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Volume 3 (1954)
- Issue 6 Pages 467-
- Issue 5 Pages 389-
- Issue 4 Pages 291-
- Issue 3 Pages 195-
- Issue 2 Pages 93-
- Issue 1 Pages 3-
Volume 3, Issue 5
Displaying 1-19 of 19 articles from this issue
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On the Determination of GermaniumYOSHINAGA OKA, TAKUJI KANNO, KAORU SHIBA1954 Volume 3 Issue 5 Pages 389-393
Published: October 15, 1954
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSPure germanium could easily be distilled from its solution in hydrochloric acid with the concentration above 7 N; distilling of 40-50 ml was sufficient and the volume before distillation had little influence. But when a few γ of germanium was distilled in the presence of large amount of ferric chloride or silicic acid, about 0.01% of germanium dioxide against the ferric oxide or silicic acid anhydride, there was a slight decrease in the yield of distilled germanium. Spectrophotometric study on the determination of germanium with the use of phenylfluorone indicated that, on left standing, the dispersed particles of the highly insoluble complex had a tendency to aggregate with each other and in consequence the change in absorbancy readings was noticed. Among reagents which had been examined, that from Consolidated Midland Corporation was the only one which gave nearly satisfactory results. With the reagent, changes in absorbancy readings were not observed at each wave length and at germanium concentration up to 0.9γ/ml for 5 hours. With 510mμ, calibration curve was nearly straight passing through the origin, though with longer wave lengths it curved upward slightly, when germanium concentration was low. Using the other reagent gave no straight line, and gave downward curves with shorter wave lengths, and upward curves with longer wave lengths. Absorption maximum was obtained at around 504 mμ, but the shape of spectral absorbancy curve was somewhat different depending on the kind of reagent used.View full abstractDownload PDF (1157K) -
Separation of Inorganc Cations by the Formation of Complex IonsMASAFUMI MAKI1954 Volume 3 Issue 5 Pages 393-397
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSComplex ions were prepared by using 4 N NH4OH-0.1M NH4tartarate solution, separated intoclassified groups in usual qualitative analysis and the migration of each ion was determined. Those Ni++, Co++, Mn++ and Zn++ which were difficult to separate in the preceding experiment (III) and those of Sb+++, Sn++; Al+++, Cr+++ which were difficult to be isolated by usual chromatography were isolated by this method. Mixed ions containing ions from different groups were separated by the difference of migration rate of ion. Changing the ratio NofH4OH:NH4tartarate can modify mutual migration rate of ions and some ions were migrated to the opposite electrode. No difference in the rate of migration of ions was observed by the change of concentration of sample solution. An example of separation of Co++ by electrochromatography suggests tis application of a mixed complex ion of the same series.View full abstractDownload PDF (1133K) -
HIROSHI NOZAKI, HIROSHI HAMADA1954 Volume 3 Issue 5 Pages 397-398
Published: October 15, 1954
Released on J-STAGE: January 14, 2010
JOURNAL FREE ACCESSPaper Partition chromatography of aliphatic carboxylic acids by means of hydroxamic acid method given by Inoue (J. Agr. Chem. Soc. Japan 23, 294, 1950) was applied for column chromatography with silica gel, using silica gel as a packing material, water as a stationary phase and n-butanol as a. mobile phase, and the experimental rate of flow was compared with that calculated from Rf value. The result showed good agreement between them, with the indication that partition chromatography was performed when hydroxamic was applied to column chromatography with silica gel with above phases.View full abstractDownload PDF (503K) -
HITOSHI KAMADA, SHIGEYUKI TANAKA, KYUICHI ARAKAWA1954 Volume 3 Issue 5 Pages 399-403
