Evaluation of focused ultrasound and ozonolysis as sample treatment for direct determination of mercury by FI-CV-AAS. Optimization of parameters by full factorial design.
Different oxidation methodologies based on ozone and focused ultrasound for the degradation of organic matter and organic-mercury compounds (spiked) present in human urine are discussed. Inorganic and total mercury can be determined in human urine. A flow-injection cold-vapour atomic absorption spectrometer system was used for mercury measurements. Optimization of cold vapour generation was performed with NaBH4 and SnCl2. A two-level full factorial design (2(4)) was applied to understand the cross-effects among the variables influencing the degradation of organic-mercurials and organic matter in urine by KMnO4/HCl/focused ultrasound, namely, KMnO4 and HCl concentration, ultrasonication time and ultrasonication amplitude. Optimization results showed that all variables were significant. New trends in the application of focused ultrasound and ozone are highlighted. As a result of the optimization procedure, one simple, rapid and accurate method was developed for the determination of total mercury in urine samples The method is based on the ultrasound assisted degradation of organo-mercurials and organic matter in urine in the presence of KMnO4/HCl/Focused Ultrasound. The procedure can be accomplished within 3 min, using 50% sonication amplitude provided by a probe ultrasonic device (63 W maximum output power, 22.5 kHz frequency). The method was applied to measure the mercury content in spiked urine from different non-exposed volunteers.
Capelo
J L
JL
Instituto Superior Técnico, Centro de Química Estrutural, Universidade Técnica de Lisboa, Torre sul, 11 andar., Avda Rovisco Pais s/n, 1049-001 Lisbon, Portugal. jlcapelom@ist.utl.pt
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D000328:Adult; D020650:Combinatorial Chemistry Techniques / Q000379:methods; D005163:Factor Analysis, Statistical; D005260:Female; D017022:Flow Injection Analysis / Q000379:methods*; D005740:Gases / Q000032:analysis / Q000737:chemistry; D006801:Humans; D008628:Mercury / Q000528:radiation effects / Q000652:urine*; D008832:Microchemistry / Q000379:methods*; D010126:Ozone / Q000737:chemistry*; D013010:Sonication; D013057:Spectrum Analysis / Q000379:methods*; D016482:Urinalysis / Q000379:methods*
D005740:Gases; D010126:Ozone; D008628:Mercury