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The present article describes fundamentals and applications of multivariate techniques used for the optimization of analytical procedures and systems involving spectroanalytical methods such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP OES), and inductively coupled plasma mass spectrometry (ICP-MS), considering the main steps of a chemical analysis. This way, applications of experimental designs in optimization of sampling systems, digestion procedures, preconcentration procedures, instrumental parameters of quantification steps of analytical methods, and robustness tests have been summarized in this work.

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This article critically overviews the state-of-the-art of slurry sampling as an approach for the minimization of sample preparation prior to the determination of metals and metalloids in complex matrices by spectroanalytical techniques. Relevant factors involved in the optimization of slurry-based analytical procedures and the dependence of the quality of the results on the calibration method selected are discussed in detail. The advantages and limitations compared to solid sampling for the analysis of solid matrices are highlighted and discussed. Analytical applications of slurry sampling reported in the literature emphasizing publications between 2004 and 2009 are comprehensively compiled covering detection by flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ET-AAS), cold vapor atomic absorption spectrometry (CV-AAS), hydride generation atomic absorption spectrometry (HG-AAS), hydride generation atomic fluorescence spectrometry (HG-AFS), inductively coupled plasma optical emission spectrometry (ICP-OES), and inductively coupled plasma mass spectrometry (ICP-MS).