紫外分光光度法测定硒氧化过程中二氧化硒  

UV spectrophotometric determination of selenium dioxide in process of selenium oxidation

作　　者：朱鸭梅[1] 崔群[1] 王海燕[1] 

机构地区：[1]南京工业大学化学化工学院,南京210009

出　　处：《分析试验室》2010年第10期60-63,共4页Chinese Journal of Analysis Laboratory

基　　金：中国石油化工股份有限公司委托科研(YZ05-07-ZS-0016)项目资助

摘　　要：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。Based on the Absorption property of 5-nitro-2,1,3-benzoselenodiazo in the UV region,UV spectrophotometric determination of Se(Ⅳ) in process of selenium oxidation was proposed.The derivative reaction conditions of Se(Ⅳ) and 4-nitro-o-phenylenediamine(NPDA) to form 5-nitro-2,1,3-benzoselenodiazo was investigated and the accuracy of determination results was analyzed.The proper derivative reaction conditions were as follows: the pH of 2,the temperature of 60 ℃,the reaction time of 10 min and the mass ratio of NPDA to Se(Ⅳ) of 168.The Absorbance had good linear relationship with the concentration of Se(Ⅳ) in the range of 0.002~0.02 g/L with good linear correlation coefficient.The selenium dioxide content in the process of selenium oxidation was measured by this method,and the repeatability of analysis result was excellent with the RSD of 0.52%.The average spiked recovery of Se(Ⅳ) was 98.12%.The method is simple,accurate and efficient for determination of Se(Ⅳ) in large selenium content system and is a good reference for other valence states of selenium.

关 键 词：硒(Ⅳ) 4-硝基邻苯二胺 5-硝基-2 1 3-苯并苤硒脑 吸光度 萃取 

分 类 号：O657.3[理学—分析化学]