摘要
样品前处理是测定土壤中重金属元素的关键步骤,为保障测定结果能如实反应土壤环境状况,比较不同的前处理方法对土壤中6种重金属元素的同时提取能力。基于电感耦合等离子体质谱技术,采用微波和石墨消解装置,探索消解过程中酸种类、加酸方式、消解装置、赶酸温度等因素对测定土壤标准品和实际样品结果的影响。结果表明,样品通过依次加入盐酸、硝酸、氢氟酸、高氯酸,并在160℃赶酸的石墨消解方式进行前处理能快速、准确地测定土壤中的Cu、Pb、Zn、Cd、Cr、Ni等6种元素,其前处理时长约8.5 h,并且消解成本比微波消解更低。在优化条件下,土壤标准样品中6种重金属元素检测结果的绝对回收率为91.5%~108%,相对标准偏差为0.80%~5.4%,方法检出限为0.02~2 mg/kg。表明方法的灵敏度高、准确度与精密度好,适用于批量土壤样品的分析。
Sample pretreatment is a key step in the determination of metallic elements in soil.In order to ensure that the determination results can accurately reflect the soil environment conditions,the simultaneous extraction ability of six metal elements in soil by different pretreatment methods were compared.Based on inductively coupled plasma mass spectrometry technology,microwave digestion device and graphite digestion device were used for sample pretreatment to explore the effects of acid type,the mode of adding acid,digestion device,acid evaporation temperature on the determination of soil standard and actual sample results.The results showed that by adding hydrochloric acid,nitric acid,hydrofluoric acid and perchloric acid in sequence for digestion,controlling acid evaporation temperature 160℃,the six elements of copper,lead,zinc,cadmium,chromium and nickel in soil could be determined more quickly and accurately with graphite digestion.The pretreatment time was about 8.5 h,and the cost is lower than that of microwave digestion.Under the optimal conditions,the recovery of six metallic elements in soil standard samples was 91.5%—108%,the relative standard deviation was 0.80%—5.4%,and the detection limit was 0.02—2 mg/kg.The method has the advantages of high sensitivity,good accuracy and precision,and is suitable to analyze large quantities of samples.
作者
姚苏芝
陈春霏
卢秋
梁晓曦
洪欣
尹娟
YAO Suzhi;CHEN Chunfei;LU Qiu;LIANG Xiaoxi;HONG Xin;YIN Juan(Guangxi Zhuang Autonomous Region Ecological and Environmental Monitoring Centre,Nanning,Guangxi 530028,China;Department of Management Science and Engineering,Guangxi University of Finance and Economics,Nanning,Guangxi 530003,China)
出处
《中国无机分析化学》
CAS
北大核心
2024年第4期386-392,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
广西自然科学基金资助项目(2021GXNSFAA075028)。
关键词
样品前处理
电感耦合等离子体质谱法
土壤
重金属元素
pretreatment method
inductively coupled plasma mass spectrometry
soil
heavy metallic elements
