BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 15, Issue 8
Displaying 1-24 of 24 articles from this issue
  • Koichi KATOH
    1966 Volume 15 Issue 8 Pages 811-816
    Published: August 05, 1966
    Released on J-STAGE: February 15, 2010
    JOURNAL FREE ACCESS
    Absorption spectra of D. Y. and B. C. G. were measured in various methanol-water mixtures containing a definite volume of acid or base, and absorbances of its absorption spectra were plotted against methanol volume %. The lines came down with methanol concentration, but a minimum point appeared in every case at about 90% and the lines went up again with much increasing methanol concentration.
    The similar behaviour also appeared in mixture with ethanol or iso-propanol in place of methanol.
    The term, log [(BH+)/(B)], represented as H* in this report, is in proportion to the proton activity. H* values were calculated from absorption spectra and plotted against organic solvent concentrations.
    Then, observed pH values and activity coefficients of hydrogen ion were calculated from these H* values in methanol-water mixtures.
    For instance, activity coefficients in the solution of 0.012 N sulfuric acid were as follows; 1.00(methanol 10%), 0.39(30%), 0.13(50%), 0.04(70%), 0.03(90%) and 0.12(100%).
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  • Tadashi HAYANII, Katsuhiko HONJO
    1966 Volume 15 Issue 8 Pages 816-821
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Colorimetric determination of phosphorus in iron and steel by molybdenum blue method has been investigated. A sample (0.11.0 g) is dissolved in 30 ml HNO3(1 : 1.2) with gentle heating and it is diluted with 30 ml water. Two per cent potassium permanganate solution is added to it drop by drop with gentle heating to convert phosphorus completely to phosphate ion until a small amount of manganese dioxide appears. A few drops of 10 per cent sodium sulfite solution is added to dissolve manganese dioxide, and the solution is heated to expel sulfur dioxide. After cooling the solution is neutralized with ammonia solution(1 : 1) until a slight amount of ferric hydroxide precipitate appears. Five to ten ml of nitric acid (1 : 1.2) is added to dissolve the precipitate again, and the solution istransfered into a 100 ml measuring flask. It is made up to the mark with water after adding 23 g am monium nitrate. One ml of the sample solution, 0.35 ml perchloric acid (60%) and 0.5 ml ammonium molybdade (5%) are put into a 10 ml centrifuge tube with a stopper and are diluted with water exactly to 5 ml. Two ml of n-butylacetate is added, the tube isshaken vigorously for 30 seconds and centrifuged for 30 min. with 2, 500 rpm. One ml of the organic layer is transfered to a 5 ml Nessler tube. To it is added 0.3 ml stannous chloride solution (5%) and the whole is diluted exactly to the mark with ethanol. The ab sorbance is measured at 725 mμ.
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  • Studies on Calcichrome as a spectrophotometric reagent. V
    Hajime ISHII, Hisahiko EINAGA
    1966 Volume 15 Issue 8 Pages 821-825
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    It has been found that Calcichrome forms a complex with titanium(IV) and the reaction has been studied spectrophotometrically to find the optimum conditions for the determination of titanium.
    The titanium(IV)-Calcichrome complex is formed gradually at about pH 4 and its composition was found to be 1 : 1. The complex has two absorption maxima approximately at 310 and 565 mμ when measured against water. Linear relationship was noticed between titanium(IV) concentration and absorbance under the conditions proposed. The molar extinction coefficient of the complex at 530 mμ was 11, 500 and the sensitivity was 4.2 × 10-3 μg Ti/cm2 for log(I0/I) =0.001. Many other metals such as copper(I and II), aluminum, iron(II and III), vanadium(V), etc. interfere with the determination. A new procedure was proposed for the determination of titanium.
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  • Determination of trace elements in cement. IV
    Hajime ISHII, Hisahiko EINAGA, Eiichi AOKI
    1966 Volume 15 Issue 8 Pages 825-829
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Traces of copper in cement were determined by solvent extraction and spectrophotometric method. The procedure established is as follows. A sample is dissolved in hydrochloric acid with ammonium chloride, and silica, being made insoluble, is filtered off. Copper in the filtrate is reduced to Cu(I) with hydroxylamine hydrochloride, and then is extracted at about pH 5.5 into iso-amyl alcohol as copper-2, 2'-biquinoline complex, which shows maximum absorbance at 550 mμ. In this case, tartaric acid has been added to prevent ferric iron and aluminum from precipitating into hydroxides.
