A method is described for the colorimetric determination of oxazolam, 10-chloro-2, 3, 5, 6, 7, 11b-hexahydro-2-methyl-11b-phenylbenzo [6, 7]-1, 4-diazepino [5, 4-b] oxazol-6-one, in pharmaceutical preparations, aqueous solution, urine, and blood serum. Oxazolam was hydrolysed with hydrochloric acid to 2-amino-5-chlorobenzophenone which was colored by the Bratton-Marshall method and the diazo dye was extracted with n-butanol. Color of the azo pigment was stable and absorbance of the solution was measured at 545 mμ. This colorimetric determination was suitable for routine use and has a detectability of 0.5-10μg/ml, it has a very acceptable recovery and reproducibility of the order of 98.5% from aqueous solution, 94.7% from urine, and 100.8% from blood serum. From these results, it was considered that this method can be applied as a reliable determination of oxazolam in forensic chemistry.

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The acute and subacute toxicity test of the selective herbicide, 2-azido-4-isopropylamino-6-methylthio-s-triazine (C-7019), newly developed by Ciba-Geigy Ltd., was examined, and results obtained were as follows : Acute toxicity (LD₅₀) value by oral administration after 48 hr was 2970 mg/kg (2434-3929 mg/kg) for male mice and was 3600 mg/kg (2951-4392 mg/kg) for male rats. Sedation, ataxia, and respiratory depression were the amin toxic signs. Intraperitoneal LD₅₀ value after 48 hr was 265 mg/kg (217-323 mg/kg) in male mice. Toxic symptoms of C-7019 by intraperitoneal administration differed from that of oral administration. Central excitation was observed which was then followed by toxic symptoms of oral administration. Three-month subacute toxicity test of C-7019 was carried out on mice and rats at dosage levels of 30, 50, 100, and 400 mg/kg/day in the diet, but the amount actually consumed was less than the planned dosages. No abnormal behavior due to toxicity was noted that could be related to C-7019, and no animals died in any of the groups during the experiment. Except for slightly reduced rate of body weight gain in rats, no remarkable differences compared to controls were observed in daily food consumption, growth (weight change) in mice, effect on blood (number of erythrocytes and leucocytes, hemoglobin, platelets, and blood picture), renal functions (urinary pH. glycosuria, proteinuria), liver functions (urobilinogen, bilirubin, activities of serum transaminase), or macroscopic observations on internal organs, their weight, and weight ratio. Animals which received C-7019 showed no adverse histopathological changes which could be related to C-7019 in the brain, lung, thymus, adrenal, spleen, testis, ovary, or bone marrow, except the infiltration of perivascular round cells in kidneys and focal cell infiltration in hepatic cells.

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Simulating a practical criminal case, six single hairs of the head from five individuals were sampled and analysed by the neutron activation analysis. Two samples which originated in the same person could be correctly selected by their analysis. As a method for hair individualization, Na, Cl, Br, and Mn in the samples were determined and examinations were made to see each element could be identified at matching limits of 10, 25, or 50%. It was concluded that 25% was usually permissable as the matching limit in practical cases. For the permission of a value more than 50% as the limit, more elements such as Zn, Hg, and others must be determined and the results must be collectively considered. There were no remarkable differences between the concentration of trace elements in a single hair and in strands of hair from the same individual.

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The possibility of blood grouping test utilizing hair samples previously irradiated with neutrons was investigated. Hair samples were collected from the individuals whose ABO blood group types were previously known by testing their blood cells. Irradiation of sample hair with neutrons was made for 1, 5, or 30 minutes from a pneumatic tube or for 5 hours in core, and integrated neutron doses were 4.7×10¹³, 2.3×10¹⁴, 1.4×10¹⁵, and 3.8×10¹⁶ n/cm², respectively. The activity in blood grouping test of the samples was inclined to decrease and the rate of misidentification increased in proportion to the integrated neutron dose. It was concluded that the usual blood grouping test is possible after irradiation with 10¹⁵ n/cm² of neutrons as the maximum dose.

