| 高压密闭消解-电感耦合等离子体光谱和质谱联合测定海洋地质样品中52种元素 |
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| 引用本文： | 高晶晶,刘季花,李先国,鄢全树,王小静,汪虹敏.高压密闭消解-电感耦合等离子体光谱和质谱联合测定海洋地质样品中52种元素[J].海洋学报(英文版),2017,36(1):109-117. |
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| 作者姓名： | 高晶晶 刘季花 李先国 鄢全树 王小静 汪虹敏 |
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| 作者单位： | 中国海洋大学, 海洋化学理论与工程技术教育部重点实验室, 青岛 266100;国家海洋局第一海洋研究所, 海洋沉积与环境地质国家海洋局重点实验室, 青岛 266061;青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室, 青岛 266061,国家海洋局第一海洋研究所, 海洋沉积与环境地质国家海洋局重点实验室, 青岛 266061;青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室, 青岛 266061,中国海洋大学, 海洋化学理论与工程技术教育部重点实验室, 青岛 266100,国家海洋局第一海洋研究所, 海洋沉积与环境地质国家海洋局重点实验室, 青岛 266061;青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室, 青岛 266061,国家海洋局第一海洋研究所, 海洋沉积与环境地质国家海洋局重点实验室, 青岛 266061;青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室, 青岛 266061,国家海洋局第一海洋研究所, 海洋沉积与环境地质国家海洋局重点实验室, 青岛 266061;青岛海洋科学与技术国家实验室海洋地质过程与环境功能实验室, 青岛 266061 |
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| 基金项目： | The China Ocean Mineral Resources Research and Development Association Research Program of the State Oceanic Administration of China under contract No. DY125-13-R-07; the National Natural Science Foundation of China under contract Nos 41322036 and 41230960; the Shandong Provincial Natural Science Foundation of China under contract No. ZR2014DP009; the Special Basic Research Funds for Central Public Research Institutes for The First Institute of Oceanography, State Oceanic Administration of China under contract Nos GY0213G06 and GY02-2012G35. |
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| 摘 要： | An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method(HPCD), is studied by an inductively coupled plasma optical emission spectrometry(ICP-OES) and an inductively coupled plasma mass spectrometry(ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error(RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials(GBW07309, GBW07311, GBW07313), rock reference materials(GBW07103, GBW07104,GBW07105), and cobalt-rich crust reference materials(GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation(RSD) and the relative error(RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.
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| 关 键 词： | 海洋地质样品 高压密闭消解 电感耦合等离子体光谱 电感耦合等离子体质谱 常量元素 微量元素 痕量元素 |
| 收稿时间： | 2015/11/16 0:00:00 |
| 修稿时间： | 2016/3/14 0:00:00 |
The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method |
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| GAO Jingjing,LIU Jihu,LI Xianguo,YAN Quanshu,WANG Xiaojing and WANG Hongmin.The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method[J].Acta Oceanologica Sinica,2017,36(1):109-117. |
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| Authors: | GAO Jingjing LIU Jihu LI Xianguo YAN Quanshu WANG Xiaojing and WANG Hongmin |
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| Institution: | Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, Qingdao 266100, China;Key Laboratory of Marine Sedimentary and Environmental Geology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;Laboratory for Marine Geology, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266061, China,Key Laboratory of Marine Sedimentary and Environmental Geology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;Laboratory for Marine Geology, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266061, China,Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, Qingdao 266100, China,Key Laboratory of Marine Sedimentary and Environmental Geology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;Laboratory for Marine Geology, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266061, China,Key Laboratory of Marine Sedimentary and Environmental Geology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;Laboratory for Marine Geology, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266061, China and Key Laboratory of Marine Sedimentary and Environmental Geology, The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China;Laboratory for Marine Geology, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266061, China |
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| Abstract: | An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO3 acid system with a high-pressure closed digestion method (HPCD), is studied by an inductively coupled plasma optical emission spectrometry (ICP-OES) and an inductively coupled plasma mass spectrometry (ICP-MS). The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion, less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO3 system, the relative error (RE) for the analytical results are all less than 6.0%. The method detection limits are 2–40 μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials (GBW07309, GBW07311, GBW07313), rock reference materials (GBW07103, GBW07104, GBW07105), and cobalt-rich crust reference materials (GBW07337, GBW07338, GBW07339), the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation (RSD) and the relative error (RE) are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples. |
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| Keywords: | marine geological sample high-pressure closed digestion method inductively coupled plasma optical emission spectrometry inductively coupled plasma mass spectrometry major element minor element trace element |
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