氨水分离-电感耦合等离子体质谱法测定化探样品中的银
| 1. | 浙江省地质矿产研究所, 浙江 杭州 310007 |
| 2. | 中国环境监测总站, 北京 100012 |
Determination of Silver in Samples for Geochemical Exploration by Inductively Coupled Plasma-Mass Spectrometry after Ammonia Complexation
| 1. | Zhejiang Institute of Geology & Mineral Resources, Hangzhou 310007, China |
| 2. | China National Environmental Monitoring Center, Beijing 100012, China |
摘要：应用电感耦合等离子体质谱法(ICP-MS)测定化探样品中的Ag时, 两个同位素107Ag和109Ag分别受90Zr16O1H、91Zr16O和92Zr16O1H、93Nb16O等的干扰, 即使采用干扰系数法校正, 测定结果误差仍较大。本文采用硝酸-氢氟酸-高氯酸封闭分解样品, 氨水沉淀分离干扰元素Zr后以103Rh为内标用ICP-MS测定, 溶液中残留Zr对107Ag的测定干扰采用干扰系数法进行校正。方法检出限(3σ)为4.1 ng/g, 相对标准偏差(n=12) 为2.5%~7.8%。经53个地球化学标准物质验证, 溶液中的Ag未见损失。本方法是在氨性介质中Ag与氨形成稳定的络合离子, 而Zr则生成氢氧化物沉淀, 实现了Ag和Zr的分离, 大大减小了Zr对Ag的测定干扰; 采用封闭分解样品, 减少用酸量, 降低了样品空白值, 操作方法比高压密闭分解和P507萃淋树脂分离方法更简便快速。
Determination of Silver in Samples for Geochemical Exploration by Inductively Coupled Plasma-Mass Spectrometry after Ammonia Complexation
ABSTRACT Isobaric ions interfere with two isotopes of Ag during determination by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), i.e., 90Zr16O1H and 91Zr16O on 107Ag, and 92Zr16O1H and 93Nb16O on 109Ag. Although an interference correction coefficient method was used for the calibration of the analytical results, the analytical errors remain serious. In the proposed method, samples were closed decomposed by nitric acid, hydrofluoric acid, and perchloric acid. Ammonia was used to precipitate Zr and the purified Ag was determined by ICP-MS using 103Rh as the internal standard. The interference caused by the residual Zr was calibrated by the interference coefficient method. The method has a detection limit (3σ) of 4.1 ng/g and relative standard deviation (n=12) ranging from 2.5% to 7.8%. Determination of Ag in 53 primary certified materials of geochemical exploration indicates no loss of Ag. Using ammonium as the reagent, separation of Zr and Ag was successfully achieved due to the formation of the stable Ag-ammonium complex and Zr-hydroxide precipitate. The separation of Ag from Zr has reduced the interferences of Zr on Ag. Compared with the high-pressure sealed decomposition method and the P507 extraction resin separation method, the closed sample decomposition method is much simpler with less acid used and a lower blank.
本文参考文献
| [1] |
徐娟, 胡兆初, 刘勇胜, 等. 膜去溶-电感耦合等离子体质谱法测定21种国际地质标样中的银[J]. 分析化学, 2008, 36(11): 1493-1498. doi: 10.3321/j.issn:0253-3820.2008.11.008 Xu J, Hu Z C, Liu Y S, et al. Direct Determination of Ag in 21 International Geological Reference Materials by Membrane Desolvation-Inductively Coupled Plasma-Mass Spectrometry[J].Chinese Journal of Analytical Chemistry, 2008, 36(11): 1493-1498. doi: 10.3321/j.issn:0253-3820.2008.11.008 |
| [2] |
段树荣. 液珠萃取比色法测定化探样品中的金银[J]. 桂林工学院学报, 2003, 23(1): 136-138. Duan S R. Analysis of Trace Gold and Silver in Geochemical Samples in Extraction Colorimetry[J]. Journal of Guilin Institute of Technology, 2003, 23(1): 136-138. |
| [3] |
牛占海, 林焰, 和督虎, 等. 石墨炉原子吸收法测定化探样品中银和镉[J]. 冶金分析, 2001, 21(6): 61-63. Niu Z H, Lin Y, He D H, et al. GFAAS Determination of Ag and Cd in Geochemical Samples[J]. Metanurgical Analysis, 2001, 21(6): 61-63. |
| [4] |
