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By Thomas M. Schmitt

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By use of a nonleveling solvent, the neutralization of the relatively weakly acidic second proton of sulfuric acid can be differentiated from the neutralization of the strongly acidic first proton and the sulfonic acid. This has been demonstrated for analysis of a-olefin sulfonate (21), alkylbenzene sulfonate (23-25), sulfated alcohols, and sulfated ethoxylated alcohols (18). Tetrabutylammonium hydroxide titrant was used in the earlier work, with acetone or acetone/water solvent. Later, cylcohexylamine in methanol or ethanol (23,24) and triethylamine in 50:50 acetonitrile/ethylene glycol (26) were recommended as more stable titrants.

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). ISO 6843 describes wet chemistry methods for separately determining PEG, sulfonated PEG, and inorganic salts in order to arrive at a value for the ether sulfate itself, but this value will still include alkylsulfate or alkylphenolsulfate (71). 1 g Na2SO4, fit a reflux condenser, and boil for 30 min.

A) Titration method Procedure (7,30) Accurately weigh about 5 g sample or about 1 g alcohol-soluble material into a flask, dissolve in about 50 mL water, and adjust to the methyl orange end point with dilute HC1. Add exactly 35 mL 1 M HC1 and boil with reflux for 2 hr after foaming has stopped (or remains constant). Cool and titrate to methyl orange with 1 M NaOH. Q where V\ and V2 are the volumes of base and acid used, respectively, and B and A are their molar concentrations. W is the sample weight in grams.

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