Mercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation

TitleMercury speciation by high-performance liquid chromatography atomic fluorescence spectrometry using an integrated microwave/UV interface. Optimization of a single step procedure for the simultaneous photo-oxidation of mercury species and photo-generation
Publication TypeJournal Article
Year of Publication2014
AuthorsDe Quadros, DPC, Campanella, B, Onor, M, Bramanti, E, Borges, DLG, D'Ulivo, A
JournalSpectrochimica Acta - Part B Atomic Spectroscopy
Volume101
Pagination312–319
ISSN05848547 (ISSN)
KeywordsAtomic fluorescence spectrometry, High performance liquid chromatography, Mercury, Mercury (metal), Mercury speciations, Mercury species, Microwave photochemical reactor, Photochemical reactor, Photochemical vapor generation, Photogeneration, Single-step, Speciation, Vapor generation
Abstract

We described the hyphenation of photo-induced chemical vapor generation with high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS) for the quantification of inorganic mercury, methylmercury (MeHg) and ethylmercury (EtHg). In the developed procedure, formic acid in mobile phase was used for the photodecomposition of organomercury compounds and reduction of Hg2 + to mercury vapor under microwave/ultraviolet (MW/UV) irradiation. We optimized the proposed method studying the influence of several operating parameters, including the type of organic acid and its concentration, MW power, composition of HPLC mobile phase and catalytic action of TiO2 nanoparticles. Under the optimized conditions, the limits of detection were 0.15, 0.15 and 0.35 $μ$g L- 1 for inorganic mercury, MeHg and EtHg, respectively. The developed method was validated by determination of the main analytical figures of merit and applied to the analysis of three certified reference materials. The online interfacing of liquid chromatography with photochemical-vapor generation-atomic fluorescence for mercury determination is simple, environmentally friendly, and represents an attractive alternative to the conventional tetrahydroborate (THB) system.

URLhttp://www.scopus.com/inward/record.url?eid=2-s2.0-84907885786&partnerID=40&md5=f6398aab4fa1ef1b6972f0ddb30e1b9e
DOI10.1016/j.sab.2014.09.019