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Volume 10, Issue 1
Displaying 1-18 of 18 articles from this issue
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Spectrophotometric studies on organometallic complexes used in analytical chemistry. XTakuji KANNO1961 Volume 10 Issue 1 Pages 3-8
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSQuercetinsulfonic acid reacted with niobium either in neutral or in acid solution, and gave respectively yellow complexes soluble in water. In neutral solution, the absorption maximum of the complex shifted to longer wavelength with increasing of pH. However, the absorption maximum of the complex was at about 408 mμ, and the absorbancy was constant in the range of pH from 5.8 to 6.5. In this range of pH, the constant absorbancy was obtained at the concentration of quercetinsulfonic acid above 7.4×10-4M (0.03%). In these conditions, the calibration curve at 410mμ followed Beer's law, and the molar absorption coefficient was calculated as 46, 400.
In sulfuric acid solution, the absorption maximum of the complex formed in the acid solution below 0.45N was at about 412mμ, while the absorption maximum of the complex formed in the solution above 1.8N was at about 428mμ. In sulfuric acid between 0.45N and 1.8N, the absorption spectrum had two isosbestic points at about 420mμ and 451 mμ. Therefore, the determination of niobium was performed utilizing the wavelength 420mμ, and the constant absorbancy was obtained in the concentration range of sulfuric acid between 0.45N and 1.8N, and of quercetinsulfonic acid. above 4.9×10-4M. In this condition, the calibration curve followed Beer's law and the molar absorption coefficient was calculated as 14, 800.View full abstractDownload PDF (978K) -
Spectrophotometric studies on organometallic complexes used in analytical chemistry. XITakuji KANNO1961 Volume 10 Issue 1 Pages 8-14
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe reactions of some of flavonoids, such as cyanidin chloride, flavonol, and naringenin, were investigated to know the functional group in the reaction between quercetinsulfonic acid and niobium. It has become clear that flavonoids react with niobium in acid solution by means of a carbonyl and a hydroxy group in ortho position each other, but they react with niobium in neutral solution by means of either two hydroxy groups in ortho position or a carbonyl and a hydroxy group in ortho position each other.
The compositions of niobium-quercetinsulfonic acid complexes have been studied by means of Job's method of continuous variations, and consequently, it has become clear that complexes formed at pH 3.5 and 6.0 consist from one molecule of niobium and two molecules of quercetinsulfonic acid, and complexes formed in 7.2N and 0.23N sulfuric acid solution, having absorption maxima at about 428 mμ and 412 mμ respectively, consist from equimolecular of niobium and quercetinsulfonic acid.View full abstractDownload PDF (1134K) -
Masao KAWAHATA, Heiichi MOCHIZUKI, Takeshi MISAKI1961 Volume 10 Issue 1 Pages 15-18
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSimple determinations of ppm quantity of iron have been investigated by use of solvent extraction and light absorbancy method with nitrosonaphthols.
The complex of α-nitroso-β-naphthol and ferrous iron could be extracted completely with a mixed solvent of ethyl acetate and butyl acetate in the pH range 4.310. 0 and it gave a stable solution. having a maximum absorption at 660 mμ. On the other hand, extraction of the complex of, β-nitroso-α-naphthol and ferrous iron with the same solvent gave only an unstable solution and methyl-isobutylketone was used for this purpose. The extraction was complete in the pH range 4.910.0 and it gave a stable solution having the maximum absorption at 670 mμ. These methods, however, were not applicable for the determination of ferrous and ferric irons separately. As examples of the applications, estimations of trace amounts of total iron in reagent acids and alkalies were made.View full abstractDownload PDF (642K) -
Mitsuo KIBOKU1961 Volume 10 Issue 1 Pages 19-22
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn oxidimetric titration of Sn (III), As (III) and Sb(III) has been attempted by use of a standard potassium ferricyanide solution. Quantitative determination of Sn (II) was made at pH 11.0 12.5 by use of Na5P3O10 or Na4P2O7 as the complex agent and cacotheline as an indicator. Although a direct oxidimetric titration of As(III) and Sb(III) was impossible, these were precipitated as As2S3 and Sb2S3, the precipitate was dissolved in 0.1N NaOH or in 10% Na2CO3 and As(III) and Sb(III) were indirectly determined by titration of S2-from AsS33-, SbOS- and SbS2- with K3Fe(CN)6using sodium nitroprusside as an indicator.View full abstractDownload PDF (785K) -
Mitsuo KIBOKU, Chozo YOSHIMURA1961 Volume 10 Issue 1 Pages 23-25
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe optimum pH ranges for quantitative precipitation of lanthanum, cerium, and neodymium with tannic acid were sought with the use of ammonium acetate-ammonia buffer solution, and it was found that each of those rare earths formed the precipitate quantitatively in the pH range 6.410.8.
