刘瑶^1,2, 刘瑾^1,2, 孙玲玲^1,2, 孙萱^1,2, 宋金明^1,2,3,4
1.中国科学院 海洋研究所 所级公共技术中心, 山东 青岛 266071;2.中国科学院 海洋大科学中心, 山东 青岛 266071;3.青岛海洋国家实验室 海洋生态与环境科学功能实验室, 山东 青岛 266237;4.中国科学院海洋研究所 海洋生态与环境科学重点实验室, 山东 青岛 266071

摘要:
准确测定海洋沉积物中重金属元素的含量，对于健康海洋的监测、维护和治理具有重要的指导意义。本文报道了电感耦合等离子体质谱法（ICP-MS）同时测定海洋沉积物中铜、锌、铅和镉四种元素微波密闭消解条件的正交试验优化结果。运用正交试验法，选取L₁₆（4⁵）正交表，按五因素四水平安排试验，研究不同酸体系和配比下，以及不同微波消解条件下沉积物样品的消解效果。经极差分析及方差分析后，得到海洋沉积物样品在称样量为0.05 g左右（精确到±0.000 1 g）情况下，最佳消解条件为HNO₃（体积分数69%）用量6.0 mL、H₂O₂（体积分数30%）用量3.0 mL、HF（体积分数49%）用量3.0 mL、第三步程序消解温度190℃、保温时间15 min。结果表明，正交优化后的方法准确度高，对三种有证海洋沉积物标准物质的测试均在标准值范围内；回收率好，各元素回收率在91.52%~107.55%之间；精密度高，重复性好，重复性的相对标准偏差为1.29%~8.21%；方法检出限低，各元素方法定量下限为0.005~0.057 μg/g。该方法准确可靠，满足海洋沉积物样品中铜、锌、铅和镉等元素含量准确测定的测试需求。
关键词:正交试验优化微波消解重金属海洋沉积物ICP-MS测定
DOI：10.11759/hykx20200824003
分类号:0657.63
基金项目:中国科学院战略性先导科技专项项目（XDA23050501）；山东省重大科技创新工程专项项目（2018SDKJ0504-1）

Optimization of microwave digestion conditions for determination of heavy metals in marine sediments by ICP-MS
LIU Yao^1,2, LIU Jin^1,2, SUN Ling-ling^1,2, SUN Xuan^1,2, SONG Jin-ming^1,2,3,4
1.Analytical Center of Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China;2.Center for Ocean Mega-Science, Chinese Academy of Sciences, Qingdao 266071, China;3.Laboratory for Marine Ecology and Environmental Science, Qingdao National Laboratory for Marine Science and Technology, Qingdao 266237, China;4.Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China
Abstract:
Accurate determination of heavy metals in marine sediments is of great significance for monitoring, maintaining, and managing healthy oceans. In this paper, the orthogonal test results of microwave digestion conditions for the simultaneous determination by inductively coupled plasma mass spectrometry (ICP-MS) of copper, zinc, lead, and cadmium in marine sediments have been reported. Using the orthogonal test method, L₁₆ (4⁵) orthogonal table was selected to study the digestion effect of sediment samples under different acid systems and ratios and under different microwave digestion conditions. After range analysis and variance analysis, the optimal digestion conditions were as follows:the added volume of HNO₃, H₂O₂, and HF were 6.0 mL, 3.0 mL, and 3.0 mL, respectively; the digestion temperature was 190℃, and the digestion time was set to 15 min. The results showed that the accuracy of the method after orthogonal optimization was high, and the test results of three certified marine sediment reference materials were all within the standard value range. The recovery rate was good, and the recovery rate of each element was 91.52%-107.55%; High precision and good repeatability, the relative standard deviation of repeatability was 1.29%-8.21%; Low detection limit of the method, the quantitative limit of each element was 0.005-0.057 μg/g. The method is accurate and reliable and can meet the requirements for accurate copper, zinc, lead, and cadmium determination in samples of marine sediments.
Key words:orthogonal experiment optimizationmicrowave digestionheavy metalsmarine sedimentsICP-MS determination





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