Advanced oxidation processes (AOPs) have known increased application to treat wastewaters containing recalcitrant compounds that are hardly degraded by conventional technologies. AOPs are characterized by the formation of strong oxidants such as hydroxyl radicals, superoxide anions, hydroperoxyl radicals and singlet oxygen, which react with the contaminant, contributing to its degradation. This paper provides an overview of the determination methods of reactive oxygen species, ROS, in the application of AOPs; the methods developed in the available literature for the detection and quantification of ROS are reviewed as a first step in the assessment and detailed description of the mechanisms involved in the oxidation reactions, focusing on the critical analysis of the main strengths and weaknesses presented by the probe molecules employed in the evaluated studies.

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The electrochemical degradation of 2-chlorophenol (2-CP) on boron-doped diamond (BDD) anodes was carried out using two electrolytes, NaCl and Na2SO4. Both electrolytes supported complete mineralization of 2-CP, but faster rates of degradation were observed in NaCl. After 4 h of oxidation, the total organic carbon (TOC) balance neared 100% with Na2SO4 for identifiable compounds, whereas 4 mM of TOC remained unidentified with NaCl. Since chlorophenols are known to be precursors of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), a rigorous assessment of intermediate products was carried out. When near complete mineralization was achieved, the use of NaCl resulted in the concentration of total PCDD/Fs increasing 2.68 × 10(4) times compared to the untreated sample, and to toxicity values several times higher than the maximum level established by U.S. Environmental Protection Agency for water ingestion. When Na2SO4 was used, the increase in total PCDD/Fs concentration was 134 times lower than with NaCl and there was no significant 2,3,7,8-PCDD/Fs formation. Thus, we emphasize the importance of electrolyte selection in electro-oxidation processes, especially when PCDD/Fs precursors are initially present or may be formed in the treated water samples.

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This work assesses the influence of the operating conditions H2O2 dose (20 or 100% of the stoichiometric amount), temperature (20 or 70°C), and the presence of chloride in the oxidation medium in the formation of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) during Fenton treatment of aqueous samples of 2-chlorophenol, 2-CP, one of the strongest precursor of PCDD/Fs. After 4h of oxidation in the experiments carried out with 20% H2O2 chlorinated phenoxyphenols and biphenyls, which are intermediates in PCDD/Fs formation, as well as PCDD/Fs were observed, resulting in concentrations 11 times higher than in the untreated sample. Additionally, when NaCl was also present in the reaction medium, PCDD/Fs were formed at higher extent, with a total concentration 74.4 times higher than in the untreated 2-CP solution. Results depicted a preferential formation of PCDFs over PCDDs, with dominance of lower chlorinated PCDD/Fs (tetra and penta-PCDD/Fs). Besides, the formation of the most toxic PCDD/Fs congeners (2,3,7,8-PCDD/Fs) was not favored under the operating conditions used in this work.