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  • Continuous-flow fractionation of selenium in contaminated sediment and soil samples using rotating coiled column and microcolumn extraction.

Continuous-flow fractionation of selenium in contaminated sediment and soil samples using rotating coiled column and microcolumn extraction.

Talanta (2012-01-24)
Elena Yu Savonina, Petr S Fedotov, Rainer Wennrich
ABSTRACT

Dynamic fractionation is considered to be an attractive alternative to conventional batch sequential extraction procedures for partitioning of trace metals and metalloids in environmental solid samples. This paper reports the first results on the continuous-flow dynamic fractionation of selenium using two different extraction systems, a microcolumn (MC) packed with the solid sample and a rotating coiled column (RCC) in which the particulate matter is retained under the action of centrifugal forces. The eluents (leachants) were applied in correspondence with a four-step sequential extraction scheme for selenium addressing "soluble", "adsorbed", "organically bound", and "elemental" Se fractions extractable by distilled water, phosphate buffer, tetramethylammonium hydroxide, and sodium sulphite solutions, respectively. Selenium was determined in the effluent by using an inductively coupled plasma atomic emission spectrometer. Contaminated creek sediment and dumped waste (soil) samples from the abandoned mining area were used to evaluate resemblances and discrepancies of two continuous-flow methods for Se fractionation. In general, similar trends were found for Se distribution between extractable and residual fractions. However, for the dumped waste sample which is rich in organic matter, the extraction in RCC provided more effective recovery of environmentally relevant Se forms (the first three leachable fractions). The most evident deviation was observed for "adsorbed" Se (recoveries by RCC and MC are 43 and 7 mg kg(-1), respectively). The data obtained were correlated with peculiarities of samples under investigation and operational principles of RCC and MC.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Sodium sulfite, BioUltra, anhydrous, ≥98% (RT)
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Tetramethylammonium sulfate, suitable for ion pair chromatography, LiChropur, ≥99.0% (T)
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Tetramethylammonium hydroxide solution, ACS reagent
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Tetramethylammonium hydroxide solution, 10 wt. % in H2O
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Tetramethylammonium chloride, reagent grade, ≥98%
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Tetramethylammonium fluoride, 97%
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Tetramethylammonium hydroxide solution, 25 wt. % in methanol
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Sodium sulfite, BioXtra, ≥98%
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Sodium sulfite, ACS reagent, ≥98.0%
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Tetramethylammonium hydroxide solution, 25 wt. % in H2O
Supelco
Tetramethylammonium chloride, suitable for ion pair chromatography, LiChropur, ≥99.0% (AT)
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Sodium sulfite, anhydrous, Redi-Dri, reagent grade, ≥98%
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Sodium sulfite, puriss. p.a., reag. Ph. Eur., anhydrous, 98-100.0% (iodometric)
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Sodium sulfite, ≥98%
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Tetramethylammonium hydroxide pentahydrate, ≥95.0% (T)
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Tetramethylammonium bromide, suitable for ion pair chromatography, LiChropur, ≥99.0% (AT)
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Tetramethylammonium bromide, 98%