研究了β型硅钼黄的形成及其被乙醇光化学还原为硅钼蓝的影响条件,建立了乙醇光化学还原-硅钼蓝分光光度法测定氧化铝载钯催化剂中硅含量的新方法。结果表明,在810 nm波长处,硅量在0~2μg/mL范围内硅钼蓝吸光度符合朗伯-比耳定律;分取溶解后的催化剂溶液,控制测定试液钼酸铵浓度为5 g/L、盐酸浓度为0.9 mol/L,以乙醇作为光催化还原剂,用UVA紫外灯为光源照射25 min,测定样品中含量为0.1%~1%的硅,RSD=1.43%(n=9),加标回收率98.5%~101%。
Photochemical reduction-silicon molybdenum blue spectrophotometry, a new analytical method, was used to measure silicon content in Pd/Al2O3 catalyst. The conditions for photo-reducingβ-silicon molybdenum yellow into silicon molybdenum blue with ethanol were investigated. The results showed that the changes in absorbance complied with Beer-Lambert law when the silicon content was in 0~2 μg/mL concentration range. The method applied to the determination of 0.1%~1% silicon contents in Pd/Al2O3 catalyst with satisfactory results. The recovery was between 98.5%~101% with aRSDof 1.43% (n=9).
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