BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 7, Issue 11
Displaying 1-16 of 16 articles from this issue
  • Studies on the determination of nitrogen in nitrocellulose and nitric acid. II
    Tetsuro MURAKAMI
    1958 Volume 7 Issue 11 Pages 681-684
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    After treating nitric oxide evolved from the Lunge nitrometer with ferrous sulfate solution, the residual gas was used for the mass spectrometry. Although there were great differences in the amount of residual gas, depending upon whether the solution had been boiled or not before the gas was absorbed, the major element in either case was nitrogen. The ratio of N2/Ar in the residual gas was determined to be about 50, which is very close to the (N2/Ar) ratio of the gas dissolved in sulfuric acid or in water.
    Therefore the absorption method for the removal of nitric oxide was found not to be recommended, and error may occur during the manipulation. Carbon dioxide in nitrometer was measured by the gravimetric method and was given about 0.15% regardless of the concentration of sulfuric acid used. But no sulfur dioxide gas was recognized in it when 94.5% or 98% sulfuric acid were used.
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  • Studies on the determination of nitogen in nitrocellulose and nitric acid. III
    Tetsuro MURAKAMI
    1958 Volume 7 Issue 11 Pages 685-690
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    By cooling with liquid oxygen, nitric oxide evolved from the Lunge nitrometer was separated into condensed and in-condensed portions. The condensed portion was further separated into two portions; by vaporization at -130°C leaving an in-condensed portion. These three portions were then used as the sample for the mass spectrometry and the composition was determined.
    0.20% nitrogen was found in the gas when both 94.5% and 98% sulfuric acid were used, and these N2/Ar atios corresponded with that of the sulfuric acid in which nitrogen and argon had been previously dissolved. Judging from this, the nitrogen cannot be formed due to the reaction in the nitrometer but rather is caused by the evolution of the nitrogen dissolved in the sulfuric acid. On the other hand nitrous oxide was a by-product produced by the reaction in the nitrometer. The formation of nitrous oxide was 0.22% when 94.5% sulfuric acid was used, and 0.39% when 98% sulfuric acid was used; the more concentrated sulfuric acid was used, when the more vigorously this side reaction occurred. The same result was obtained when the sample was potassium nitrate. Nitrocellulose samples gave about 0.17% carbon dioxide when either 94.5% or 98% sulfuric acid was used. The percentage of carbon monoxide evolved was 0.02% when 94.5% sulfuric acid was used, and was 0.24% when 98% acid was used; potassium nitrate samples showed a difference in that they yielded no carbon dioxide cr carbon monoxide.
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  • Fumikazu KAWAMURA, Hiroshi NAMIKI
    1958 Volume 7 Issue 11 Pages 691-695
    Published: November 05, 1958
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    In order to determine phosphine in acetylene rapildy, method to determine the light absorbancy of molybodenum blue has been investigated. A gaseous sample of 2550 ml contained in a 100ml capacity injector is introduced into an absorption vessel, large sized test tube, containing 20ml of 0.3% bromine water in 1 min. The sample is oxidized and transferred into a 50 ml measuring flask after 10% sodium sulfite is added dropwise for reduction of the excess bromine, 5 ml of a mixture of 6.5 N H2SO4-1.5% ammonium molybdate and 0.25 ml of 2% SnCl2 are added to the solution. The sample solution is allowed to stand for 10 min at 25°C and the absorbancy of blue colored solution is measured with photoelectric colorimeter. The calibration curve was prepared by using a solution of a standard phosphate solution containing an equal amount of bromine and sodium sulfite to the sample solution and by developing a molybedenum blue after reduction with SnCl2. Acetylene evolved from calcium carbide is collected in a gas holder and the phosphine content is determined by this method and by the JIS method. Good agreements are observed between the results of both methods. In order to avoid the loss of phosphine in acetylene while standing for long time, an apparatus indicated in Fig. 1 was made. By this method, phosphine can be determined in 15 min. This method is also applicable for rapid determination of phosphine in acetylene in plant operation.
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  • Fumio AOKI, Seishi YAJIMA, Toshio KUROSAWA
    1958 Volume 7 Issue 11 Pages 695-699
    Published: November 05, 1958
    Released on J-STAGE: February 15, 2010
    JOURNAL FREE ACCESS
    A sample solution of fission products which had passed about 2 years since its arrival was measured by a gamma-ray scintillation spectrometer. And Ce-Pr-144, Ru-Rh-106 and Cs-Ba_??_-137 were identified by their photopeaks in the spectrometer scan. Further, the sample was separated into several fractions through a cation exchange resin column. The relative activities of the nuclides cited above and Zr-Nb-95 (which was identified in a fraction separated) were roughly obtained from their photopeaks of their principal gammas. Comparing the activities obtained with those of Hunter and Ballou's graph, the cooling time of the fission products was estimated about 2.5 years.
