β-Hydroxybutyric acid-p-phenetidide (B), ethoxybenzamide (EB), and caffeine in antipyretic preparations were determined by gas-liquid chromatography with hydrogen flame ionization detector on a 2-m column of 1.3% Epon resin at 165°. B was changed to trimethylsilyl derivative by using a silyl reagent consisting of hexamethylidisilazane and trimethylchlorosilane. EB was slightly affected by using hexamethyldisilazane : trimethylchlorosilane (8 : 2) directly. Then the reagent was diluted withte trahydrofuran : chloroform (1 : 1) mixture and the effect can be eliminated. Determination was made successfully by the internal standard method using phenanthrene.

View full abstract

Acetylsalicylic acid, phenacetin, and caffeine in antipyretic preparations were determined by gasliquid chromatography with hydrogen flame ionization detector on 2-m column of 8% SE-52, at 170°. Acetylsalicylic acid was changed to trimethylsilyl derivative at room temperature by using hexamethyldisilazane and trimethylchlorosilane. Determination was made successfully by the internal standard method using dibutyl phthalate.

View full abstract

Aluminium-acetylsalicylic acid (Asp-Al), phenacetin, caffeine, and acetaminophen were determined by gas-liquid chromatography with hydrogen flame ionization detector on a 2-m column of 10% QF-1, at 170°. i) For Asp-Al, phenacetin, and caffeine preparations, mixture of these three was added to 40 ml of 0.5% sodium fluoride solution (0.2N HCl) at room temperature. After 20 min, only Asp-Al was decomposed to acetylsalicylic acid, and acetylsalicylic acid, phenacetin, and caffeine were extracted with chloroform. The solvent was evaporated from the extract on a water bath and the cooled residue was silanized. ii) For Asp-Al, AA and caffeine preparations, AA and caffeine were extracted with chloroformacetone (1 : 1) mixture, and the residue which contains Asp-Al was added to 40 ml of 0.5% sodium fluoride solution (0.2N HCl) at room temperature. After 20 min, acetylsalicylic acid was extracted with chloro-form. This chloroform solution was mixed with the former chloroform-acetone solution, and this was evaporated on a water bath. The cooled residue was silanized. Determination was made successfully by the internal standard method using dipropyl phthalate.

View full abstract

In a series of the studies, the antioxidant effect of D, L-α-tocopherol and the synergistic effects of some kinds of organic acids on the oxidation of methyl linoleate (ML) with oxygen were reported in this paper. Samples and experimental conditions were same as those described in the previous paper. Oxygen was passed through purified ML with or without the antioxidant and the synergists, then the samples obtained were estimated for peroxide value. Antioxidant effect of α-tocopherol on the oxidation at 105°was shown little in the absence of the synergist, but was remarkable in the presence of ascorbic acid or citric acid. The effect of α-tocopherol on the oxidation at 70°was clearly observed even without any synergist, but the addition of it increased markedly the antioxidant offect of α-tocopherol. The effect of α-tocopherol was compared with that of butyl hydroxy anisol (BHA), which had been reported in the previous paper. It was shown that the effect of BHA was more active than that of α-tocopherol ; even a half equivalent of BHA was more effective than α-tocopherol on the oxidation at 70°. Sixteen kinds of organic acids and esters were examined for the synergistic effect with α-tocopherol and eight of them were found to be effective in preventing oxidatien of methyl linoleate ; D, L-malic, L-tartaric, oxaloacetic, malonic, citric, L-ascorbic, and D, L-gliceric acids and diethyl malate were effective ; succinic (weak +), tartronic, propionic, lactic, β-hydroxybutyric, and pyruvic acids, gluconolactone, and triethyl citrate were ineffective. The mechanism of the synergistic action of these organic acids seemed to be complicated, but the synergist was assumed to act as a hydrogen donor to α-tocopherol (or its oxidation products).

View full abstract

Chromium in water or soil was oxidized to a sexivalent state with potassium permanganate and extracted from the acidic aqueous solution with methyl isobutyl ketone containing trioctylamine, and then determined by atomic absorption spectrophotometry with air-acetylene flame. Extraction fficiency was about 100% by single extraction. This method was not interfered even in the presence of a large quantity of many other metals such as iron, nickel, copper, aluminium, zinc, lead, and manganese.

View full abstract

Fundamental studies were carried out on the removal of polychlorinated biphenyls (PCB) contained in polluted source of supplying water. Activated carbon and coagulants such as aluminium sulfate and polyaluminium chloride (PAC) were used for removing PCB from water. In the present work, method for determination of PCB was also studied. Gaschromatographic determination of decachlorobiphenyl (DCB), which was obtained by complete chlorination of PCB with SbCl₅, gave a good result. Among several preparations of PCB, Kanechlor-600 in water was determined as DCB in a good yield by gaschromatography, after extraction with n-hexane, concentration with Kuderna-Danish condenser, and chlorination with SbCl₅ in a sealed glass tube at 200°for 1 hr. Removal of PCB from water was tested with Kanechlor-600 usnig the above method of determination. Two processes of treatment for aqueous solution containing 1ppm of Kanechlor-600 showed about 90% removal. One of them was the addition of activated carbon powder and coagulant at the same time, and the other was to pass the solution through a column of granular activated carbon. These processes were used in the purification system of water supplying work in some instances. It is considered that such higher purification system will be effective in removal of PCB from polluted water.

View full abstract