摘要
用HNO3+HCl分解样品,采用Fe3+-柠檬酸混合溶液作抑制剂,研究了下氢化物发生-原子荧光光谱法测定痕量硒时的干扰及其机理,探讨了NO3-和NO2-残留的影响,并用正交试验设计结合单因素试验研究了不同浓度Fe3+盐、盐酸、柠檬酸、硼氢化钾等条件下Se的回收率。该方法的检出限为0.15μg.L-1,样品中Se含量为27.01μg.L-1的相对标准偏差在3.1%～4.2%之间(n=11),加标回收率为96.1%～102.3%。用于实际样品的测定,结果满意。
The samples were decomposed with HNO3＋HCl,and Fe3＋-citric acid mix solution was added to eliminate interferences.The elimination and mechanism of tellurium interference with selenium determination by HG-AFS were studied,and the residuary influence of NO-3 and NO-2 was investigated.The interference of ferric trichloride,hydrochloric acid,citric acid and PBH concentration with the fluorescence intensity of selenium was observed by the orthogonal test design combined with the mono-factor test.The detection limit was 0.15 μg·L-1.The relative standard deviation of a solution containing 27.01 μg·L-1 selenium in sample was in the range of 3.1%~4.2%（n=11）,and the recoveries of selenium were 96.1%~102.3%.The results obtained were satisfied,and the method was successfully applied to the determination of selenium in high purity tellurium samples.
出处
《光谱学与光谱分析》
SCIE
EI
CAS
CSCD
北大核心
2011年第11期3123-3125,共3页
Spectroscopy and Spectral Analysis
基金
国家自然科学基金项目(20807012)
广东省自然科学基金项目(9151065003000010)资助
关键词
高纯碲
硒
干扰及消除
原子荧光光谱
High purity tellurium
Selenium
Interference and elimination
Atomic fluorescence spectrometry
