利用 LA-ICP-Q-MS 实验中的短单脉冲响应进行深度剖面定量分析

IF 3.1 2区 化学 Q2 CHEMISTRY, ANALYTICAL Journal of Analytical Atomic Spectrometry Pub Date : 2024-06-04 DOI:10.1039/D4JA00082J
Maximilian Podsednik, Florian Fahrnberger, David Ken Gibbs, Birgit Achleitner, Silvia Larisegger, Michael Nelhiebel, Herbert Hutter and Andreas Limbeck
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摘要

LA-ICP-MS 实验中对高分辨率成像和高样品吞吐量的需求促使人们开发低色散的快速反应消融细胞。这些烧蚀池可以获得称为单脉冲响应 (SPR) 的短瞬态信号,其宽度在个位数毫秒范围内,最大值为 1%。然而,与 ICP-Q-MS 结合使用时,由于要对选定的 m/z 比率进行顺序测量,记录这些短信号会带来问题。如果目标是一个以上的 m/z 比率,四极杆检测系统的时间分辨率就不足以准确测定短 SPR。这项工作的重点是利用快速反应烧蚀电池,在 SPR 模式下使用基于四极杆的检测系统分析多种元素。为此,配备了快速响应烧蚀室的 ArF-准分子激光器与具有 0.2 毫秒及以下短沉降时间的 ICP-MS 相耦合。在 NIST SRM 612 中分析了两种天然存在的琼-同位素,以优化停留时间,获得理想的数据。数据显示,停留时间和沉降时间的比值起着至关重要的作用。通过优化参数,可以确定 107Ag 和 109Ag 在 10 ms FW0.01M 瞬态信号中的自然比率。随后,LA-ICP-MS 的这一概念被应用于掺铝碳化硅(一种宽带隙半导体)的深度剖面分析。该程序在大约 2 分钟内获得了 30 个不同样品位置的深度剖面图,深度分辨率高达 55 纳米。
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Quantitative depth profile analysis using short single pulse responses in LA-ICP-Q-MS experiments†

The demand for high-resolution imaging, and high sample throughputs in LA-ICP-MS experiments has led to developing rapid-response ablation cells with low dispersion. These cells can achieve short transient signals called single pulse responses (SPRs), whose width is in the single-digit millisecond range at 1% of the maximum. However, coupled with ICP-Q-MS, recording those short signals poses a problem due to the sequential measurement of selected m/z ratios. If more than one m/z ratio is targeted, the time resolution of quadrupole detection systems is insufficient for accurately determining short SPRs. This work focuses on utilizing rapid response ablation cells for the analysis of multiple elements with quadrupole-based detection systems in the SPR mode. To achieve this, an ArF-excimer laser equipped with a rapid-response ablation chamber is coupled to an ICP-MS with a short settling time of 0.2 ms and below. The two naturally occurring Ag-isotopes were analyzed in the NIST SRM 612 to optimize the dwell times for ideal data acquisition. The data shows that the ratio of the dwell time and the settling time, plays a crucial role. With the optimized parameters, the natural ratio of 107Ag and 109Ag within a 10 ms FW0.01M transient signal could be determined. This concept of LA-ICP-MS was then applied for depth profiling analysis of Al-doped SiC, a wide bandgap semiconductor. This procedure acquired depth profiles on 30 different sample locations in approximately 2 minutes with an exceptional depth resolution of 55 nm.

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来源期刊
CiteScore
6.20
自引率
26.50%
发文量
228
审稿时长
1.7 months
期刊介绍: Innovative research on the fundamental theory and application of spectrometric techniques.
期刊最新文献
Back cover Evaluation of miniaturized ultrasonic nebulization for high-efficiency sampling in characterization of silver nanoparticles by single particle inductively coupled plasma mass spectrometry† Atomic spectrometry update: review of advances in the analysis of metals, chemicals and materials Assessing the performance of handheld LIBS for predicting soil organic carbon and texture in European soils† Research on a bimodal fusion detection method for surface defects of metal AM components based on LIBS
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