BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 12, Issue 9
Displaying 1-18 of 18 articles from this issue
  • Mitsuo KIBOKU
    1963 Volume 12 Issue 9 Pages 797-799
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Determination of carbon disulfide was made by using a standard potassium ferricyanide solution. A wighed amount of sample containing carbon disulfide was taken into 10% alcoholic alkali and allowed to stand for 3060 min. for the formation of xanthate. It was oxidized with a definite amount of excessive potassium ferricyanide and a little osmic acid as a catalyst, being kept for 15 min. at 20°C.
    The remaining potassium ferricyanide was titrated with ferrous sulfate using dimethylglyoxime as an indicator at pH 710, whereby the end point was estimated by the appearance of red coloration, and the carbon disulfide was determined from the amount of ferricyanide consumed by the xanthate. The xanthate gave sulfate and formate by the oxidation with potassium ferricyanide and the equivalent number against the oxidizing agent was 14.
    Download PDF (462K)
  • Kakuzo TADA, Hikoroku HORIGUCHI
    1963 Volume 12 Issue 9 Pages 799-803
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A rapid control method is proposed for the determination of cobalt, titanium and tantalum in cemented carbides. The sample is dissolved in a mixture of hydrofluoric and nitric acids, and evaporated to dryness. The residue is dissolved in dilute hydrofluoric acid, and then transferred to a column of strong quaternary amine anionexchange resin.
    Cobalt alone passes through the column, while titanium, tungsten and tantalum remain adsorbed. Titanium and tungsten are removed by elution with a hydrochloric-hydrofluoric acid. Tantalum is collected in a separate eluate of ammonium chloride and ammonium fluoride solution. Cobalt is determined by chelatometry using EDTA, after eliminating hydrofluoric acid from the first eluate. Boric acid is added to the second and the third eluates to complex the hydrofluoric acid. Titanium is precipitated with tannin from ammoniacal solution, and tantalum is precipitated with cupferron from acidic solution.
    Titanium is determined by chelatometry after pyrosulfate fusion of the ignited oxide containing a little tungsten, and tantalum is determined by weighing the oxide.
    The time required for an analysis is approximately 8 hours.
    Download PDF (874K)
  • Studies on controlled potential electroanalysis. XIV
    Masao TANAKA
    1963 Volume 12 Issue 9 Pages 804-807
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Electrodeposition of various metals on platinum electrode in 0.1M oxalic acid with 0.4M potassium oxalate has been investigated. The deposition potentials of metals were +0.30 V (vs. S. C. E.) for Hg, -0.25 V for Cu, -0.30 V for Se, -0.50 V for Sb, -0.60 V for Pb, -0.75 V for Sn, -0.80 V for Cd and < -1.00 V for Fe, Ni, Co and Zn.
    Among these, respective determination of Hg, Cu, Cd, Fe, and Zn at controlled potential was possible. Hg-Cu, Cu-Cd, Cd-Fe and Cd-Zn were separatorily determined.
    Download PDF (653K)
  • Studies on controlled potential electrolysis.XV
    Masao TANAKA
    1963 Volume 12 Issue 9 Pages 808-810
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Electrodeposition of various metals on platinum electrode in 0.5N sodium hydroxide has been investigated. The deposition potentials of metals were 0.00 V (vs. S. C. E.) for Au, -0.35 V for Pd, -0.80 V for Pb, -1.00 V for Sb and -1.50 V for Zn. Among these metals, electrolytic determination of Au, Pb and Zn at the controlled potential was possible. Au-Zn and Pb-Zn were separatorily determined.
    Download PDF (471K)
  • Akira KAWASE
    1963 Volume 12 Issue 9 Pages 810-817
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The reaction of ο- (2-thiazolylazo) phenol compounds and nickel gives products with red-purple or blue coloration, and the chelates can be extracted with chloroform. Their molecular extinction coefficient at their maximum absorption wavelengths around 600700 mμ are 35 × 104 (Table VI) and they can be applied for determination of trace nickel.
