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NARUHITO YOKOUCHI
1954 Volume 3 Issue 1 Pages
3-7
Published: February 15, 1954
Released on J-STAGE: January 14, 2010
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In the previous paper of this series, the writer reported on the gravimetric determination of magnesim in cast or pig iron, but this method was found to be rather tedious in field operation so that an oxine colorimetry was devised. After decomposition of the sample with an acid, potassium cyanide solution is added to remove the majority of iron as a complex salt. The remainder of iron and manganese are removed as a hydroxide (Fe) or dioxide (Mn), calcium is removed as an oxalate, and magnesium is precipitated with oxine. This precipitate is collected by filtration, dissolved in hydrochloric acid, and colorimetrically determined with the use of sulfanilic acid and sodium nitrite. This present method is simple in procedures, necessitates only a small amount of reagents as compared to the gravimetric method, and the time of analysis is shortened.
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YASUSHI KITANO, HIDEMATSU TAKAKUWA
1954 Volume 3 Issue 1 Pages
7-10
Published: February 15, 1954
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The so-called iodometry has been used as an International Standard Method for the determination of hydrogen sulfide or sulfur dioxide in air but this method gives an extremely erroneous results if caution is not exercised in various points. For such reasons, air entirely devoid of hydrogen sulfide and sulfur dioxide was submitted to this method for examination. From the results thereby obtained, it has become clear that following points should be noted in using this method for a quantitative determination:
(1) Iodine is easily lost by vaporization, the amount of loss being extremely great, when air is bubbled or when the atmospheric temperature is high.
(2) In order to trap escaping iodine, a tube containing sodium thiosulfate must be attached by means of a ground-glass joint. Rubber tubing must never be used.
(3) The distilled water and starch reagent used must be those which have previously consumed iodine.
(4) The reaction itself can be used as such for quantitative determination.
(5) It is desirable te chill the iodine tube with ice to be maintained at around 0°C.
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MASAO MARUYAMA, KIYOHISA MARUYAMA
1954 Volume 3 Issue 1 Pages
11-16
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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Reduction potentials of 2, 4-dinitro-6- and 2, 4-dinitro-4-cyclohexylphenol was measured at pH 1-10. It was thereby found that the separatory determination of 2, 4-dinitro-6-cyclohexylphenol in a mixture is possible by the polarographic method if carried out in a buffer solution of around pH 7. The errors in the determination were influenced naturally by the temperature, pH, and the concentration of alcohol, but an unexpected source of great error was found to appear if extreme care is not taken in the measurement of wave height. Absolute errorr of ±2% should be taken into consideration for samples containing around 85% of 2, 4-dinitro-6-cyclohexylphenol.
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Absorption and Explosion Method
ATSUSHI MIZUIKE
1954 Volume 3 Issue 1 Pages
17-21
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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Analysis of carbon dioxide, carbon monoxide, oxygen, hydrogen, and methane, contained in a minute quantity, such as total volume of 10
-3cc. (normal state) or less, is often demanded.
The writer carried out detailed studies on absorption analysis of gases by the measurement of change under a microscope, of the diameter of bubles by treating sample gas trapped as a bubble in a liquid with various absorptions solution. Further, a special explosion pipette was devised and fairly satisfactory results were obtained by combustion analysis of hydrogen and methane. In general, both absorption and explosion methods can be carried out rapidly with an error of a few per cent. However. a sample containing methane was found to give a larger rate of error, This method is simple in procedure, does not need skill, and the apparatus can be easily obtained or made. Some summarized example are also described.
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Studies on the Simultaneous Spectrochemical Analysis of Inorganic Constituents with Logarithmic Sector Disc.
NAOICHI OHTA, YASUO TOMITA
1954 Volume 3 Issue 1 Pages
22-25
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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The inorganic ccnstituents in biological materials are so small in content and their relative contents differ so much that although their (simultaneous) determination had been desired such was found difficult by the ordinary spectralanalysis. The writers attempted a spectrochemical analysis using a logarithmic sector disc and examined analytical conditions for the determination of Na, K, Mg, Ca, Sr, Ba, Zn, B, Al, and Mn. The spectrograph used was the Zeiss Q. U. 24. The sample was reduced to ash with fuming nitric acid and 30% hydrogen peroxide, derived to a chloride, and placed on an auxiliary electrode of copper. This was excited by continuous arc of 4A, 150V, D, C, for one minute, the paralleled light entering the slit was shielded by a logarithmic sector disc, and record the spectra on the Fuji Al dry plate. The plate was developed by D76 developer and the length of the spectral line was measured under a projector. Nickel was preliminarily added to the sample to be measured as an internal standard. A linear quantitative curve was obtained with each pair of lines as to the relationship between the difference of line length and logarithm of concentration, within a specific concentration range. The analyses were carried out with the brain, liver. heart, kidney, muscle, and lung of five cases of normal rabbit and it was found that a (simultan eous) determination of Na, K, Mg, Ca, and Fe was possible.
