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机构地区:[1]上饶师范学院化学化工学院,江西上饶334001 [2]江西省煤田地质局226地质队,江西萍乡337000
出 处:《分析科学学报》2015年第6期863-866,共4页Journal of Analytical Science
基 金:教育部第四批高等学校特色专业建设点资助项目(No.TS11524)
摘 要:实验发现在pH=4.2的HAc-NaAc缓冲溶液中,以抗坏血酸为增敏剂,痕量Sc(Ⅲ)可催化KBrO3氧化灿烂甲酚蓝的褪色反应,据此建立了一种测定痕量Sc(Ⅲ)的催化动力学光度分析新方法。优化了相关的测定条件,考察了其它离子对测定的影响,在选定的实验条件下,测得催化褪色反应的表观活化能为77.3kJ·mol-1,方法的线性范围为0.012~0.28μg·mL-1,Sc(Ⅲ)的检出限为4.7×10-4μg·mL-1。该方法用于煤样中痕量Sc(Ⅲ)的分析,5次测定的相对标准偏差≤5.14%,样品加标回收率在92.9%~109%之间。A catalytic kinetic spectrophotometric method for the determination of trace Sc(Ⅲ)based on the oxidation reaction between KBrO3 and brilliant cresyl blue in the presence of ascorbic acid as an sensitizer in HAc-NaAc buffer solution(pH =4.2)has been developed.The related determination condition and the dosage of reagents were optimized.Under the optimal experimental condition,the apparent activation energy of catalytic fading reaction was 77.3kJ·mol-1,and the linear range of method was 0.012-0.28μg·mL-1,with the detection limit of 4.7×10-4μg·mL-1.The proposed method was applied to the determination of trace scandium in coal samples.The relative standard deviations were less than 5.14%(n=5),and the recoveries of standard addition were 92.9%-109%.
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