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The head space is purged with nitrogen, then the tube is stoppered and placed within a pressure tube in a heating block. After heating at 185eC for 10 min, the tube is cooled and 3 mL water is added. The resulting alkyl iodides are extracted with three 1 -mL portions of petroleum ether. The combined extracts are washed free of iodine with two 1-mL portions of 20% aqueous sodium thiosulfate solution, then evaporated to dryness on a water bath. Analysis is by gas chromatography on a 5-ft column of 10% polyethylene glycol diadipate on Celite.
Sulfonation does not change the distribution, and the high 2-phenyl isomer content LAS is more water soluble, other things being equal. Analytical methods are available for very thorough characterization of the impurities in the alkylbenzene raw material used to produce LAS. These include trace levels of tetralins and of di- and polyaromatic compounds. Analysis is via preparative HPLC separation into the major classes, followed by capillary GC/MS identification and quantification of individual components (52).
Liquid-Liquid Extraction There are a number of standard methods for this analysis, for example, ASTM D1568 for alkylaryl sulfonates, ASTM D1570 for analysis of alkyl sulfates, ISO 1104 for alkanesulfonates and certain non-LAS alkylarylsulfonates, and ASTM D3673 for oc-olefin sulfonates (6-9). As with any extraction, it is advisable to check the isolated oil by IR 14 Chapter 1 spectroscopy to determine if any anionic material has also been extracted under the conditions used. Recovery of oil is good for sulfonates, but several extractions are necessary for alkyl sulfates, while recovery from alkyl ether sulfates is quite low (10).