BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 13, Issue 1
Displaying 1-23 of 23 articles from this issue
  • Identification of BHT and BHA in antioxidant mixtures
    Naochika NAKAMURA, Toshiko YOSHIDA, Shunji KUSUMOTO
    1964Volume 13Issue 1 Pages 3-5
    Published: January 05, 1964
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
    A new color reaction of BHT (butylated hydroxy toluene) was reported previously in Part 1, which comprized a reaction of BHT with p-nitrobenzene-diazonium salt after treating BHT with an alcoholic hydrogenchloride reagent. In this report the method was extended to the identification of BHT and BHA in mixtures of phenolic or aminocontaining antioxidant by a simple procedure.
    The azo dye which was obtained by the method previously reported could be separated on a sheet of paper treated with aluminum hydroxide or on a small aluminum hydroxide column, using petroleum ether as the developing solvent. The identification limit is 60 μg each of BHT and BHA in 0.3 ml of a sample, but it can be made more sensitive by treating the dye with an alkaline dimethylforamide reagent.
    Download PDF (462K)
  • Application to the determination of iron (III) in water
    Mitsuo ITÔ, Sôichirô MUSHA
    1964Volume 13Issue 1 Pages 6-10
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    Design and use of a photometer for the flowing samples are described. The photometer consists essentially of a double-beam optical system, an amplifier, and a continuous flow cell assembly. The amplifier contains two devices : first, the logarithmic amplifier which provides direct readings of absorbancies and, second, the electronic switching systems using a phototube and transistors. The comparison was made in stabilities between the proposed photometer and a conventional spectrophotometer with stationary solutions. Standard deviations for the two photometers were of the same order.
    Besides, the continuous flow cell and the proportioning compartment for mixing reagents with samples at constant ratio are described. Iron(III) in water was continuously determined with thiocyanate as the colorant in the range of 1.87 to 8.99 ppm within 4% of variation.
    Download PDF (847K)
  • Takashi ASHIZAWA, Kanji HARUYAMA, Kikuo NAGASAWA, Yoshio MORIMOTO
    1964Volume 13Issue 1 Pages 11-16
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    Polonium (210Po) was extracted with dithizonecarbon tetrachloride solution (5×10-4M) in 1N nitric acid, decomposed with conc. nitric acid, dried in a on a planchet, and then α-activity was measured by a gas flow proportional counter or a Geiger-Muller counter, the counting efficiencies of which were 34.6±2.7% and 5.77±0.14% (95% C. L.), respectively.
    The percent extraction of polonium by one extraction was 99.4% and its separation from 100 mg copper, 20 mg mercury, 500 mg bismuth and 500 mg tellurium was possible by selecting suitable extracting condition.
    Lead and nickel did not interfere. Halogen ions showed disturbance in acid medium. The extraction from alkaline solution containing cyanide ions was possible. This method is suitable for control analysis of polonium in uranium refining process and the time required for an analysis is about 2 hours. The error of analysis is 10% (95% C. L.).
    Download PDF (1011K)
  • Hidehiro GOTO, Shigero IKEDA, Akira ONUMA
    1964Volume 13Issue 1 Pages 16-19
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    An argon carrier gas fusion capillary trap condensation method was applied for the determination of oxygen in zircalloy. The investigation was carried out mainly to find out optimum metal baths for the gas extraction. Iron was not suitable to be used as a metal bath, as the gas could not be extracted completely in spite of the presence of a large amount of iron. A tin-iron mixed bath containing iron as much as 20 times of sample in weight gave a good result for the determination of oxygen by extracting it at 1900°C.
    The procedure is appreciably rapid and easy to be operated. When platinum was used as the bath metal, an amount only eight times as much as the sample weight is enough to obtain the reproducible result. In this case, however, platinum should be added at the same time when the sample was charged in the crucible and the gas extraction should be carried out at 2000°C.
    Download PDF (786K)
  • Keishi NAKAHARA, Taeko DANZUKA
    1964Volume 13Issue 1 Pages 20-22
    Published: January 05, 1964
    Released on J-STAGE: April 28, 2009
    JOURNAL FREE ACCESS
    A new colorimetric method is devised for the determination of trace amount of iron (0.0005%) in the reagent grade disodium ethylenediaminetetraacetate by using bathophenanthroline as a colorimetric reagent. One gram of sample was digested gently with 6 ml of 60% nitric acid in a semi-micro Kjeldahl digestion flask until the content became clear, then it was concentrated to about 1 ml. After diluting the content to 20 ml, to it were added 2ml of 10% hydroxylamine hydrochloride, 2ml of 0.03% bathophenanthroline and 2ml of 20% ammonium acetate.
