NDLI: Evaluation of the detection and quantification limits in electroanalysis using two popular methods: application in the case study of paraquat determination

Content Provider	Royal Society of Chemistry (RSC)
Author	Machado, Sergio A. S. Silva, Osmair Benedito da
Copyright Year	2012
Abstract	In this work, the reduction reaction of paraquat herbicide was used to obtain analytical signals using electrochemical techniques of differential pulse voltammetry, square wave voltammetry and multiple square wave voltammetry. Analytes were prepared with laboratory purified water and natural water samples (from Mogi-Guaçu River, SP). The electrochemical techniques were applied to 1.0 mol L−1 Na2SO4 solutions, at pH 5.5, and containing different concentrations of paraquat, in the range of 1 to 10 μmol L−1, using a gold ultramicroelectrode. 5 replicate experiments were conducted and in each the mean value for peak currents obtained −0.70 V vs. Ag/AgCl yielded excellent linear relationships with pesticide concentrations. The slope values for the calibration plots (method sensitivity) were 4.06 × 10−3, 1.07 × 10−2 and 2.95 × 10−2 A mol−1 L for purified water by differential pulse voltammetry, square wave voltammetry and multiple square wave voltammetry, respectively. For river water samples, the slope values were 2.60 × 10−3, 1.06 × 10−2 and 3.35 × 10−2 A mol−1 L, respectively, showing a small interference from the natural matrix components in paraquat determinations. The detection limits for paraquat determinations were calculated by two distinct methodologies, i.e., as proposed by IUPAC and a statistical method. The values obtained with multiple square waves voltammetry were 0.002 and 0.12 μmol L−1, respectively, for pure water electrolytes. The detection limit from IUPAC recommendations, when inserted in the calibration curve equation, an analytical signal (oxidation current) is smaller than the one experimentally observed for the blank solution under the same experimental conditions. This is inconsistent with the definition of detection limit, thus the IUPAC methodology requires further discussion. The same conclusion can be drawn by the analyses of detection limits obtained with the other techniques studied.
Starting Page	2348
Ending Page	2354
Page Count	7
File Format	HTM / HTML PDF
ISSN	17599660
Volume Number	4
Issue Number	8
Journal	Analytical Methods
DOI	10.1039/c2ay25111f
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Open
Subject Keyword	U River Voltammetry IUPAC Ultramicroelectrode Herbicide Mojiguaçu River Pesticide International Union of Pure and Applied Chemistry Electrochemistry PH Positive-definite matrix Paraquat Differential pulse voltammetry Square wave
Content Type	Text
Resource Type	Article
Subject	Analytical Chemistry Engineering Chemical Engineering

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