The analytical method to determine a small amount of ABS in toothpaste is successfully completed : In order to eliminate sodium alkylsulfates and other methylene blue active materials, alcohol extract of toothpaste is refluxed for 2 hr with 1 : 2 hydrochloric acid. If ABS exists in the hydrolysed solution, it can be determined by Abbott's method. Thus, about 0.05% ABS which is previously mixed with toothpaste is quantitatively determined by this method.
Condensation products of oleic acid and paraformaldehyde in acetic acid solution were saponified and then fractionated by recrystallization, and the following two substances were obtained [1 part of oleic acid reacted with 2 parts of formaldehyde effectively in 1 hr when 1% of HClO4 was used as a catalyst (Fig. 3)]. One of them had mp 117-118°C and seemed to have pyranol-4 structure because of its characteristics (Table 1 & Fig.-1) and it was considered as 3-octyl-4-hydroxy-5-carboxyhexyltetrahydropyran (or 3-heptyl-4-hydroxy-5-carboxyheptyltetrapyran). Pigulevskii assumed in his report about the same reaction that the product had pyranol-3 structure. And the other was C18H36O3, mp 70-71°C, A.V. 184.5, and from the IR spectrum (shown in Fig.-2), it was considered as monohydroxystearic acid (mixture of 9-and 10-hydroxy acids). As the catalyzers, perchloric acid was most effective, and sulfuric acid and borontrifluoride etherate were also fairly effective (Table 3).
Authors investigated the condensation of octadecene-1 with formaldehyde in acetic acid at the presence of perchloric acid as, the catalyst. The reaction products were saponified and fractionated by recrystallization and chromatography, and three substances were separated. The characteristics of these substances were corresponded to those of nonadecadiol-1, 3 (mp 75-75.5°C), 3-pentadecatetrahydropyranol-4 (mp 65-66°C) and octadecanol (mp 41-44°C., mixture of alkanol-2 and-3), respectively. The presence of alkyl-1, 3-dioxan, known as one of the main products of lower olefine condensed with formaldehyde, was also recognized in this case from IR spectrum of the lower melting fractions of the filtrate, but it was not isolated because of its small quantity. As the catalyzer, perchloric acid was more effective than followed sulfuric acid and borontrifluoride etherate in the above reactions. The larger the quantity of paraformaldehyde used against olefine, the greater the yield of the products obtained, but more pyranol was obtained in case of 1 : 1 molar ratio than other cases (Table 1). The saponification value of the product was the highest at 3 hr reaction time, and the reaction was seemed to proceed easily (Fig. 4). Octadecene-1 did not react with formaldehyde without acetic acid in inert solvent such as ethanol or in the presence of 50% acetic acid, also it did not react with aqueous formalin even in acetic acid (Table 3).
In the previous report, authors described on the bis-cyanoethylation of cetyl amine. In this paper, studies on the bis-cyanoethylation of hexyl amine and nonyl amine are reported. In this experiment, the relation between the reaction in polar solvent or in non-polar solvent and the composition of cyanoethylate was investigated. As a result, cyanoethylation to form mono-compound and his-compound was a successive reaction and bis-compound was obtained with a yield of about 90% under the suitable condition in methanol solvent, whereby a mixture of 2 parts of solvent per part of amine and 3 mol of acrylonitrile per mol of amine was used and the mixture was refluxed at reaction temperature of 70°C in atmospheric pressure and maintained at reflux for 48 hr. Optimum conditions in the reaction to hexyl amine and to that of nonyl amine were nearly the same except that the reaction velocity of the former was something fast. At the reaction in benzene solvent, under the same condition abovementioned, mono-compound obtained from the both amines was at yield from 94 to 97%, and bis-compound from the both was at yield of about 3% respectively. In the case of non-solvent, under the same condition, mono-compounds from the both amines were at yield of about 85%, and about 15% for his-compounds. Authors found it as the difference in reaction velocity between those amines and cetyl amine in the bis-cyanoethylation, that the change in reaction temperature ranging from 20 to 70°C had no exceeding influence upon the yield of the bis-compounds of the both amines, and that the reaction velocity to form bis-compound with both amines in the methanol was slower than that of cetyl amine.
