Journal
MICROCHIMICA ACTA
Volume 183, Issue 4, Pages 1289-1297Publisher
SPRINGER WIEN
DOI: 10.1007/s00604-016-1766-y
Keywords
Fe3O4@Al2O3; Nanoadsorbent; Sol-gel; XRD; SEM; EDX; Speciation; Optical emission spectrometry
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Funding
- University of Johannesburg (Applied Chemistry, Centre for Nanomaterial Science Research Centre)
- National Research Foundation (NRF, South Africa) [98745]
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The authors have developed a rapid and efficient preconcentration method for speciation of Mo(VI), Sb(V) and V(V) that is based on ligandless ultrasound-assisted dispersive solid phase microextraction (UDSPME) using Fe3O4@Al2O3 nanoparticles (NPs) as a sorbent. The NPs were characterized using XRD, SEM, EDX and surface area (BET). The experimental parameters affecting the preconcetration system were optimized using fractional factorial design. The target analytes were preconcetrated, eluted with dilute nitric acid, and then determined by ICP-OES. Under optimum conditions, the limits of detection (for n = 20) for the analytes range from 0.16 to 0.18 ng L-1 and the limits of quantification range from 0.5 to 0.6 ng L-1. The repeatability (intra-day precision; for n = 15) and reproducibility (inter-day precision; for n = 7) ranged from 2.1 to 3.9 % and 4.5 to5.3 %, respectively. The accuracy of the UDSPME method was checked by analysing certified reference material (CRM) and standard reference materials (SRM). Finally, a non-chromatographic method was developed for speciation of Mo, Sb and V at trace levels and successfully applied for the determination of analytes in environmental water samples.
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