b lodometric methods reported in the literature for analysis of ferf-butyl peresters are inconvenient, require long reaction times, and are of relatively low accuracy. Traces of iron salts in the acetic acid and sodium iodide accelerate iodine liberation from the reaction of peresters with iodide ion, thus permitting an improvement of the Wheeler method for analysis of tertbutyl peresters. The new procedure employs 0.00270 ferric chloride hexahydrate in glacial acetic acid as solvent. Reaction times are reduced to 5 to 10 minutes and the method does not require extensive precautions for oxygen exclusion. The method gives precise and accurate results (standard deviation of determinations, =t 0.4270; average per cent deviation between calculated and found values, 0.2970).Both aliphatic and aromatic tert-butyl peresters can be analyzed. A redoxfree radical mechanism is proposed to account for the stoichiometry and products of reaction.N ACCURATE procedure was re-
was concluded that sulfonation of 2,6-lutidine occurred in the 3-position.The S-benzylisothiuronium salts was obtained as an oil which could not be induced to crystallize.Spectra. The infrared spectra of all the materials were obtained using a Perkin Elmer recording instrument, Model 21, Ser. 140. Acknowledgment. We wish to thank Mrs. C. S. Tang-Yeh and Mrs. S. L. Margerum for the analyses and Mrs. B. Pollster for the infrared measurements.Lafayette, Ind.
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