混合酸比例对ICP-MS/OES测定地球化学样品中多元素的影响
四川省冶金地质勘查局六〇五大队分析测试中心, 四川 眉山 610860 |
The Effect of Mixed Acid Ratio on the Determination of Multielements in Geochemical Samples by ICP-MS/OES
Analysis & Testing Center of the No. 605 Team, Sichuan Metallurgy Geological Survey, Meishan 610860, China |
摘要：应用电感耦合等离子体质谱/发射光谱仪（ICP-MS/OES）测定地球化学样品中的多元素时，通常采用混合酸（盐酸-硝酸-氢氟酸-高氯酸）分解试样，但不同比例的混合酸对试样的分解效果影响极大，导致测试结果中经常出现铬、锰、铁、铝、钛及部分稀土元素测定结果偏低、精密度不理想的情况。本文通过改变混合酸中各类酸的混合比例，采用逆王水-氢氟酸-高氯酸分解试样，逆王水提取，使上述元素获得了较为理想的分解效果，特别是这些元素含量较高的样品分解效果的改善尤为显著。实验证明：当取样量为0.100 g时，采用8 mL逆王水、6 mL氢氟酸、3 mL高氯酸分解试样，8 mL逆王水提取，用国家一级标准物质进行验证，测试结果的相对标准偏差（n=6）为0.34%~4.02%，本方法精密度和准确度均满足地质实验室质量管理规范要求，可快速、准确、批量测定地球化学样品中的多元素。
The Effect of Mixed Acid Ratio on the Determination of Multielements in Geochemical Samples by ICP-MS/OES
ABSTRACT When determining elements in geochemical samples, the sample is usually decomposed by mixed acid (hydrochloric acid-hydrofluoric acid-perchloric acid) by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) and Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). However, the different proportions of mixed acid have a great influence on sample decomposition, resulting in lower analytical results of chromium, manganese, iron, aluminum, titanium and parts of rare earth elements, and bad analytical precision. In this study, samples are digested by mixed solution of inverse aqua regia, hydrofluoric acid, and perchloric acid, and then extracted by inverse aqua regia. This improves the decomposition of the above elements, especially for samples with high contents of these elements. Results show that the relative standard deviation (n=6) ranges from 0.34% to 4.02% for repeated determination of national level standard materials when 0.1 g sample was digested by 8 mL inverse aqua regia, 6 mL hydrofluoric acid, and 3 mL perchloric acid, and then extracted by 8 mL inverse aqua regia. The accuracy and precision of this method can satisfy the quality control standard requirements of the geology laboratory. This method establishes a fast and accurate approach to batch determination of multielements in geochemical samples.
本文参考文献
| [1] | Gray A L,Houk R S,Jarvos K E. Handbook of Inducti-vely Coupled Plasma Mass Spectrometry[M] . England: Chapmananad Hall, 1992 |
| [2] |
Qi L, Grégoire D C. Determination of trace elements in twenty six Chinese geochemistry reference materials by inductively coupled plasma-mass spectrometry[J].Geostandards Newsletter, 2000, 24: 51-63. doi: 10.1111/ggr.2000.24.issue-1 |
| [3] |
Diegor W, Longerich H, Abrajano T, et al. Applicability of a high pressure digertion technique to the analysis of sediment and soil samples by inductively coupled plasma-mass spectrometry[J].Analytica Chimica Acta, 2001, 431(2): 195-207. doi: 10.1016/S0003-2670(00)01339-8 |
| [4] |
Monecke T, Bombach G, Klemm W, et al. Determination of trace elements in the quartz reference material UNS-SpS and in natural quartz samples by ICP-MS[J].The Journal of Geostandards and Geoanalysis, 2000, 24: 73-81. doi: 10.1111/ggr.2000.24.issue-1 |
| [5] |
李冰,杨红霞. 电感耦合等子体质谱原理和应用[M] . 北京: 地质出版社, 2005: 109-110, 116. Li B,Yang H X. The Principle and Application of Inductively Coupled Plasma-Mass Spectrometry[M] . Beijing: Geological Publishing House, 2005: 109-110, 116. |
| [6] |
贾双琳, 赵平, 杨刚, 等. 混合酸敞开或高压密闭溶样-ICPMS测定地质样品中稀土元素[J]. 岩矿测试, 2014, 33(2): 186-191. Jia S L, Zhao P, Yang G, et al. Quick determination of rare earth elements in geological samples with open acid digestion or high-pressure closed digestion by inductively coupled plasma-mass spectrometry[J]. Rock and Mineral Analysis, 2014, 33(2): 186-191. |
| [7] |