It has been found there exist two types in the deterioration of frying oils, and they are named J and S types from their respective deterioration types. J is original deterioration type which appear in most oils, while some oils belong to S type inhere unstable factors such as that they were stored in undesirable condition or color reversion were developed fastly in them. Each type has always its induction and subsequent weariness periods (so called TSUKARE), and latter develops rapidly after the former period. The TSUKARE (weariness) has been ordinally identified by the change of foaming conditions to be occurred during frying. However, it often occurred that the induction period was not seen, because the sampling is generally made on a periodical basis in the evaluation test of frying stability. In this study, the potato chips (at the rate of 1 kg an hour) were fried at 190°C by using 1.5 kg of five kinds of soybean oil. Those sampling for the objective test were fixed on the basis of the foaming conditions, giving up the periodical sampling. The results of this experiment were as follows : 1) The change in iodine value, carbonyl value, viscosity and ultra violet absorption spectra have been found extremly useful in evaluating the induction and subsequent weariness period, but the others (refractor, color and acid value) were not so helpful. 2) The absorption band of conjugated dienoic acid (at about 230 mμ), which showed a broad range and increased slowly during the induction period, were developed intensely and rapidly with progress of the TSUKARE (weariness). On the other hand, it was also found that those absorptions of conjugated trienoic acid (at 259, 268, 279 mμ) were very clearly indicated during induction period, but tended to disappear in the order of 259, 279, 268 mμ as the TSUKARE advances. 3) After the TSUKARE appeared in the frying, the sampling must be done frequently to take hold of progress in the induction and weariness periods.
The authors contemplated to prepare triol polyether by liquid phase polymerisation of propylene oxide using glycerine, trimethylolplopane or 1, 2, 6 hexanetriol as starting material and found that catalyst concentration and mole ratio of starting material to the oxide effected to the reaction velocity of polymerisation and the average molecular weight, colour and unsaturation of the polymer. It was also studied to prepare polyether with tetraol or hexaol. Further investigations were made on the conditions of purification of crude polyether such as neutralizing agent, filtering method and stripping method under reduced pressure.
In this paper, polyoxyethylene nonylphenyl ether EO 10 mol (PEG-N10) and dodecyl benzene sulfonate (Na-DBS) were investigated on the relationship of detergency and quantity of surface active agent absorbed by fabric. It was found that there was a close relationship between quantity of surface active agent absorbed and whiteness retention with wool, and the reason why PEG-N10 is somewhat inferior to Na-DBS in maximum detergency is justifiable because of its lower whitenness retention.
Contamination of fruit and vegetables such as grape, cabbage, turnip and cucumber by the detergent solution of sodium dodecylbenzene sulfonate (SUBS) have been investigated by means of the radiotracer method using SUBS labeled with radioisotope 35S. The measurement of contamination was chiefly made for cabbage under varying conditions of the difference in the part and in water content of cabbage leaf, concentration of the detergent solution, dipping time and temperature, and rinsing time. The effect of sodium sulfate as a builder was also studied. Under the usual condition of dipping in 0.1% detergent solution for five min at 1618°C, followed by rinsing twice with 100 cc of water for 20 sec, the contaminations observed were 0.29 γ/cm2 for the surface and 1.8 γ/cm along the cracks and damages of cabbage leaf. Air dried cabbage leaf suffered from stronger contamination than the fresh one. The contamination of grape was about the same but those of turnip and cucumber were three or four times as much as that of cabbage when compared in the unit of contamination per area, but the results were just opposite when the usual unit of contamination per 100 g of the sample was used. We considered the latter expression to be unreasonable.