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Thirty-three water samples were collected around the outflow of the Shioiri River at Tateyama City and each sample was analysed for the most probable number (MPN) of coli-form bacteria and for the concentration of NaCl. A significant correlation between the logarithm of the MPN value and the concentration of NaCl was ascertained by statistical analysis.

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Separation and identification of chlorinated phenoxy herbicides were examined by thin-layer chromatography using polyamide. The herbicides were developed with 14 kinds of solvent systems and visualized by spraying with silver nitrate, o-tolidine or o-dianisidine solution and irradiating ultraviolet ray. All the herbicides tested were distinctly separated by the solvent system composed of non polar solvent and acetic acid, e.g., benzene-acetic acid (9 : 1) or dichloromethane-acetic acid (19.5 : 0.5), and detected at the levels of 1-4 μg.

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Naphazoline contained in mixed eye-lotion was converted into N-acetyl and N-butyryl derivatives and determined by gas chromatography supported on 1.5% OV-17 along with chlorpheniramine maleate and T-caine, the consituents commonly present. The amount of sample corresponding to about 10 mg of naphazoline was taken, made alkaline with ammonia, and extracted with chloroform or carbon tetrachloride. The extract was dehydrated over anhydrous sodium sulfate and evaporated to dryness under reduced pressure below 40°. The residue was dissolved in 4.0 ml of 0.2% dioctyl phthalate solution, when T-caine was not present. To this solution was added 10 μl of acetic anhydride and shaken for 15 min. Excess reagent was decomposed by adding 2 ml of 10% sodium hydrogen carbonate solution. The chloroform layer was separated and dehydrated over anhydrous sodium sulfate, 1.0-2.0 μl of this chloroform solution was injected into gas chromatography. When T-caine was present, the residue was dissolved in 4.0 ml of chloroform solution of 0.2% dicyclohexyl phthalate, added with 20 μl of butyric anhydride, and shaken for 30 min. The excess reagent was decomposed with 2 ml of 10% sodium hydrogen carbonate solution. The chloroform solution was treated and applied to gas chromatography in the same manner as N-acetyl derivative. The decomposed products of naphazoline such as ethylenediamine, 1-naphthylacetic acid, and 1-naphtylacetylethylenediamine did not interfere in this method.

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In connection with oxidation of methyl linoleate with oxygen at 70-110°reported previously, the carbonyl compounds produced from hydroperoxides formed by this oxidation were examined. Besides the known methyl ester of formyloctanoic acid and hexanal, reported to have been formed by autoxidation of methyl linoleate, 2-octenal, 2, 4-nonadienal, methyl monoepoxyoctadecenoate, and another smalll quantity of substance assumed to be methyl formylundecenoate were detected as the oxidation products of methyl linoleate by means of gas chromatography and thin-layer chromatography of their p-nitro and 2, 4-dinitro-phenylhydrazones. The oxidation products of methyl linoleate by oxygen were compared with those obtained by periodate oxidation of epoxidized methyl linoleate (methyl monoepoxyoctadecenoate). Formation of malonaldehyde from methyl linoleate by air oxidation was also discussed.

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Chemical methylation of inorganic mercurial compounds with methylcobalamin, a vitamin B₁₂ analog, was examined. Quantitative determination of methylated mercury by gas chromatography and analysis of the products by thin-layer chromatography revealed that thh methylation proceeded at a markedly high rate by simply mixing methylcobalamin with inorganic mercury, and the reaction gave dimethylmercury as the initial and methylmercury as the final products. Comparative experiments using several other metal halides under the same condition indicated that mercuric chloride is a unique acceptor of the methyl moiety from methylcobalamin among these metal halides tested.

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Concentration of carbon dioxide and dust were measured in the underground market-streets, in subway trains, on the platforms of subway stations, in tearooms, cinemas, bowling alley, and department stores in Osaka city. Determination period were October, 1969∼January, 1970, December, 1970∼January, 1971, and November, 1967. It was found that air in the underground market-street was better than in subway trains, etc.

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