This work proposes a simple, fast and inexpensive method to determine As in natural waters, using X-ray fluorescence. 50 µL of each sample containing 100 mg L-1 of yttrium as internal standard were deposited over a 2.5 µm thickness MylarTM film. The samples were dried at 50 °C for 2 h. X-ray spectra were obtained using an EDXRF apparatus. The accuracy was determined by analyte addition/recovery and by comparison with Hydride Generation Atomic Absorption Spectrometry (HG AAS). A recovery of about 100% was obtained and the results were in good agreement with HG AAS. The method showed a relative standard deviation of 6.8% and a detection limit of 10.5 µg L-1 of As.

Este trabalho descreve um método para a pré-concentração de cádmio com sílica gel modificada com cupferron e sua determinação por espectrometria de absorção atômica com chama. O efeito do pH, a quantidade do material adsorvente, a concentração de eluente, volume da amostra e quantidade do analito adsorvido foram otimizados. O efeito de interferentes foi avaliado para diversos íons mostrando que a extração de cádmio somente é afetada por Zn(II) e Cu(II), dependendo da concentração dos mesmos, mas pode ser minimizada pela adição de 0,05 mmol de KI. Foi obtido um fator de enriquecimento de até 30 vezes. Os limites de detecção e de quantificação foram de 0,5 µg L-1 (3sigma) e 2,0 µg L-1 (10sigma), respectivamente, com rsd de 1,1% (n=10). A exatidão foi avaliada com material de referência certificado e o resultado obtido (3,93 ± 0,01 µg g-1) concordou com o valor certificado (4,15 ± 0,38 µg g-1). O teor de cádmio em esmalte de unhas foi determinado, obtendo-se recuperações quantitativas para as amostras enriquecidas com o analito. O método proposto caracteriza-se pela simplicidade, eficiência e baixo custo.

A method for the determination of cadmium by flame atomic absorption spectrometry (FAAS) after its preconcentration onto a column containing silica gel modified with cupferron was developed. The pH, amount of adsorbent material, concentration of eluent, volume of sample and amount of Cd were optimized. The effect of several foreign ions was also investigated and showed that the retention of cadmium depended on the amounts of Zn(II) and Cu(II) present and that these interferences could be overcome by using a 0.05 mmol KI. An enrichment factor of up to 30 was obtained , the LOD was 0.5 µg L-1 (3sigma) and the LOQ was 2.0 µg L-1 (10sigma) with rsd of 1.1% (n = 10). The accuracy of the proposed method was ascertained by using certified reference material and the obtained result (3.93 ± 0.01 µg g-1) agrees with the certified value (4.15 ± 0.38 µg g-1). The determination of Cd in nail polish showed quantitative recoveries for the spiked samples. The proposed method is characterized by simplicity, efficiency and low cost.