BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 14, Issue 8
Displaying 1-23 of 23 articles from this issue
  • Makoto OTOMO
    1965 Volume 14 Issue 8 Pages 677-682
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Iron (III) reacts with an excess of Xylenol Orange to form 1:1 and 1:2 complexes with their absorption maxima at 545 and 500 mμ, respectively, while only a 1:1 complex with its absorption maximum at about 586 mμ is formed when an excess of iron is present. The molar extinction coefficients and the apparent formation constants of these complexes were spectrophotometrically determined.
    As little as 3μg/25ml of iron was determined successfully with any one complex of the former two, and as little as 0.025μmol/25ml and of Xylenol Orange with the latter. The absorbance in every case conforms well to Beer's law.
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  • Naoichi OHTA, Hiroshi MORITA
    1965 Volume 14 Issue 8 Pages 682-687
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The spectrophotometric method for glucose by picric acid was studied and improved.
    On the concentration of picric acid as a color developing agent, alkaline picric acid reagent in Lewis-Benedict method was too thick to measure the absorbance of the reacted solution against the reagent blank at its maximum absorbing wavelength 460mμ. On the other hand, the highest and constant absorbance of the reacted solution was obtained only in the presence of picric acid more than five times of glucose. The authors recommended 0.05M aqueous solution of picric acid.
    The comparison of alkali reagents showed that the maximum color development was obtained in 0.4N NaOH medium, but the discoloration occurs at above 0.4N. When Na2CO3 or K2CO3 was used, the color development showed a positive correlation with the concentration of the alkali reagent, and the absorbance of the solution reached almost constant value by Na2CO3 above 0.6g/5ml.
    The authors proposed the following procedure. Add 1ml 0.05M picric acid and 3ml 20g/100ml Na2CO3 to 1ml sample solution containing 010-5mol glucose (or reducing sugar). Mix and heat on boiling water for 10 minutes. Cool and dilute to 25ml with distilled water. Measure the absorbance of colored solution at 460mμ against reagent blank or 520mμ against H2O.
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  • Takashi HATTA, Masamichi KUROSAKI, Toshihisa SUNADORI, Hironori HASHIM ...
    1965 Volume 14 Issue 8 Pages 688-691
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method was proposed for the determination of 1-chloro-1, 2-dibromoethane (CDB) in the oils and emulsions by using a two-stage gas chromatography equipped with a four-way cock between the first column and the second one. The peak of CDB was apparently separated from those of the oils and emulsions on the second stage of gas chromatogram. The first column (4 mm × 2 m, stainless steel) of the apparatus stated hereinbefore contained 15 weight per cent of high vacuum silicone grease and 2 weight per cent of stearic acid as the stationary phase and the column temperature was maintained at 120°C. On the other hand, the second column (4 mm × 3 m, copper) contained 10 weight per cent of Thermol-2 as the phase on the support of Shimalite and its temperature was adjusted to 110°C. Analysis of the sample containing anisole (AN) as the internal standard was made by employing helium as the carrier gas with the flow rate of 60 ml per minute on the Shimadzu Gas Chromatograph 2A and 2B. The standard deviation and the mean recovery by the abovementioned method were 0.5 to 0.6% and 99.5 to 100.7%, respectively.
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  • Akira YAMAMOTO
    1965 Volume 14 Issue 8 Pages 692-697
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Glass shows a continuous change of viscosity accompanied with several transformations in an extremely wide temperature range by heating, and the characteristics in this range have a special importance. The conventional viscosimetric or dilatometric methods of measurement about these characteristics can be applied only at a narrow temperature interval.
    The author recommended the DTA method as a useful one for the continuous measurement of glass characteristics throughout the above mentioned temperature range, i. e. from room temperature up to the fusing temperature.
    The suitable selected analytical conditions of the DTA as well as its optimum structual design enabled us to obtain accurate and stable DTA records of glass samples.
    DTA data on commercial glasses, e. g. lead glass, boro-silicate glass, non-alkali glass, and several optical glasses are examined, and a method of detecting the characteristic points of these glasses, including transformation points tg, annealing point ts, incipient deformation point Mg, softening point tsoft, sintering point tsint, flow point tf, and working point tw, is proposed from the exo- and endo-therm peak features.
    By the temperature readings of these characteristics points according to the up mentioned method and these corresponding viscosity values which decided by definitions, the possibility of drawing the temperature-viscosity curves for individual samples is suggested.
