冷原子汞发生-原子荧光光谱法测定地球化学样品中痕量汞
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摘要
称取样品0.200 0g,加入盐酸-硝酸(9+1)混合酸5mL,于沸水浴中加热2h,冷却后加入75g·L~(-1)硫脲-75g·L~(-1)抗坏血酸混合溶液5mL,混匀后,用含5g·L~(-1)酒石酸的3mol·L~(-1)盐酸溶液定容至25mL,摇匀后供冷原子汞发生-原子荧光光谱法分析。所选择的仪器工作条件为:(1)光电倍增管负高压230V;(2)主阴极峰值电流25mA,辅助阴极峰值电流0;(3)2g·L~(-1)氢氧化钾-0.05g·L~(-1)硼氢化钾混合液为还原剂;(4)载气(氩气)流量800mL·min~(-1);(5)原子化器温度200℃;(6)原子化器高度7mm。结果表明:汞的质量在12.00ng以内与荧光强度呈线性关系,方法的检出限(3s)为0.24ng·g~(-1)。方法用于测定地球化学国家一级标准物质中的痕量汞,测定值与认定值相符,测定值的相对标准偏差(n=12)小于8.0%。
The sample(0.200 0 g) was added into 5 mL of a mixture of hydrochloric acid and nitric acid(9+1),and the solution was heated in boiling water for 2 h.After cooling,5 mL of a solution containing 75 g·L~(-1) thiourea and 75 g·L~(-1) ascorbic acid was added and mixed well.Then the volume of the solution was made up to25 mL with 3 mol·L~(-1) hydrochloric acid solution containing 5 g·L~(-1) tartrate.After shaking,the sample solution was used for cold atomic mercury generation-atomic fluorescence spectrometry analysis.Working conditions of the instrument were chosen as follows:(1) negative high voltage of photomultiplier tube was 230 V;(2) peak currents of main cathode and auxiliary cathode were 25 mA,0,respectively;(3)a mixed solution containing 2 g·L~(-1) KOH and 0.05 g·L~(-1) KBH_4 was used as reducing agent;(4)flow-rate of carrier gas(argon) was 800 mL·min~(-1);(5)temperature of atomizer was 200℃;(6) height of atomizer was 7 mm.It was showed that,linear relationship was found between fluorescence intensity and mass of mercury within 12.00 ng,with detection limit(3 s) of 0.24 ng·g~(-1).The proposed method was applied to determination of mercury in GBWs for geochemistry,giving results in consistency with certified values and RSDs(n=12) less than 8.0%.
The sample(0.200 0 g) was added into 5 mL of a mixture of hydrochloric acid and nitric acid(9+1),and the solution was heated in boiling water for 2 h.After cooling,5 mL of a solution containing 75 g·L~(-1) thiourea and 75 g·L~(-1) ascorbic acid was added and mixed well.Then the volume of the solution was made up to25 mL with 3 mol·L~(-1) hydrochloric acid solution containing 5 g·L~(-1) tartrate.After shaking,the sample solution was used for cold atomic mercury generation-atomic fluorescence spectrometry analysis.Working conditions of the instrument were chosen as follows:(1) negative high voltage of photomultiplier tube was 230 V;(2) peak currents of main cathode and auxiliary cathode were 25 mA,0,respectively;(3)a mixed solution containing 2 g·L~(-1) KOH and 0.05 g·L~(-1) KBH_4 was used as reducing agent;(4)flow-rate of carrier gas(argon) was 800 mL·min~(-1);(5)temperature of atomizer was 200℃;(6) height of atomizer was 7 mm.It was showed that,linear relationship was found between fluorescence intensity and mass of mercury within 12.00 ng,with detection limit(3 s) of 0.24 ng·g~(-1).The proposed method was applied to determination of mercury in GBWs for geochemistry,giving results in consistency with certified values and RSDs(n=12) less than 8.0%.
引文
[1] DZ/T 0011-2015 中华人民共和国地质矿产行业标准地球化学普查规范(1∶50000)[S].
[2] 徐文军.顺序注射氢化物发生-原子荧光光谱法同时测定环境水样中铋和汞[J].冶金分析,2009,29(11):61-64.
[3] 杨芬,卢业友.氢化物发生-原子荧光光谱法测定水系沉积物中的铋和汞[J].理化检验-化学分册,2011,47(1):70-72.
[4] 戴礼洪,刘潇威,刘岩,等.全自动汞分析系统在土壤总汞测定中的应用[J].理化检验-化学分册,2014,50(7):845-848.
[5] 张锦茂,冯先进,周志恒,等.ATC 005原子荧光光谱分析技术[M].北京:中国标准出版社,2011:47-49.
[6] 陈丽琼,杨晓红,张榆霞,等.原子荧光光谱法测定大气颗粒物中砷、汞的研究现状及展望[J].理化检验-化学分册,2015,51(8):1203-1207.
[7] 张延妮,董娟丽.氢化物发生-原子荧光光谱法同时测定水中砷和汞[J].理化检验-化学分册,2009,45(3):316-318.
[8] 张耀奎,肖海斌.高锰酸钾-过硫酸钾消化氢化物发生-原子荧光光谱法测定水中汞[J].四川地质学报,2012,32(3):356-366.
[2] 徐文军.顺序注射氢化物发生-原子荧光光谱法同时测定环境水样中铋和汞[J].冶金分析,2009,29(11):61-64.
[3] 杨芬,卢业友.氢化物发生-原子荧光光谱法测定水系沉积物中的铋和汞[J].理化检验-化学分册,2011,47(1):70-72.
[4] 戴礼洪,刘潇威,刘岩,等.全自动汞分析系统在土壤总汞测定中的应用[J].理化检验-化学分册,2014,50(7):845-848.
[5] 张锦茂,冯先进,周志恒,等.ATC 005原子荧光光谱分析技术[M].北京:中国标准出版社,2011:47-49.
[6] 陈丽琼,杨晓红,张榆霞,等.原子荧光光谱法测定大气颗粒物中砷、汞的研究现状及展望[J].理化检验-化学分册,2015,51(8):1203-1207.
[7] 张延妮,董娟丽.氢化物发生-原子荧光光谱法同时测定水中砷和汞[J].理化检验-化学分册,2009,45(3):316-318.
[8] 张耀奎,肖海斌.高锰酸钾-过硫酸钾消化氢化物发生-原子荧光光谱法测定水中汞[J].四川地质学报,2012,32(3):356-366.
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