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  • Studies on the metallurgical polarographic analysis. V
    Yoshiaki MIURA
    1958 Volume 7 Issue 11 Pages 699-702
    Published: November 05, 1958
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Rapid and simultaneous determinations of copper and iron in aluminum and its alloys by polarographic method have been investigated and the following method was established. The sample is taken up in sodium hydroxide solution and sodium sulfide solution is added to separate a precipitate containing copper and iron sulfides. The precipitate is taken up in a solution of a dilute nitric acid containing bromine water and simultaneous polarographic determinations of copper and iron are carried out by the use of supporting electrolytes of 0.5 M ethylenediamine tartrate and 0.1 M pyrophosphate. Satisfactory results were obtained by using a calibration curve method and an absolute method for standard samples secured from National Bureau of Standards and factory samples.
    The time required for the analysis of the two components was about 7080 min.
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  • Yasushi MASHIKO, Noboru HOSOYA, Minoru AKIMOTO
    1958 Volume 7 Issue 11 Pages 702-706
    Published: November 05, 1958
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    In Heyrovsky circuit for derivative polarography, a current corresponding to ΔE always flows through the recording meter, and when the zero point of recording meter is adjusted, the value of ΔE is altered.
    The Heyrovsky circuit was therefore improved as shown in Fig. 3. The experimental results obtained with the circuit of Fig. 3 were as follows.
    (1) The recording meter does not remove its zero point on application of ΔE potential, after the bridge circuit is balanced.
    (2) Under a satisfactory state of balance, the pulse current with dropping mercury electrode disappears, if the drops of two mercury electrodes are synchronized.
    (3) The derivative polarogram recorded by this circuit shows a symmetrical curve against maximum potential. This maximum potential is in good agreement to the half wave potential, if IR drop and recording lag of the recorder are corrected.
    (4) The values of peak current are generally reproducible to ±1.6% difference, and they are strictly linear function of the concentration.
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  • Nakaaki ODA, Masaji KUBO
    1958 Volume 7 Issue 11 Pages 707-711
    Published: November 05, 1958
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Methods of quantitative determination of chlorine in metallic titanium so far adopted were examined and a rapid method was proposed as the results of the examination. Hydrofluoric acid (20 cc per 5 g of sample) is taken as the best reagent to decompose the sample without any loss of chlorine (Table 1 and 2). Nitric acid added to hydrofluoric acid worked as an oxidizing agent to eliminate hydrolysis of titanium (Table 3). Chlorine was centrifuged in the form of silver chloride and turned to separable form (Table 4). Micro-glass filter and a small drying box helped the rapid filtration and drying of silver chloride (Fig. 1 and Table 8). This method showed 100% recovery (Table 5) of total chlorine in metallic titanium being contained in the forms of chloride and chlorate. The precision is assumed 5% and the lower limit of the determination is 0.005% Cl (Table 6). The time required for analysis was 40?70 min. a sample (Table 8).
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  • Tsugio TAKEUCHI, Fukuzoo HAYAKAWA
    1958 Volume 7 Issue 11 Pages 712-716
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Quantitative determination of a small amount of saturated hydrocarbons in a special grade benzene by gas chromatography has been investigated. Gas chromatograms, were obtained by using a column of tricrecylphosphate or carbowax as a liquid phase and using hydrogen gas as a developing gas. Before the appearance of the peak of benzene, four peaks were obtained. Pure saturated hydrocarbon which was though to be present as an impurity in benzene was added each by each to the pure benzene sample and gas chromatogram for this specimen was obtained in the same way as for the sample benzene. Then qualitative determination of the impurities was made by the comparison to the peak of known substances. In the quantitative determination, a definite amount of ethyl ether was added as an internal standard substance and the relative intensities of the spectra were measured with respect to that of the internal standard. A calibration curve prepared by plotting the relative intensity of the peak of the impurity as the function of its concentration in ether was used for quantitative determination.
    As an example of the analysis, the presence of 0.16% n-heptane, 0.08% cyclohexane, 0.07% methylcyclohexane, and a small amount of n-hexane and an unknown impurity was found. By the fractional crystallization, a pure benzene showing no impurity by the above gas chromatography was prepared.
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  • [in Japanese]
    1958 Volume 7 Issue 11 Pages 717-718
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 718-720
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 720
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 721
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 721a-724
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 725-732
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1958 Volume 7 Issue 11 Pages 732-736
    Published: November 05, 1958
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese]
    1958 Volume 7 Issue 11 Pages 737-741
    Published: November 05, 1958
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
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