4.0 Article

Determining Mercury in Sediment Samples by Extraction Using a Novel-Chelating Reagent Dithiothreitol (DTT) Followed by Cold Vapor Atomic Fluorescence Spectrometry (CV-AFS)

Journal

JOURNAL OF THE BRAZILIAN CHEMICAL SOCIETY
Volume 31, Issue 12, Pages 2553-2560

Publisher

SOC BRASILEIRA QUIMICA
DOI: 10.21577/0103-5053.20200133

Keywords

dithiothreitol; mercury; sediments; cold vapor; direct Hg analyzer

Funding

  1. Brazilian National Counsel of Technological and Scientific Development (CNPq) [INCT 465497/2014-4, 442187/2018-1]
  2. Coordination for the Improvement of Higher Education Personnel, Brazil (CAPES) [001]

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A new analytical protocol has been developed for the determination of mercury in surface sediments using dithiothreitol (DTT) as a new chelating reagent for the extraction. This protocol requires a small sample mass (250 mg), 4.0 mL of a 0.1 M (pH = 9.0) aqueous DTT solution, and sonication for 30 min, followed by cold vapor atomic fluorescence spectrometry (CV-AFS). The limits of detection and quantification determined were 6 and 18 ng g(-1), respectively. The method was validated using three standard reference materials, SRM NIST 1646a, PACS-2, and MESS-3, with recoveries in the range of 102-124%. The new analytical protocol was successfully applied in riverine surface sediments, revealing concentrations in the range of 220-340 ng g(-1). The results obtained by CV-AFS were compared to those obtained by DMA-80 (direct mercury analyzer). The linear regression equation obtained was [CV-AFS] = (0.91 +/- 0.07)[DMA-80] + (0.04 +/- 0.02), revealing no systematic difference between the analytical methods. Hence, the proposed method does not require the complete digestion of the sediment, and was found to be comprehensive, simple, accurate and suitable to be employed for determination of mercury in sediment samples.

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