Separation and Detection of Sulfur-Containing Anions Using Single-Column Ion Chromatography

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Abstract
The five principal sulfur-containing anions in oil shale retort by-product waters are separated and detected using a high-performance liquid chromatograph (HPLC) with a simple mercury emission (254 nm) photometric detector. The anions (sulfide, sulfite, sulfate, thiosulfate, and thiocyanate) are studied on silica-based and resin-based anion exchangers over a range of conditions with two types of eluents. The eluents are phthalate- or gluconate-based to accommodate indirect or direct photometric detection. With a silica-based column, sulfite and sulfate are not resolved unless sulfite is derivatized. With the resin-based column and a gluconate-based eluent, either sulfite and sulfate or thiosulfate and thiocyanate are left unresolved at a single set of conditions. Alternatives for determining all of the subject anions in a single isocratic run are discussed. These include complexation of sulfite or electrochemical discrimination of sulfite in the presence of sulfate, and discrimination of thiosulfate in the presence of thiocyanate by a combination of electrochemical and 195-nm photometric detection. The photometric detection systems are compared with conventional conductivity detection and electrochemical detection. Indirect photometric for general or universal detection is shown to be comparable to conductivity detection in the separation and detection of the subject species of sulfur-containing anions. Direct photometric detection of sulfide is shown to have an advantage over electrochemical detection in some of the oil shale retort by-product water matrices because of apparent electrode poisoning effects caused by the organic-laden waters.

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