A novel strategy for direct elemental determination using laser-induced breakdown spectroscopy: fluence calibration,Journal of Analytical Atomic Spectrometry

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A novel strategy for direct elemental determination using laser-induced breakdown spectroscopy: fluence calibration
Journal of Analytical Atomic Spectrometry ( IF 3.1 ) Pub Date : 2021-07-30 , DOI: 10.1039/d1ja00229e
Raquel C. Machado ₁ , Diego Victor Babos ₁ , Daniel F. Andrade ₁ , Edenir Rodrigues Pereira-Filho ₁

Affiliation

Quantitative analysis requires a lot of effort to obtain an adequate calibration method to overcome matrix effects employing direct solid analysis by laser-induced breakdown spectroscopy (LIBS). To this end, in this study, a new calibration strategy using different laser fluence values, named Fluence Calibration (FC), was developed and evaluated for LIBS quantitative analysis. In FC-LIBS, only one single calibration standard (a pellet with a known concentration of the analyte) and pellets of the sample are used to build a linear model from the emission signals acquired at different laser fluence values, optimized for each matrix sample used in the method development (printed circuit board – waste PCB and fertilizer samples). Satisfactory trueness was obtained for the determination of Al (94 to 115%) and Pb (98 to 100%) in PCB samples and Al, K, Mg, Na and P (ranging from 81 to 120%) in fertilizer samples, in which one sample of each matrix was used as a standard for calibration. For some fertilizer samples, the plasma normalization process did not occur and the matrix effects were not efficiently overcome using FC-LIBS. Standards for calibration were also prepared from salts and adequate figures of merit (i.e. accuracy and precision) were achieved using FC-LIBS for Al (trueness ranged from 82 to 114% and relative standard deviation – RSD 14%) in PCB samples and for Al and P (trueness ranged from 82 to 114% and RSD from 11 to 31%) in fertilizer samples. The FC-LIBS method is an alternative among the nontraditional methods of calibration that allows faster and simpler pellet preparation compared to traditional univariate calibration strategies, acquisition and data treatment for the direct analysis of complex solid samples.

中文翻译：

使用激光诱导击穿光谱直接测定元素的新策略：通量校准

定量分析需要付出大量努力才能获得适当的校准方法，以通过激光诱导击穿光谱 (LIBS) 进行直接固体分析来克服基质效应。为此，在本研究中，开发了一种使用不同激光注量值的新校准策略，称为 Fluence Calibration (FC)，用于 LIBS 定量分析。在 FC-LIBS 中，仅使用一个单一的校准标准（具有已知分析物浓度的颗粒）和样品颗粒来根据在不同激光注量值下获得的发射信号构建线性模型，并针对所使用的每个基质样品进行优化在方法开发中（印刷电路板 - 废 PCB 和肥料样品）。测定 PCB 样品中的铝（94 至 115%）和铅（98 至 100%）以及铝、钾、镁、肥料样品中的 Na 和 P（范围为 81% 至 120%），其中每种基质的一个样品用作校准标准。对于某些肥料样品，未发生等离子体标准化过程，并且使用 FC-LIBS 无法有效克服基质效应。校准标准也由盐和足够的品质因数制备（即准确度和精密度）是使用 FC-LIBS 实现的，用于 PCB 样品中的铝（真实度范围为 82 至 114%，相对标准偏差 - RSD 14%）以及铝和磷（真实度范围为 82 至 114%，RSD 为 11到 31%) 在肥料样品中。FC-LIBS 方法是非传统校准方法中的一种替代方法，与用于直接分析复杂固体样品的传统单变量校准策略、采集和数据处理相比，它可以更快、更简单地制备颗粒。

更新日期：2021-08-24

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