电感耦合等离子体质谱法测定地球化学样品中的硼碘锡锗
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摘要
在多目标的配套方法中,硼、碘、锡、锗四个元素的分析涉及三个配套方法,发射光谱法测定硼、锡,原子荧光光谱法测定锗,分光光度法或电感耦合等离子体质谱法(ICP-MS)测定碘,分析成本高、检测效率低。本文建立了一种ICP-MS同时测定地球化学样品中硼、碘、锡、锗的方法。样品用过氧化钠熔矿,使难熔元素锡分解完全,熔盐经水提取后加入铼内标,再用阳离子交换树脂分离大量钠盐及大部分阳离子,保证了盐分满足质谱测定的要求。方法检出限分别为硼0.92μg/g、碘0.10μg/g、锡0.29μg/g、锗0.09μg/g,满足多目标测试要求。用国家一级标准物质验证,测定值与认定值一致,相对标准偏差(RSD,n=12)≤5%,适用于批量地球化学样品中硼、碘、锡、锗的测定,样品处理过程简便,检测效率高。
BACKGROUND: In the multi-objective method, the analysis of four elements of boron, iodine, tin and germanium involves three supporting methods. Boron and tin were determined by Emission Spectrometry, germanium was determined by Atomic Fluorescence Spectrometry, and iodine was determined by Spectrophotometry or Inductively Coupled Plasma-Mass Spectrometry. The analysis cost is high and the detection efficiency is low. OBJECTIVES: To establish an easy, highly efficient and precise, low-cost method for determination of boron, iodine, tin and germanium in geochemical samples by Inductively Coupled Plasma-Mass Spectrometry.METHODS: The sample is fused with sodium peroxide to completely decompose the refractory element tin. The molten salt is extracted by water and the internal standard is added, and then the cation exchange resin is used to separate a large amount of sodium salt and most of the cations, ensuring that the salt meets the requirements of mass spectrometry analysis.RESULTS: The element detection limits were 0.92μg/g, 0.10μg/g, 0.29μg/g, 0.09μg/g for boron, iodine, tin and germanium, respectively. The relative standard deviation(RSD, n=12) was smaller than 5%. The method was verified by certified reference materials, and the measured values were consistent with the certified values.CONCLUSIONS: The method is suitable for the determination of boron, iodine, tin and germanium in batch geochemical samples.
BACKGROUND: In the multi-objective method, the analysis of four elements of boron, iodine, tin and germanium involves three supporting methods. Boron and tin were determined by Emission Spectrometry, germanium was determined by Atomic Fluorescence Spectrometry, and iodine was determined by Spectrophotometry or Inductively Coupled Plasma-Mass Spectrometry. The analysis cost is high and the detection efficiency is low. OBJECTIVES: To establish an easy, highly efficient and precise, low-cost method for determination of boron, iodine, tin and germanium in geochemical samples by Inductively Coupled Plasma-Mass Spectrometry.METHODS: The sample is fused with sodium peroxide to completely decompose the refractory element tin. The molten salt is extracted by water and the internal standard is added, and then the cation exchange resin is used to separate a large amount of sodium salt and most of the cations, ensuring that the salt meets the requirements of mass spectrometry analysis.RESULTS: The element detection limits were 0.92μg/g, 0.10μg/g, 0.29μg/g, 0.09μg/g for boron, iodine, tin and germanium, respectively. The relative standard deviation(RSD, n=12) was smaller than 5%. The method was verified by certified reference materials, and the measured values were consistent with the certified values.CONCLUSIONS: The method is suitable for the determination of boron, iodine, tin and germanium in batch geochemical samples.
引文
[1] 程素敏,王娟,张岩,等.分光光度法测定土壤中碘的方法改进[J].中国无机分析化学,2015,5(4):41-43. Cheng S M,Wang J,Zhang Y,et al.Method improvement on the determination of iodine in soil by ectrophotometry[J].Chinese Journal of Inorganic Analytical Chemistry,2015,5(4):41-43.
[2] 张文华,王彦东,吴冬梅,等.交流电弧直读光谱法快速测定地球化学样品中的银、锡、硼、钼、铅[J].中国无机分析化学,2013,3(4):16-19. Zhang W H,Wang Y D,Wu D M,et a1.Rapid determination of silver,tin,boron,molybdenum and lead in geochemical samples by AC Arc direct-reading spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(4):16-19.
