动能歧视模式ICP-MS测定地球化学样品中14种痕量元素
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摘要
应用传统ICP-MS法测定勘查地球化学样品中Ag、Cd等痕量元素,基体效应和多原子离子干扰严重,准确测定的难度较大。本文基于当前ICP-MS消除干扰技术,分析了ICP-MS标准模式(STD)及动能歧视模式(KED)测定地球化学样品中Ag、Cd等14种痕量元素的有效性,通过比较这两种模式的测定效果,在此基础上确定了各元素的有效测定模式。结果表明:在KED模式下,基体元素如Zr、Nb氧化物的产率降低,基本上消除了Zr、Nb氧化物对痕量元素Ag、Cd的多原子离子干扰。KED模式提高了信噪比,降低了方法检出限,如Ag、Cd的检出限分别为0. 004mg/kg、0. 005mg/kg,其他12种元素的检出限也低于多目标地球化学调查76种元素分析方案中的检出限。测定痕量元素的准确度显著优于STD模式。实验中采用简单的硝酸-氢氟酸-高氯酸消解样品,残渣用王水复溶,结合KED模式下优选出干扰较小的同位素作为测定同位素,以Rh作为内标校正仪器产生的信号漂移,将样品溶液稀释至1000倍,基体效应降低至最小。本方法经国家一级标准物质的验证,测定结果与认定值相符,可为勘查地球化学提供高质量数据。
BACKGROUND: Traditional inductively coupled plasma-mass spectrometry( ICP-MS) determination of trace elements such as Ag and Cd in geochemical samples is seriously affected by the matrix effect and multiple polyatomic ions,making it difficult to measure these elements accurately.OBJECTIVES: To compare the results of ICP-MS standard mode( STD) and kinetic energy discrimination mode( KED),and determine the valid determination modes of each element.METHODS: The samples were digested by HNO3-HF-HClO4,and the residue was dissolved in aqua regia.Under the KED mode,the isotopes with less interference were selected as the determination isotopes. Rh was used as the internal standard element to correct the signal drift,and the sample solution was diluted by 1000. Under these conditions,the matrix effect was minimized.RESULTS: The productivity of matrix elements such as Zr and Nb oxides was reduced,and the interference of oxides on Ag and Cd was minimized under the KED mode. The KED mode improved the signal-to-noise ratio and reduced the detection limits of this method with Ag and Cd,detection limits of 0. 004 mg/kg and 0. 005 mg/kg,respectively. The detection limits of the other 12 elements were also lower than those of 76 element analysis schemes in a multi-objective geochemical survey. The accuracy of determination of trace elements was significantly better than that of the STD mode.CONCLUSIONS: The method has been verified by the first-class national reference material and the analytical results are in good agreement with the certified values. The method provides high-quality data for exploration geochemistry.
BACKGROUND: Traditional inductively coupled plasma-mass spectrometry( ICP-MS) determination of trace elements such as Ag and Cd in geochemical samples is seriously affected by the matrix effect and multiple polyatomic ions,making it difficult to measure these elements accurately.OBJECTIVES: To compare the results of ICP-MS standard mode( STD) and kinetic energy discrimination mode( KED),and determine the valid determination modes of each element.METHODS: The samples were digested by HNO3-HF-HClO4,and the residue was dissolved in aqua regia.Under the KED mode,the isotopes with less interference were selected as the determination isotopes. Rh was used as the internal standard element to correct the signal drift,and the sample solution was diluted by 1000. Under these conditions,the matrix effect was minimized.RESULTS: The productivity of matrix elements such as Zr and Nb oxides was reduced,and the interference of oxides on Ag and Cd was minimized under the KED mode. The KED mode improved the signal-to-noise ratio and reduced the detection limits of this method with Ag and Cd,detection limits of 0. 004 mg/kg and 0. 005 mg/kg,respectively. The detection limits of the other 12 elements were also lower than those of 76 element analysis schemes in a multi-objective geochemical survey. The accuracy of determination of trace elements was significantly better than that of the STD mode.CONCLUSIONS: The method has been verified by the first-class national reference material and the analytical results are in good agreement with the certified values. The method provides high-quality data for exploration geochemistry.
引文
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[2]李小莉，安树清，徐铁民，等．超细粉末压片制样X射线荧光光谱测定碳酸岩样品中多种元素及CO2[J]．光谱学与光谱分析，2015,35(6):1741-1745.Li X L,An S Q,Xu T M,et al. Ultra-fine pressed powder pellet sample preparation XRF determination of multi-elements and carbon dixide in carbonate[J].Spectroscopy and Spectral Analysis,2015,35(6):1741-1745.
