Comparação de métodos na determinação de elementos em cinzas volantes: Comparing methods for the determination of elements on fly ashes

The characterization of solid materials through flame atomic absorption spectrophotometry requires the total dissolution of the samples. This pre-treatment, besides being analytically time consuming, increases the risks of sample contamination. For this reason, there is an increasing interest in developing more efficient analytical processes aiming the simplification, especially in the reduction of costs, human participation and number of samples preparation phases. The use of microwaves as source of heat in the solubilization or sample digestion is being vulgarized in the late years, not only because of the decrease in the digestion time as well as the minimization of the loses by volatilization. The present work aims the comparison of two methods of solubilization. Method 1 consists in the solubilization of the samples by aqua regia HCl:HNO3, 3:1 v/v, while in method 2 the samples solubilization is done with a mixture of three acids HCl:HNO3:HF, 1:5:2, v/v, using a microwave with controlled pressure and temperature as heat source. The material used in the analytical process was an ash sample from the incineration of urban solid residues, the same ash sample previously submitted to five different processes of contaminant removal, and sample a reference (NIST-2690). After the samples mineralization, they were analysed by atomic absorption spectrophotometry in relation to the concentration of Cd, Cr, Cu, Fe, Ni, Pb and Zn. In relation to the reference sample used, the values obtained for the recovery of elements, in general, were lower than 100%, with the exception of Cd (114%), in both methods, and of Pb (100%), in the microwave. However, the values obtained through the extraction with method 2 (Fe – 97%, Ni 85% e Zn – 96%) were higher than the values obtained with method 1 (Fe – 85%, Ni 58% e Zn – 58%), with the exception of Cr that had the same recovery. In relation to Cu, although there is no established value for the reference sample, with method 2 the value obtained (61.2 mg kg) was higher than the one obtained with method 1 (39.8 mg kg). Concerning the samples in study, statistically, the results obtained with both methods did not differ in relation to the extraction of Cd, Cu, Ni. The concentration of Cu and Zn in the ashes from the EIRSU presented values higher than those from the extraction by the method 2, while in the other samples there were no significant differences. In relation to Fe and Pb, the method of extraction by aqua regia presented values significantly higher comparing to those obtained by the other method. REVISTA DE CIENCIAS AGRARIAS 218