    The combining ratio of the metal to the reagent was 1 : 2 (Fig. 9 and 10), and the presence of 1 : 1 chelate in an aqueous medium at low pH (Fig. 10 and 11) was also recognized.
    The conditions for determination of nickel by these reagents were established (Table IV). NT and HMT were suitable for the photometric determination, and SNT, RT, MT, and DMT were superior as metal indicators. p. 80 (1959), (Iaterscience).
    Download PDF (1223K)
  • Akira KAWASE
    1963 Volume 12 Issue 9 Pages 817-821
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The reaction of ο- (2-thiazolylazo) phenol compounds with cobalt gives products with red-purple or blue coloration and the chelates can be extracted with chloroform. Since they have molecular extinction coefficients of 25×104 at their maximum absorption wavelengths of 550600 mμ (Table I and Fig. 1 and 2), the determination of a small amount of cobalt by them may be possible.
    The combining ratio of the metal to the reagent was found to be 1:2 (Fig. 6).
    The conditions for determination of cobalt by these reagents have been investigated. NT and HMT were suitable as reagents for extraction and SNT, MT, DMT and RT were excellent as metal indicators.
    Download PDF (752K)
  • Hiroko OKADA, Keiji KANEKO, Shoichi GOSEKI
    1963 Volume 12 Issue 9 Pages 822-826
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Yttrium or lanthanum forms a stable, blue complex with methylthymol blue (MTB) at about pH 6 or above which is supposed to have a 1 to 1 composition. MTB has an absorption maximum at about 440 mμ and its complex has it at 610 mμ, respectively, at pH 6.4.
    Beer's law is obeyed over a range of 0 to 120 mμ of yttrium or lanthanum in 25 ml, and the molar extinction coefficient of the complex at 610 mμ is 2.60×104 for yttrium or 2.54×104 for lanthanum.
    Some of heavy metal ions and large amounts of citrate, fluoride, phosphate, and tartrate ions decrease the absorbance considerably.
    Download PDF (738K)
  • Yoshitaka KOBAYASHI, Saburo KANNO, Masumi TAKUMA
    1963 Volume 12 Issue 9 Pages 826-830
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Among a number of methods for determinations of alkyl benzene sulfonate(ABS) in water, colorimetric methods using methylene blue are most useful, because of their simplicity.
    But, the methods are relatively nonspecific and subject to many interferences especially of anionic detergents outside of ABS. A modification of the Longwell-Maniece method (L. M. method) which have been introduced to reduce interferences, particularly of anionic detergents, is described.
    One hundred ml of sample water is taken and concentrated to about 50 ml (0.020.14 mg as ABS is required to be contained). Twenty five ml of HCl is added to it and boiled for one hour in a round-bottom flask with a water-cooling condenser (for instance, 1 mg of sodium lauryl sulfate can be decomposed by this procedure). After cooling, a few drops of phenolphthalein solution and sodium hydroxide solution are added till neutrality and the L. M. method is applied.
    Available range for determination in the proposed method is from 0.02 to 0.14 mg of ABS/50 ml CHCl3, at 654 mμ in a 10 mm cell, using pure chloroform as a reference blank.
    Download PDF (870K)
  • Yoshikazu HASHIMOTO, Yoshiaki KOBAYASHI
    1963 Volume 12 Issue 9 Pages 831-835
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    An internal standard electrode was prepared by packing graphite powder with a definite amouut of internal standard substances into the capillary of a soaking-up electrode. Various method of adding the standard into graphite were examined, amomg which was recommended the following.
    The graphite powder was immersed in a nitric acid solution containing zinc (20%) and dried in an electric furnace at about 250°C. Then the powder was packed into the capillary of the electrode and the hydrochloric acid (1 : 5) was soaked up to the top of it. The electrode was heated gently by slowly raising the temperature (the rate should not exceed 50°C/hr.), and kept for 30 min. at 200°C.