张雪梅, 张勤. 发射光谱法测定勘查地球化学样品中银硼锡钼铅[J]. 岩矿测试, 2006, 25(4): 323-326. Zhang X M, Zhang Q. Determination of Silver, Boron, Tin, Molybdenum and Lead in Geochemical, Exploration Samples by Emission Spectrometry[J]. Rock and Mineral Analysis, 2006, 25(4): 323-326. |
| [5] |
何红蓼, 李冰, 韩丽荣, 等. 封闭压力酸溶-ICP-MS法分析地质样品中47个元素的评价[J]. 分析试验室, 2002, 21(5): 8-12. He H L, Li B, Han L R, et al. Evaluation of Determining 47 Elements in Geological Samples by Pressurized Acid Digestion-ICPMS[J]. Chinese Journal of Analysis Laboratory, 2002, 21(5): 8-12. |
| [6] |
曹心德, 尹明, 王小蓉, 等. 微波消解-电感耦合等离子体质谱法测定土壤中微量稀土元素[J]. 分析化学, 1999, 27(6): 679-683. Cao X D, Yin M, Wang X R, et al. Determination of Trace Rare Earth Elements in Soils by Inductively Coupled Plasma-Mass Spectrometry after Microwave Digestion for Sample Preparation[J]. Chinese Journal of Analytical Chemistry, 1999, 27(6): 679-683. |
| [7] |
周国兴, 刘玺祥, 崔德松, 等. 碱熔ICP-MS法测定岩石中稀土等28种金属元素[J]. 质谱学报, 2010, 31(2): 120-124. Zhou G X, Liu X X, Cui D S, et al. Determination of 28 Elements Including Rare Earth Elements by ICP-MS in Alkali Melted Rock Sample[J]. Journal of Chinese Mass Spectrometry Society, 2010, 31(2): 120-124. |
| [8] |
黄慧萍, 李艳玲, 陶德刚, 等. 电感耦合等离子体质谱法测定铬铁矿中痕量稀土元素[J]. 冶金分析, 2005, 25(6): 42-45. Huang H P, Li Y L, Tao D G, et al. Determination of Trace Rare Earth Elements in Monomineralic Rocks of Chromite by Inductively Coupled Plasma-Mass Spectrometry[J]. Metanurgical Analysis, 2005, 25(6): 42-45. |
| [9] |
周丽萍, 李中玺. 王水提取-电感耦合等离子体质谱法同时测定地质样品中微量银、镉、铋[J]. 分析试验室, 2005, 24(9): 20-25. Zou L P, Li Z X. Determination of Silver, Cadmium and Bismuth in Geological Samples by Inductively Coupled Plasma Mass Spectrometry with Aqua Regia Treatment[J]. Chinese Journal of Analysis Laboratory, 2005, 24(9): 20-25. |
| [10] |
范凡, 温宏利, 屈文俊, 等. 王水溶样-等离子体质谱法同时测定地质样品中砷锑铋银镉铟[J]. 岩矿测试, 2009, 28(4): 333-336. Fan F, Wen H L, Qu W J, et al. Determination of Arsenic, Antimony, Bismuth, Silver, Cadmium and Indiumin Geologgical Samples by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Sample Digestion[J]. Rock and Mineral Analysis, 2009, 28(4): 333-336. |
| [11] |
闵广全. CCT-ICP-MS测定土壤中微量元素银[J]. 农业科技与装备, 2012, (10): 17-18. doi: 10.3969/j.issn.1674-1161.2012.10.009 Min G Q. Determination of Soil Microelement Ag with CCT-ICP-MS[J].Agricultural Science & Technology and Equipment, 2012, (10): 17-18. doi: 10.3969/j.issn.1674-1161.2012.10.009 |
| [12] |
Guo W, Hu S H, Zhang J Y, et al. Elimination of Oxide Interferences and Determination of Ultra-trace Silver in Soils by ICP-MS with Ion-Molecule Reactions[J].Science of the Total Environment, 2011, 409: 2981-2986. doi: 10.1016/j.scitotenv.2011.04.011 |
| [13] |
邢智, 漆亮. P507萃淋树脂分离-电感耦合等离子体质谱法快速测定化探样品中的银[J]. 岩矿测试, 2013, 32(3): 398-401. Xing Z, Qi L. Separation with P507 Levextrel Resin for Rapid Determination of Ag in Geochemical Exploration Samples by ICP-MS[J].Rock and Mineral Analysis, 2013, 32(3): 398-401. |
引证文献（本文共被引用4次）
| [1] |
钛铁试剂共振散射法测定废胶片中的银含量[J]. 翟好英,胡尧,张金洋. 化学试剂. 2016(09) |
| [2] |
电感耦合等离子体质谱法测定硒时多元素干扰的碰撞/反应研究及其在地质样品中的应用[J]. 程秀花,王海蓉,黎卫亮,王鹏. 冶金分析. 2015(12) |
| [3] |
盐酸介质下火焰原子吸收光谱法测定铅精粉中的高含量银[J]. 刘高令,姜贞贞,吴文清,王祝,邵蓓,邬国栋,李明礼. 岩矿测试. 2016(06) |
| [4] |
电感耦合等离子体质谱直接测定化探样品中微量银[J]. 李永林. 西藏科技. 2016(08) |
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