Abstract:Mercury and arsenic belong to the controlled elements in soil environmental quality monitoring. Due to the great difference in content between two elements, it is difficult to accurately determine them simultaneously by hydride generation-atomic fluorescence spectrometry. If inductively coupled plasma atomic emission spectrometry (ICP-AES) are employed to determine arsenic and mercury, the problem is that the sensitivity is low.A simple hydride generation device combined with inductively coupled plasma atomic emission spectrometer (HG-ICP-AES) was self-made for the simultaneous determination of mercury and arsenic in soil. The soil sample was digested with aqua regia (1+1). The acidity of sample solution was kept at 15% containing 15 g/L potassium borohydride as the reducing agent. The optimal working conditions of ICP-AES were as follows: the incident power was 1 450 W, the peristaltic pump speed was 1.7 mL/min, the plasma gas flow was 16 L/min, and the atomizing gas flow was 0.45 L/min. The linear range of mercury and arsenic was 0.50-10.0 μg/L and 5.00-100 μg/L, respectively. The linear correlation coefficients were both 0.999 8. The limits of detection of mercury and arsenic were 0.016 μg/g and 0.12 μg/g, and limits of quantification were 0.064 μg/g and 0.48 μg/g, respectively. The contents of mercury and arsenic in certified reference materials and actual samples of soil were determined according to the experimental method. The measured values of reference materials were consistent with the certified values. The relative standard deviations (RSD, n=6) of determination results for the actual sample were between 3.1% and 4.8%. Meanwhile, the contents of mercury and arsenic in actual sample of soil were determined according to the experimental method and atomic fluorescence spectrometry. The t test indicated that the determination results of two methods had no significant difference. The proposed method was suitable for the simultaneous determination of mercury and arsenic in soil.
王记鲁, 郝苗青, 李静, 王鑫, 刘跃. 氢化物发生-电感耦合等离子体原子发射光谱法测定土壤中汞和砷[J]. 冶金分析, 2023, 43(5): 74-78.
WANG Jilu, HAO Miaoqing, LI Jing, WANG Xin, LIU Yue. Determination of mercury and arsenic in soil by hydride generation- inductively coupled plasma atomic emission spectrometry. , 2023, 43(5): 74-78.
[1] 孙晶,李伟,吕学斌,等.中国重要湿地土壤中汞、砷的分布与污染概况[J].环境科学与技术,2021,44(9):100-110. SUN Jing,LI Wei,LÜ Xuebin,et al.Distribution and pollution situation of mercury and arsenic in important wetlands soil in China[J].Environmental Science & Technology,2021,44(9):100-110. [2] 贺攀红,杨珍,荣耀,等.氢化物发生-电感耦合等离子体原子发射光谱法测定尾矿渣固体废物水浸出液中痕量铅[J].冶金分析,2014,34(7):43-46. HE Panhong,YANG Zhen,RONG Yao,et al.Determination of trace lead in leaching solution of tailings solid waste by hydride generation-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(7):43-46. [3] 傅慧敏,周益奇,王巧环.氢化物发生电感耦合等离子体原子发射光谱同时测定土壤中十四种微量元素[J].环境化学,2013,32(6):1094-1095. FU Huimin,ZHOU Yiqi,WANG Qiaohuan.Simultaneous determination of 14 trace elements in soil by hydride generation inductively coupled plasma atomic emission spectrometry[J].Environmental Chemistry,2013,32(6):1094-1095. [4] 吴峥,熊英,王龙山.自制氢化物发生系统与电感耦合等离子体发射光谱法联用测定土壤和水系沉积物中的砷锑铋[J].岩矿测试,2015,34(5):533-538. WU Zheng,XIONG Ying,WANG Longshan.Determination of As, Sb and Bi in soil and stream sediment by a selfdeveloped hydride generation system coupled with inductively coupled plasma-optical emission spectrometry[J].Rock and Mineral Analysis,2015,34(5):533-538. [5] 贺攀红,杨珍,龚治湘.氢化物发生-电感耦合等离子体发射光谱法同时测定土壤中的痕量砷铜铅锌镍钒[J].岩矿测试,2020,39(2):235-242. HE Panhong,YANG Zhen,GONG Zhixiang.Simultaneous determination of trace arsenic,copper,lead,zinc,nickel and vanadium in soils by hydride generation-inductively coupled plasma-optical emission spectrometry[J].Rock and Mineral Analysis,2020,39(2):235-242. [6] 叶建平,周西林.氢化物发生-电感耦合等离子体原子发射光谱法测定球墨铸铁中砷、锑、铋[J].理化检验(化学分册),2013,49(9):1073-1075. YE Jianping,ZHOU Xilin.HG-ICP-AES Determination of As,Sb and Bi in ductile iron[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2013,49(9):1073-1075. [7] 刘攀,李治亚,杜米芳,等.氢化物发生电感耦合等离子体发射光谱法测定钢中微量砷[J].中国测试,2021,47(1):76-81,95. LIU Pan,LI Zhiya,DU Mifang,et al.Determination of trace arsenic in steel by hydride generation inductively coupled plasma emission spectrometry[J].China Measurement and Test,2021,47(1):76-81,95. [8] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 22105—2008 土壤质量 总汞、总砷、总铅的测定 原子荧光法[S].北京:中国标准出版社,2008. [9] 生态环境部.HJ 168—2020环境监测分析方法标准制订技术导则[S].北京:中国环境科学出版社,2020. [10] 环境保护部.HJ 680—2013 土壤和沉积物 汞、砷、硒、铋、锑的测定 微波消解/原子荧光法[S].北京:中国环境科学出版社,2013. [11] 朱晓丹,王炜,魏君,等.酸化吹气-气相分子法测定固体废物中硫化物[J].中国环境监测,2021,37(3):186-191. ZHU Xiaodan,WANG Wei,WEI Jun,et al.Determination of sulfide in solid waste by acidification blowing-gaseous molecules method[J].Environmental Monitoring in China,2015,37(3):186-191.