基于硅钼黄分光光度法建立了分析柠檬酸液中溶硅的方法,探讨了柠檬酸浓度、钼酸铵浓度、柠檬酸与钼酸铵浓度比、盐酸浓度和显色时间对硅钼黄络合物吸光度的影响.研究表明,反应体系为CCA/CAM=1/3,HCI浓度为0.35mol/L,低于3.0%的柠檬酸液中显色10min.在λ=410nm处,吸光度(A)与质量浓度(C)成线性关系,Si的量在0.1~16.0mg/L内符合比尔定律,硅的测定回归方程为A=0.030+0.060C(R2 =0.9982),其检出限为0.1 mg/L,方法重复性的RSD和精密度均小于1.0%,加标回收率为99.5%~102.4%.此法快速、简便,可准确分析柠檬酸液中的溶硅.%Nanocolloidal silicon content in citric acid solution based on the spectrophotmetric analysis method was established in this work, the effects of CA concentration, AM concentration, the mass ratio of citric acid and ammonium molybdate, HC1 concentration and coloration time on the absorbance of molybdosilicate yellow were analyzed in detail. Results indicated that the optimal reaction condition was CCA/ CAM = 1/3 and 0. 35 mol/L HC1. Also,the optimal coloration time was 10 min below 3.0% of citric acid solution. A good linear relationship between absorbance (A and silicon mass ( C) was obtained at 410 nm. The mass concentration of Si was 0. 1 ~ 16. 0 mg/L and fitted Beer' s law. The equation was expressed as A = 0.030 + 0.060C( R2 = 0.9982) , and its limited detection was 0.1 mg/L. The RSD of reproducibility and precision were both less than 1.0% with recoveries of 99.5% ~ 102. 4%. This method can be applied to covenient,accurate and rapid determination of nanocolloidal silicon in the citric acid.
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