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GAO Jingjing,LIU Jihua,LI Xianguo,YAN Quanshu,WANG Xiaojing,WANG Hongmin. 2017. 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. Acta Oceanologica Sinica, 36(1):109－117

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

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

Received:November 16, 2015 Revised:March 14, 2016

DOI：10.1007/s13131-017-0991-5

Key words: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

中文关键词: 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

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.

Author Name	Affiliation	E-mail
GAO Jingjing	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
LIU Jihua	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	jihliu@fio.org.cn
LI Xianguo	Key Laboratory of Marine Chemistry Theory and Technology of Ministry of Education, Ocean University of China, Qingdao 266100, China
YAN Quanshu	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
WANG Xiaojing	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
WANG Hongmin	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.

中文摘要:

建立了硝酸-盐酸-氢氟酸高压密闭消解样品，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个常量、微量、痕量元素的方法。实验优化了仪器工作参数，确定了最佳测定条件。考察了光谱和质谱干扰、消解方法和酸体系对元素测定结果的影响。选择了分析元素的最佳分析谱线和同位素，选取了Rh作为内标元素，以补偿基体效应和分析信号的漂移。相比于电热板消解法和微波消解法，高压密闭消解法具有酸用量少，消解完全，消解过程损失少等优点。硝酸-盐酸-氢氟酸体系能有效地分解海洋地质样品，测定结果的相对误差均低于6%。方法检出限：ICP-OES为2~40 μg·g-1，ICP-MS为6~80ng·g-1。所建立的分析方法用于海洋沉积物标准物质（GBW07309、GBW07311、GBW07313）、岩石标准物质（GBW07103、GBW07104、GBW07105）和富钴结壳标准物质（GBW07337、GBW07338、GBW07339）的验证，测定值与标准值吻合，其相对标准偏差和相对误差均小于6%。该分析方法适用于大批海洋地质样品中52种元素的测定。

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