    Copper-2, 2'-biquinoline complex is completely extracted at pH 4.56.5 under the conditions proposed, and is stable at least for two hours.
    As little as 0.001% copper in cement was determined with satisfactory results, which showed the presence of 0.0020.01% of copper in commercial products.
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  • Ryoei ISHIDA
    1966 Volume 15 Issue 8 Pages 829-834
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Chromazurol S reacts with yttrium to form a reddish violet complex in a nearly neutral medium (Barbital sodium-hydrochloric acid buffer) and it was applied to the determination of yttrium. Several conditions for the color development, the composition of the colored. complex and the influence of coexisting ions were in vestigated.
    The maximum absorption wavelength of the complex against the reagent blank at about pH 7.0 or higher was 562 mμ. Absorption curves against water blank at pH 7.6 have an isosbestic point at about 487 mμ which depends on the amount of reagent.
    The optimum pH for the color development is at about 7.6.
    A linear relationship exists between the absorbance and the yttrium concentration (Beer's law). The optimum concentration range determined by Ringbom's plot is between 6 and 35μg. of yttrium in 10 ml. The molar extinction coefficient of the complex at 562 mμ is 22, 600.
    The molar ratio of yttrium and chromazurol S in the complex is estimated to be 1 : 2 by a continuous variation method and by a mole ratio method. The complex has a formation constant of 1.5 × 1010 under the conditions studied.
    Anions such as phosphate, EDTA, fluoride, oxalate, tartrate etc. inhibit the color development, and cations such as Be(II), UO2(II) etc. give an overestimation of yttrium. Several heavy metals precipitate under the conditions and interfere with the determination.
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  • Wataru FUNASAKA, Tsugio KOJIMA, Kazumi FUJIMURA, Sue KUSHIDA
    1966 Volume 15 Issue 8 Pages 835-840
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A method of separation of o-, m- and p-chlorobenzoic acids by salting-out chromatography and of their determination by U. V. spectrophotometry has been presented, in which the stationary phase is weak-acid resin Amberlite CG-50 (sodium form), the mobile phase is acidic aqueous salt solution of varying concentrations, and the salting-out agent is aqueous or alcoholic aqueous solution of sodium chloride. The distribution coefficients of three isomers increased with increasing sodium chloride concentration and with decreasing pH over the range 2.05.0. That of m-isomer also increased with increasing concentration of ethyl alcohol over the range 05%.
    Quantative separation of the three isomers has been accomplished by a column of φ 10 mm × 150 mm and 2 M aqueous solution of sodium chloride of pH 3.5 containing 5% ethy J alcohol.
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  • Studies on inorganic thin layer chromatography. VIII
    Shoji TAKITANI, Noriko FUKUOKA, Yuko MITSUZAWA
    1966 Volume 15 Issue 8 Pages 840-845
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Thin layer chromatography was carried out on 12 common metallic ions, i e., [A] Pb(II), Cr(III), Mn(II), Ni(II), Cu(II), Co(II), [B] Hg(II), Zn(II), Bi(III), Fe(III) and [C] Ba(II), Sr(II). Ions of A, B, and C groups were developed, respectively, with acetone-3 N HCl(99 : 1), n-butanol-benzene-1 N HNO3-1 N HCl (50 : 46 : 2.6 : 1.4) and n-butanol-methanol-conc. HCl (10 : 80 : 10). The chromatograms obtained by appropriate color reagents were applied to the densitometric determination of respective ions. Standard error of mean (S. E. M.) 0.22.1 was not small, but the method seemed to fit for the semiquantitative dedetermination. In the area method of chromatographic determination, most ions showed a linearity between the logarithmic quantity (log W) and the square root of the spot area (√A).
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  • Teiji ÔKUBO, Masuo KOJIMA
    1966 Volume 15 Issue 8 Pages 845-849
    Published: August 05, 1966
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A spectrophotometric method for the determination of rhenium with thiourea and stannous chloride is studied, and it is used for determination of rhenium in platinumrhenium alloys and in several rhenium compounds. Analytical procedure is as follows. A sample solution containing 0.05 to 2 mg of rhenium is introduced into a 100 ml volumetric flask, followed by addition of 25 ml of concentrated hydrochloric acid, 12 ml of 5% thiourea solution and 6 ml of 1 M stannous chloride in 4 M hydrochloric acid solution. It is made up to the mark with water and mixed thoroughly. After 50 minutes or later, the absorbance is measured at 390 mμ or 445 mμ and rhenium is determined referring to the analytical curve which was linear in the range of 0 to 2 mg of rhenium. The method is applicable to the accurate determination of rhenium.