    The pH of the resulting solution was adjusted to 4.5 with a few drops of ammonia water. After warming the solution for 5 min. in a boiling water bath, the colored complex was extracted with 5 ml of iso-amylalcohol-iso-propylether (1:1), and the absorbancy of the organic layer was observed at 530 mμ against a reagent blank. The proposed method is more sensitive and suffers less from the deviation than the dry ashing method adopted as an official method in, JIS K 8107.
    Download PDF (566K)
  • Saichiro ONUKI, Kunihiko WATANUKI, Yukichi YOSHINO
    1964Volume 13Issue 1 Pages 23-27
    Published: January 05, 1964
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
    Small amounts of iron (0.0020.10%) in solder, white metal, type metal, Sn-metal and Pb-metal were determined spectrophotometrically with ο-phenanthroline in the presence of EDTA, by which were masked diverse metal ions such as Zn, Cu, Sn, Pb, Bi and Sb.
    An aliquot of the sample solution was heated with ascorbic acid and EDTA, and then an appropriate amount of buffer solution and ο-phenanthroline were added, and pH was adjusted to 5 with ammonium acetate. After heating the solution, it was diluted with water to a definite volume.
    The absorbance of the iron-ο-phenanthroline complex was measured at 510 mμ.
    Download PDF (765K)
  • Chromatographic determination with hydroxamized filter paper. II.
    Keiya KOTSUJI
    1964Volume 13Issue 1 Pages 27-32
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    The proposed hydroxamized paper gives blue color with vanadyl ion and grayish violet color with chromic ion.
    When vanadium (IV) is developed by the ascending elution with dilute sulfuric acid, a narrow blue band (detectable>3 μg V) is obtained on a strip of the paper without spraying any reagent for its detection. The influence of overlapping chromium (III) band is overcome by forming the acetate complex of chromium.
    When a sample solution (pH 2.42.6) containing vanadium, chromium and molybdenum is absorbed on this paper strip (19.5×1 cm) and eluted with sulfuric acid (pH 1.61.7), vanadium (320 μg) is separated from chromium (<200 μg) and molybdenum (<10 μg) after development for 120 min. The band is cut out, and vanadium is extracted with dilute sulfuric acid and determined spectrophotometrically with 8-quinolinol using 550 mμ.
    Download PDF (1087K)
  • Determination of rare earth elements in nuclear fuel materials by isotope dilution method. I.
    Takuji KOMORI, Shuzo TAMURA, Misao OUCHI, Katsubumi GUNJI, Hiroshi HAS ...
    1964Volume 13Issue 1 Pages 32-38
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    Concentractions of neodymium, samarium and europium in nuclear fuel materials were measured by the isotope dilution method. The electromagnetically enriched isotopes of samarium and europium (147Sm, 151Eu) and neodymium obtained from fission products were used as spike isotopes.
    After dissolution of the samples, known quantities of the spike solutions were added respectively, and rare earth elements were separated from the samples by thiocyanate-tri-n-butylphosphate extraction or oxinate extraction and tri-n-butylphosphate extraction. The isotopic composition of separated rare earth elements was measured by a surface ionization type mass spectrometer (CEC 21-702B) without the mutual separation of rare earth elements, while the concentractions of neodymium, samarium and europium were calculated from the results of the isotopic assay.
    The method can be applied to the determination of some rare earth elements, such as neodymium, samarium and europium, in the range from ppm to ppb in nuclear fuel materials with satisfactory precision and accuracy.
    Download PDF (1342K)
  • Wataru FUNASAKA, Teiichi ANDO, Yoshiro TOMIDA
    1964Volume 13Issue 1 Pages 38-41
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    X-ray fluorescence method was applied to the determination of thorium in monazite, and the addition method combined with the internal standard method (Sr as internal standard) was found suitable.
    Procedure:-After strontium carbonate (50 mg) and thorium oxide (0, 30, or 60 mg) are added to the monazite (500 mg), the mixture is fused with potassium hydrogen sulfate (5g). The fused matter is crashed to fine powders, and the intensities of Th Lα1-1 and Sr Kα1-1 of the three powdered samples thus prepared are measured.
    The content of thorium in each monazite was calculated either from the ratio ITh/ISr, or from ITh by applying the theoretical equation (1) or (2), respectively. The former gave results close to those by chemical analysis, while the latter gave a little higher ones.
