We developed a simple, rapid, and solventless method for analyzing trihalomethanes in beer samples using headspace solid-phase microextraction. The effects of varying experimental parameters, such as extraction temperature and time, addition of sodium chloride, and agitation speed, on extraction yield were studied using a univariate experimental design. Limits of detection between 0.22 and 0.46 µg L- 1 and wide linear ranges were achieved for trihalomethanes. We measured the trihalomethane recoveries and precision (as the standard deviation of repeat measurements) and demonstrated the applicability of the proposed method by analyzing 32 beer samples.

Neste estudo foi desenvolvida uma metodologia analítica para determinação de 2,4-dinitrofenol (2,4-DNP) em amostras de águas de chuva de regiões de Santa Catarina utilizando a voltametria de onda quadrada (VOQ) e de forma ex situ. O estudo envolveu a aplicabilidade de utilizar o eletrodo de carbono vítreo modificado com filme de bismuto. A formação do filme de bismuto foi otimizada por voltametria cíclica e em seguida, estudos de pH e eletrólito de suporte foram investigados para a redução do 2,4-DNP. Os parâmetros analíticos que afetam a sensibilidade da VOQ foram otimizados. Na sequência, as figuras analíticas de mérito foram obtidas: faixa linear de trabalho de 3,2 x 10-7 - 4,6 x 10-6 mol L-1, coeficiente de correlação de 0,996, RSD% = 17,5 (1,3 x 10-6 mol L-1, n = 6), 11,7 (2,5 x 10-6 mol L-1, n = 6) e 6,4 ( 4,5 x 10-6 mol L-1, n = 6), limite de detecção de 1,2 x 10-7 mol L-1. E, finalmente estudos de recuperação foram realizados para avaliar a exatidão da metodologia. Valores obtidos ficaram entre 84-112% (2,5 x 10-6 mol L-1) e 89 - 113% (4,5 x 10-6 mol L-1).

In this study an analytical methodology for determination of 2,4-dinitrofenol (2,4-DNP) in rainwater samples of regions of Santa Catarina was developed using the square wave voltammetry (SWV). The study involved the applicability to use the modified glass carbon electrode with bismuth film. The formation of the bismuth film was optimized by cyclic voltammetry and after that, studies of pH and electrolyte support were investigated for the reduction of 2,4-DNP (ex situ form). The analytical parameters that affect the sensitivity of the SWW were optimized. In order, the analytical figures of merit were obtained: linear working range of 3,2 x 10-7 - 4,6 x 10-6 mol L-1; excellent coefficient of correlation of 0,996; RSD% = 17,5 (1,35 x 10-6 mol L-1, n = 6), 11,7 (2,5 x 10-6 mol L-1, n = 6) e 6,4 ( 4,6 x 10-6 mol L-1, n = 6); limit of detection of 1,2 x 10-7 mol L-1. Recovery studies were performed to evaluate the accuracy of the methodology. The values obtained were between 84 - 112% (2,7 x 10-6 mol L-1 ) and 89 - 113% (4,3 x 10-6 mol L-1).