【引用本文】 乔磊, 叶永盛, 李鹰, 等. 固体直接进样-电热蒸发-电感耦合等离子体质谱联用分析土壤中的重金属元素[J]. 岩矿测试, 2020, 39(1): 99-107. doi: 10.15898/j.cnki.11-2131/td.201907170107
QIAO Lei , YE Yong-sheng , LI Ying , et al. Determination of Heavy Elements in Soil by ETV-ICP-MS with Direct Solid Injection[J]. Rock and Mineral Analysis, 2020, 39(1): 99-107. doi: 10.15898/j.cnki.11-2131/td.201907170107

固体直接进样-电热蒸发-电感耦合等离子体质谱联用分析土壤中的重金属元素

1. 聚光科技(杭州)股份有限公司, 浙江 杭州 310000;

2. 浙江大学, 浙江 杭州 310000

收稿日期: 2019-07-17  修回日期: 2019-09-07 

基金项目: 国家重点研发计划项目"重大科学仪器设备开发"(2017YFF0108203);杭州市重大科技创新项目"基于质谱技术的全自动重金属智能分析系统研制"(20182011A25)

作者简介: 乔磊,硕士,应用工程师,主要从事质谱应用技术开发。E-mail:qiaolei0023@163.com。。

Determination of Heavy Elements in Soil by ETV-ICP-MS with Direct Solid Injection

1. Focused Photonics Inc, Hangzhou 310000, China;

2. Zhejiang University, Hangzhou 310000, China

Received Date: 2019-07-17
Revised Date: 2019-09-07

摘要:为解决高基质土壤样品中痕量重金属元素检测前处理操作繁琐、样品易二次污染或损失等问题,本文建立了采用固体直接进样-电热蒸发-车载电感耦合等离子体质谱定量分析环境现场土壤样品中Cr、Cu、Zn、As、Cd、Hg和Pb元素的分析方法。该方法采用高温电热蒸发石墨炉作为原子化器,称量后样品经梯度升温选择性蒸发,再结合双通道伴热传输石英管、两路氩气在线稀释、ICP-MS瞬时扫描、基体匹配外部校正等策略,有效解决了土壤直接进样过程中传输效率低、基体效应大的问题。在优化的仪器条件下,按照实验方法称取20mg土壤标准物质GBW07401、GBW07406、GBW07407、GBW07430和GBW07456建立外部校正曲线,样品中7种元素的校准曲线线性相关系数≥ 0.999;并按照实验方法测定了杭州市滨江区两处田间土壤样品中Cr、Cu、Zn、As、Cd、Hg和Pb,相对标准偏差(RSD)<7%,相对误差<2.7%,检出限为1.2~32ng/g,回收率为91%~113%。该方法是一种有实用价值的现场样品分析技术,适合现场中大批量土壤样品的分析监测。

关键词: 土壤, 双通道石英管, 在线稀释, 伴热传输, 电热蒸发, 车载电感耦合等离子体质谱

Determination of Heavy Elements in Soil by ETV-ICP-MS with Direct Solid Injection

KEY WORDS: soil, double channel quartz tube, on-line dilution, heat transfer, electrothermal vaporization, mobile inductively coupled plasma-mass spectrometry

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固体直接进样-电热蒸发-电感耦合等离子体质谱联用分析土壤中的重金属元素

乔磊, 叶永盛, 李鹰, 付永强, 周建光, 俞晓峰