Characterization of estuarine sediments by near infrared diffuse reflectance spectroscopy
It has been developed a partial least squares near infrared (PLS-NIR) method for the determination of estuarine sediment physicochemical parameters. The method was based on the chemometric treatment of first order derivative reflectance spectra obtained from samples previously lyophilized and sieved through a lower than 63 μm grid. Spectra were scanned from 833 to 2976 nm, averaging 36 scans per spectrum at a resolution of 8 cm-1, using chromatographic glass vials of 9.5 mm internal diameter as measurement cells. Models were built using reference data of 31 samples selected through the use of a hierarchical cluster analysis of NIR spectra of sediments obtained from the Ria de Arousa estuary…
Microwave-assisted distillation of iodine for the indirect atomic absorption spectrometric determination of iodide in milk samples
To complete these microwave distillation studies, a method for iodide determination in milk-type samples is proposed. The iodide contained in the sample is oxidized to iodine, which is distilled by means of microwave energy and reduced back to iodide. This iodide is combined with Hg(II) and 2,2′-dipyridyl to give an ion pair, which is selectively extracted into IBMK. Mercury is determined in the extract by ETAAS in order to determine iodide. The yield of the distillation process (100%) was evaluated using the Sandell–Kolthoff reaction. In addition, for the solvent extraction, no buffer was needed; 3/5 was the best phase ratio (organic/aqueous); 30 s was the shaking time and the extracts wer…
Estuarine sediment quality assessment by Fourier-transform infrared spectroscopy
Partial least squares Fourier-transform infrared (PLS-FTIR) models were developed for the quality assessment of estuarine sediments through the evaluation of several physico-chemical parameters. Models were based on the chemometric treatment of attenuated total reflection (ATR) spectra directly obtained from samples previously lyophilized and sieved through a lower than 63 μm grid. Spectra were scanned from 3997 to 523 cm-1, averaging 36 scans per spectrum with a nominal resolution of 8 cm-1. Models were built using reference data obtained for sediment samples collected from Ria de Arousa estuary. Hierarchical cluster classification of sediment ATR spectra was employed for the establishment…