and treated by nitric acid solution. The reaction time of silicomolybdate yellow was 30 min. The standard solution series was matched and determined by the experimental method. The results show that there is a linear relationship between the mass concentration of silicon and the absorbance of the silicon between 0 渭 g / mL and 1 渭 g / mL. The linear regression equation of dissolved sample is 蟻 1. 333 A 0.004, the correlation coefficient is 0. 999, the detection limit of the method is 0. 013, the linear regression equation of nitrate 13) is 蟻 1. 277 A 0.0068, the correlation coefficient is 0. 999, the detection limit of the method is 0. 014. The detection limit is 0. 014 under the optimized conditions. Don't dissolve in sulfuric acid, Three carbon steel standard samples were treated by nitric acid dissolution method. The silicon content was determined by the experimental method. The measured value was in agreement with the determined value. The relative standard deviation (RSDN ~ (10)) was between 0.26% and 1.1%.
【作者单位】：国家纺织机械产品质量监督检验中心(山西);
【分类号】：TG115

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