摘要
建立了微波消解-电感耦合等离子体原子发射光谱(ICP-AES)法同时测定土壤中多种主次元素的分析方法。采用硝酸-氢氟酸-双氧水体系在微波消解仪中消解土壤样品,待消解完成后加入高氯酸驱赶氢氟酸,盐酸溶解盐类物质,将土壤中所有元素的矿物晶格破坏使待测溶液全部进入试液,采用ICP-AES法测定。通过筛选合适分析谱线和合理设置背景扣除位置提高样品分析中的精密度和准确度。选用国家土壤标准物质进行方法验证,绝大多数实验结果与标准值吻合,相对标准偏差(RSD)小于5%。方法具有同时测定土壤样品中多种元素、试剂用量少、操作简单等优点,表明方法适合大批量土壤中主次元素的快速检测。
An analytical method for the simultaneous determination of various main and secondary elements in soil by microwave digestion-inductively coupled plasma emission spectrometry was established.The nitrogen-hydrofluoric acid-hydrogen peroxide water system was used to digest soil samples in the microwave ablator.After digestion,added perchloric acid to drive hydrofluoric acid,added hydrochloricacid to dissolve the salt material,and the mineral lattice of all elements in the soil were destroyed.All the solution to be tested entered the test liquid,then determined by inductively coupled plasma emission spectroscopy.The precision and accuracy of sample analysis were improved by screening suitable analytical lines and setting reasonable background deduction positions.The National soil standard material was used to verify the method.Most of the experimental results were consistent with the standard value,and the RSD was less than 5%.The method has the advantages of simultaneous determination of various elements,less reagent use,and simple operation,which indicates that the method is suitable for rapid detection of main and secondary elements in large amounts soil.
引文
[1]杨苏才,南忠仁,曾静静.土壤重金属污染现状与治理途径研究进展[J].安徽农业科学(Anhui Journal of Agricultural Science),2006,34(3):549-552.
[2]孙鹏,刘海涛,李崇江,等.电热蒸发-直接进样-冷原子吸收光谱法测定土壤以及沉积物中汞[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2018,8(1):6-10.
[3]杨丽华.微波消解ICP-MS法测定土壤中的十种金属元素[J].福建分析测试(Fujian Journal of Analytical Testing),2017,26(2):59-62.
[4]盖荣银,孙友宝,马晓玲,等.二乙烯三胺五乙酸提取结合火焰原子吸收光谱法测定土壤中的有效态元素[J].环境化学(Journal of Environmental Chemistry),2016,35(5):1096-1097.
[5]张艳,吴峥,张飞鸽,等.电感耦合等离子体原子发射光谱法测定锰矿石中主次量元素[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2014,4(1):41-45.
[6]REHAN I,GONDAL M A,REHAN K.Determination of lead content in drilling fueled soil using laser induced spectral analysis and its cross validation using ICP-OES method[J].Talanta,2018,182:443-449.
[7]吴永盛,徐金龙,庄姜云,等.微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定土壤中8种重金属元素[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2017,7(4):16-20.
[8]李刚,胡斯宪,陈琳玲.原子荧光光谱分析技术的创新与发展[J].岩矿测试(Rock and Minera lAnalysis),2013,32(3):358-376.
[9]杨远,邓飞跃,肖立青,等.湿法消解-电感耦合等离子体发射光谱法测定烟叶中22种元素[J].中国烟草学报(Chinese Journal of Tobacco),2013(3):11-17.