[3] 黄辉,李本涛,李颖,等.ICP-AES法测定低合金钢中的微量硼[J].化学分析计量,2016,25(1):47-49. Huang H,Li B T,Li Y,et al.Determination of trace boron in low-alloy steel by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2016,25(1):47-49.
[4] 宋伟娇,代世峰,赵蕾,等.微波消解-电感耦合等离子体质谱法测定煤中的硼[J].岩矿测试,2014,33(3):327-331. Song W J,Dai S F,Zhao L,et al.Determination of boron in coal samples with microwave digestion by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(3):327-331.
[5] 池卫廷.硼测定方法的研究现状[J].职业与健康,2010,26(3):335-338. Chi W T.Study status of boron determination[J].Occupation and Health,2010,26(3):335-338.
[6] 赵峰,李瑞仙,祝建国,等.氢化物发生-原子荧光光度法直接测定环境土壤中的痕量锗[J].分析测试技术与仪器,2011,17(1):56-58. Zhao F,Li R X,Zhu J G,et al.Direct determination of trace germanium in environmental soil by atomic fluorescence spectrometry[J].Analysis and Testing Technology and Instruments,2011,17(1):56-58.
[7] 杨佳,薛瑞,张超.氢化物发生-原子荧光光谱法测定铀矿石中的锗元素[J].中国无机分析化学,2016,6(2):16-19. Yang J,Xue R,Zhang C.Determination of germanium in uranium ores by hydride-generation atomic fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2016,6(2):16-19.
[8] 陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196. Chen B,Liu H Q,Xing Y X.Simultaneous determination of Ge,Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196.
[9] 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 a1.Evaluation of determining 47 elements in geological samples by pressurized acid digestion-ICPMS[J].Chinese Journal of Analysis Laboratory,2002,21(5):8-12.
[2] 张文华,王彦东,吴冬梅,等.交流电弧直读光谱法快速测定地球化学样品中的银、锡、硼、钼、铅[J].中国无机分析化学,2013,3(4):16-19. Zhang W H,Wang Y D,Wu D M,et a1.Rapid determination of silver,tin,boron,molybdenum and lead in geochemical samples by AC Arc direct-reading spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(4):16-19.
[3] 黄辉,李本涛,李颖,等.ICP-AES法测定低合金钢中的微量硼[J].化学分析计量,2016,25(1):47-49. Huang H,Li B T,Li Y,et al.Determination of trace boron in low-alloy steel by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Meterage,2016,25(1):47-49.
[4] 宋伟娇,代世峰,赵蕾,等.微波消解-电感耦合等离子体质谱法测定煤中的硼[J].岩矿测试,2014,33(3):327-331. Song W J,Dai S F,Zhao L,et al.Determination of boron in coal samples with microwave digestion by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(3):327-331.
[5] 池卫廷.硼测定方法的研究现状[J].职业与健康,2010,26(3):335-338. Chi W T.Study status of boron determination[J].Occupation and Health,2010,26(3):335-338.
[6] 赵峰,李瑞仙,祝建国,等.氢化物发生-原子荧光光度法直接测定环境土壤中的痕量锗[J].分析测试技术与仪器,2011,17(1):56-58. Zhao F,Li R X,Zhu J G,et al.Direct determination of trace germanium in environmental soil by atomic fluorescence spectrometry[J].Analysis and Testing Technology and Instruments,2011,17(1):56-58.
[7] 杨佳,薛瑞,张超.氢化物发生-原子荧光光谱法测定铀矿石中的锗元素[J].中国无机分析化学,2016,6(2):16-19. Yang J,Xue R,Zhang C.Determination of germanium in uranium ores by hydride-generation atomic fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2016,6(2):16-19.
[8] 陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196. Chen B,Liu H Q,Xing Y X.Simultaneous determination of Ge,Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196.
[9] 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 a1.Evaluation of determining 47 elements in geological samples by pressurized acid digestion-ICPMS[J].Chinese Journal of Analysis Laboratory,2002,21(5):8-12.
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