Sulphonate salts chromatographic

Taylor and Nickless [1] have described a paired-ion high performance liquid chromatographic technique for the separation of mixtures of linear alkylbenzene sulphonates and p-sulphophenylcarboxylate salts,... 

Stable esters coming formally from alkynols and carboxylic, sulphonic or dialkyl phosphoric acids were prepared for the first time via alkynyliodonium salts with the corresponding anion. Several alkynyl carboxylates were obtained by anion exchange of alkynyl iodonium tosylates the initially formed salts, PhI+C=CR RCO2, were converted spontaneously into the esters on elution through a chromatographic column packed with an anion-exchange resin (Pol+ArCOj) ... 

A solution of the iodonium salt (912 mg, 2 mmol) in chloroform (10 ml) was added to a solution of sodium p-chlorobenzene sulphinate (496 mg, 2.5 mmol) and triethylbenzylammonium chloride (22.8 mg, 0.1 mmol) in water (10 ml). The mixture was stirred at room temperature for 5 h then the organic layer was separated, the water layer extracted with chloroform (3 x 10 ml) and the combined organic layers washed with water (3 x 20 ml) and dried. After concentration, the residue was chromatographed on silica gel (hexane-chloroform) to give the pure sulphone (472 mg, 92%) m.p. 80-82°C. 

An alternative method is to use an ion chromatograph, where the sample is ashed for about 10 h at 750°C, the residue dissolved in HNO3, diluted with distilled water to a given volume and an aliquot eluted with 0.02% methane sulphonic acid (CH3SO3H), which forms the Na salt and the conductivity is then checked against known Na standards. 

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