ABSTRACT
The chromium speciation procedure was optimized using magnetic polyaniline nanoparticles (Fe3O4@PANI NPs) solid-phase extraction coupled with microsampling injection-flame atomic absorption spectrometry (MIS-FAAS). Chromium speciation was successfully achieved by Fe3O4@PANI NPs at pH 8.0. The recoveries obtained for Cr(III) and Cr(VI) were above 95% and under 5%, respectively. Recoveries of over 95% for Cr(III) from 40.0 mL of the sample were obtained using 25 mg Fe3O4@PANI NPs and 500 µL of 0.2% (w/v) thiourea (TU) solution prepared in 2 mol L-1 HCl as eluent. Total chromium as Cr(III) was extracted quantitatively after reducing the Cr(VI) to Cr(III). The linear range, detection limit, preconcentration factor, and precision of the optimized method for Cr(III) in aqueous solution were 2.5-94.0 µg L-1, 0.335 µg L-1, 80, and 3.07%, respectively. The validation of the method was controlled using SPS-WW2 Batch 114 wastewater and BCR-715 industrial wastewater as standard reference materials (SRMs) for environmental water, and the obtained results were in close agreement with the certified values.
ABSTRACT
An aminated Amberlite XAD-resin as a solid phase extractant was tested for speciation of inorganic mercury, Hg(II) and methylmercury, MeHg(I) in water and fish tissue samples. It was found that Hg(II) and MeHg(I) ions could be simultaneously retained by a column filled with AAXAD-4 resin at pH 4 and the sequential quantitative elutions of Hg(II) and MeHg(I) were achieved using 10â¯mL of 0.1%(m/v) thiourea in 3%(v/v) HCl and 10â¯mL of 6â¯molâ¯L-1 HCl, respectively. Hg(II) in the eluent was directly determined and MeHg(I) in the second eluent is quantified using FI-CVG-AAS after its oxidative digestion with KMnO4. The limits of detection for Hg(II) and MeHg(I) ions were found to be 0.148 and 0.157⯵gâ¯L-1, respectively. The method was validated by analysing a certified reference material. The relative errors for Hg(II), MeHg(I) and T-Hg were in range of -1.8% and -3.2%.
