In this paper, a feasible method was proposed for the chlorine and fluorine determination in eye-pencil samples using ion chromatography (IC). The microwave-induced combustion (MIC) was used to digest up to 200 mg of a sample, with 50 mg of microcrystalline cellulose as a combustion aid and only water for analytes absorption. Cl and F recoveries were 105 ± 1 and 93 ± 5%, respectively, when standard solutions were used in the recovery tests. Certified reference materials (CRM) were also digested mixed to the sample, and no significant difference between the obtained results and the certified values was observed. Precision was assessed in terms of repeatability and intermediate precision, with relative standard deviations (RSD) lower than 9%. Limits of detection (LOD) for Cl and F were 37 and 4 mg kg-1, respectively. Ultrasound-assisted extraction (UEA) was also evaluated; however, the results were not satisfactory. The proposed method was suitable for Cl and F determination in eye-pencil because it proved to be accurate, precise and safe, and also minimized waste generation and had high throughput.

Dry ashing, dissolution in aqueous medium or wet digestion methods were evaluated for sample preparation of shampoo for the subsequent indirect determination of sulfur by UV-Vis spectrophotometry. Among the sample preparation methods evaluated, microwave-assisted wet digestion using 7 mol L-1 HNO3 was the most suitable method for this purpose. Accuracy of the proposed method was evaluated by recovery test using standard solution, and the recovery was about 96%. Moreover, for comparison of results, S (as SO42-) was also determined by ion chromatography, after microwave-assisted wet digestion using concentrated HNO3, and no significant difference was observed between the obtained results (according to the t-test for a 95% confidence level, p = 0.288). Relative standard deviations were always lower than 10% and the limit of detection was 0.007% w/v. Finally, the proposed method was applied for analysis of sixteen shampoos used to many types of hair, from different brands produced in Brazil, and the concentration of S ranged from 0.78 to 2.82% w/v.