硅钼蓝分光光度法测定水玻璃旧砂中的硅酸钠
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摘要
本文建立了硅钼蓝分光光度法测定水玻璃旧砂中硅酸钠的分析方法。使用硫酸提高酸度促使硅形成稳定的硅钼蓝络合物,根据紫外可见吸收光谱中的吸收峰和摩尔吸收系数,进行定性分析,从而计算出溶液中硅酸钠的含量。探讨了溶液酸度、显色时间、显色剂和还原剂等因素对硅钼蓝吸光度的影响。同时,对优化后的硅钼蓝分光光度法进行精密度和准确度评定,标准偏差小于1.57,加标回收率在98.36～101.3之间。对湿法再生砂和干法再生砂中硅酸钠含量测定并分析,优化后的硅钼蓝分光光度法具有良好的重现性和精密度。硅酸钠含量的测定为水玻璃再生砂的使用性能提供了评价指标。
An analysis method based on the silicon molybdenum blue spectrophotometry is established to measure the amount of sodium silicate in used sodium silicate sand. The content of sodium silicate in solution was calculated by qualitative analysis based on the absorption peak and molar absorption coefficient in the ultraviolet visible absorption spectrum. The effects of solution acidity, color development time, colorant and reducing agent on the absorbency of molybdenum blue were discussed. At the same time, the precision and accuracy test of the optimized silicon molybdenum blue spectrophotometry was carried out. The standard deviation of repeated measurements was less than 1.57, and the standard recovery rate was between 98.36 and 101.3. The content of sodium silicate in wet and dry recycled sand was determined and analyzed. The optimized molybdenum blue spectrophotometry had satisfied reproducibility and precision. The determination of sodium silicate content provides an evaluation index for the performance of sodium silicate recycled sand.
An analysis method based on the silicon molybdenum blue spectrophotometry is established to measure the amount of sodium silicate in used sodium silicate sand. The content of sodium silicate in solution was calculated by qualitative analysis based on the absorption peak and molar absorption coefficient in the ultraviolet visible absorption spectrum. The effects of solution acidity, color development time, colorant and reducing agent on the absorbency of molybdenum blue were discussed. At the same time, the precision and accuracy test of the optimized silicon molybdenum blue spectrophotometry was carried out. The standard deviation of repeated measurements was less than 1.57, and the standard recovery rate was between 98.36 and 101.3. The content of sodium silicate in wet and dry recycled sand was determined and analyzed. The optimized molybdenum blue spectrophotometry had satisfied reproducibility and precision. The determination of sodium silicate content provides an evaluation index for the performance of sodium silicate recycled sand.
引文
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[2] 朱纯熙,卢晨.水玻璃硬化的认识过程[J].无机盐工业, 2001, 33(1): 22～25.
[3] 卢记军,谭远友,闻向东,汪华方,陈锐,王成.水玻璃旧砂再生脱膜率评价方法初探[J].热加工工艺, 2014, 43(7): 74～76.
[4] 夏文宝,姜宏,鲁鹏,等.高铝硅酸盐玻璃中铝配位的XPS研究[J].材料科学与工程学报, 2013, 31(5): 715～717.
[5] 王发洲,刘云鹏,胡曙光.硅酸盐水泥与阳离子乳化沥青颗粒的相互作用机理[J].材料科学与工程学报, 2013, 31(2): 186～190.
[6] 高学峰.重量法及EGTA滴定法联合测定硅钡钙铁合金中硅、钡、钙[J].冶金分析, 2002, 22(1): 44～46.
[7] 高庆福,张长瑞,冯坚,等.氧化硅气凝胶隔热复合材料研究进展[J].材料科学与工程学报, 2009, 27(2): 302～306.
[8] 谷松海,李旭辉.X射线荧光光谱法测定工业硅中铁、铝、钙[J].光谱学与光谱分析, 2001, 21(4): 569～571.
[9] 化学试剂 硅酸盐测定通用方法[S]. GB/T 9742-2008.