氢化物发生-原子荧光光谱法测定硫磺中微量铋  

Determination of micro bismuth in sulfur by hydride generation atomic fluorescence spectrometry

作　　者：程先忠[1] 何启生[2] 李小丹[2] 邵坤[1] 张瑞华[1] 

机构地区：[1]武汉工业学院化学与环境工程学院,湖北武汉430023 [2]宜昌地质矿产研究所,湖北宜昌443003

出　　处：《冶金分析》2009年第9期10-14,共5页Metallurgical Analysis

基　　金：湖北省科技厅自然科学基金重点项目(2008CDA100)资助

摘　　要：本文建立了氢化物发生-原子荧光光谱法直接测定硫磺中微量铋的方法。为避免硫磺样品分解时使用大量的强酸和有毒试剂,采用微波消解,以HNO3-H2O2作为消化试剂,能够完全将硫磺消解,制备的溶液直接进行原子荧光光谱法测定铋。实验中对影响仪器测定的条件如负高压、灯电流、原子化高度进行了优化,并对载气、屏蔽气、硼氢化钾、酸度介质的影响进行了探讨。方法的检出限为0.023ng/mL,对升华硫磺、食品级硫磺、工业硫磺3种类型样品进行了精密度和回收率试验,回收率在96%～106%,相对标准偏差为0.92%～4.5%(n=7)。方法满足硫磺样品中微量铋的测定,并且避免了废气对环境的污染。A new method was developed for the direct determination of micro bismuth in sulfur samples by hydride generation atomic fluorescence spectrometry. Microwave digestion was employed to avoid the use of large amounts of strong acid and toxic reagents. HNOa-H2O2 was used as the digestion reagent so that sulfur could be digested completely and the sample solution could be determined by atomic fluorescence spectrometry. The analytical parameters, such as negative high voltage, lamp current and atomized height were optimized. The effects of carrier, masking gas, sodium bonohydride and acidity were explored. The detection limit （3σ） of bismuth was 0. 023 μg/L. The relative standard deviation （RSD） for seven replicate measurements of the sulfur samples was 0. 92%--4.5% （n=7） ; the standard addition recovery was 96%- 106%. The proposed method was suitable for the determination of bismuth in sulfur samples without the risk of environmental contamination

关 键 词：氢化物发生-原子荧光光谱法 微波消解 硫磺 铋 

分 类 号：TQ125.11[化学工程—无机化工]