论文部分内容阅读
利用5-硝基-2,1,3-苯并苤硒脑对紫外光的吸收特性,用紫外分光光度计测定硒氧化过程中硒(Ⅳ)含量。研究了硒(Ⅳ)与4-硝基邻苯二胺(NPDA)生成5-硝基-2,1,3-苯并苤硒脑的衍生反应条件,验证了测定结果的准确性。结果表明:衍生反应适宜条件为pH2,反应温度60℃,反应时间10 min,NPDA试剂用量为硒(Ⅳ)的168倍。在0.002~0.02 g/L硒(Ⅳ)范围内,硒(Ⅳ)浓度与衍生产物5-硝基-2,1,3-苯并苤硒脑的吸光度线性关系良好。用该法测定硒氧化过程中二氧化硒含量,RSD为0.52%。硒(Ⅳ)的平均加标回收率为98.12%。本文建立的紫外分光光度法为硒含量较大的体系中硒(Ⅳ)定量分析提供了准确、便捷的测定方法,对于其它价态硒(Ⅵ价、Ⅱ价、0价)测定有借鉴作用。
Using 5-nitro-2,1,3-benzodiazepine selenium brain UV absorption characteristics, determination of selenium (Ⅳ) content by selenium oxidation with UV spectrophotometer. The derivatization conditions of selenium (Ⅳ) and 4-nitro-o-phenylenediamine (NPDA) to generate 5-nitro-2,1,3-benzodiazepine selenium were studied, and the accuracy of the determination results was verified. The results showed that the suitable conditions for the derivatization reaction were pH2, reaction temperature 60 ℃, reaction time 10 min, and the amount of NPDA reagent was 168 times of selenium (Ⅳ). In the range of 0.002-0.02 g / L selenium (Ⅳ), the concentration of selenium (Ⅳ) has good linear relationship with the absorbance of 5-nitro-2,1,3-benzodiazepine selenium. The determination of selenium dioxide selenium content by this method, RSD was 0.52%. The average recovery of selenium (Ⅳ) was 98.12%. The UV spectrophotometry established in this paper provides an accurate and convenient method for the quantitative analysis of selenium (Ⅳ) in the system with large selenium content. It can be used as a reference for the determination of other valences of selenium (Ⅳ, Ⅱ, 0).