张霖琳, 梁宵, 加那儿别克·西里甫汗, 等.在土壤及底泥重金属测定中不同前处理和分析方法的比较[J].环境化学, 2013, 32(2):302-306. Zhang L L, Liang X, Xlph J, et al. Comparison of different pretreatment and analytical method of heavy metals in soil and sediment samples[J]. Environmental Chemistry, 2013, 32(2):302-306. |
| [8] |
王君玉, 吴葆存, 李志伟, 等. 敞口酸溶-电感耦合等离子体质谱法同时测定地质样品中45个元素[J]. 岩矿测试, 2011, 30(4): 440-445. Wang J Y, Wu B C, Li Z W, et al. Determination of elemental content in geological samples by one-time acid dissolution and inductively coupled plasma-mass spectrometry[J]. Rock and Mineral Analysis, 2011, 30(4): 440-445. |
| [9] |
Stewart I I, Olesik J W. The effect of nitric acid concen-tration and nebulizer gas flow rates on aerosol properties and transport rates in inductively coupled plasma sample introduction[J].Journal of Analytical Atomic Spectrometry, 1998, 13: 1249-1256. doi: 10.1039/a804966a |
| [10] |
马生凤, 温宏利, 马新荣, 等. 四酸溶样-电感耦合等离子体原子发射光谱法测定铁、铜、锌、铅等硫化物矿石中22个元素[J]. 矿物岩石地球化学通报, 2011, 30(1): 65-72. Ma S F, Wen H L, Ma X R, et al. Determination of 22 elements in iron, copper, zinc, and lead sulphide ores by ICP-AES with four acids digestion[J]. Bulletin of Mineralogy, Petrology and Geochemistry, 2011, 30(1): 65-72. |
| [11] |
岩石矿物分析编委会. 岩石矿物分析(第四版第一分册)[M] . 北京: 地质出版社, 2011: 201-208. The Editorial Committee of Rock and Mineral Analysis . Rock and Mineral Analysis (The Fourth Edition, The First Volume)[M] . Beijing: Geological Publishing House, 2011: 201-208. |
| [12] |
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. |
| [13] |
Yokoyama T, Makishima A, Nakamura E, et al. Evaluation of the coprecipitation of incompatible trace elements with fluoride during silicate rock dissolution by acid digestion[J].Chemical Geology, 1999, 157: 175-187. doi: 10.1016/S0009-2541(98)00206-X |
| [14] |
李清彩, 赵庆令, 孙宁, 等. 电感耦合等离子体发射光谱测定区域地球化学样品中Cu、Mo、Pb、Sn、W、Zn元素[J]. 分析试验室, 2008, 27(Supplement): 317-319. Li Q C, Zhao Q L, Sun N, et al. Determination of Cu, Mo, Pb, Sn, W and Zn in geochemical samples by inductively coupled plasma-atomic emission spectrometry[J]. Chinese Journal of Analysis Laboratory, 2008, 27(Supplement): 317-319. |
相似文献（共20条）
| [1] |
林光西. 氢化物发生-原子荧光光谱法直接测定地球化学样品中痕量碲. 岩矿测试, 2008, 27(2): 151-152. |
| [2] | |
| [3] |
曹成东, 魏轶, 刘江斌. 发射光谱法同时测定地球化学样品中微量银铍硼锡铋钼. 岩矿测试, 2010, 29(4): 458-460. |
| [4] |
沈宇, 张尼, 高小红, 李皓, 马怡飞. 微波消解电感耦合等离子体质谱法测定地球化学样品中钒铬镍锗砷. 岩矿测试, 2014, (5): 649-654. |
| [5] |
吴健玲, 刘亚轩, 张勤. 电感耦合等离子体质谱法直接同时测定地球化学样品中镓铟铊. 岩矿测试, 2003, (1): 21-27. |
| [6] |
汪君, 王頔, 邓长生, 张建梅, 羊鸫, 王斌堂, 朱素霞. 电感耦合等离子体发射光谱法测定地球化学样品中的钍. 岩矿测试, 2014, 33(4): 501-505. |
| [7] | |
| [8] |
徐崇颖, 付爱瑞, 肖凡, 邢刚. 碘化钾-甲基异丁基甲酮萃取-火焰原子吸收分光光度法连续测定地球化学样品中痕量银镉铊. 岩矿测试, 2007, 26(1): 67-70. |
| [9] |
施意华, 杨仲平, 熊传信, 徐华. 蒸馏分离-电感耦合等离子体质谱法测定地球化学样品中痕量钌和锇. 岩矿测试, 2010, 29(4): 350-354. |
| [10] |
白金峰, 张勤, 孙晓玲, 董永胜, 范辉, 徐进力, 刘亚轩. 高分辨电感耦合等离子体质谱法测定地球化学样品中钪钇和稀土元素. 岩矿测试, 2011, 30(1): 17-22. |
| [11] |
徐进力, 邢夏, 郝志红, 刘彬, 白金峰. 聚氨酯泡塑吸附-电感耦合等离子体质谱法测定地球化学样品中的微量铊. 岩矿测试, 2012, 31(3): 430-433. |
| [12] |
白金峰, 薄玮, 张勤, 王海鹰. 高分辨电感耦合等离子体质谱法测定地球化学样品中的 36种元素. 岩矿测试, 2012, 31(5): 814-819. |
| [13] | |
| [14] |
俞晓峰, 李锐, 寿淼钧, 郑存江, 胡勇平. E5000型全谱直读型电弧发射光谱仪研制及其在地球化学样品分析中应用. 岩矿测试, 2015, 34(1): 40-47. doi: 10.15898/j.cnki.11-2131/td.2015.01.005 |
| [15] |
代素芳, 郑浩. 在高氯酸—酒石酸—硫脲介质中原子吸收法测定多种矿石中的银. 岩矿测试, 2000, (4): 301-303. |
| [16] |
冯静. P350萃取色谱分离无火焰原子吸收光谱法测定地球化学样品中的铟. 岩矿测试, 2005, (2): 138-140. |
| [17] |
邢夏, 徐进力, 何晓辉, 孙晓玲, 张芳. 石墨炉原子吸收光谱法测定地球化学样品中微量铬. 岩矿测试, 2011, 30(3): 333-336. |
| [18] |
王鹤龄, 李光一, 曲少鹏, 钱玉平, 仇秀梅, 董学林. 氟化物固体缓冲剂-交流电弧直读发射光谱法测定化探样品中易挥发与难挥发微量元素. 岩矿测试, 2017, 36(4): 367-373. doi: 10.15898/j.cnki.11-2131/td.201608230125 |
| [19] | |
| [20] |
李勇. Z-2000偏振塞曼石墨炉原子吸收分光光度计测定地球化学样品中痕量金. 岩矿测试, 2008, 27(4): 305-309. |
计量
- PDF下载量(59)
- 文章访问量(8227)
- HTML全文浏览量(3338)
- 被引次数(0)