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSDue to the lack of a suitable method of analysis of quinoline and isoquinoline fractions in high boiling portion of coal-tar bases, these are estimated from infrared absorption spectra. The results indicate that the sample of quinoline fraction is found to contain two components, consisting of quinoline. and isoquinoline The content of each component is estimated. Also, the sample from isoquinoline fractionis is found to contain four components, quinoline, isoquinoline, 2-methylquinoline and 8-methylquinoline, and these are estimated. Since the estimation of the four component-system gives too complicated absorption spectrum and gives large error, a modified two component compensation method of measuring of 2-methyl-and 8-methylquinoline is applied after estimation of quinoline and iso-quinoline inorder to minimize the error.View full abstractDownload PDF (1292K) -
TAKERO SUDO, DAIZO SHIMOE, TAKATOMO TSUJII1954 Volume 3 Issue 5 Pages 403-408
Published: October 15, 1954
Released on J-STAGE: January 14, 2010
JOURNAL FREE ACCESSQuantitative microdetermination of N-methyl groupe is one of the most difficult analysis in structural analysis and although many improved methods are proposed, these require careful attention and high skill, furthermore, their accuracies are rather obscure and the data of practical operations are lacking in numbers. Attempts have been made to test on heretofore known quantitative microdetermination methods of N-methyl group with the result of considarable + errors due to an incomplete removal of obstructive gases. Although this difficuly was removed by lowering the rate of gaseous flow to 1 bubble/2-3 seconds, but the operation was rather difficult, The authors used a washing tube containing solid sodium thiosulfate and an improved liquid washer in order to remove iodine vapor and hydrogen iodide which cause + error. Further improvement is made by setting a double distilling system. The result of testing on 11 kinds of samples indicated that the average error was -0.12% and the square root of unbiased estimate of variance was 0.18%. This improved method has merits in accuracy, shortening the time of operation and simplification of the operation than the other methods, especially, the rate of flow of carbon dioxide can be increased several times more than the other methods; also it can be operated 2 sets at the same time.View full abstractDownload PDF (1417K) -
TADASHI NAGAOKA, SEIICHI YAMAZAKI1954 Volume 3 Issue 5 Pages 408-409
Published: October 15, 1954
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSDue to the lack of method for correct estimation of FeO in chromite or chromite brick heretofore, this investigation was carried out, and the following procedure was found to give the satisfactory results: Pulverized sample amounting to 0.25 g are dissolved in a mixture of 0.1 g V2O5, 10cc phosphoric acid and 20 cc sulfuric acid by heating for 12-13 minutes at about 200°C, cobalt sulfate solution is added in the ratio of Cr:Co = 1:3 (by weight) for discoloration of Cr ion, andV4+ produced from the reduction of V2O5 by FeO is titrated with N/10 KMnO4.View full abstractDownload PDF (507K) -
TOMOYUKI AKIYAMA1954 Volume 3 Issue 5 Pages 410-412
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSBeryllium salt is treated with hydrazine carbonate solution for formation of basic beryllium carbonate, heated to precipitate as Be(OH)2, filtered, washed with warm water, dried, ignited and weighed as BeO; there was almost no error of estimation, Using of ethylamine solution gives Be(OH)2 at pH. 5.56.0, while using of ethylamine carbonate gives basic beryllium carbonate at pH 6.3, which turns to Be(OH)2 on heating. Accordingly, it can be estimated as BeO by usual method. Methylamine or its carbonate solution gives a similar result and the estimation can be carried out simply. For precipitation of Be as BeNH4PO4·xH2O, the solution at pH. 7.27.6. BeO is found from its pyrophosphate by using the factor 0.2565. Crystalline berylliumammonium phosphate is found to be Be NH4PO4·41/2 H2O. The presence of tartaric acid or potassium salt in the solution has large influence on the estimation of beryllium.View full abstractDownload PDF (589K) -
KENSUKE YASHIRO1954 Volume 3 Issue 5 Pages 413-415
Published: October 15, 1954
Released on J-STAGE: January 14, 2010
JOURNAL FREE ACCESSTo apply the Karl Fischer titrimetric method to the determination of water in Nylon, a simple titration flask with attached condenser is devised and the sample is heated with cresol for dissolution in this flask. The result indicated that the method could be carried out rapidly with the error of ±0.05%, when the Nylon contained no antiaging agents nor plasticizers, etc.
