Analytical and Bioanalytical Chemistry vol:376 issue:6 pages:890-901
A five-step sequential extraction procedure was applied on dried and wet Ballastplaat Scheldt estuary sediments. When wet (fresh) sediments were used, all sample handling up to the 3rd extraction step, inclusive, was carried out under inert atmosphere. The repeatability of the procedure was very good on dry samples. For Fe as for Mn, RSD values are lower than 4%, except for Mn in the fifth extraction step where a spread of 10% is observed. The observed RSDs for Pb are of the same order of magnitude as those for Mn. On wet samples the spread of the results is higher than on dried ones. The highest RSDs observed for Fe amount to 20%, for Mn to 15% but for Pb an RSD of up to 44% was found. Better homogenization of the solid sediment part of lyophilized sediments and different porosities of wet sediment sub-samples may be the explanation. These results also indicated that drying/oxidizing of the sediment sample causes a shift from less available/mobile metal fractions to more available/mobile fractions. The Mn and Fe oxyhydroxide spikes added to a wet sediment sample were recovered between 100+/-10%. The results obtained after changing the sequence of the extraction steps (multiple rotations and inversions were tested) corroborated the progressive increase in the aggressive nature of the extraction solutions in our standard scheme. Although there is also no need to change the ratio volume of extractant to amount of sediment, increasing the number of extraction repetitions in steps 1 to 3 resulted, for some of those extraction steps, in a partially modified analyte distribution. Finally the method was applied to sandy and muddy sediment cores of the Scheldt estuary and revealed clear differences between metal distributions in both types of sediment.