Determination of 18 Elements in Soil by Combined System of Super Microwave Digestion and Automatic Heavy Metal Analysis
摘 要
以超级微波消解-全自动重金属分析联用系统测定土壤中18种元素(锂、铍、钒、铬、锰、钴、镍、铜、锌、砷、钼、银、镉、锑、铊、铅、铋、铀)的含量。取0.1 g土壤于消解管中,将消解管加载至上述联用系统,按照以下步骤自动完成加酸、消解、稀释、测定:加入1 mL水润湿样品,再加入1.5 mL硝酸、0.5 mL盐酸和0.5 mL氢氟酸,并程序升温至260℃,保温30 min;冷却、泄压、用水稀释后,用电感耦合等离子体质谱法测定。结果表明:18种目标元素的质量浓度均在一定范围内与其对应的信号强度与内标元素铑信号强度的比值呈线性关系,检出限(3s)为0.001~0.300 μg·L-1;方法用于土壤成分分析标准物质GSS-2、GSS-13和GSS-27的分析,测定值均在认定值的不确定度范围内,其相对标准偏差(n=6)为1.3%~5.3%。方法消解用酸量仅为HJ 803-2016的50%,且自动化程度高、分析快速,适用于大批量土壤样品的分析。
Abstract
A combined system of super microwave digestion and automatic heavy metal analysis was applied to determination of 18 elements (Li, Be, V, Cr, Mn, Co, Ni, Cu, Zn, As, Mo, Ag, Cd, Sb, Tl, Pb, Bi, U) in soil. The soil of 0.1 g was taken and loaded on the above combined system to automatically complete acid addition, digestion, dilution and determination as the following steps:1 mL of water was added to wet the sample, then 1.5 mL of nitric acid, 0.5 mL of hydrochloric acid, and 0.5 mL of hydrofluoric acid were added, and the mixture was heated to 260℃ by program temperature and kept for 30 min; after cooling, depressurization, and dilution with water, inductively coupled plasma mass spectrometry was used for determination. It was shown by the results, the mass concentrations of 18 target elements were linearly related to their corresponding signal intensity ratios between target element and internal standard element of Rh in definite ranges, with detection limits (3s) in the range of 0.001-0.300 μg·L-1; the proposed method was used for the analysis of standard substances for soil composition analysis (GSS-2, GSS-13 and GSS-27), and the determined values were in the uncertainty ranges of the certified values, with RSDs (n=6) of the determined values in the range of 1.3%-5.3%. The amount of acid used for digestion was only 50% of that of HJ 803-2016, and the method had a high degree of automation and rapid analysis, which was suitable for the analysis of large batches of soil samples.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202205005
所属栏目 工作简报
基金项目 杭州市重大科技创新项目(20182011A25)
收稿日期 2021/1/12
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备注张维权,工程师,硕士,主要研究方向为样品前处理及质谱分析,13067966573@163.com
引用该论文: ZHANG Weiquan,LU Shuimiao,XIA Xiaofeng,NI Dazhao,LI Ying,LI Jian. Determination of 18 Elements in Soil by Combined System of Super Microwave Digestion and Automatic Heavy Metal Analysis[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(5): 523~527
张维权,卢水淼,夏晓峰,倪大钊,李鹰,李剑. 超级微波消解-全自动重金属分析联用系统测定土壤中18种元素的含量[J]. 理化检验-化学分册, 2022, 58(5): 523~527
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参考文献
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【3】侯鹏飞,江冶,曹磊.土壤样品石墨消解法在ICP-MS分析中的应用[J].安徽地质, 2020,30(3):233-236.
【4】李媛媛,纪轶.微波消解技术在环境化学分析中的应用研究[J].中国资源综合利用, 2020,38(10):74-76.
【5】杨叶琴,赵昌平,赵杰.微波消解-电感耦合等离子体原子发射光谱法测定土壤中8种重金属元素的含量[J].理化检验-化学分册, 2019,55(1):63-67.
【6】卢丽,刘二龙,詹业添,等.超级微波消解-电感耦合等离子体发射光谱测定小麦中总铝含量[J].食品安全质量检测学报, 2018,9(3):564-569.
【7】赵一霖,霍霈霖,李吉龙,等.超级微波消解-电感耦合等离子体发射光谱/质谱法高效测定不同基质食品中27种矿物质元素[J].食品安全质量检测学报, 2018,9(10):2404-2410.
【8】孙杰,吴玥,蒋沄泱,等.稀酸酸解-电感耦合等离子体质谱法测定土壤中14种无机元素的含量[J].理化检验-化学分册, 2017,53(3):315-321.
【9】王雪枫,李湘,康文贵.碱性溶液微波消解-氢化物发生-原子荧光光谱法测定土壤中锡[J].理化检验-化学分册, 2020,56(3):344-348.
【10】赵翊,聂融,魏静,等.超级微波消解-电感耦合等离子体质谱法测定PM2.5滤膜中6种痕量重金属[J].疾病预防控制通报, 2016,31(5):66-68.
【11】张守杰,乔晴,邢荣花,等.H2O2-超级微波消解-ICP-MS法测定乳粉中铅含量[J].中国口岸科学技术, 2020(2):32-37.
【12】MULLER E I, SOUZA J P, MULLER C C, et al. Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-AES and ICP-MS[J]. Talanta, 2016,156/157:232-238.
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【17】苏子鹏,叶剑芝,杨春亮,等.溶液酸度对ICP-MS测定大米中镉和铜的影响[C]//农产品质量安全与现代农业发展专家论坛论文集.北京:[出版者不详], 2011:202-206.
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