For samples containing the above compounding agents, this method cannot be applied directly unless a test is made upon determinating whether or not there is any reaction between the Karl Fischer reagent and these compounding agents.View full abstractDownload PDF (744K) -
Extraction of Cyanamide in Calcium Cyanamide.SHINSUKE TAKEI1954 Volume 3 Issue 5 Pages 415-416
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSThe stabilyty of cyanamide in acetic acid was investigated; no change was observed by immersing it for 5 hours in 1N acetic acid at below 15°C and pH. 2. 43. Based on this fact, the cyanamide in calcium cyanamide was extracted with acetic acid and a satisfactory result was obtained by stirring 2g sample for 30 minutes in 450cc 0.1N acetic acid or for 15 minutes in 450cc 0.5N acetic acid, then the extact was proceeded for analysis.View full abstractDownload PDF (472K) -
Micro-determination of Cobalt and Iron by Induced Precipitations with Zinc Mercuric Thiocyanate ComplexSHUKICHT SAKURABA1954 Volume 3 Issue 5 Pages 417-420
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSA solution containing a small amount of metal ions, e. g. Cu+2, Fe+3, Co+2 or Ni+2, and a largeamount of Zn+2 (or Cd+2) is treated with (NH4)2[Hg(CNS)4] reagent for precipitation of Zn [Hg(CNS)4] together with these metal ions by the induced precipitation. The precipitate shows a characteristic coloration and it turns to a characteristic colored solution by dissolving it in acetone-methanol (1:1) containing 10% NH4CNS, i. e. red-brown by the presence of Fe+3, greenish blue by the Co+2 and red-brown by the Cu+2. 550γ of Fe+3 or 5120γ of Co+2 in 25200ml. of the sample solution may be determined by means of photometric measurement of the colored solution above mentioned. The determination of Cu+2 is difficult due to the rapid discoloration. The conditions for obtaining the best induced precipitation, e. g. the amount of Zn+2 to be added, the amount of precipitating agent against the definite volume of sample, and the stability of the colored solution to be tested are discussed. Also, the procedure for photometric estimation of a single ion and the interference are investigated. A satisfactory result is obtained for simultaneous estimation of Fe and Co in the solution.View full abstractDownload PDF (1116K) -
KANICHI OGAWA, TERUHIKO NAITO1954 Volume 3 Issue 5 Pages 421-423
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
JOURNAL FREE ACCESSAs a method of estimating the concentration of chlorine dioxide in air, potential of chlorine-dioxide-gas-electrode in chlorite solution was measured : ClO2+e→ClO2-; E=Eo+RT/nF(PClO2/AClO2-).
Keeping the active amount of ClO2- constant, the relation between electrode potential and logarithm of partial pressure of ClO2 could be expressed in a straight line under constant temperature. In order to keep the active amount of ClO2- constant, a saturated solution of hardly soluble chlorite, such as of lead or silver chlorite, was used. By bubbling chlorine dioxide gas around the platinum electrode immersed in the above solution, satisfactory results were obtained.
Further attempts were made to apply this method for an industrial use, and a continuous indicator of the chlorine dioxide gas concentration in air was successfully constructed.View full abstractDownload PDF (647K) -
[in Japanese]1954 Volume 3 Issue 5 Pages 424-425
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese]1954 Volume 3 Issue 5 Pages 425
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese]1954 Volume 3 Issue 5 Pages 425a-426
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese], [in Japanese]1954 Volume 3 Issue 5 Pages 426
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese]1954 Volume 3 Issue 5 Pages 426a-427
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese], [in Japanese]1954 Volume 3 Issue 5 Pages 428-435
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese], [in Japanese]1954 Volume 3 Issue 5 Pages 436-445
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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[in Japanese]1954 Volume 3 Issue 5 Pages 446-451
Published: October 15, 1954
Released on J-STAGE: April 28, 2009
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