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  • Tetsuhei TACHIKAWA
    1965 Volume 14 Issue 8 Pages 697-701
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The potentiometric titration of copper (II) with EDTA and the reverse titration were carried out by use of two bimetallic electrode couples: platinum-tungsten and platinum-molybdenum. Titration curves were constructed and the magnitudes of change in potential at the end point (ΔE/ΔV) were compared. Furthermore, the influence of the addition of ethyl alcohol on them was investigated.
    In case of the titration of copper (II) with EDTA, both platinum-tungsten and platinum-molybdenum couples gave S-shaped titration curves. The magnitudes of change in potential at the end point at pH 4 were greater than that at pH 10 for both couples. The addition of ethyl alcohol was slightly inclined to decrease the magnitude of ΔE/ΔV with a few exceptions.
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  • Ohiko KAMMORI, Isamu TAGUCHI, Kazuyoshi TAKAHASHI, Toshio KOIKE
    1965 Volume 14 Issue 8 Pages 702-707
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The photometric method for determination of palladium with thiooxine has been newly improved for iron and steel. The MIBK extraction and the thiourea washing methods have been successfully adopted to remove the interfering elements.
    For the determination of 0.30.005% palladium, 0.4 g of sample is decomposed with aqua regia. Iron and molybdenum are removed with MIBK extraction method after nitric acid drived off. One-half % of thiooxine solution and 10 m/ of hydrochloric acid are added to the one tenth aliquot to form a red complex in 6N hydrochloric acid. The complex is extracted with chloroform and washed with 5ml of 1% thiourea-6N HCl solution to remove the co-extracted copperthiooxinate. Palladium is determined with the absorbance at 505 mμ. Five samples were analyzed in about five hours within an absolute error of 0.003%. Elements commonly present in iron and steel scarcely interfered.
    The determination of 0.010002% palladium in pure iron with micro sample spectrophotometer is also described.
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  • Keiichi FURUYA, Hitoshi KAMADA
    1965 Volume 14 Issue 8 Pages 708-710
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    There were discussions on the adsorption mechanisms of carbon monoxide by manganese in the vacuum fusion furnace. Thanheiser reported that manganese films deposited on the walls of the vacuum fusion furnace adsorbed carbon monoxide, while Wood et al. and Sawa reported that carbon monoxide adsorption by manganese occured when it was depositing. Carbon monoxide was allowed to circulate in a furnace and gas adsorption curves by manganese and chromium were measured at the different furnace conditions. By means of this method whether the adsorption of carbon monoxide occured at the depositing metal vapor or on the deposited films were partly clarified. Much more carbon monoxide was adsorbed by chromium vapor than chromium films on the furnace walls, although in the case of manganese it was adsorbed rather by films than vapor. The adsorption speed by manganese vapor was about 300 times greater than that by chromium vapor.
    In the analysis of steel samples containing manganese the adsorption mechanism by manganese might be affected by other components.
    These results will give useful informations for designing the apparatus.
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  • Shigeyuki TANAKA, Yukio ONO
    1965 Volume 14 Issue 8 Pages 711-716
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The infrared spectrometric determination of safrole in red camphor oils was disturbed by the ovelapping absorption bands of the coexisting components. This made the selection of the key band quite difficult and hinder the direct application of the I. R. spectrometry.
    The pretreatments of the sample including, thin layer chromatography and silica gel chromatography for removing interfering components was investigated, in which successive variation of developing solvents enabled the quantitative separation of safrole. Taking the absorption 1040 cm-1 of safrole and 1380 cm-1 of n-hexane usually remaining in the safrole fraction of the eluate as the key bands, the amount of safrole was determined accurately on the above two component system.
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  • [in Japanese], [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 717-720
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1965 Volume 14 Issue 8 Pages 720-723
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 723-725
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 725-728
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 728-730
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 731-732
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 732-735
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 735-737
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 737-739
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1965 Volume 14 Issue 8 Pages 739-742
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 742-745
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 745-748
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
  • [in Japanese]
    1965 Volume 14 Issue 8 Pages 749-755
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1965 Volume 14 Issue 8 Pages 756-763
    Published: August 05, 1965
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese]
    1965 Volume 14 Issue 8 Pages 764-777
    Published: August 05, 1965
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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