Rationale In this review, works published in the past 25 years for fluorine, chlorine, bromine, and iodine determination in several matrices by inductively coupled plasma mass spectrometry (ICP‐MS) were covered. Usually, the determination of halogens has been performed by ICP‐MS using a previous sample preparation step or, more recently, by direct analysis of solid or liquid samples. Methods Methods based on combustion, extraction, pyrohydrolysis, sample dilution in organic or aqueous medium, and wet digestion, among others, are discussed. Moreover, the recent applications of methods based on laser ablation (LA) and electrothermal vaporization (ETV) coupled to ICP‐MS are discussed. Results The main challenge for methods using sample preparation has been to obtain a final solution compatible with ICP‐MS, as well as to overcome problems related to analyte losses and contamination. Interferences due to the presence of dissolved organic compounds in solution, enhancement or suppression of ionization of analytes, and related matrix effects have been of concern when using ICP‐MS. For the determination of halogens by ICP‐MS using LA and ETV systems, some limitations related to the difficulty of calibration are pointed out, impairing the widespread use of this approach. Conclusions A critical view is presented for further halogen determination by ICP‐MS, mainly for matrices considered difficult to digest using conventional protocols.

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Microwave-assisted solid sampling analysis coupled to flame furnace atomic absorption spectrometry (MW-SS-FF-AAS) was used for Cd and Pb determination in food-contact polymer samples, with the aim of minimizing reagents and laboratory waste. Operational parameters, such as the FF tube design, the oxygen flow rate, the flame stoichiometry, the sample mass, among others, were evaluated and optimized. Calibration was performed using only reference solutions, and the limits of quantification were 1.7 and 4.6 μg g−1 for Cd and Pb, respectively. Accuracy was assessed by the analysis of certified reference materials (CRMs), and by comparison with the results obtained by inductively coupled plasma mass spectrometry after microwave-assisted wet digestion. The MW-SS-FF-AAS results for the CRMs showed no statistical difference with the certified values, and good agreement was observed with the results of the digestion method. The MW-SS-FF-AAS method was considered suitable for Cd and Pb determination in food-contact polymers. The concentrations of Cd and Pb in the analyzed samples varied from <1.7 to 628 μg g−1, and from <4.6 to 614 μg g−1, respectively. As sample digestion is not necessary, the use of concentrated acids can be avoided by using the proposed MW-SS-FF-AAS method, greatly reducing waste generation.

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In this study, two methods based on the use of diluted acids were developed: microwave-assisted wet digestion (MAWD) and microwave-assisted ultraviolet digestion (MAWD-UV). These methods are evaluated for the digestion of oral pharmaceutical drugs and further determination of elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). Commercial drugs for the treatment of type 2 diabetes are used. No prior comminution is performed. For MAWD, the optimized conditions were 2 mol L−1 or 3 mol L−1 HNO3, 1 mL of 50% H2O2 and a 45 min or 55 min irradiation program. For MAWD-UV, the condition using 1 mol L−1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program enabled the digestion of all samples. In this way, efficient methods are proposed for the digestion of commercial pharmaceutical tablets for further determination of class 1 and 2A elemental impurities (ICH Q3D guidelines).

The aim of this study was to characterize the limnological parameters and analyse the biological effects of different ponds in a commercial fish farm in the Pará State, Brazil. One pond is designated for fingerling production (N) while the other is for fattening and termination (F). The other three ponds are named supply tanks, from which the water from the Parauapebas River is collected to fill N and F tanks. For the physical–chemical analysis, samples from N and F ponds were collected at a depth of 50 cm close to the water's outlets of the ponds, with the aid of a commercial kit for water analysis. Caenorhabditis elegans nematodes were used for water quality biomonitoring and exposed for 24 h to samples from all five tanks collected during three different days, being assessed through physiological endpoints. During the study, values of transparency and pH were higher in N, both with significant differences between the ponds. The other parameters did not show any differences among them in the different days and times analysed. The results showed that the water quality of N and F ponds is in accordance with the current legislation in the country. Despite being in accordance with legislation and with acceptable metal levels, samples caused toxicity to worms, which indicate that for fish production, a continuous supervision is essential for the success of the activity. Therefore, the limnological variables in relation to biomonitoring should be constantly assessed in fish farm enterprises in order to maintain a more efficient and sustainable productive system.

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