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Elemental sulfur in sediments: analytical problems

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Abstract

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 S8 and selection of the most optimal conditions for S8 analysis with GC-MS. The presented studies have shown that the temperature of the injector and the chromatographic column during S8 determination should not exceed 180 °C. At temperatures over 180 °C, the sulfur S8 is 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 S8 is badly extended and asymmetric. To minimize the problems of S8 decomposition 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 S8 in bottom sediments, collected in the Gulf of Gdansk (southern Baltic Sea), has been performed. The concentration of S8 fell 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.

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References

  • Al-Zahrani I, Aneel Mohammed MH, Basheer C, Siddiqui MN, Al-Arfaj A (2015) Membrane assisted simultaneous extraction and derivatization with triphenylphosphine of elemental sulfur in arabian crude samples by gas chromatography/mass spectrometry. J Chem Doi. doi:10.1155/2015/792914

    Google Scholar 

  • Burton ED, Bush RT, Sullivan LA (2006a) Elemental sulfur in drain sediments associated with acid sulfate soils. Appl Geochem 21:1240–1247

    Article  CAS  Google Scholar 

  • Burton ED, Bush RT, Sullivan LA (2006b) Fractionation and extractability of sulfur, iron and race elements in sulfidic sediments. Chemosphere 64:1421–1428

    Article  CAS  Google Scholar 

  • Cetkauskaite A, Pessala P, Södergren A (2004) Elemental sulfur: toxicity in vivo and in vitro to bacterial luciferase, in vitro yeast alcohol dehydrogenase, and bovine liver catalase. Environ Toxicol 19:372–386

    Article  CAS  Google Scholar 

  • Chen YW, Joly H, Belzile N (1997) Determination of elemental sulfur in environmental samples by gas chromatography-mass spectrometry. Chem Geol 137:195–200

    Article  CAS  Google Scholar 

  • Chou C-L (2012) Sulfur in coals: a review of geochemistry and origins. Int J Coal Geol 100:1–13

    Article  CAS  Google Scholar 

  • Fabbri D, Locatelli C, Tarabusi SA (2001) A new procedure, based on combustion to sulphate and ion chromatography for the analysis of elemental sulfur in sediments. Chromatographia 53:119–121

    Article  CAS  Google Scholar 

  • Giordano M, Norici A, Hell R (2005) Sulfur and phytoplankton: acquisition, metabolism and impact on the environment. New Phytol 166:371–382

    Article  CAS  Google Scholar 

  • Hua R, Li Y, Liu W, Zheng J, Wei H, Wang J, Lu X, Kong H, Xu G (2003) Determination of sulfur-containing compounds in diesel oils by comprehensive two-dimensional gas chromatography with a sulfur chemiluminescence detector. J Chromatogr A 1019:101–109

    Article  CAS  Google Scholar 

  • Jasińska A, Burska D, Bolałek J (2012) Sulfur in the marine environment. Oceanol Hydrobiol St 41:72–82

    Google Scholar 

  • Kudłak B, Rogowska J, Wolska L, Kałas M, Łęczyński L, Namieśnik J (2012) Toxicity assessment of sediments associated with the wreck of s/s Stuttgart in the Gulf of Gdańsk (Poland). J Environ Monit 14:1231–1236

  • Kuklińska K, Cieszyńska M, Wolska L, Namieśnik J (2013) Analytical and bioanalytical problems associated with the toxicity of elemental sulfur in the environment. Trac-Tren. Anal Chem 48:14–21

    Google Scholar 

  • Madigan MT, Martinko JM, Parker J (1997) Brock biology of microorganisms. Prentice-Hall, London

    Google Scholar 

  • Mechlińska A, Wolska L, Namieśnik J (2012) Removal of sulfur from a solvent extract. Trac-Tren. Anal Chem 31:129–133