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  • Yusuke NAKAYAMA, Yoshimasa TAKASHIMA
    1966 Volume 15 Issue 8 Pages 850-852
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Precipitation reactions of meta-, hexa-, and pyrovanadates with hexamminecobalt(III) chloride were studied in detail to find the optimum conditions for the gravimetric and radiometric determination of vanadium.
    Recommended procedures for both gravimetric and radiometric analysis of vanadium are as follows. Neutral or acidic sample solution containing 530 mg of vanadium is adjusted to pH 13 by adding sodium hydroxide solution. After allowing to stand for 30 minutes, the excess reagent solution is added to the sample solution. The precipitate obtained is filtered and washed. The weight of the precipitate is measured after drying at 110°C. Radiometric determination is done under the same conditions but on microscale using radioactive cobalt compound.
    The gravimetric method is applicable to the determination of milligram amounts of vanadium, while the radiometric method is useful for microgram amounts of vanadium.
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  • Shizuya MAEKAWA, Kiyotoshi KATO, Masanori SAKURAI
    1966 Volume 15 Issue 8 Pages 852-855
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    One half gram of iron or steel sample is decomposed by treating with the mixture of 15 ml sulfuric acid (1+9)and 10 ml hydrogen peroxide (15% v/v).
    After being cooled, interfering elements are removed by electrolysis with mercury cathode. The acidity of the solution is adjusted to pH about 4 with ammonia water (1+1) and hydrochloric acid(5 M) using p-nitrophenol as an indicator, then the solution is diluted exactly to 100 ml with water. A 25 ml aliquot is transferred to a 100 ml measuring flask, and 1 ml of ascorbic.acid solution (1% w/v), 5.0 ml of aluminon-buffer composite solution (prepared by dissolving 500 g of ammonium acetate, 0.8 g of aluminon and 90 ml of acetic acid in 1 liter of water) and 2 ml of gum arabic solution (5%, w/v) are added.
    Then the solution is heated on a water bath or on a hot plate, cooled, diluted to the mark with water, and mixed. The absorbance is measured at 532 mμ in a 20 mm cells. The proposed method has three advantages over the JIS method; the sensitivity is higher by about thirty percent, the procedure is simpler, and the color is more stable (stable for at least 24 hours).
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  • Noboru KOBAYASHI
    1966 Volume 15 Issue 8 Pages 855-856
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    An improved apparatus for semimicro steam distillation of ammonia and other volatile substances is described.
    It is the characteristics of the apparatus that both sample-distilling vessel and drain-exhaust cylinder are installed inside the steam-generating flask. In this way, heating the sample-distilling vessel and keeping it warm are simultaneously achieved, and removal of the sample solution after distillation is found to be easy and rapid.
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  • Isao FUJII, Haruo MUTO
    1966 Volume 15 Issue 8 Pages 856-858
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    The oxygen content of titanium metal was determined by bombarding samples with 14 MeV neutrons from a Cockcroft-Walton machine and measuring the 7.35 second nitrogen-16 gamma activity produced by the reaction 16O(n, p)16N. In this paper, optimum condition for the measurement of gamma rays of 16N, a correction for the absorption of gamma-rays by samples are discussed. The analytical results by this method are in good agreement with those by the vacuum fusion method. The sensitivity for oxygen is about 1000 counts/mg of oxygen and the standard deviation of the method at the level of oxygen concentration 0.1% is 4%.
    This method may be used to study the accuracy and the precision of the conventional method because the method is non-destructive.
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  • Sadao SANO, Hiroshi MATSUI, Ryozo NAKAGAWA
    1966 Volume 15 Issue 8 Pages 858-860
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Using A R L's 1.5 m Industrial Research Quantometer, analyses of rare earth elements and zirconium in magnesium alloys have been carried out by the point to-plane method. High voltage spark discharge (L= 360 μH, C=0.007 μF, R=residual, V=20 kV) is used for excitation. Elements analysed and the range of their concentration are : La 0.061.4%, Ce 0.041.9%, Pr 0.160.5%, Nd 0.43.5% and Zr 0.7%, and these elements are determined with the coefficient in the variation of about 13%.