On the other hand, a minute amount of cerium gave a coloration with tannic acid showing a maximum absorption at 420 mμ at pH 9.2, and quantitative determination of cerium 1.810.6γ/ ml was possible. Determination of cerium in the presence of lanthanum and neodymium was made.View full abstractDownload PDF (390K) -
Jutaroh SETO1961 Volume 10 Issue 1 Pages 25-29
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThere has thus far been no easy way of separating histamine from histidine and determining their quantities. In determining the small quantities of histamine contained in large quantities of histidine, biological assays with cats have hitherto been used, by which the said quantities are only indirectly estimable.
In order to overcome such inconvenience, the author has invented a circular paper chromatography of a simple design and succeeded in a rapid identification of the contents by using the said device after giving the sample a simple preliminary treatment (Fig. 1, 3). The Rf of histidine was 0.05 and that of histamine 0.35.
Also by using the ascending method, the small quantities of histamine contained in large quantities of histidine could be determined easily and with sensitivity of below ca. 1γ (Fig. 4).
1) Solvent : Acetone CHCl3·28% NH4OH·H2O
(30:15:0.4:12)
Revelation reagent : 0.2% Ninhydrinin in n-C4H9OH solution or 0.1% iodine-C2H5OH solution
The Toyo filter paper No. 50
Development time : 30 ± 5 min.
Sensitivity : below ca. 0.1γ
2) Solvent : Phenol·H2O (4:1)
Revelation reagent : 0.2% Ninhydrinin in n-C4H9OH solution
The Toyo filter paper No. 51View full abstractDownload PDF (891K) -
Isao MATUBARA, Shukuo KINOSHITA1961 Volume 10 Issue 1 Pages 29-33
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGas chromatography, using a column packed with 10% triethanolamine on Celite 545 or 20% Tween-80-glycerol mixture (3:1) on C-22, was shown to be a useful method for rapid determination of solvents such as n-butanol, acetone and ethanol in acetone-butanol fermentation broth. When the triethanolamine column was used, n-butanol peak was separated incompletely from water peak, but the time required for elution was only 9 minutes. When the Tween-80 column was used, a complete separation of four components was achieved, but it took 17 minutes.
The column was held at 90°C and the flow rateof carrier gas (H2) was 50 ml/min. Each solvents were determined from relative heights of the peaks in accordance with that of n-propanol added. The results obtained showed good agreement with those obtained by the conventional methods.View full abstractDownload PDF (726K) -
Kozo MOMOKI1961 Volume 10 Issue 1 Pages 34-40
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAttempts for accurate determination of Mn by fluorescent X-ray spectrometry have been unsuccessful for special steel, which usually contains some amount of Cr, owing to the overlapping interference by Cr Kβ line to Mn Kα line. The degree of the enhancement of Mn Kα peak by Cr Kβ lines was, however, found to have a simple linear relation only to Cr content of the sample, and to be corrected easily for the percentages of Cr if the latter was known.
