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Volume 6, Issue 4
Displaying 1-13 of 13 articles from this issue
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Analytical studies on microgram quantities of antimony. IIINiro MATSUURA, Shizue TOMURA1957 Volume 6 Issue 4 Pages 205-210
Published: April 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPaperchromatographic spots of antimony split into three or four bands according to the treatment of the sample and the oxidation state of the developer. A main peak of the chromatogram has been found to appear at the acid front if the spotted sample of trivalent antimony chloride or of pentavalent chloroantimonic acid in concentrated hydrochloric acid medium is treated with a developer such as butanol containing hydrochloric acid together with hydrogen peroxide or nitrite as an oxidizing agent. On the other hand, a sample previously oxidized in slightly acid solution or a sample of irradiated unit of 124SbCl3 solution (presumably oxidized into the pentavalent state by prolonged irradiation with β and γ rays) has shown a main spot at the start and partly tracing bands in succession up to the acid front. The tracing bands in some cases showed maxima, the Rf value of each of which was dependent on the period of migration, and might be properly named "kinetic bands" formed by the reaction of hydrolysed products of pentavalent chloroantimonic acid with conc. hydrochloric acid in the mobile phase. Experiments also showed that a sample of antimony (V) chloride in the conc. hydrochloric medium or trivalent antimony chloride produced a quite similar sharp peak at the acid front. Therefore, by the use of n-butanol containing conc. hydrochloric acid as a developer, the Rf values of 0.80-0.72 for Sb (V) and of 0.69-0.76 for Sb (III) can not be distinguished. The typical pentavalent chloroantimonic acid chromatograms are composed of four spots : namely, first, a hydrolysed product of chloroantimonic acid at the start; second, a diffused band of a reaction product at the intermediate zone; third, a sharp chloroantimonic acid peak at the acid front; and fourth, a faint extracted chloroantimonic acid at the developer zone.View full abstractDownload PDF (892K) -
Iwaji IWASAKI, Takashi KATSURA, Minoru YOSHIDA, Toshikazu TARUTANI1957 Volume 6 Issue 4 Pages 211-215
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid method of analysis of FeO, Fe2O3, TiO2, V2O3, SiO2, and MnO in magnetite and ilmenite has been established. The FeO content is determined by decomposing (30 sec to 2 min) 0.1g sample in 1 cc HF and 20 cc H2SO4 (1 : 1) and titrating with N/20 KMnO4 solution. The sample solution after the titration is reduced with Zn-Hg and the sum of Fe and Ti is calculated from titration with N/20 KMnO4 solution. This is then reduced with 2 % Zn-Hg and the Ti is determined by Fe3+ solution, using 7 cc 30 % solution of KSCN as an indicator. The content of Fe2O3 is calculated from the above result. The effect of the presence of V in the above analytical procedure has been investigated. The SiO2 was determined by colorimetric method. Also, there was an indication of possibility of colorimetric determination of Mn by decomposing the sample solution with HF and H2SO4 and by treating it with H3BO3 without removing the HF.View full abstractDownload PDF (949K) -
Mutsuaki SHINAGAWA, Toshifumi MURATA, Takashi YOSHIDA1957 Volume 6 Issue 4 Pages 215-219
Published: April 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPolarographic analysis of tin in the presence of lead and antimony has been studied, and the following conclusions obtained :
(1) In a solution of tartrate, stannic ion does not give the reduction wave, but stannous ion gives both the oxidation and the reduction waves. The half-wave potentials of these waves vary with the pH values; and under the conditions that the concentration of tartrate and the pH value are respectively in the ranges between 3 and 4, the oxidation wave gives a defined diffusion current without interference by lead and antimony ions.
(2) The optimum conditions under which tin is determinable can be obtained after the effect of the reduction products (sodium chloride and aluminium chloride) has been taken into account.
(3) The diffusion current of the oxidation wave is proportional to the concentration of stannous ion between 5 and 50×10-3M.
