Microwave-Assisted Photochemical Reactor for the Online Oxidative Decomposition and Determination of p-Hydroxymercurybenzoate and Its Thiolic Complexes by Cold Vapor Generation Atomic Fluorescence Detection
Anno: 2011
Autori: Angeli V., Ferrari C., Longo I., Onor M., D’Ulivo A., Bramanti E.
Affiliazione autori: Consiglio Nazionale delle Ricerche, Istituto di Chimica dei Composti OrganoMetallici, Area di Ricerca, Via G. Moruzzi 1 56124 Pisa, Italy; Consiglio Nazionale delle Ricerche, Istituto Nazionale di Ottica, UOS PISA, Area di Ricerca, Via G. Moruzzi 1, 56124 Pisa, Italy
Abstract: We developed a photochemical method for the online oxidation of p-hydroxymercurybenzoate (PHMB), an organic mercury species widely used for mercaptan and thiolic compound labeling. The method is based on a fully integrated online UV/microwave (MW) photochemical reactor for the digestion of PHMB, followed by cold vapor generation atomic fluorescence spectrometry (CVG-AFS) detection. The MW/UV process led to the quantitative conversion of PHMB and thiol-PHMB complexes to Hg(II), with a yield between 91% and 98%, without using chemical oxidizing reagents and avoiding the use of toxic carcinogenic compounds. This reaction was followed by the reduction of Hg(II) to Hg(0) performed in a knitted reaction coil with NaBH(4) solution, and AFS detection in an Ar/H(2) miniaturized flame. The low MW power applied (18 W) allowed us to keep constant the temperature of the photochemical reactor (21 +/- 1 degrees C), using a flowing water bath. This avoided peak widening due to diffusion processes generally occurring at high temperatures and in the additional cooling coil. This method has been applied to the determination of thiols in human plasma, blood, and wine.
Giornale/Rivista: ANALYTICAL CHEMISTRY
Volume: 83 Da Pagina: 338 A: 343
Parole chiavi: MicrowaveDOI: 10.1021/ac102462xCitazioni: 32dati da “WEB OF SCIENCE” (of Thomson Reuters) aggiornati al: 2024-04-14Riferimenti tratti da Isi Web of Knowledge: (solo abbonati) Link per visualizzare la scheda su IsiWeb: Clicca quiLink per visualizzare la citazioni su IsiWeb: Clicca qui