In low alloy steel containing 0.21.0% of Mn and 07% of Cr, Cr correcting intensities for Mn Kα overlapping intensities was 52.8× (Cr%) (cps) for the measuring conditions. The values were evaluated from Fig. 3 of the paper, in which Mn overlapping intesities of Mn-constant (ca. 0.4%) samples were plotted against varying Cr%. By subtracting these correction terms from Mn Kα overlapping intensities, the characteristic intensities of imaginable Cr-free samples were given for the determination of Mo. At the same time, a method was given in which a nomograph was effectively applicable for evaluating Mn% simply from the intensities measured of both MnKα overlapping and Cr Kα lines of a sample.
The method was most successful for the deter minations of Mn in low alloy steel of high or too low Cr content, whereas the nomograph was applicable even to eliminate some absorption effect by W.View full abstractDownload PDF (1398K) -
Kozo MOMOKI1961 Volume 10 Issue 1 Pages 40-47
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAs standard type X-ray spectrograph gives only absolute intensities of analytical lines at a time, results of routine analyses with this apparatus suffer from lack of precision by daily variations of measured intensities, if a definite calibration curve is used every day. Usually some sorts of checks of the calibration curve using several standard samples are necessary for the situation.
A new nomographic method has been proposed to give very simple control of these variations in routine analyses, in which each intensity of the same sample changes usually with a constant ratio over the whole range of a calibration curve. Two types of nomograph, one for low concentrations of measuring elements (in Fig. 3) and the other only for high content range (in Fig. 6) are presented.
Determinations of Ni in low alloy steel by Fig. 3 and that in stainless steel by Fig. 6 have been conducted with standard deviations of less than 0.065 % Ni and 0.13% Ni, respectivery, even if there are some mis-setting of goniometer, pulse height analyzer, or primary tube current and voltage, through the intensity measurements.View full abstractDownload PDF (1749K) -
Hot atom effects of metal complexes of 8-hydroxyqui-noline. IIHiroshi EBIHARA, Kenji YOSHIHARA1961 Volume 10 Issue 1 Pages 48-53
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPreparation of some radioisotopes in a high specific activity was studied utilizing the SzilardChalmers effects of some metal oxinates (8-hydroxyquinolinates). The experimental results obtained for molybdenum, indium and tungsten oxinates were given.
Dehydrated oxinates irradiated in JRR-1 were dissolved in an organic solvent. The organic solution of oxinates was shaken with Michaelis' buffer solutions of various pH values. Comparing radioactivities of the layers, the extractability was calculated. On the other hand, the amount of metals coming into the aqueous phase was determined. Basing upon those values each enrichment factor was calculated.
The experiments of separation with molybdenum showed that about 0.52% activity was found in the aqueous solution at pH 2.05.6 after shaking with the organic solution, whereas the oxinate was kept in the organic phase. The total amount of molybdenum was determined by coloration of its thiocyanate, and the enrichment factor of 10430 was obtained. The daughter of molybdenum, technetium-99m produced by β-disintegration was also separated from molybdenum by an ion exchange method.
The experimental data about indium showed that nearly 100% activity was found in the aqueous phase of 1N sodium hydroxide solution, but the total amount of indium in the aqueous solution was so small that it could not be detected by colorimetric method. So the quantities of indium were determined by activation analysis because of its large activation cross section. In this way, the enrichment factor of 106 was obtained.
Tungsten was extracted with an aqueous solution of pH 7. The experiments showed that about 34% activity was found in the aqueous solution after shaking with the organic solution. The total amount of tungsten was determined by the thiocyanate method. Thus, the enrichment factor of 430 was obtained in the best case tested for tungsten oxinate.View full abstractDownload PDF (946K) -
[in Japanese]1961 Volume 10 Issue 1 Pages 54-55
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese]1961 Volume 10 Issue 1 Pages 55-57
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1961 Volume 10 Issue 1 Pages 57-58
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1961 Volume 10 Issue 1 Pages 58-61
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese]1961 Volume 10 Issue 1 Pages 61-62
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1961 Volume 10 Issue 1 Pages 63
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese]1961 Volume 10 Issue 1 Pages 64-71
Published: January 05, 1961
Released on J-STAGE: February 16, 2010
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[in Japanese]1961 Volume 10 Issue 1 Pages 72-76
Published: January 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS
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