(4) As much as a few percent of tin in lead is determinable with an error less than 10% (as proven by analysis of synthesized samples).View full abstractDownload PDF (1106K) -
Analyses of drugs and chemicals by paper electrophoresis. IVYahyoe KINOSHITA, Shigetaka MORIYAMA, Toshiko SHIMIZU1957 Volume 6 Issue 4 Pages 219-224
Published: April 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSWith the use of the apparatus described in Report III of this series, experiments on electrophoresis have been carried out in three buffer solutions of Clark-Lubs, Sorensen, and Kolthoff. The maximum mutual differences of migration distance of sulfamines in any of these buffer solutions were shown at pH 7.0, and the differences of migration distance of anilides were great at pH 2.0. The separation and identification of those with these pH values were possible by carrying out the test at 400 V, 1mA/cm, and at 15°C for 60 minutes. The detection of migration zones was accomplished by spraying a solution composed of 3 g p-dimethylaminobenzaldehyde and 7 g conc H2SO4 in 100 ml water on the air-dried paper used for electrophoresis. This treatment caused the sulfamines to give an orange color up to 0.2γ and the anilides to give a yellow color with the limit of detection up to 0.25γ.View full abstractDownload PDF (949K) -
EDTA MethodYoshihide ENDO, Hidetaro TANIHARA, Kunihiro HATTORI1957 Volume 6 Issue 4 Pages 224-228
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of lime and magnesia in iron ore has generally been carried out by the volumetric method after converting them to oxalate and phosphate, respectively. The present method deals with a volumetric method of using EDTA. The separation of the iron was effected by using ether, a mercury cathode, and ion exchange resin, and the remainder of the iron was precipitated by aqueous ammonia. The filtrate was divided into two portions: the one was used for the determination of the sum of lime and magnesia by the EBT-EDTA volumetric method, and the other was used for the separation of the lime by ammonium oxalate. The filtrate from this separation was used for the estimation of magnesia by the EBT-EDTA volumetric method, from which the lime was calculated by the difference in weights of these two determinations. Also, the disturbing effect of Mn and other trace elements and salts was evaluated by masking. The results are summarized as follows : 1). Masking of Mn up to 15 mg in the test solution was possible by adding 15 ml 20% KCN; the presence of other elements and salts in the solution showed no effect under this treatment. 2). In the determination of magnesia in the presence of a trace of Ca2+, the aging of the precipitate was incomplete, and it was necessary to accelerate the aging by adding about 5 ml of 0.01 M Ca2+. 3). The above method was applied to synthetic and experimental samples, and it was superior in both speed and accuracy to the usual method.View full abstractDownload PDF (905K) -
Analysis using hydrofluotitanic acid hydrogen peroxide reagent. IHisao FUKAMAUCHI, Mieko SEKIGUCHI, Kazuko IIYOSHI1957 Volume 6 Issue 4 Pages 229-232
Published: April 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt has been found that when a substance such as silicic acid which produces a more stable fluorocomplex than that of titanium, is added to a mixture of hydrofluotitanic acid and hydrogen peroxide, the mixture becomes yellowish-colored due to the formation of pertitanic acid, and it may therefore be used as a coloring reagent for such substances. Some pertitanic acid is formed merely by mixing hydrogen peroxide with sodium fluotitanate solution, so a solution of the mol-ratio, Na2TiF61 : NaF4 : H2O21, is suitable for using asa coloring reagent. The reaction of silicic acid with the reagent is best observed in 1 N or more strongly acidified solution. The confirmation limits in the presence of contrast solutions, were SiO2 1 mg/5 cc in weak HF-acidic solution, and SiO2 0.05 mg/0.6 cc and SiO2 0.5 mg/10 cc in about 1.2 NH2SO4-acidic solution. By the use of a photoelectric colorimeter, at a wave-length of 420 mμ, a layer of 1 cm, and an acidity of 1 N H2SO4, SiO2 0.1 mg/10 cc was detected. As the reagent reacts with glass, all of the test-tubes, burets, cells of the colorimeter, and other vessels used were made of synthetic resin.View full abstractDownload PDF (797K) -
Shin KIMURA1957 Volume 6 Issue 4 Pages 232-237
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe method of sampling is the biggest problem in the gas analysis of iron and steel, and it is important to know the exact constituents of gasses in the sample without the formation of mold cavity or uneven distribution of gases. In order to clarify this problem, the size of the metal mold for casting the experimental sample for analysis and the position of the casted metal to be taken for sampling have been investigated. The results indicated that using a smaller metal mold and taking the sample from the centre of a rod sample gave better values for deriving an average value and without showing any uneven distribution of gases. The experiments are described in detail.View full abstractDownload PDF (1058K) -
Separation and semimicro determination of iodine in organic compounds containing other halogensAsaji KONDO1957 Volume 6 Issue 4 Pages 238-240
Published: April 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method of selective separation and determination of iodine on a semimicro scale in organic compounds containing chlorine or bromine has been established. The decomposition of the sample was effected by the use of sodium peroxide and a microbomb. Some improvements were made in the mixing of the sample and the sodium peroxide. The product of decomposition was dissolved in water, the hydrogen peroxide was driven off by gentle boiling with platium foil, and the solid impurities were filtered off. The pH of the filtrate was then adjusted to below 1 with conc HCl. PdCl2 and hydrazine were added, and the precipitate of PdI2 was let stand for 1 day, then filtered, washed, and dried. The errors were less than 0.3 %.View full abstractDownload PDF (604K) -
[in Japanese]1957 Volume 6 Issue 4 Pages 241-242
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
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[in Japanese]1957 Volume 6 Issue 4 Pages 242-243
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1957 Volume 6 Issue 4 Pages 243-245
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1957 Volume 6 Issue 4 Pages 246-255
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
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[in Japanese]1957 Volume 6 Issue 4 Pages 256-260
Published: April 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS
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