    So far as the monazites used in this study are concerned, the intensities of Th Lα1-1 and of γ-rays emitted from the monazites themselves were both nearly proportional to the values obtained by the above procedure.
    Download PDF (707K)
  • Wataru FUNASAKA, Tsuguo KOJIMA, Kazumi FUJIMURA
    1964Volume 13Issue 1 Pages 42-46
    Published: January 05, 1964
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
    A salting-out chromatographic separation of maleic and fumaric acids has been carried out using weakly acidic cation exchange resins.
    From an acidic aqueous solution of calcium chloride, maleic and fumaric acids were adsorbed on Amberlite CG-50. The distribution coefficient of these acids increased with increasing calcium chloride concentration and also with decreasing pH value.
    In the chromatographic separation of the acids, the mixture was placed on the column of 500mm × 17mmφ, packed with 200400 mesh of Amberlite CG-50 buffering at pH 1.5, and the development was carried out at 40°C using 4M calcium chloride of pH 1.5 as a developer. After the separation, the acids in effluent was determined by u. v. spectrophotometry and good results were obtained.
    Moreover, the elution behavior of the acids when eluted with 5M sodium chloride of pH 1.5 and with mixture of butyl alcohol and 4M calcium chloride of pH 1.5 has also been investigated.
    Download PDF (774K)
  • Effect of hydrogen flow rates on the relative correction factor, false response and analysis of carbonyl sulfide
    Takamasa AONUMA, Ryuji NINOMIYA, Tadao SHIBA
    1964Volume 13Issue 1 Pages 46-51
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    The cause of daily variation of relative correction factor was attributed to the change of flow rate of hydrogen against nitrogen. By some stationary phases, amines were adsorbed on the carrier resulting a disappearence of the expected peak, and a false peak of ammonia appeared by the replacing absorption after passing hydrocarbon.
    An analysis of carbonyl sulfide was possible by use of the reaction column
    Download PDF (945K)
  • Studies on 2-substituted pyridines as analytical reagent. II.
    Atsushi SUGII, Motoko DAN, Hiroko OKAZAWA
    1964Volume 13Issue 1 Pages 51-54
    Published: January 05, 1964
    Released on J-STAGE: May 07, 2010
    JOURNAL FREE ACCESS
    Synthesized 1-picolinoylthiosemicarbazide was found to have a sensitive reaction with iron(III) to give a water-soluble yellow complex in weakly acidic media.
    Investigations on its application as an analytical reagent showed that the complex had two absorption maxima at 405 mμ and 650 mμ.
    The estimation of 0.55 ppm iron (III) was possible by use of the more sensitive 405 mμ. The composition of the complex was determined by the continuous variation method and by the molar ratio method to be 1:2 for iron(III): reagent.
    Download PDF (641K)
  • [in Japanese], [in Japanese]
    1964Volume 13Issue 1 Pages 55-56
    Published: January 05, 1964
    Released on J-STAGE: April 28, 2009
    JOURNAL FREE ACCESS
    Download PDF (309K)
  • [in Japanese], [in Japanese]
    1964Volume 13Issue 1 Pages 56-58
    Published: January 05, 1964
    Released on J-STAGE: April 28, 2009
    JOURNAL FREE ACCESS
    Download PDF (349K)
  • [in Japanese]
    1964Volume 13Issue 1 Pages 58-59
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    Download PDF (239K)
  • [in Japanese]
    1964Volume 13Issue 1 Pages 59-61
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
  • [in Japanese]
    1964Volume 13Issue 1 Pages 61-62
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese]
    1964Volume 13Issue 1 Pages 62-64
    Published: January 05, 1964
    Released on J-STAGE: April 28, 2009
    JOURNAL FREE ACCESS
    Download PDF (460K)
  • [in Japanese]
    1964Volume 13Issue 1 Pages 64-66
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
  • [in Japanese], [in Japanese]
    1964Volume 13Issue 1 Pages 66-68
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    Download PDF (436K)
  • [in Japanese], [in Japanese]
    1964Volume 13Issue 1 Pages 68-70
    Published: January 05, 1964
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
  • [in Japanese]
    1964Volume 13Issue 1 Pages 71-78
    Published: January 05, 1964
    Released on J-STAGE: January 14, 2010
    JOURNAL FREE ACCESS
    Download PDF (1587K)
  • [in Japanese]
    1964Volume 13Issue 1 Pages 79-84
    Published: January 05, 1964
    Released on J-STAGE: April 28, 2009
    JOURNAL FREE ACCESS
    Download PDF (1211K)
feedback
Top