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脉冲微放电与电感耦合等离子体质谱联用对固体金属样品进行元素分析。

Pulsed microdischarge with inductively coupled plasma mass spectrometry for elemental analysis on solid metal samples.

出版信息

Anal Chem. 2015 May 5;87(9):4871-8. doi: 10.1021/acs.analchem.5b00397. Epub 2015 Apr 17.

Abstract

Pulsed microdischarge employed as source for direct solid analysis was investigated in N2 environment at atmospheric pressure. Compared with direct current (DC) microdischarge, it exhibits advantages with respect to the ablation and emission of the sample. Comprehensive evidence, including voltage-current relationship, current density (j), and electron density (ne), suggests that pulsed microdischarge is in the arc regime while DC microdischarge belongs to glow. Capability in ablating metal samples demonstrates that pulsed microdischarge is a viable option for direct solid sampling because of the enhanced instantaneous energy. Using optical spectrometer, only common emission lines of N2 can be acquired in DC mode, whereas primary atomic and ionic lines of the sample are obtained in the case of pulsed mode. Calculations show a significant difference in N2 vibrational temperatures between DC and pulsed microdischarge. Combined with inductively coupled plasma mass spectrometry (ICPMS), pulsed microdischarge exhibits much better performances in calibration linearity and limits of detection (LOD) than those of DC discharge in direct analysis of samples of different matrices. To improve transmission efficiency, a mixture of Ar and N2 was employed as discharge gas as well as carrier gas in follow-up experiments, facilitating that LODs of most elements reached ng/g.

摘要

在大气压的 N2 环境中研究了用作直接固体分析源的脉冲微放电。与直流(DC)微放电相比,它在样品的烧蚀和发射方面具有优势。包括电压-电流关系、电流密度(j)和电子密度(ne)在内的综合证据表明,脉冲微放电处于电弧状态,而 DC 微放电属于辉光放电。对金属样品的烧蚀能力表明,由于增强的瞬时能量,脉冲微放电是直接固体采样的可行选择。使用光学光谱仪,仅在 DC 模式下可以获得 N2 的常见发射线,而在脉冲模式下可以获得样品的主要原子和离子线。计算表明,N2 振动温度在 DC 和脉冲微放电之间存在显著差异。与直流放电相比,脉冲微放电与电感耦合等离子体质谱(ICPMS)相结合,在直接分析不同基质的样品时,在校准线性度和检测限(LOD)方面表现出更好的性能。为了提高传输效率,在后续实验中,将 Ar 和 N2 的混合物用作放电气体以及载气,使大多数元素的 LOD 达到 ng/g。

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