光谱学与光谱分析
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ICP-MS测定电吸附找矿泡塑样品中微量元素
施意华,杨仲平,黄俭惠,周奇明,熊传信
桂林矿产地质研究院,广西 桂林 541004
Determination of Trace Elements in Electrical Absorption Prospecting Polyform Sample by Inductively Coupled Plasma Mass Spectrometry
SHI Yi-hua, YANG Zhong-ping, HUANG Jian-hui, ZHOU Qi-ming, XIONG Chuan-xin
Guilin Research Institute of Geology for Mineral Resources, Guilin 541004, China
摘要 : 建立了电感耦合等离子质谱法(ICP-MS)测定电吸附找矿泡塑样品中钒、铬、锰、钴、镍、铜、锌、镓、铌、钼、银、镉、金、铊、铅和铋等16种微量元素的方法。进行了灰化法-王水提取、硝酸-过氧化氢消解-王水提取和沸水浴王水提取试样的比较实验,以硝酸-过氧化氢-王水提取法为最佳样品分解方法。对仪器工作参数进行了优化, 选取103 Rh和185 Re作为测定元素的内标元素, 进行了测定同位素的选择及干扰的消除等实验, 测定元素校准曲线的相关系数都在0.999 8以上, 各元素的检出限分别为0.001~2.2 μg·g-1 , 精密度介于1.39%~4.84%之间, 样品加标回收率为94.86%~105.2%。方法简便快速,已应用于大量泡塑样品分析。
关键词 :电感耦合等离子质谱法;电吸附找矿;泡塑样品;微量元素
Abstract :An ICP-MS method was established for the determination of sixteen trace elements, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Nb, Mo, Ag, Cd, Au, Tl, Pb and Bi in electrical absorption prospecting polyform. Three methods for polyform samples (ashing method, extraction by HNO3 +H2 O2 and digestion with aqua regia) were compared and the results showed that the second method is the best one. The best operational paramenters of X series ICP-MS were confirmed, the inner standard 103 Rh and 185 Re were selected for the determination of elements, and analysis of isotopes interference correction equations was established. Satisfactory linearity of working curves of the sixteen trace elements was obtained, giving all their correlation coefficients over 0.999 8. The determination limit of the analytes was in the range of 0.001-2.2 μg·g-1 . The precision was 1.39%-4.84%, and the recoveries were between 94.86% and 105.2%. The method is sensitive, quick and simple and has been applied to the analysis of a great number of polyform samples.
Key words :Inductively coupled plasma mass spectrometry(ICP-MS);Electrical absorption prospecting;Polyform sample;Trace elements
收稿日期: 2008-08-10
修订日期: 2008-11-20
通讯作者:
施意华
E-mail: syhua2000@163.com
[1] ZHOU Qi-ming,ZHOU Li-hong, DONG Shu-zheng(周奇明, 周立宏, 董树政). Geophysical & Geochemical Exploration(物探与化探), 2004, 28(3): 199. [2] ZHOU Qi-ming, HUANG Shu-jun, YANG Fang-fang, et al(周奇明,黄书俊, 杨芳芳, 等). Mineral Resources and Geology(矿产与地质), 2005, 19(6): 660. [3] WANG Ying, XIN Shi-gang(王 莹, 辛士刚). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2004, 24(2): 226. [4] SONG Xiao-nian, FENG Tian-pei(宋小年, 冯天培). Rock and Mineral Analysis(岩矿测试), 2006, 25(3): 282. [5] HOU Jing, GAO De-yu, LI Hong, et al(侯 静, 高德玉, 李 红, 等). Journal of Isotopes(同位素), 2004, 17(3): 135. [6] CHEN Lin, HE Yu-ping(陈 林, 贺与平). Metallurgical Analysis(冶金分析), 2007, 27(5): 59. [7] LI Chun-sheng, CHAI Zhi-fang, MAO Xue-ying, et al(李春生, 柴之芳, 毛雪瑛, 等). Chinese Journal of Analytical Chemistry(分析化学), 2001, 29(5):534. [8] ZHANG Lei, DING Xi-xiang, FANG Chao-meng(张 蕾, 丁锡祥, 方朝萌). Journal of Instrumental Analysis(分析测试学报), 2003, 22(2): 97. [9] LI Bing, YANG Hong-xia(李 冰, 杨红霞). The Principle and Application of Inductively Coupled Plasma Mass Spectrometry(电感耦合等离子体质谱原理与应用). Beijing: Geological Publishing House(北京: 地质出版社), 2005: 142. [10] HE Xiao-qing, LIU Xiang-sheng, CHEN Weng-xiang, et al(何小青, 刘湘生, 陈翁翔, 等). Metallurgical Analysis(冶金分析), 2004, 24(6): 26. [11] SONG Juan-e, LIANG Yue-qin, YU Shui(宋娟娥,梁月琴,于 水). Chinese Journal of Analytical Chemistry(分析化学), 2007, 35(3):423. [12] WANG Song-jun, CAO Lin, CHANG Ping, et al(王松君, 曹 林, 常 平, 等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2006, 26(7): 1330. [13] WANG Song-jun, CHANG Ping, WANG Pu-jun, et al(王松君, 常 平, 王璞珺, 等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2007, 27(1): 151. [14] SUN De-zhong, HE Hong-liao(孙德忠, 何红蓼). Rock and Mineral Analysis(岩矿测试), 2007, 26(1): 21. [15] LI Man, LI Dong-lei, LIU Xi-xiang, et al(李 曼, 李东雷, 刘玺祥, 等). Journal of Chinese Mass Spectrometry(质谱学报), 2006, 27(2): 100. [16] ZHOU Qi-ming, ZHAO You-fang, HUANG Hua-luan, et al(周奇明, 赵友方, 黄华鸾, 等). Geophysical & Geochemical Exploration(物探与化探), 2001, 25(13): 169.
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