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
-
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。
-
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
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. -
Álvarez M B, Garrido M, Lista A G, et al. 2008. Three-way multivariate analysis of metal fractionation results from sediment samples obtained by different sequential extraction procedures and ICP-OES. Anal Chim Acta, 620(1-2):34-43 Barreto S R G, Nozaki J, De Oliveira E, et al. 2004. Comparison of metal analysis in sediments using EDXRF and ICP-OES with the HCl and Tessie extraction methods. Talanta, 64(2):345-354 Chand V, Prasad S. 2013. ICP-OES assessment of heavy metal contamination in tropical marine sediments:a comparative study of two digestion techniques. Microchem J, 111:53-61 Cruz S M, Schmidt L, Nora F M D, et al. 2015. Microwave-induced combustion method for the determination of trace and ultratrace element impurities in graphite samples by ICP-OES and ICP-MS. Microchem J, 123:28-32 de Sousa Á S, Ferreira E M M, Cassella R J. 2008. Development of an integrated flow injection system for the electro-oxidative leaching of uranium from geological samples and its spectrophotometric determination with Arsenazo III. Anal Chim Acta, 620(1-2):89-96 Dolor M K, Helz G R, McDonough W F. 2009. Sediment profiles of less commonly determined elements measured by Laser Ablation ICP-MS. Mar Pollut Bull, 59(4-7):182-192 Feist B, Mikula B, Pytlakowska K, et al. 2008. Determination of heavy metals by ICP-OES and F-AAS after preconcentration with 2, 2'-bipyridyl and erythrosine. J Hazard Mater, 152(3):1122-1129 Frena M, Quadros D P C, Castilho I N B, et al. 2014. A novel extraction-based procedure for the determination of trace elements in estuarine sediment samples by ICP-MS. Microchem J, 117:1-6 Gao Jingjing, Liu Jihua, Qiao Shuqing, et al. 2010. Determination of major and minor elements in oceanic sediments by ICP-OES.Chin J Spectr Lab (in Chinese), 27(3):1050-1054 Gao Jingjing, Liu Jihua, Zhang Hui, et al. 2012. Determination of rare earth elements in the marine sediments by inductively coupled plasma-mass spectrometry with high-pressure closed digestion. Rock Miner Anal (in Chinese), 31(3):425-429 Gao Jingjing, Zhu Aimei, Bai Yazhi, et al. 2013. Determination of fifty elements in cobalt-rich crusts by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry. Adv Mar Sci (in Chinese), 31(3):398-405 Hein J R, Spinardi F, Okamoto N, et al. 2015. Critical metals in manganese nodules from the Cook Islands EEZ, abundances and distributions. Ore Geol Rev, 68:97-116 Hu Ningjing, Huang Peng, Liu Jihua, et al. 2015. Tracking lead origin in the Yellow River Estuary and nearby Bohai Sea based on its isotopic composition. Estuar Coast Shelf Sci, 163:99-107 Hu Shenghong, Wang Xiuji, Ge Wen, et al. 2004. Simultaneous determination of major-to-ultratrace elements in the oceanic polymetallic nodules materials by inductively coupled plasma mass spectrometry combined with inductively coupled plasma optical emission spectrometry. Chin J Anal Chem (in Chinese), 32(9):1139-1144 Landajo A, Arana G, de Diego A, et al. 2004. Analysis of heavy metal distribution in superficial estuarine sediments (estuary of Bilbao, Basque Country) by open-focused microwave-assisted extraction and ICP-OES. Chemosphere, 56(11):1033-1041 Li Chuanshun, Shi Xuefa, Kao Shunji, et al. 2013. Rare earth elements in fine-grained sediments of major rivers from the highstanding island of Tai wan. J Asian Earth Sci, 69:39-47 Lunderberg J M, Bartlett R J, Behm A M, et al. 2008. PIXE as a complement to trace metal analysis of sediments by ICP-OES. NuclInstrum Methods Phys ResSect B Beam Interac Mater Atoms, 266(21):4782-4787 Papaefthymiou H, Papatheodorou G, Christodoulou D, et al. 2010.Elemental concentrations in sediments of the Patras Harbour, Greece, using INAA, ICP-MS and AAS. Microchem J, 96(2):269-276 Pinho J, Canário J, Cesário R, et al. 2005. A rapid acid digestion method with ICP-MS detection for the determination of selenium in dry sediments. Anal Chim Acta, 551(1-2):207-212 Qiao Shuqing, Shi Xuefa, Gao Jingjing, et al. 2013. The distribution and variation of elements in sediments off the Huanghe (Yellow) River mouth. Chin J Oceanol Limnol, 31(4):876-885 Röllin S, Sahli H, Holzer R, et al. 2009. PU and NP analysis of soil and sediment samples with ICP-MS. Appl RadIsot, 67(5):821-827 Tarafder P K, Thakur R. 2005. Surfactant-mediated extraction of iron and its spectrophotometric determination in rocks, minerals, soils, stream sediments and water samples. Microchem J, 80(1):39-43 Yan Quanshu, Castillo P, Shi Xuefa, et al. 2015. Geochemistry and petrogenesis of volcanic rocks from Daimao Seamount (South China Sea) and their tectonic implications. Lithos, 218-219:117-126
点击查看大图
计量
- 文章访问数: 1046
- HTML全文浏览量: 76
- PDF下载量: 834
- 被引次数: 0