Determination of 12 Heavy Metal Elements in Soil by Inductively Coupled Plasma Mass Spectrometry with Automatic Graphite Digestion
摘 要
分取约0.100 0 g处理后的土壤样品,用少量水润湿,以3 mL硝酸、3 mL氢氟酸和1 mL高氯酸为酸体系,采用全自动石墨炉消解仪于150 ℃消解样品2.0 h。消解完成后,赶酸,消解液和水冲洗液一起转移至50 mL容量瓶中,再用水定容,混匀,过0.45 μm滤膜,滤液按照电感耦合等离子体质谱仪工作条件进行测定。结果表明:钒、铬、锰、钴、镍、铜、锌、砷、镉、铅、钼、锑等12种重金属元素的质量浓度均在200 μg·L-1以内与所对应的响应强度与内标响应强度比呈线性关系,检出限(3s)为0.008~0.250 μg·g-1;对土壤标准样品GSS-13、GSS-19、GSS-23进行准确度和精密度试验,测定值均在认定值的不确定度范围内,并且测定值的相对标准偏差(n=6)均不大于4.0%;方法用于5个实际土壤样品分析,12种重金属元素测定值均未超过国家土壤环境质量二级标准。
Abstract
An aliquot about 0.100 0 g of treated soil sample was taken, and wetted with a small amount of water. Nitric acid (3 mL), hydrofluoric acid (3 mL) and perchloric acid (1 mL) were used as acid system, and the sample were digested at 150 ℃ for 2.0 h by a automatic graphite furnace digester. After the digestion was completed, the acid was removed, and the digestion solution and water rinsing solution were transferred into a 50 mL-volumetric bottle, and then diluted with water to volume. After mixing well, the above solution was filtered through a 0.45 μm filter membrane, and the filtrate was determined according to the working conditions of the inductively coupled plasma mass spectrometer. It was shown that linear relationships between the values of mass concentrations of 12 heavy metal elements including vanadium, chromium, manganese, cobalt, nickel, copper, zinc, arsenic, cadmium, lead, molybdenum and antimony and response intensity ratios of their to internal standards were within 200 μg·L-1, with detection limits (3s) in the range of 0.008-0.250 μg·g-1. Tests for accuracy and precision on the soil standard samples GSS-13, GSS-19 and GSS-23 were carried out, and the determined values were within the uncertainty ranges of the confirmed values, and RSDs (n=6) of the determined values were less than 4.0%. The method was used to analyze 5 actual soil samples, and the determined values of 12 heavy metal elements did not exceed the national secondary standard of soil environmental quality.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202310016
所属栏目 工作简报
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收稿日期 2022/7/24
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备注杨连潭,助理工程师,主要研究方向为污水、土壤检测以及污水处理技术等,Yzouxiangshijie@163.com
引用该论文: YANG Liantan,HUANG Jianhui,PAN Qingshan. Determination of 12 Heavy Metal Elements in Soil by Inductively Coupled Plasma Mass Spectrometry with Automatic Graphite Digestion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(10): 1202~1207
杨连潭,黄建辉,潘青山. 全自动石墨消解-电感耦合等离子体质谱法测定土壤中12种重金属元素的含量[J]. 理化检验-化学分册, 2023, 59(10): 1202~1207
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【12】耿广善,郑建明,艾明.ICP-AES测定土壤中的重金属[J].广州化工, 2011,39(3):117-118.
【13】周资凯,鲍益帆,叶昌林,等.混合酸消解变化影响原子荧光法测定土壤和沉积物中砷元素[J].四川环境, 2020,39(6):1-6.
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