By Thomas M. Schmitt
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Additional info for Analysis Of Surfactant
Puschmann and Wickbold have described comprehensive procedures for quantitative determination of the components in alkyl ether sulfates by wet chemical methods (68,69). Nowadays, these tests are usually performed by HPLC. Cloud point determination, a measure of EO content, is described in Chapter 2 with characterization of nonionic surfactants. 1. Total Active Matter ISO 6842 defines total active matter as ethanol solubles, which includes not only the ether sulfate but also alkyl or alkylphenol sulfate, PEG sulfate, and unsulfated nonionic material including PEG (70).
1. Total Inorganic Salts An accurate value for total inorganic salts can be obtained by weighing that portion of the sample insoluble in alcohol. The following procedure specifies use of isopropanol. ASTM methods D1568 and D1570 specify ethanol (6,7). Procedure: Gravimetric Method for Determination of Total Inorganic Salts in Anionic Surfactants (Alcohol Insoluble Matter) Dissolve an accurately weighed quantity of sample of about 10 g in 200 mL anhydrous 2-PrOH in a 400-mL beaker. Boil for 5 min with stirring.
Procedure (7) Weigh a sample of 1-5 g into a suitable flask and dissolve in about 50 mL water. Adjust to the methyl orange end point with HC1 or KOH solution, then add 50 mL 1 M HC1 solution. 5 hr to complete hydrolysis. Cool to about 50°C and rinse the condenser into the flask with water and petroleum ether. This step is vital because the alcohols are steam-distilled from the flask and trapped in the condenser (62). Transfer the flask contents to a separatory funnel and extract several times with 40-or 50-mL aliquots of petroleum ether.