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机构地区:[1]东华理工大学核资源与环境教育部重点实验室,江西南昌330013 [2]东华理工大学应用化学系,江西抚州344000
出 处:《化工时刊》2007年第11期44-46,共3页Chemical Industry Times
摘 要:在硫酸介质中,痕量铌对溴酸钾氧化结晶紫的褪色反应有良好的催化作用,作者由此建立了测定痕量铌的催化动力学光度法。通过绘制吸收曲线,选定实验的测定波长为545 nm。运用单因素实验方法,选择了最佳的实验条件:1.0 mol/L的硫酸用量为2.0 mL,0.10 mol/L的溴酸钾用量为2.5 mL,0.50 g/L结晶紫用量为0.5 mL,反应时间为4 min,反应温度为100℃。该方法的线性范围在0-50μg/L之间,工作曲线的线性方程为ΔA=0.926CNb-3.64×10^-3(相关系数r=0.999 3),检出限达到6.1×10^-10g/mL。将该方法应用于合金钢样品中痕量铌的测定,结果令人满意。A new method for the determination of trace niobium by kinetic spectrophotometry was developed. This method was based on the catalytic effect of trace niobium on discoloring reaction of crystal violet oxidized by potassium bromate in sulphuric acid solution. The absorption curves were drew. The detective wavelength of this experiment was 545 nm. The single factor method was used to choice the best experiment conditions. The amount of H2SO4 (1.0 mol/L) was 2.0 mL, the amount of KBrO3(0.10 mol/L) was 2.5 mL, and the amount of crystal violet (0.50 g/L) was 0.5 mL. The reaction times was 4 min, and the reaction temperature was 100℃. The linear range of this method was 0 - 50 μg/L for niobium. The linear equation was ΔA = 0.926 CNb - 3.64 × 10^-3(r = 0.9993)and the detection limit was 6.1 × 10^-10 g/ mL. The method could be applied to the determination of trace niobium in alloy steel with satisfactory results.
分 类 号:TG115.33[金属学及工艺—物理冶金]
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