Determination of 15 Trace Elements in Soil Samples by LA-ICP-MS
摘 要
在土壤标准样品中加入内标元素铼,将其压片后直接进样,将激光聚焦在样品表面下100 μm,在以下条件下进行激光剥蚀(LA):1剥蚀载气氦气流量为600 mL·min-1;2剥蚀光斑直径为110 μm;3剥蚀速率为50 μm·s-1。剥蚀后形成的气溶胶进入电感耦合等离子体质谱仪(ICP-MS),对其中15种微量元素(铍、钒、铬、钴、镍、铜、锌、镓、砷、镉、锡、锑、铊、铅、铋)进行测定。采用标准加入法,通过校准曲线外推得到各目标元素的含量。检出限(3s)为0.01~0.08 μg·g-1;用此方法分析了2个土壤标准样品(GSS-3和GSS-14),除铍、锑和镉,其他元素所得测定值均在认定值的允许不确定度范围内,且相对误差(RE)均不超过10%;对土壤标准样品(GSS-14)重复测定5次,15种元素测定值的相对标准偏差(n=5)均在10%以内。
Abstract
Rhenium as internal standard element was added to the soil standard sample, and the sample was injected directly after pressing into tablet. Laser beam was focused at 100 μm below the sample surface, and LA was performed as follows: 1 the flow rate of helium as carrier gas was 600 mL·min-1; 2 the diameter of ablation light spot was 110 μm; 3 the ablation rate was 50 μm·s-1. The ablation particles obtained were introduced into ICP-MS and 15 trace elements (i.e. Be, V, Cr, Co, Ni, Cu, Zn, Ga, As, Cd, Sn, Sb, Tl, Pb, Bi) were determined. The standard addition method was used to extrapolate to obtain the content of target elements by the calibration curve. Detection limits (3s) found were in the range of 0.01-0.08 μg·g-1. Two soil standard samples (GSS-3 and GSS-14) were analyzed by this method. Except for Be, Sb and Cd, the determined values of other elements were all within the allowable uncertainty ranges of the certified values, with relative error (RE) less than 10%; the soil standard sample (GSS-14) was analyzed for 5 times, and RSDs (n=5) of the measured values of 15 elements were all within 10%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202101013
所属栏目 工作简报
基金项目
收稿日期 2019/12/23
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作者单位点击查看
联系人作者李小佳(pimoxiu@163.com)
备注王小龙,博士研究生,主要从事ICP-MS应用研究工作
引用该论文: WANG Xiaolong,LI Man,LU Yixin,HU Rui,LI Xiaojia. Determination of 15 Trace Elements in Soil Samples by LA-ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(1): 67~71
王小龙,李曼,陆翌欣,胡锐,李小佳. 激光剥蚀-电感耦合等离子体质谱法测定土壤中15种微量元素[J]. 理化检验-化学分册, 2021, 57(1): 67~71
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参考文献
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【14】李自强,胡斯宪,李小英,等.水浴浸提-氢化物发生-原子荧光光谱法同时测定土壤污染普查样品中砷和汞[J].理化检验-化学分册, 2018,54(4):480-483.
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【2】OLIVARES J A, HOUK R S. Ion sampling for inductively coupled plasma mass spectrometry[J]. Analytical Chemistry, 1985,57(13):2674-2679.
【3】于兆水,张勤.激光剥蚀-电感耦合等离子体质谱法测定微量溴和碘[J].理化检验-化学分册, 2010,46(10):1193-1195.
【4】LIMBECK A, GALLER P, BONTA M, et al. Recent advances in quantitative LA-ICP-MS analysis:Challenges and solutions in the life sciences and environmental chemistry[J]. Analytical and Bioanalytical Chemistry, 2015,407(22):6593-6617.
【5】ZHU H, LIU M, GUO T, et al. Laser ablation single particle aerosol mass spectrometry for the direct analysis of raw coal samples[J]. Journal of Analytical Atomic Spectrometry, 2018,33(7):1158-1167.
【6】周慧,汪正,朱燕,等.激光剥蚀电感耦合等离子体质谱法测定碳化硅器件中杂质元素[J].分析化学, 2014,42(1):123-126.
【7】赵令浩,胡明月,詹秀春,等.激光剥蚀电感耦合等离子体质谱法在玻璃产品质量控制中的应用[J].理化检验-化学分册, 2015,51(11):1515-1519.
【8】ASH R D, HE M. Details of a thallium poisoning case revealed by single hair analysis using laser ablation inductively coupled plasma mass spectrometry[J]. Forensic Science International, 2018,292:224-231.
【9】罗倩华,陈玉红,王海舟.激光剥蚀-电感耦合等离子体质谱法测定不锈钢中17种元素[J].冶金分析, 2013,33(9):1-7.
【10】胡净宇,王海舟.激光剥蚀-电感耦合等离子体质谱对高温合金中17种痕量元素的测定[J].分析测试学报, 2010,29(4):359-363.
【11】石蕊,金献忠.激光剥蚀电感耦合等离子体质谱法测定纯铝及铝丝中铁、硅、铜、锰、镁、钛、锌、铬和镍[J].理化检验-化学分册, 2015,51(6):837-841.
【12】赵小学,成永霞,王玲玲,等.盐酸溶样-原子荧光光谱法测定土壤和沉积物中的砷[J].理化检验-化学分册, 2016,52(6):709-711.
【13】孙杰,吴玥,蒋沄泱,等.稀酸酸解-电感耦合等离子体质谱法测定土壤中14种无机元素的含量[J].理化检验-化学分册, 2017,53(3):315-321.
【14】李自强,胡斯宪,李小英,等.水浴浸提-氢化物发生-原子荧光光谱法同时测定土壤污染普查样品中砷和汞[J].理化检验-化学分册, 2018,54(4):480-483.
【15】姜劲锋,徐鸿志,郭伟,等.粉末压饼LA-ICP-MS测定土壤样品中微量元素[J].分析试验室, 2007,26(11):20-24.
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