优化BCR法-ICP-MS在土壤重金属化学形态分析中的应用
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摘要
为了研究土壤重金属元素的化学形态,以优化的BCR法模拟自然环境条件,连续提取了不同土壤标准物质中Cd、Cr、Cu、Ni、Pb、Zn的交换态、还原态、氧化态;采用微波混酸(5mL HNO_3+2 mL HCl+1 mL HF)消解土壤样品,电感耦合等离子体质谱法(ICP-MS)分析测定,在碰撞反应池模式(CCT)下以~(115)In和~(209)Bi双内标加入法进行信号漂移补偿和干扰校正;以形态分析标准参考物质(欧盟RCR-701)验证了方法的准确性。结果表明,CCT动态模式能有效地降低检测过程中多原子离子的干扰作用,检测分析方法的检出限均小于0. 2 ng/g,RSD <1. 35%(n=5),方法验证性实验说明所选方法准确可靠;土壤样品中各元素3种化学形态与残渣中含量的加和均与总量参考值接近,回收率在95%～110%之间;该法适于土壤重金属形态的提取和分析测定,对研究土壤重金属的赋存特征、迁移转化规律及影响因素、重金属元素的来源及土壤重金属污染的治理与修复有一定的指导意义。
Natural environment conditions were simulated by improved BCR method in order to study the chemical forms of heavy metals in soil and exchangeable form,reducible form,oxidable form,residual form of heavy metals( Cd,Cr,Cu,Ni,Pb,Zn) in soil certified reference material were extracted continuously. The mixed system of microwave digestion was composed of 5 mL HNO_3,2 mL HCl and 1 mL HF. Content of elements in each form was determined by inductively coupled plasma mass spectrometry. The internal standard elements ~(115)In and ~(209)Bi were used to compensate for matrix suppression effect and sensitivity drift based on the CCT model. Accuracy of the extraction method was verified using standard reference materials for speciation analysis( EU BCR701). The result showed that interference of polyatomic ions can be effectively reduced by CCT mode in the process of detection and analysis. The detection limits was less than 0. 20 ng/g and RSD < 1. 35%( n = 5). The sum of the content of each element was close to the total amount and recovery rate was 95%-110%. Results of confirmatory experiments showed that the coincidence degree was fine. Method validation experiments showed that the selected method was accurate and reliable.The method was suitable for extraction and analysis of heavy metal forms in soil. It has important guiding significance for studying the occurrence characteristics,migration and transformation rules and influencing factors of heavy metals,sources of heavy metals and remediation and remediation of heavy metal pollution in soil.
Natural environment conditions were simulated by improved BCR method in order to study the chemical forms of heavy metals in soil and exchangeable form,reducible form,oxidable form,residual form of heavy metals( Cd,Cr,Cu,Ni,Pb,Zn) in soil certified reference material were extracted continuously. The mixed system of microwave digestion was composed of 5 mL HNO_3,2 mL HCl and 1 mL HF. Content of elements in each form was determined by inductively coupled plasma mass spectrometry. The internal standard elements ~(115)In and ~(209)Bi were used to compensate for matrix suppression effect and sensitivity drift based on the CCT model. Accuracy of the extraction method was verified using standard reference materials for speciation analysis( EU BCR701). The result showed that interference of polyatomic ions can be effectively reduced by CCT mode in the process of detection and analysis. The detection limits was less than 0. 20 ng/g and RSD < 1. 35%( n = 5). The sum of the content of each element was close to the total amount and recovery rate was 95%-110%. Results of confirmatory experiments showed that the coincidence degree was fine. Method validation experiments showed that the selected method was accurate and reliable.The method was suitable for extraction and analysis of heavy metal forms in soil. It has important guiding significance for studying the occurrence characteristics,migration and transformation rules and influencing factors of heavy metals,sources of heavy metals and remediation and remediation of heavy metal pollution in soil.
引文
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[10]程秀花,王海蓉,黎卫亮,等.电感耦合等离子体质谱法测定硒时多元素干扰的碰撞/反应研究及其在地质样品中的应用[J].冶金分析,2015,35(12):5-9.
[11]王家恒,刘冬云.动态反应池-电感耦合等离子体质谱法同时测定地质样品中的金和银[J].分析试验室,2017(7):819-822.
[12]赵小学,赵宗生,王玲玲.水中汞的电感耦合等离子体-质谱法测定[J].中国测试,2013,39(6):50-52.
[13]张修景.微波消解-气相色谱法测定罗汉参中硒的含量[J].食品与发酵工业,2014,40(1):198-201.
[14]聂西度,符靓. ICP-MS法测定食品级二甲基硅油中的As、Cd、Hg、Pb毒理性元素[J].现代食品科技,2014(6):229-232.
[2]王书航,张博,姜霞,等.采用连续分级提取法研究沉积物中磷的化学形态[J].环境科学研究,2015,28(9):1382-1388.
[3]吴慧梅,李非里,牟华倩,等.两步连续提取法测定植物中重金属的形态[J].环境科学与技术,2012,35(7):133-137.
[4]张思思,陈旭峰,李春萍,等.尾矿及其浸出液中重金属形态分析与评价[J].应用化工,2017,46(6):1108-1112.
[5]化玉谨,张敏英,陈明,等.炼金区土壤中汞形态分布及其生物有效性[J].环境化学,2015(2):234-240.
[6]王国莉,陈孟君,范红英,等.四种土壤重金属形态分析方法的对比研究[J].浙江农业学报,2015,27(11):1977-1983.
[7]张朝阳,彭平安,宋建中,等.改进BCR法分析国家土壤标准物质中重金属化学形态[J].生态环境学报,2012(11):1881-1884.
[8]姚军,迪里木拉提·毛里明,武钰,等.微波消解-ICP-MS测定新疆哈药金雀花药材中20种微量元素[J].应用化工,2016,45(4):778-780.
[9]施意华,阳兆鸿,徐华,等.改进化学顺序提取-电感耦合等离子体质谱法应用于铅锌尾矿中铜铅锌镉镍的化学形态分析[J].冶金分析,2016,36(7):83-89.
[10]程秀花,王海蓉,黎卫亮,等.电感耦合等离子体质谱法测定硒时多元素干扰的碰撞/反应研究及其在地质样品中的应用[J].冶金分析,2015,35(12):5-9.
[11]王家恒,刘冬云.动态反应池-电感耦合等离子体质谱法同时测定地质样品中的金和银[J].分析试验室,2017(7):819-822.
[12]赵小学,赵宗生,王玲玲.水中汞的电感耦合等离子体-质谱法测定[J].中国测试,2013,39(6):50-52.
[13]张修景.微波消解-气相色谱法测定罗汉参中硒的含量[J].食品与发酵工业,2014,40(1):198-201.
[14]聂西度,符靓. ICP-MS法测定食品级二甲基硅油中的As、Cd、Hg、Pb毒理性元素[J].现代食品科技,2014(6):229-232.