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The method below is based on hydrolysis of sulfate groups, followed by column chromatographic separation of derivatives of the resulting alcohols and alcohol ethoxylates. Only the unethoxylated material elutes from a silica gel column. Procedure: Gravimetric Determination of Alkyl Sulfate in Alcohol Ethoxysulfates (76) Dissolve about 10 g sample, accurately weighed, in 250 mL 1 M H2SO4 in a flask with ground glass neck. Fit a condenser and heat at reflux for 90 min. Dilute with an equal volume of EtOH in a 1-L separatory funnel and extract 3 times with 150-mL aliquots of pentane, combining the extracts in a flask with a ground glass neck.
H2SO4 to 1 L water), and 15 mL CHC13 are added. As a blank, the remainder of the unhydrolyzed column eluate is analyzed in another separatory funnel. 1 M H2SO4 solution is omitted with the blank. The extraction is performed, then repeated with a second 15-mL portion of CHC^. The extracts are combined into 50mL volumetric flasks, diluted to volume, and the absorbance is measured at 642 nm, calibrating with solutions of sodium hexadecanesulfonate analyzed in the same way. (c) Liquid chromatography.
GC may also be used after cleavage of the sulfate group, as discussed in Chapter 8. 1. Assay Assay is conventionally performed by two-phase or one-phase titration with benzethonium chloride, as described in Chapter 16. Assay may also be performed by determination of 26 Chapter 1 ester SO3 as described subsequently. For example, ISO 2271 specifies purity determination of sodium lauryl sulfate (used as a reagent) by a variation of the ester 803 method (5,30). 2. Alkyl Chain Length Distribution The alkyl chain length distribution is readily determined by HPLC or GC.