QUANTITATIVE DETERMINATION OF ARYLSULFONIC ACIDS AND SALTS BY ALKALI FUSION

A method to determine arylsulfonic acids and salts based on alkali fusion and measurement of either the resultant sulfite or phenol is described. Sulfite was measured volumetrically. Phenols were measured by gas chromatography. The sulfonates were fused with potassium hydroxide at 380-400 °C under nitrogen or helium atmosphere. The sulfite-measuring approach gives an analysis for total sulfonate; a standard deviation of better than 3%; a high degree of selectivity since sulfite can come only from the sulfonate; and a fairly wide range of application. The phenol-measuring approach gives an analysis of micro-sized samples; a standard deviation of 1 to 3%; high selectivity; and a fairly rapid method of analysis. The phenol method is also extremely valuable for analyzing complex mixtures of homologs and isomers. With this method the fusion reaction is carried out in a small heated chamber connected directly to a gas chromatograph. The neutralized fusion products are swept into the gas chromatograph. © 1969, American Chemical Society. All rights reserved.