The procedure for tertiary amines described above is the most efficient for these compounds in the presence of primary or secondary amines.The procedure for primary amines as described above is the only known method for determining these compounds in the presence of secondary amines. However, if the mixture to be analyzed consists of a primary and tertiary amine, the primary amine is best determined by the acetylation procedure of Ogg, Porter, and Willits (S), which is faster than the salicylaldehyde method. Alcohols interfere with the acetylation method.The acetylation method is also the best way of determining secondary amines in the presence of tertiary amines; it is more 1297 direct than determining total amines and su1itr:ictiiig the tertiary amine.
topic mixtures as test liquids, and indicated that preliminary experiments had been successful.Hawkins suggested a mixture of ethylbenzene and chlorobenzene as an ideal test mixture for columns with up to 80 plates, and also for tests a t both atmospheric and subatmospheric pressures.Its relative volatility ranges from 1.10 a t 760 mm. to about 1.12 at 20 mm. of mercury pressure. The use of an n-heptanemethylcyclohexane mixture a t reduced pressures was also suggested.F. E . Williams of Hercules Powder Go. pointed out the lack of test mixtures composed of compounds other than hydrocarbons. Rossini felt this was because hydrocarbons were more easily obtained in the pure state than other types of compounds. INTERPRETATION OF DATAWilliams pointed out the complexities of analyzing break cuts to obtain over-all composition, and the desirability of being able to calculate composition directly from the boiling point or refractive index curves. Schoenberger recommended the use of the equal-area cut-point method for low temperature distillations, but also indicated this method had definite limitations. Rossini observed that from accurate boiling points and vapor pressuretemperature curves it is possible to calculate the boiling point of an equimolar mixture and thus establish the cut point. The additional difficulties which result from the presence of a third component during the break were noted.Hawkins described the calibration of columns with known mixtures, in order to obtain arbitrary correction factors for locating cut points and account quantitatively for the material subjected to analytical distillation.
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