Determination of copper, lead, zinc, cadmium, chromium, nickel and arsenic in road dust by inductively coupled plasma mass spectrometry with acid digestion in closed system
1. Hebei Research Center for Geoanalysis, Baoding 071051, China; 2. Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Hebei Province, Baoding 071051, China
Abstract:The accurate determination of heavy metals (Cu, Pb, Zn, Cd, Cr, Ni and As) in road dust samples is of great significance for the prevention and control of environmental pollution in urban roads. The samples were digested by acid dissolution in closed system in HF-HNO3 system. 52Cr, 60Ni, 63Cu, 66Zn, 75As, 111Cd and 208Pb were selected as the measuring isotopes. The contents of Cr and As were determined by collision reaction cell technique using mode of He. The determination results of Cd were corrected by the interference correction equation equipped in the instrument. Consequently, the determination method of Cu, Pb, Zn, Cd, Cr, Ni and As in road dust samples by inductively coupled plasma mass spectrometry (ICP-MS) was established. The sample dissolution conditions were optimized. The results showed that 0.1 g of sample could be fully dissolved by 7.0 mL of mixed acid (HF∶HNO3=1∶6, volume ratio) after digestion in closed system at 160 ℃ for 2 h. Under the optimized experimental conditions, the correlation coefficient of the calibration curve was higher than 0.999. The limit of detection ranged from 0.012 to 0.096 μg/g, and the limit of quantification was between 0.040 μg/g and 0.32 μg/g. The proposed method was applied to the determination of Cu, Pb, Zn, Cd, Cr, Ni and As in road dust samples. Moreover, the spiked recovery tests were also conducted. The relative standard deviations (RSD, n=12) of determination results were all less than 4%, and the spiked recoveries were between 95% and 104%. The road dust samples were analyzed according to the experimental method. The measurement results were basically consistent with those obtained by high-pressure microwave digestion-ICP-MS for Cu, Pb, Zn, Cd, Cr and Ni, and hydride generation atomic fluorescence spectrometry (HG-AFS) for As.
[1] 武媛媛,李如梅,彭林,等.运城市道路扬尘化学组成特征及来源分析[J].环境科学,2017,38(5):1799-1806. WU Yuanyuan,LI Rumei,PENG Lin,et al.Chemical compositions and source apportionment of road dust in Yuncheng[J]. Environmental Science,2017,38(5):1799-1806. [2] 张金,姬亚芹,邢雅彤,等.天津市高校夏季道路扬尘PM2.5中水溶性离子污染特征及来源[J].环境科学学报,2020,40(5):1604-1610. ZHANG Jin,JI Yaqin,XING Yatong,et al.Characteristics and sources of water-soluble ions in road dust PM2.5 during summer in university campuses of Tianjin[J].Acta Scientiae Circumstantiae,2020,40(5):1604-1610. [3] 郭广慧,雷梅,陈同斌,等.交通活动对公路两侧土壤和灰尘中重金属含量的影响[J].环境科学学报,2008,28(10):1937-1945. GUO Guanghui,LIE Mei,CHEN Tongbin,et al.Effect of road traffic on heavy metals in road dusts and road side soils[J].Acta Scientiae Circumstantiae,2008,28(10):1937-1945. [4] 陈波,刘洪青,邢应香.电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J].岩矿测试,2014,33(2):192-196. CHEN Bo,LIU Hongqing,XING Yingxiang.Simultaneous determination of Ge, Se and Te in geological samples by inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2014,33(2):192-196. [5] 程秀花,黎卫亮,王海蓉.封闭酸溶样ICP-MS法直接测定地质样品中镓、铟、铊、锗[J].分析试验室,2015,34(10):1204-1208. CHENG Xiuhua,LI Weiliang,WANG Hairong.Determination of gallium, indium, thallium and germanium in geological samples after pressurized acid digestion by inductively coupled plasma mass spectrometry[J].Chinese Journal of Analysis Laboratory,2015,34(10):1204-1208. [6] 李冰,马新荣,杨红霞,等.封闭酸溶-电感耦合等离子体原子发射光谱法同时测定地质样品中硼砷硫[J].岩矿测试,2003,22(4): 241-247. LI Bing,MA Xinrong,YANG Hongxia,et al.Determination of boron,arsenic and sulfur in geological samples by inductively coupled plasma atomic emission spectrometry with sample treatment by pressurized decomposition[J].Rock and Mineral Analysis,2003,22(4): 241-247. [7] 马生凤,温宏利,马新荣,等,四酸溶样-电感耦合等离子体原子发射光谱法测定铁、铜、锌、铅等硫化物矿石中22个元素[J]矿物岩石地球化学通报,2011,30(1):65-72. MA Shengfeng,WEN Hongli,MA Xinrong,et al.Determination of 22 elements in iron, copper, zinc, and lead sulphide ores by ICP-AES with four acids digestion[J].Bulletin of Mineralogy, Petrology and Geochemistry,2011,30 (1):65-72. [8] 彭杨,吴婧,巢静波,等.土壤/沉积物中14种金属元素的 ICP-MS 准确测定方法[J].环境化学,2017,36(1):175-182. PENG Yang,WU Jing,CHAO Jingbo,et al.A method for the the accurate determination of 14 metal elements in soils/sediments by ICP-MS[J].Environmental Chemistry,2017,36(1):175-182. [9] 边朋沙,李晓敬,申玉民,等.电感耦合等离子体质谱法测定地质样品中痕量碲[J].冶金分析,2018,38(6): 25-30. BIAN Pengsha,LI Xiaojing,SHEN Yumin,et al.Determination of trace tellurium in geological sample by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2018,38(6):25-30. [10] 赵朝辉,李可及,邹利平,等.ICP-MS同时测定土壤样品中的镓铟锗[J].矿产综合利用,2012(3):52-54. ZHAO Chaohui,LI Keji,ZOU Liping,et al.Simultaneous determination of Ga,In and Ge in soil samples by ICP-MS[J].Multipurpose Utilization of Mineral Resources,2012(3):52-54. [11] 李晓敬,边朋沙,金倩,等.高压微波消解-电感耦合等离子体质谱法测定地质样品中分散元素镓铟铊锗碲镉[J]冶金分析,2019,39(4): 38-44. LI Xiaojing,BIAN Pengsha,JIN Qian,et al.Determination of disperse elements of gallium, indium, thallium, germanium, tellurium and cadmium in geological samples by inductively coupled plasma mass spectrometry with high-pressure microwave digestion[J].Metallurgical Analysis,2019,39(4):38-44. [12] 王佳翰,李正鹤,杨峰,等.偏硼酸锂碱熔-电感耦合等离子体质谱法同时测定海洋沉积物中48种元素[J].岩矿测试,2021,40(2):306-315. WANG Jiahan,LI Zhenghe,YANG Feng,et al.Simultaneous determination of 48 elements in marine sediments by ICP-MS with lithium metaborate fusion[J].Rock and Mineral Analysis,2021,40(2):306-315. [13] 李冰,杨红霞.电感耦合等离子体质谱原理和应用[M].北京:地质出版社,2005:98-100. [14] 岩石矿物分析编委会.岩石矿物分析[M].4版.北京:地质出版社,2011.