富铀矿岩石样品中痕量镉的精确测量方法
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摘要
由于富铀矿岩石中伴生有大量的钼矿,而电感耦合等离子体质谱法测定痕量镉含量时,钼的氧化物会直接叠加到镉的质谱峰,造成质谱干扰,影响测量镉的正确度及精密度。研究了三种模式电感耦合等离子体质谱(ICP-MS)法测定富铀矿岩石中痕量镉Cd分析方法:膜去溶等离子体质谱(MCN-ICP-MS)法测定富铀矿岩石中痕量镉Cd含量的方法,能够高效降低钼的氧化物产率避免质谱干扰,将镉的灵敏度提高一个数量级,该方法的检出限为0.003μg·g,精密度小于5.52%,正确度为2.31%;以He气为碰撞气的碰撞池等离子体质谱法(KED-ICP-MS)测定富铀矿岩石中痕量镉Cd含量的方法,能够有效减少钼的氧化物干扰,同时也降低了镉的灵敏度,该方法的检出限为0.011μg·g~(-1),精密度小于8.63%,正确度为9.71%;氢化物发生等离子体质谱法(HG-ICP-MS)测定富铀矿岩石中痕量镉Cd含量的方法,该方法的检出限为0.003μg·g~(-1),精密度小于7.33%,正确度为3.68%。
Because there are a large number of molybdenum ores associated with uranium-rich rocks,the spectral of molybdenum oxides will directly superimpose on the mass spectrum peaks of cadmium which will cause mass spectrum interference and affect the accuracy and precision of cadmium measurement in the content determination of trace cadmium by Inductively Coupled Plasma Mass Spectrometry(ICP-MS). In this paper, three modes of Inductively Coupled Plasma Mass Spectrometry(ICP-MS)were developed for the determination of trace Cadmium in uranium-rich rocks. The first modes is the membrane dissolution plasma mass spectrometry(MCN-ICP-MS). The mode can effectively reduce the yield of molybdenum oxides and avoid the interference of mass spectrometry,and increase the sensitivity of cadmium by one order of magnitude. The detection limit of this method is0.003 μg·g~(-1), the precision is less than 5.52 %, and the accuracy is 2.31 %. The second mode is the collision pool plasma mass spectrometry( KED-ICP-MS) with He as collision gas, the mode can effectively reduce the interference of molybdenum oxides and reduce the sensitivity of cadmium. The detection limit of this method is 0.011 μg·g~(-1), the precision is less than 8.63 %, and the accuracy is9.71 %. The third mode is the Hydride Generation Plasma Mass Spectrometry(HG-ICP-MS). The detection limit of this mode is 0.003 μg·g~(-1), the precision is less than 7.33 % and the accuracy is3.68 %.
Because there are a large number of molybdenum ores associated with uranium-rich rocks,the spectral of molybdenum oxides will directly superimpose on the mass spectrum peaks of cadmium which will cause mass spectrum interference and affect the accuracy and precision of cadmium measurement in the content determination of trace cadmium by Inductively Coupled Plasma Mass Spectrometry(ICP-MS). In this paper, three modes of Inductively Coupled Plasma Mass Spectrometry(ICP-MS)were developed for the determination of trace Cadmium in uranium-rich rocks. The first modes is the membrane dissolution plasma mass spectrometry(MCN-ICP-MS). The mode can effectively reduce the yield of molybdenum oxides and avoid the interference of mass spectrometry,and increase the sensitivity of cadmium by one order of magnitude. The detection limit of this method is0.003 μg·g~(-1), the precision is less than 5.52 %, and the accuracy is 2.31 %. The second mode is the collision pool plasma mass spectrometry( KED-ICP-MS) with He as collision gas, the mode can effectively reduce the interference of molybdenum oxides and reduce the sensitivity of cadmium. The detection limit of this method is 0.011 μg·g~(-1), the precision is less than 8.63 %, and the accuracy is9.71 %. The third mode is the Hydride Generation Plasma Mass Spectrometry(HG-ICP-MS). The detection limit of this mode is 0.003 μg·g~(-1), the precision is less than 7.33 % and the accuracy is3.68 %.
引文
[1]新华社.联合国制定铅镉含量新标准[J].中国食品学报, 2006,(4):136.
[2] The comission of European Communities. Commission directive 2005/31/EC of 29 April 2005 amending council directive 84/500/EEC as regards a declaration of compliance and performance criteria of the analytical method for ceramic articles intended to come into contact with foodstuffs[S]. 2005.
[3]郭冬发,武朝辉,裴玲云,等.膜去溶进样高分辨等离子体质谱技术测定岩石样品中的17个镧系和锕系元素[J].质谱学报, 1999, 20(3, 4):103-104.
[4]彭谦,王光建,张克荣.冷蒸气发生原子吸收光谱法测定食品中痕量镉[J].理化检验-化学分册,2003, 39(3):133-134.
[5]吴政宙,陈文君.食品中痕量镉的测定[J].光谱实验室, 2005, 22(4):814-818.
[6]龚治湘.微型多功能进样装置:中国, ZL 200420084256.7[P].
[2] The comission of European Communities. Commission directive 2005/31/EC of 29 April 2005 amending council directive 84/500/EEC as regards a declaration of compliance and performance criteria of the analytical method for ceramic articles intended to come into contact with foodstuffs[S]. 2005.
[3]郭冬发,武朝辉,裴玲云,等.膜去溶进样高分辨等离子体质谱技术测定岩石样品中的17个镧系和锕系元素[J].质谱学报, 1999, 20(3, 4):103-104.
[4]彭谦,王光建,张克荣.冷蒸气发生原子吸收光谱法测定食品中痕量镉[J].理化检验-化学分册,2003, 39(3):133-134.
[5]吴政宙,陈文君.食品中痕量镉的测定[J].光谱实验室, 2005, 22(4):814-818.
[6]龚治湘.微型多功能进样装置:中国, ZL 200420084256.7[P].