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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