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  • Shizuo FUJIWARA, Kozo NAGASHIMA, Taiki KOBAYASHI
    1966 Volume 15 Issue 8 Pages 860-862
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    ESR spectra of Mn(II) ions in sulfides of the group IV cations were examined. The sulfides were prepared by the usual precipitation technique using (NH4)2S, and the distribution of Mn(II) ion in the precipitates was investigated. Precipitates containing Zn, Co, and Ni together with various amounts of Mn were tested. X-ray powder studies of these mixed sulfides showed amorphous character. No ESR spectrum was observed for nickel sulfide contaminated with manganese (II) ion. ESR hfs was observed for zinc and cobalt sulfides containing small amounts of manganese, and it shows a homogeneous distribution of manganese (II) ion in the precipitation. When treated with 1 N HCl, the ESR hfs of (Co, Mn)S disappeared completely. This probably means the dissolution, and reprecipitation of CoS in process.
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  • Yoshinori TAKATA, Giichi MUTO
    1966 Volume 15 Issue 8 Pages 862-864
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A method is described for the analysis of palladium alloy by controlled potential coulometry. Silver was determined coulometrically at the potential of -0.15V (vs. SCE) in the electrolyte of 0.1M NH4Cl-1M NH4OH. A mixed solution of Au, Pt and Pd was electrolysed at -0.18-0.19 V in 0.1M NH4Cl-1M NH4OH, and at +0.55 V and 0.00V in 0.1M Na2HPO4-0.5M H3PO4, that correspond to the electrolysis of Au+Pt, Au and Au+Pt +Pd respectively. From the quantities of electricity for these electrolysis, the percent ages of these elements composing palladium alloy were caluculated.
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  • Yoshio SAIKI
    1966 Volume 15 Issue 8 Pages 864-866
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    In the SBR latex as the compounding agent of portland cement mortar, many kinds of minor components besides SBR polymer were generally involves; they are, for example, surface active agents, antiforming agents, and polymerization modifier, etc. In this paper, the separation of these substances by the solvent extraction method and the analysis by infra-red spectrophotometric method were described. Surface active agents (polyoxyethylene alkyl ether and alkylbenzene sulfonate) were separated by the methyl alcohol extraction and antiforming agents (silicone) by the carbon. tetrachroride extraction. On the other hand, polymerization modifier (quinone derivatives) was separated as a precipitate from the solution of the methyl alcohol extraction by keeping it for 2 days at room tempreature. Only silicone was determined from the rate of the absorption intensity of 800 cm-1(silicone) and 840 cm-1 (SBR).
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  • Jitsuo SUGITA, Yukio IMAI
    1966 Volume 15 Issue 8 Pages 866-868
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    An accurate and simple method for determination of N-chloro-5-methyl-3-isoxazole-carboxamide (N-chloroamide) and a small amount of an excess NaOCl in the Hofmann reaction is described. NaOCl is determined potentiometrically with hydrazine sulphate, followed by the iodometric determination of N-chloroamide. This method shows the relative errors of ±2% for NaOCl and ± 1% for N-chloroamide, and is recommended to be applicable to the reaction control.
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  • Norio FUKUSHI
    1966 Volume 15 Issue 8 Pages 868-870
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A method using phosphorous trichloride-platinous chloride coordination compound, was adopted for the sample preparation in the case of microdetermination of phosphorus in silicon tetrachloride. A spectrographic study was made to estimate its analytical use on the complex and then a neutron-activation analysis was applied to the determination of the trace amount of phosphorus in silicon tetrachloride according to this preparation method.
    The method proposed for sample preparation may be available enough to the determination of phosphorus in silicon tetrachloride samples and it has such an advantage as simplicity, rapidness and less contamination with reagents used over other preparation methods.
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  • [in Japanese], [in Japanese]
    1966 Volume 15 Issue 8 Pages 871
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
  • [in Japanese]
    1966 Volume 15 Issue 8 Pages 872-881
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1966 Volume 15 Issue 8 Pages 882-885
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1966 Volume 15 Issue 8 Pages 886-893
    Published: August 05, 1966
    Released on J-STAGE: February 15, 2010
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1966 Volume 15 Issue 8 Pages 894-898
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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  • [in Japanese]
    1966 Volume 15 Issue 8 Pages 899-904
    Published: August 05, 1966
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
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