Elemental sulfur in sediments: analytical problems.
In the paper, a modified method for elemental sulfur (S8) determining using gas chromatography coupled with mass spectrometry (GC-MS) is proposed with estimation of selected validation parameters. The aim of this work was a review of problems associated with the determination of S8and selection of the most optimal conditions for S8analysis with GC-MS. The presented studies have shown that the temperature of the injector and the chromatographic column during S8determination should not exceed 180 °C. At temperatures over 180 °C, the sulfur S8is decomposed to the other sulfur species such as S2, S3, S4, S5, and S6. During decreasing injector and column temperature below 180 °C the chromatographic peak eluted as S8is badly extended and asymmetric. To minimize the problems of S8decomposition to other sulfur species during chromatographic process also other parameters of the GC-MS have been selected. In order to apply the proposed method for real sediments samples, determination of sulfur S8in bottom sediments, collected in the Gulf of Gdansk (southern Baltic Sea), has been performed. The concentration of S8fell in the range from below the limit of detection to 0.1432 ± 0.0095 mg/g d.w. The research has also shown that addition of approx. 200 mg of activated copper is effective for removing sulfur from bottom sediment extracts.
Department of Environmental Toxicology, Faculty of Health Sciences, Medical University of Gdansk, 80-204 Gdansk, 23 Debowa Str, Gdansk, Poland. justyna.rogowska@gumed.edu.pl.
Justyna
J
Rogowska
Department of Environmental Toxicology, Faculty of Health Sciences, Medical University of Gdansk, 80-204 Gdansk, 23 Debowa Str, Gdansk, Poland.
Joanna
J
Sychowska
Department of Environmental Toxicology, Faculty of Health Sciences, Medical University of Gdansk, 80-204 Gdansk, 23 Debowa Str, Gdansk, Poland.
Monika
M
Cieszynska-Semenowicz
Department of Environmental Toxicology, Faculty of Health Sciences, Medical University of Gdansk, 80-204 Gdansk, 23 Debowa Str, Gdansk, Poland.
Lidia
L
Wolska
D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D019015:Geologic Sediments / Q000032:analysis / Q000737:chemistry; D057230:Limit of Detection; D013455:Sulfur / Q000032:analysis / Q000737:chemistry
D013455:Sulfur
Analytical problems; Aquatic environmental; Elemental sulfur; Environmental pollution; Gas chromatography; Sediments
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