    Aluminum sample solutions acidic with nitric acid (1 : 2) were soaked up and excited with a. c. intermittent are of 3A. Steady intensity ratios of spectral lines Zn 3072.1Å/Al 3082.8Å were obtained in the range of 1 to 3 min. from the beginning of the excitation.
    100 to 500 μg/ ml of Al were determined under these conditions with standard deviations about 15%.
    Download PDF (968K)
  • Radiometric Polarography.II
    Mutsuaki SHINAGAWA, Hiroyuki NEZU, Tadaharu TAMAI
    1963 Volume 12 Issue 9 Pages 836-840
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A coulometry through the measurement of radioactivity of deposits was examined with several kinds of microelectrodes. The solution (50 ml) containing 5 × 10-3F Hg (NO3)2-0.1F HNO3 and 103 μc 60Co was the best among the solutions examined. The electrolysis was performed at the controlled potential of -1.50 V versus S. C. E. To determine the amounts of cobalt electro-reduced to metallic state, γ-rays from cobalt-60 were utilized and were measured with a scintillation counter.
    From the experimental results, it was found that the weight of cobalt deposited or the quantity of the electricity passing through the electrode could be determined with a sensitivity of 2.87 × 10-8g Co or 0.94 × 10-4 coulombs.
    Download PDF (931K)
  • Tsugio TAKEUCHI, Takayoshi YOSHIMORI, Takashi KATO
    1963 Volume 12 Issue 9 Pages 840-844
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    An accurate and simple method was described for the determination of U (VI) in uranium dioxide. The method was based on the constant current coulometry using titanium sulfate electrolyte proposed by Kennedy and Lingane (Anal. Chim. Acta, 18, 240, 1958). The sample (0.10.5g) was dissolved readily in a mixture of 2N sulfuric acid and 12 drops of hydrofluoric acid, which was more preferable than the strong phosphoric acid. An aliquot of the solution was added to 3540ml of the electrolyte consisting of 78M sulfuric acid, 0.60.8M titanium sulfate, 10 mg of ferrous ion, 50100 mg of uranium (IV) ion and a few drops of hydrofluoric acid. Uranium (VI) was determined coulometrically using a sensitive amperometric end point procedure.
    Satisfactory results were obtained for 131240 μg of uranium(VI) when the indicator circuit potential was chosen at 0.140.16 V vs. S. C. E. Results of stoichiometric analysis of uranium oxides (UO2 and U3O8) were also tabulated.
    Download PDF (1059K)
  • Saichiro ONUKI
    1963 Volume 12 Issue 9 Pages 844-848
    Published: September 05, 1963
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method of spectrophotometric determination of bismuth as its iodide complex (460 mμ) after anion exchange separation has been presented, by which trace amounts of Bi in solder alloys have been determined with satisfactory results.
    An anion exchange resin, Diaion SA # 100(100200 mesh, Cl-form), was used for separating Bi in solder alloys.
    Pb was eluted with 8M HCl, then Sn (IV) with 2M HNO3 and finally Bi with 0.5M HNO3. Other impurities, such as Cu, Fe, Al, As, and Zn did not interfere the photometric measurements.
    Download PDF (825K)
  • [in Japanese]
    1963 Volume 12 Issue 9 Pages 849-850
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (393K)
  • [in Japanese], [in Japanese], [in Japanese]
    1963 Volume 12 Issue 9 Pages 850-853
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (618K)
  • [in Japanese]
    1963 Volume 12 Issue 9 Pages 853-854
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (341K)
  • [in Japanese], [in Japanese], [in Japanese], [in Japanese], [in Japane ...
    1963 Volume 12 Issue 9 Pages 854-857
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (702K)
  • [in Japanese]
    1963 Volume 12 Issue 9 Pages 858-864
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Download PDF (1186K)
  • [in Japanese]
    1963 Volume 12 Issue 9 Pages 880-884
    Published: September 05, 1963
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
feedback
Top