A process of separatory determination of monochioroacetic acid (M. C. A.) and monoiodoacetic acid (M. I. A.) by use of ion exchange resin has been investigated. A strongly basic R-NO3 type resin, Amberlite IRA-410, of 100-150 mesh size was used for the test.The adsorbed acids were liberated by using NaNO3 as a liberating agent in order of M. C. A.and M. I. A. The effluent was hydrolyzed with alkali and the Cl- or I- liberated was determined by titration with Volhard's method to give respective acid content.By application of design of column based on a plate theory, the design of column size was made for a complete separation of them and this was applied for a general separatory method. Quantitative determinations were carried out on various samples prepared under different conditions and satisfactory results were obtained.
Relative reaction velocities for thermal chlorination of trichloroethylene and perchloroethylene were 20, 30 and 70, and 6-8, 10 and 15 at 350°C, 400°C and 450°C, respectively, when a thermal decomposition velocity of a pure tetrachloroethane*2 at 400°C was set as 10 (Preceeding Report I). The thermal chlorination of tetrachloroethane was followed by the following competitive reactions and an optimum reaction temperature was around 475-500°C for formation of perchloroethylene: Tetrachloroethane (1) trichloroethylene (2) pentachloroethane (3) perchloroethylene (4) hexachloroethane. The reaction velocities of each of these reactions at above 400°C were in order of (1)>(3)>(2)>(4). The dehydrochlorinating reaction of (1) was far rapider than that of the thermal decomposition system of tetrachloroethane with an addition of a small amount of chlorine. However, in case of a poor mixing of chlorine, which caused the thermal decomposition of a part of tetrachloroethane without chlorine, the reaction velocity of (1) was decreased considerably.This fact may be attributed to the formation of a retarder by the thermal decomposition of tetrachloroethane. The side reaction in the thermal chlorination of tetrachloroethane was mainly caused by the thermal change of trichloroethylene which was produced by the thermal decomposition of tetrachloroethane.It was assumed that this side reaction had a close relation with the formation of retarder.
In order to examine the properties of condensation products of diphenic acid, obtained by the oxidation of phenanthrene, with ethylene glycol and ethylenediamine, the condensation reactions have been carried out. Dimethyl diphenateand ethylene glycol are used for esterification reaction, and a salt of diphenicacid and ethylenediamine is used as the raw material for amide formation byapplying usual condensation reactions. Both of these reactions yield a largeamount of volatile oligomer and it was found that high molecular condensatescan not be obtained. Tests on elementary analysis, saponification value and thedetermination of molecular weight indicated that these by-product oligomers are assumed to be cyclic condensates.