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Examination of Stannous Chloride-Potassium Thiocynate Method
HIROSHI NISHIDA
1954 Volume 3 Issue 1 Pages
25-29
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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In the colorimetry of tungsten, coloration with the Wellknown stannous chloride, potassium thiocyanate, hydrochloric and sulfuric acids was comparatively examined in detail using photoelectric colorimeter. It was thereby confirmed that a rapid and accurate results can be obtained by following the conditions listed below, and some considerations were made: A sample solution containing up to 3 mg./100 ml. should be kept below 20 ml., to which are aded 5-10 ml. of sulfuric acid, approx. 20 ml. of hydrochloric acid, and 5 ml. of 2M stannous chloride. This mixture is cooled to below 25°, is diluted to 100 ml. with 10 ml. of 20% potassium thiothianate and 30 ml. water, and measured at once.
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FUMIKAZU KAWAMURA, KOZO MOMOKI, SHIGETAKA SUZUKI
1954 Volume 3 Issue 1 Pages
29-32
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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A rapid microdetermination of salicylic acid by coulometric titration using electrolytically generated bromine and cuprous ion was studied. A satisfactory result was found to be obtained with a simple constant current source and an amperometric indicator system.
A potential difference of 250 mV was applied between the indicator electrodes immersed in the electrolyte composed of 0.3
N hydrochloric acid, 0.1
N copper sulfate, and 0.1
N potassium bromide. Mearsurering the time of electrolysis at a constant current of 10mA, an excess of bromine was generated for completing reaction with salicylic acid. After standing for 2 minutes, the excess bromine was back-titrated electrolytically generated cuprous ion. The end point was obtained amperornetrically by observing the current flow between the indicator electrodes. From the number of coulombs of electricity required to generate bromine reacted with salicylic acid, 50-300ϒ of salicylic acid was determined within 5-7 minutes.
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Determination of Beryllium by Hydrogen Sulfide with the Ether Method
TOMOYUKI AKIYAMA
1954 Volume 3 Issue 1 Pages
33-34
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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As has already been reported, the ammonium sulfide method is comparatively satisfactory in isolating beryllium from iron, nickel, cobalt, and manganese in a solution containing tartaric acid but it is difficult to completely separate it from iron, and the writer has pointed out the necessity of removing majority of iron by the ether method. In the present method, the sample solution is rendered alkaline with ammonia and hydrogen sulfide is applied in the presence of tartaric acid to precipitate the sulfides of nickel, cobalt, and iron. After the separation of these sulfides, ammonia is added to the filtrate to allow formation of the hydroxides of aluminum and beryllium. These are then dissolved in 6
N hydrochloric acid, and the minute amount of iron that remains is extracted with a mixture of ether and hydrochloric acid. The aqueous solution of hydrochloric acidity remaining here is treated by the oxine method to remove aluminum as Al(C
9H
6ON)
3, and the filtrate is submitted to the quantitative determination of beryllium as beryllium oxide. Satisfactory results were obtained.
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Determination by Selenous Acid
TOMOYUKI AKIYAMA
1954 Volume 3 Issue 1 Pages
35-37
Published: February 15, 1954
Released on J-STAGE: April 28, 2009
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Determination of beryllium with selenous acid gives better results than with ammonia water. By this method, the writer obtained a basic salt of the composition, BeO·2BeSeO
3·6H
2O. The separation of beryllium from other metals was effected by the use of a mixture of acetic acid and ammonium acetate, adjusting the reaction of the solution to pH 4.2-5.5, by which Hg, Cu, Ag, Cd, Al, Mn, Ni, Co, Fe, Zn, Pb, Cr, Bi, and Ti precipitated. From the point of solubility, the separation of beryllium was possible from Cu, Mn, Bi, Ti, and Hg, but rather incomplete from Al and Ni. If a large amount of ammonium salt is present during the determination of beryllium with selenous acid, the value obtained will be far smaller. The experimental error by the present method is within ±0.3% as BeO.
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[in Japanese]
1954 Volume 3 Issue 1 Pages
38
Published: February 15, 1954
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[in Japanese]
1954 Volume 3 Issue 1 Pages
39-40
Published: February 15, 1954
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[in Japanese]
1954 Volume 3 Issue 1 Pages
40-42
Published: February 15, 1954
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[in Japanese], [in Japanese]
1954 Volume 3 Issue 1 Pages
42
Published: February 15, 1954
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[in Japanese], [in Japanese]
1954 Volume 3 Issue 1 Pages
42a-44
Published: February 15, 1954
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[in Japanese]
1954 Volume 3 Issue 1 Pages
45-52
Published: February 15, 1954
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[in Japanese]
1954 Volume 3 Issue 1 Pages
53-56
Published: February 15, 1954
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[in Japanese]
1954 Volume 3 Issue 1 Pages
57-64
Published: February 15, 1954
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1954 Volume 3 Issue 1 Pages
e1b
Published: 1954
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1954 Volume 3 Issue 1 Pages
e1c
Published: 1954
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1954 Volume 3 Issue 1 Pages
e1d
Published: 1954
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1954 Volume 3 Issue 1 Pages
e1e
Published: 1954
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1954 Volume 3 Issue 1 Pages
e1f
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1954 Volume 3 Issue 1 Pages
e1g
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1954 Volume 3 Issue 1 Pages
e1h
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1954 Volume 3 Issue 1 Pages
e1i
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1954 Volume 3 Issue 1 Pages
e1j
Published: 1954
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1954 Volume 3 Issue 1 Pages
e1a
Published: 1954
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