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Determination of Cd and Pb in biological reference materials by electrothermal atomic absorption spectrometry: A comparison of three ultrasonic-based sample treatment procedures
Authors:Maduro C  Vale G  Alves S  Galesio M  da Silva M D R Gomes  Fernandez C  Catarino S  Rivas M G  Mota A M  Capelo J L
Institution:a REQUIMTE, Departamento de Química Faculdade de Ciências e Tecnología, Universidade Nova de Lisboa, Quinta da Torre, 2829-516 Monte de Caparica, Portugal
b Centro de Química Estrutural, Instituto Superior Técnico de Lisboa, Avda Rovisco Pais, s/n, 1049-001 Lisboa, Portugal
c Laboratório de Análises do IST, Instituto Superior Técnico de Lisboa, Avda Rovisco Pais, s/n, 1049-001 Lisboa, Portugal
d INIAP, Estação Vitivinícola Nacional, 2565-191 Dois Portos, Portugal
Abstract:Three different ultrasonic-based sample treatment approaches, the automated ultrasonic slurry sampling, the ultrasonic assisted acid solid-liquid extraction (ASLE) and the enzymatic probe sonication (EPS) were compared and discussed for the determination of Cd and Pb by ET-AAS in biological reference materials. The sample mass chosen to perform the analysis was 10 mg and the liquid volume was 1 ml of nitric acid 1 M. The best results were obtained with the slurry procedure with which it was possible accurate and precise determination of the Cd and Pb content in four of the five reference materials studied. Optimum performance (total metal extraction) of ASLE assisted by ultrasound for Cd was only achieved in two of the four materials assessed whereas total Pb recovery was only possible in three of the five samples. Total extraction with the enzymatic probe sonication was only obtained for Cd in oyster tissue. Neither ASLE nor EPS were able to extract Cd or Pb from spruce needles. Pb concentration obtained after EPS was found to be highly dependent from sample centrifugation speed and time.
Keywords:Acid leaching  Ultrasonic treatment  Microwave digestion  ET-AAS  Enzymatic probe sonication
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