摘要
采用王水/HBr溶解样品,酒石酸掩蔽锑,用甲基异丁基甲酮(MIBK)将汞萃取到有机相中,建立了有机相进样—断续流动注射原子荧光光谱法测定锑锭和氧化锑中汞含量的方法。研究了溶样方法和共存离子可能引起的干扰,优化了仪器工作条件、萃取条件、酸度及其他影响因素。结果表明,在最佳条件下,汞含量在0.02～50μg/L范围内线性关系良好,方法检出限为0.013μg/L。将方法应用于锑锭和氧化锑实际样品分析,测得结果与电感耦合等离子体原子发射光谱法一致,相对标准偏差(RSD,n=6)在0.65%～2.4%之间,加标回收率为94%～99%。
After the samples were dissolved in aqua regia/HBr and tartaric acid was added to mask antimony, then mercury in antimony ingot and antimony oxide was extracted into the organic phase with methyl isobutyl ketone （MIBK） and determined by organic phase injection-intermittent flow injection atomic fluorescence spectrometry. Sample dissolution methods and interferences caused by coexisting ions were investigated, and instrument working conditions, extraction conditions, acidity and other factors were optimized. The results showed that under optimal conditions, the mercury content within the range of 0.02 to 50 μg/Lwas in good linear relationship, and the detection limit was 0. 013 μg/L. This method was applied to the actual antimony ingot and antimony oxide sample analysis. It was found that the results were consistent with those obtained by inductive coupled plasma atomic emission spectrometry with relative standard deviations （RSDs, n=6） of 0. 65%-2.4% and recoveries of 94 %-99%.
出处
《冶金分析》
CAS
CSCD
北大核心
2012年第9期43-46,共4页
Metallurgical Analysis
基金
国家自然科学基金(No.51168001)
关键词
甲基异丁基甲酮
萃取
氢化物发生原子荧光光谱法
锑锭
氧化锑
汞
methyl isobutyl ketone
extraction
hgdride generation atomic fluorescence spectrometry
antimony ingot
antimony oxide
mercury
