Iron, cobalt and nickel in refined soybean oils were determined by neutron activation analysis followed by radiochemical purification of the resulting radioactive iron, cobalt and nickel. After neutron irradiation of the oils in a small reactor of TRIGA-II type, followed by chemical separation based mainly on ion exchange of the iron and cobalt, the nickel was separated by Ni-dimethylglyoxime precipitation method. These elements were determined by β- decay and γ-spectrometory. The sensitivity limits were about × 10-7 grams for iron, × 10-8 grams for cobalt and × 10-9 grams for nickel when 13 grams samples are irradiated for 0.5150 hrs. in a thermal neutron flux of about 1012 n/cm2/sec.
Methyl 10-undecenoate and mercuric acetate were allowed to react in acetic acid to give methyl acetoxy acetoxy mercuri-undecenoate. The mercurial adduct was then reacted in acetic acid with benzene, toluene, o-xylene, m-xylene, p-xylene, phenol, catechol, o-cresol, m-cresol, p-cresol and anisol in 1 : 10 mole ratio each at 6065°C for 5 hours in the presence of perchloric acid as aa catalyst, which gave methyl 11-aryl-9-undecenoates corresponding to the respective arylic compounds.. The yields of these compounds were 36.968.5%. The solubilizing power of aqueous solutions of sodium salts therefrom, using dimethylaminoazo benzene as solubilizate, was excellent ; namely 9.4 dye g/mol sodium salt for 11- (3, 4-dihydroxyphenyl) -9-undecenoate and 6.2 dye g/mol sodium salt for 11-phenyl-9-undecenoate.
Authors studied the isolation technique and some properties (NMR, UV, IR, GLC, TLC, and saponification rate) of the trimethyl esters of mono-maleic anhydride adducts of oleic acid and trans-trans conjugated octadecadienoic fatty acid. The silicic acid column chromatography or thin-layer chromatography technique using silica coated plate and solvent system consisting of petroleum ether-diethyl ether=7 ; 35 : 5 (vol/vol) resulted in good effects on the isolation of mono-maleic anhydride adducts. In the case of oleic acid adduct, it was found that a-methylene group adjacent to double bond disappared (by NMR) and cis-double bond was converted to traps form (by IR and NMR), then it was conjectured that the succinic acid type adduct was formed. In the case of trans-trans conjugated octadecadienoic fatty acid adduct, cyclohexene type adduct was formed which differed from oleic acid adduct. The separation of cyclohexene type adduct and succinic acid type adduct each other from their mixture was found to be possible by the programmed gas liquid chromatography technique using 3 % SE-30/chromosorb W column and hydrogen flame ionization detector. The peak temperature of the former was 203°C, and the latter was 194 °C. In addition, surface active properties of their tripotassium salts were discussed.
A polymerization o acrolein was carried out with benzoyl peroxide as a catalyst in the presence or the absence of a solvent. The methods, which measured chemical properties of the white poly-acrolein obtained, were established before the investigation of the polymerization. Thus residual double bonds and the residual aldehyde group in the polymer could be measured by means of a Wijs method and a sodium bisulfite method, respectively; these measurements taking 120 and 48 hrs for the quantitative analyses, respectively. Polyacrolein grew abruptly with increase in the reaction temperature and the acrolein concentra-tion, but the kind o solvents (benzene and n-hexane) did little effect on the formation. The poly-mer was found to have more residual double bonds under lower reaction temperature and a lower acrolein concentration, whereas the residual aldehyde group became less when reaction temperature wass lowered. The sum of both residual groups, to cite instance of the bulk polymerization, was 9095% at 90°C, 6070% at 70 °C and 4550% at 50 °C. Thus, the consumption of functional groups, especially aldehyde group, increased with lowering of the reaction temperature. Furthermore, these two functional groups decreased with lapse of the reaction time. In order to explain these findings, polyacrolein was separated into its pyridine-soluble and -insolble parts, and the ratio of both parts and their respective residual functional groups were measured. Consequently, by the use of benzoyl peroxide, acrolein was polymerized mainly through its cleavage of the carbon-carbon double bond. The polymers thus formed as a result o the cleavage were subjected to react secondarily by themselves; intermolecular cross-linkings by mutual aldehyde groups especially in the case of lower temperature and acrolein concentration, and intermolecular cross-likings through double bonds and aldehyde group in the case of higher temperature and acrolein concentration.
The shake culture method was adopted as the Testing Method for Biodegradability of Synthetic Detergent in the Japanese Industrial Standard in April 1967. Japanese Ministry of International Trade & Industry is executing its administrative recommendation toward the change-over to biodegradable detergents. Detergent industry is promoting the change-over by its own initiative prior that recomendation. The authors estimated that the proportion of biodegradable surf actants with straight alkyl chain was ca. 54% of the total anionic surfactants for use of household detergent and that of linear alkylate sulfonates within the alkylbenzene sulfonates used was ca. 38% in the middle of 1967, and that these proportions turned to ca. 61% and 48%, respectively, at the end of 1967. At that turning stage, determinations of the content of linear alkylate self onates in total of the alkylbenzene sulfonates in raw municipal sewages, effluents from sewage treatment plants, and river waters were carried out in Aug.-Sept., 1967 and Feb.-March, 1968. It was found that the content of linear alkylate sulfonates were <531% (Aug.-Sept., 1967) and <540% (Feb.-March, 1968). This rather higher figures of some 30 or 40% obtained with river waters indicate the direct discharge of domestic sewage into rivers and necessity for treating the sewage in sewage treatment plants. From those results, it is believed that remarkable effect of the change over is difficult to expect under the present situation, some 120% of pervasion of sewerage systems.
Various phthalates and aliphatic diesters were analysed by gas-liquid chromatography qualitatively and quantitatively. Two columns of lower content liquid phase, such as 1.4% neopentylglycol sebacate or 1.2% SE-30 on Diasolid-M, were used in order to separate the esters having higher boiling points. By using the internal standard method, those esters were successfully separated and analysed quantitatively with considerable good accuracy. The vapour pressures of several esters could be estimated from relative retention times (Rr) against the standard substances such as DEP or DOA. By inserting these values in Clausius-Clapeyron's equation, the latent heat values Δ H were calcurated. Rr was discussed in terms of activity coefficient r and latent heat ΔH. Consequently, the corrected Rr could be revealed only by the difference of Δ H between the samples and the standard substance, and was indifferent with the kind of columns.