Laser-Induced Breakdown Spectroscopy Optimization Using Response Surface Methodology

Rodrigo Rossi De Araújo, D. Milori, M. C. Mitsuyuki, C. Montes, A. Melfi
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Abstract

Laser-induced breakdown spectroscopy (LIBS) is a modern analytical technique that is capable of fast, multi-elemental, lowcost and environmental friendly analysis, which does not require complex sample preparation. Albeit its potential, LIBS analysis still presents many limitations in terms of sensitivity and reproducibility, especially when analyzing complex matrices such as of sediments and soil samples. In order to reduce these matrix related effects, it is highly recommended that the system temporal parameters, which are responsible for controlling plasma evolution and signal collection, are optimized beforehand. In this work, we proposed the design of experiments (DOE) tool – specifically, the response surface methodology (RSM) – as an approach to optimize LIBS’s most important parameters (delay-time, interpulse delay, gate width and accumulated pulse). Signal-to-noise ratio (SNR) of the emission lines for Zn, Cd, Mg, Al, Ni, Cu, Ca, Cr, Sr, Fe were the response variable assessed during the procedure. The results showed that the RSM was an effective optimization tool for LIBS parameters and the final condition improved SNR ratios by up to a 48 ratio, when comparing to the not-optimal conditions.
利用响应面方法优化激光诱导击穿光谱法
激光诱导击穿光谱(LIBS)是一种现代分析技术,能够进行快速、多元素、低成本和环境友好型分析,无需复杂的样品制备。尽管潜力巨大,但激光击穿光谱分析在灵敏度和重现性方面仍有许多局限性,尤其是在分析沉积物和土壤样品等复杂基质时。为了减少这些与基质相关的影响,强烈建议事先优化负责控制等离子体演变和信号收集的系统时间参数。在这项工作中,我们提出了实验设计(DOE)工具--特别是响应面方法(RSM)--作为优化 LIBS 最重要参数(延迟时间、脉冲间延迟、门宽度和累积脉冲)的一种方法。在此过程中,锌、镉、镁、铝、镍、铜、钙、铬、锶、铁发射线的信噪比(SNR)是需要评估的响应变量。结果表明,RSM 是一种有效的 LIBS 参数优化工具,与非最佳条件相比,最终条件的信噪比提高了 48%。
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