    Google Scholar 

  • Meyer B (1976) Elemental sulfur. Chem Rev 76:367–388

    Article  CAS  Google Scholar 

  • Nair KK, Siddiqi WA, Kumar R, Niwas R, Gogoi R, Srivastava C, Gopal M (2014) Sensitive and rapid determination of elemental nanosulfur/sulfur by liquid chromatography. J Sep Sci 37:1126–1133

    Article  CAS  Google Scholar 

  • Norici A, Hell R, Giordano M (2005) Sulfur and primary production in aquatic environments: an ecological perspective. Photosynth Res 86:409–417

    Article  CAS  Google Scholar 

  • Pardos M, Benninghoff C, Thomas RL, Khim-Heang S (1999) Confirmation of elemental sulfur toxicity in the Microtox® assay during organic extracts assessment of freshwater sediments. Environ Toxicol Chem 18:188–193

    Article  CAS  Google Scholar 

  • Pauls RE (2010) Determination of elemental sulfur in gasoline by gas chromatography with on-column injection and flame ionization detection following derivatization with triphenylphosphine. J Chromatogr Sci 48:284–288

    Article  Google Scholar 

  • Ranzan C, Ranzan L, Trierweiler LF, Trierweiler JO (2015) Sulfur determination in diesel using 2D fluorescence spectroscopy and linear models IFAC-papers On Line 48–8: 415–420

  • Ricking M, Neumann-Hensel H, Schwarzbauer J, Svenson A (2004) Toxicity of octameric elemental sulfur in aquatic sediments. Environ Chem Lett 2:109–112

    Article  CAS  Google Scholar 

  • Rogowska J, Wolska L, Namieśnik J (2010) Impacts of pollution derived from ship wrecks on the marine environment on the basis of s/s Stuttgart (Polish coast, Europe. Sci Total Environ 408:5775–5783

    Article  CAS  Google Scholar 

  • Rogowska J, Mechlińska A, Wolska L, Namieśnik J (2013) Polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs): sediments and water analysis. In: Jorgensen SE (ed) Encyclopedia of environmental management. Taylor & Francis, New York, pp. 2186–2207

    Google Scholar 

  • Svenson A, Viktor T, Remberger M (1998) Toxicity of elemental sulfur in sediments. Environ Toxicol Water Qual 13:217

    Article  CAS  Google Scholar 

  • Van Stempvoort DR, Kwong YTJ (2010) Sulfur analyses as tracers of microbial degradation of hydrocarbons in the capillary fringe. J Contam Hydrol 114:1–17

    Article  CAS  Google Scholar 

  • Wardencki W (1998) Problems with the determination of environmental sulfur compounds by gas chromatography. J Chromatogr A 793:1–19

    Article  CAS  Google Scholar 

  • Welz B, Lepri FG, Araujo RGO, Ferreira SLC, Huang MD, Okruss M, Becker-Ross H (2009) Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces—a review. Anal Chim Acta 647:137–148

    Article  CAS  Google Scholar 

  • Yin C, Li H, Liu H, Zhao L, Bai Z, Wang Y, Zhang S, Liu C (2014) Study on the formation, determination, and removal of elemental sulfur in ultra-low sulfur gas oil. Fuel Process Technol 120:16–20

    Article  CAS  Google Scholar 

  • Yücel M, Konovalov S, Moore T, Janzen C, Luther GW (2010) Sulfur speciation in the upper Black Sea sediments. Chem Geol 269:364–375

    Article  Google Scholar 

Download references

Acknowledgments

The authors would like to thank for the financial support to the Polish Ministry of Science and Higher Education (project MN–01-0095/08).

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Correspondence to Justyna Rogowska.

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Responsible editor: Philippe Garrigues

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Rogowska, J., Sychowska, J., Cieszynska-Semenowicz, M. et al. Elemental sulfur in sediments: analytical problems. Environ Sci Pollut Res 23, 24871–24879 (2016). https://doi.org/10.1007/s11356-016-7739-1

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  • DOI: https://doi.org/10.1007/s11356-016-7739-1

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