The catalytic addition reaction of diester of fumaric acid to safflower fatty acid methyl esters by flow method was investigated. It was found that the addition of diethyl fumarate to safflower fatty acid methyl esters is easily carried out by continuously passing the mixed sample of the methyl esters and diethyl fumarate at molar ratio of 1 : 1 over a high surface-area synthetic silica-alumina catalyst composed of 70% of SiO2 and 29% of Al2O3. The adduct separated by column chromatography was analyzed to have a cyclohexene ring structure by IR, NMR, and MS spectral measurement, and was confirmed to be formed by the Diels-Alder addition of diethyl fumarate to conjugated octadecadienoate.
The separating and estimating conditions for anionic surfactants by TLC were studied. 1) Sodium salts of dodecylbenzenesulfonate (LAS), dodecyl sulfate (LS-Na) and 1-dodecanesulfonate (SAS) were prepared and used as standard materials and samples. 2) The optimum conditions for TLC were as follows; Stationary phase : Silica Gel G impregnated with 10% ammonium sulfate. Activating temperature and time : 110°C, 80min. Developing solvent : 2-methyl-4-pentanone·propyl alcohol·0.1N acetic acid·acetonitrile (volume ratio, 20 : 6 : 1.6 : 1). Charring temperature and time : 250°C, 15min. Detecting reagent : No use. 3) Mixtures of LAS, LS-Na and SAS were separated and estimated each other by TLC under the above optimum conditions. The experimental error and coefficient of variation were 0.23.8% and 0.374.75 respectively.
The effect of the types of solvents on the solubilization of water in nonaqueous solutions of purified sodium 1, 2-bis- (2-ethylhexyloxycarbonyl) -1-ethanesulfonate (Aerosol OT) has been studied. The characteristic temperature, at which the solubilization of water is abruptly increasing, was found in certain nonaqueous solvent systems of purified Aerosol OT, such as benzene, toluene, tetrachloroethylene systems etc.. The characteristic temperature tends to be higher if the solubility parameter and/or the dielectric constant of solvent is large. The effect of NaCl added on the solubilization of water in nonaqueous solutions of purified Aerosol OT has been also studied. The maximum temperature of solubilization of water elevated and maximum amount of solubilization increased by adding a small amount of NaCl. It was also found that the solubilization curve for insufficiently purified Aerosol OT are mainly affected by water-soluble impurities (electrolytes).
An automated conductometric method for the determination of carbonates in detergents has been developed. Using Technicon Auto Analyzer II, sample solutions were injected automatically into the continuous flow of acidic solution with air segmentation. The evolved carbon dioxide was introduced into the flow of deionized water, and then detected automatically by electric conductometry. The surface of sample solutions was covered with liquid paraffin to prevent the contamination of carbon dioxide from air. The range of the determination for sodium carbonate was from 10 to 200mg/l and the proposed method was applied to the determination of carbonates in several commercial detergents. The results agreed with those of conventional gas chromatographic method. The capacity of this method is 30samples/h.
Infrared spectrophotometric methods for the determination of isolated trans isomers in fats and oils were studied collaboratively, using methyl elaidate, methyl stearate, and methyl esters of partially hydrogenated vegetable oils. A study was made to compare the AOCS tentative method with the IUPAC standard method. As the results of the collaborative tests, the IUPAC method was found to be more accurate than the AOCS tentative method. More accureate results, however, could be attainable by using a modified base line from 1050cm-1 to 940cm-1 in the AOCS tentative method. Furthermore, the influence of the methods of preparing methyl esters on the determination of isolated trans isomers was studied. Both the BF3-and H2SO4-methanol methods were consequently suitable for the preparation of methyl esters on the determinatiton of isolated trans isomers in fats and oils.
The mechanism of catalytic addition reaction of maleic anhydride to castor fatty acid methyl esters by flow method was investigated. It was found that the mono ester of maleic acid with the hydroxyl group of methyl ricinoleate, 1-hexyl-11-methoxycarbonyl-3-undecenyl hydrogen maleate, was formed in 40% yield at 130°C by continuously passing the mixed solution of methyl ricinoleate and maleic anhydride at molar ratio of 1 : 1 over a high surface-area synthetic silica-alumina catalyst composed of 70% of SiO2 and 29% of Al2O3. Then, it was assumed that the mono ester plays a role as intermediate in the dehydration reaction of methyl ricinoleate for producing methyl octadecadienoate.