Polysulfides: synthesis and analysis

Igene, Harrison Akhaze (2013) Polysulfides: synthesis and analysis. Masters thesis, Memorial University of Newfoundland.

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Abstract

Polysulfides of the general form ⁻SSπS⁻ occur naturally in sulfur rich waters and can be formed by the reaction of sulfide with elemental sulfur to yield water soluble polysulfides. Inorganic polysulfides have been found to form organic polysulfanes in the environment, and in water, oxidation of polysulfides can produce thiosalts and sulfuric acid, resulting in acidification of aquatic environments. Polysulfides are unstable and readily undergo changes in speciation, analysis is challenging and complicated by lack of standards. A series of polysulfides were synthesized to be used as standards. They were stabilized by methylation to form dimethylpolysulfanes and analyzed by gas chromatography-mass spectrometry (GC-MS), high performance liquid chromatography (HPLC) with UV detection, and matrix assisted laser desorption MS (MALDI-MS). The various dimethylpolysulfanes were fractionated using semi-preparatory HPLC; the fractions containing individual dimethylpolysulfanes were analyzed for sulfur content by inductively coupled plasma-optical emission spectrophotometry (ICP-OES). Stability studies were also carried out to confirm that the stabilization approach was effective.

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