A combustão iniciada com micro-ondas (MIC) foi aplicada para decomposição de amostras de tabaco de cigarro e subsequente determinação de bromo e cloro por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Massas de amostra de até 500 mg foram decompostas em frascos fechados e pressurizados com 20 bar de oxigênio. A combustão foi completada em menos de 30 s e os analitos foram absorvidos em solução diluída de (NH 4 ) 2 CO 3 . A exatidão foi avaliada usando materiais de referência certificados e mediante a determinação utilizando ICP-MS. A concordância foi melhor do que 98% usando 50 mmol L -1 de (NH 4 ) 2 CO 3 como solução absorvedora e 5 min de refluxo. A temperatura durante a combustão foi superior a 1400 °C e o conteúdo de carbono residual nos digeridos após MIC foi menor que 1%. Até oito amostras podem ser decompostas simultaneamente. Limites de quantificação utilizando MIC e determinação por ICP OES foram de 12 e 6 µg g -1 para Br e Cl, respectivamente.The microwave-induced combustion (MIC) was applied for cigarette tobacco samples digestion and further determination of bromine and chlorine by inductively coupled plasma optical emission spectrometry (ICP OES). Samples masses up to 500 mg were combusted in closed vessels using 20 bar of oxygen. Combustion was complete in less than 30 s and analytes were absorbed in diluted (NH 4 ) 2 CO 3 solution. Accuracy was evaluated using certified reference materials with similar matrix composition and comparison with results obtained using ICP-MS. The agreement was better than 98% using 50 mmol L -1 (NH 4 ) 2 CO 3 as absorbing solution and 5 min of reflux. Temperature during combustion was higher than 1400 °C and the residual carbon content in digest obtained after MIC was lower than 1%. Up to eight samples could be processed simultaneously and a single absorbing solution was suitable for both Br and Cl. Limit of quantification by MIC and further ICP OES determination was 12 and 6 µg g -1 for Br and Cl, respectively.Keywords: microwave-induced combustion, cigarette, bromine, chlorine, ICP OES
IntroductionTobacco leaves may be used in different forms such as smoking, chewing or sniffing. All of these forms result in a number of negative side effects on human health that are well-documented.1 Chlorine and bromine are essential for growth of the plants and minor constituents of tobacco. The content of bromine and chlorine in tobacco could vary depending on tobacco type, soil and climatic conditions. Typical concentration ranges for Br and Cl reported in tobacco are 100 to 200 and 700 to 30000 µg g -1 , respectively. Over 85% of the all halogenated compounds found in tobacco and smoke are either halogenated agrochemicals, impurities found in the agrochemicals, or decomposition products from the agrochemicals. Up to 2.4% of the bromine and chlorine can be transferred to smoke. There are 242 identified halogenated compounds in tobacco and/or tobacco smoke and chlorine and bromine are present in 192 and 12 different compounds, respectively.
2Bromine...