碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中无机元素

付爱瑞; 陈庆芝; 罗治定; 姜云军; 金倩; 王芸

碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中无机元素

1.
河北省地矿中心实验室, 河北保定 071051
2.
河北省地矿中心实验室, 河北保定 071051
3.
河北省地矿中心实验室, 河北保定 071051
4.
河北省地矿中心实验室, 河北保定 071051
5.
河北省地矿中心实验室, 河北保定 071051
6.
河北省地矿中心实验室, 河北保定 071051

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- 收稿日期: 2011-04-27

Quantification of Inorganic Elements in Aerosol Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Alkali Melting

1.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China
2.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China
3.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China
4.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China
5.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China
6.
Hebei Geology and Mineral Central Laboratory, Baoding 071051, China

摘要

摘要: 大气颗粒物(TSP和PM₁₀)中Si、Al、Ca、Mg、K、Fe、Na等元素含量较高,是颗粒物源分析的指示性元素。目前分析大气颗粒物样品中无机元素的方法有中子活化分析法、X射线荧光光谱法、微波消解(或高压釜消解)电感耦合等离子体发射光谱法和电感耦合等离子体质谱法。本文建立了碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中Si、Al、Ca、Mg、Fe、Ti、Ba、Sr、Zr等无机元素的分析方法,样品于镍坩埚中530~550℃灰化60 min后用NaOH融熔,水提取,再用2 mL 50%的HCl酸化,钠基体匹配消除干扰,解决了大气颗粒物滤膜样品中Si易产生的溶解不完全等问题,提高了Ti、Ba、Sr、Zr等主、次量元素测定的精密度和准确度。讨论了坩埚和熔剂的选择、灰化温度、灰化时间、酸度、干扰等影响因素。在选定条件下,测定结果相对误差(RE)<4%,相对标准偏差(RSD,n=12)<5%, 检出限为0.0047~1.2 ng/g。方法所需设备简单,分析成本低,快速简便,精密度好,准确度高,适宜批量样品的测定。
- 大气颗粒物 /
- 无机元素 /
- 碱熔 /
- 电感耦合等离子体发射光谱法
Abstract: In atmospheric particles (TSP and PM₁₀), the high contents of some inorganic elements including Si, Al, Ca, Mg, K, Fe and Na are the proxy elements for the particles source analysis. At present, there are several methods to analyze inorganic elements for atmospheric particles such as neutron activation analysis, X-ray Fluorescence Spectrometry (XRF), Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) after dissolving by microwave (or high-pressured cauldron). The established method for determining Si, Al, Ca, Mg, Fe, Ti, Sr, Ba and Zr in aerosols by ICP-AES with alkali melting solved the problems of incomplete dissolving for Si caught in an atmospheric particles filter diaphragm, and improved the precision and accuracy of the determinations of major and trace elements such as Ti, Ba, Sr, Zr. In the paper, the formula of flux is also discussed, the temperature and time for ashing, acidity, and interference effect. This method was developed by ashing the samples at a temperature of 530-550℃ for 60 min in a nickel crucible with sodium hydroxide, extracted by hot water, acidificated by 2 mL HCl (50%), eliminated interference by sodium-matrix-matching and measured by ICP-AES. The results were in good agreement with certified values with an accuracy of RE<4%, precision of<5% and detection limits of 0.0047-1.2 ng/g under the selected experimental conditions. This method is inexpensive, rapid, convenient and suitable for a large number of bulk samples with high accuracy and precision.
- aerosol /
- inorganic /
- elements /
- alkali

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碱熔-电感耦合等离子体发射光谱法测定大气颗粒物样品中无机元素

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出版历程

Quantification of Inorganic Elements in Aerosol Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry with Alkali Melting

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出版历程

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