[3]戴尽璇，黄赛杰，徐立高．微波消解-原子吸收分光光度法测定海洋沉积物中的铜、锌、铅、镉、铬[J]．化工时刊，2017,31(9):20-25.Dai J X,Huang S J,Xu L G. Determination of copper,zinc,chrome,chromium and cadmium in marine sediment by graphite furnace atomic absorption spectrophotometry with microwave digestion[J]. Chemical Industry Times,2017,31(9):20-25.
[4]卢兵，杜少文，盛红宇，等．AAS、ICP-AES、ICP-MS及XRF测定地质样品中铜铅锌锰的对比研究[J]．黄金，2014,35(9):78-81.Lu B,Du S W,Sheng H Y,et al. Contrast research on determination of Cu,Pb,Zn,Mn by AAS,ICP-AES,ICP-MS and XRF in geological samples[J]. Gold,2014,35(9):78-81.
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[8] Khorge C R,Patwardhan A A. Separation and determination of REEs and Y in columbite-tantalite mineral by ICP-OES:A rapid approach[J]. Atomic Spectroscopy,2018,39(2):75-80.
[9] Barros J A V A,Alex V,Schiavo D,et al. Determination of ultra-trace levels of Mo in plants by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)[J]. Microchemical Journal,2017,133:567-571.
[10] Yang B,Duan F M,Ding J L,et al. Determination of heavy metals in tobacco by ICP-MS and analysis of uncertainty[J]. Asian Agricultural Research,2016,8(10):51-54.
[11]赵志南，严冬，何群华，等．ICP-MS测定《全国土壤污染状况详查》项目中14种元素[J]．环境化学，2017,36(2):448-452.Zhao Z N,Yan D,He Q H,et al. Determination of 14elements in China Soil Pollution Survey by ICP-MS[J]. Environmental Chemistry,2017,36(2):448-452.
[12] Ahmed M,Chin Y H,Guo X X,et al. Microwave assisted digestion followed by ICP-MS for determination of trace metals in atmospheric and lake ecosystem[J]. Journal of Environmental Sciences,2017,55:1-10.
[13] Satyanarayanan M,Balaram V,Sawant S S,et al. Rapid determination of REEs,PGEs,and other trace elements in geological and environmental materials by high resolution inductively coupled plasma mass spectrometry[J].Atomic Spectroscopy,2018,39(1):1-15.
[14] Chen S Z,Zhu S P,Lu D B. Dispersive micro-solid phase extraction coupled with dispersive liquid-liquid microextraction for speciation of antimony in environmental water samples by electrothermal vaporization ICP-MS[J]. Atomic Spectroscopy,2018,39(2):55-61.
[15]王佳翰，冯俊，王达成，等．电感耦合等离子体质谱法测定地球化学样品中钼镉钨铀锡[J]．冶金分析，2017,37(6):20-25.Wang J H,Feng J,Wang D C,et al. Determination of molybdenum,cadmium,tungsten,uranium and tin in geochemical samples by inductively coupled plasma mass spectrometry[J]. Metallurgical Analysis,2017,37(6):20-25.
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[18]乔军，佟克兴，李安．电感耦合等离子体质谱(ICPMS)法测定葡萄酒中的铜、镉、铅[J]．中国无机分析化学，2017,7(4):33-36.Qiao J,Tong K X,Li A. Determination of copper,cadmium,lead in wine by inductively coupled plasma mass spectrometry(ICP-MS)[J]. Chinese Journal of Inorganic Analytical Chemistry,2017,7(4):33-36.
[19]宋阳，李现忠，黄文氢，等．ICP-MS技术在石油化工中的应用[J]．石油化工，2016,45(10):1279-1287.Song Y,Li X Z,Huang W Q,et al. Application of ICPMS in petrochemical industry[J]. Petrochemical Technology,2016,45(10):1279-1287.
[20]王静，王鑫，耿哲，等．碰撞池-电感耦合等离子体质谱测定海水重金属[J]．环境工程学报，2016,10(4):2139-2143.Wang J,Wang X,Geng Z,et al. Determination of heavy metal in marine waters by collision cell inductively coupled plasma mass spectrometry[J]. Chinese Journal of Environmental Engineering, 2016, 10(4):2139-2143.
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