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Volume 8, Issue 6
Displaying 1-16 of 16 articles from this issue
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Nobuo SUZUKI1959 Volume 8 Issue 6 Pages 349-353
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWell refined 10 -65×10-5M dithizone-carbon tetrachloride is prepared, and a definite amount after standing for a certain number of days is shaked with excessive silver solution containing 110Ag tracer. The solvent layer is separated and its radioactivity is estimated. Similarly, carbon tetrachloride solutions consisting of dithizone and silver salt, and that of silver salt in excess of dithizone are allowed to stand for certain number of days, and the stability from aging is estimated by determining their radioactvities. A dilute solution of dithizone is completely decomposed by standing in a room for one month. The silver salt at a concentration of about 10-5M in the presence of dithizone in excess is very stable, but that of 10-6M is not especially stable even in the presence of an excessive amount of dithizone. The decomposition by exposing it to light is very rapid. If kept in the dark, it is fairly stable but there is no great difference from that kept in a room. Also there is no great difference in the stability of solutions prepared by using either first grade or further purified carbon tetrachlorides.View full abstractDownload PDF (869K) -
Analysis using fluotitanic acid-hydrogen peroxide reagent. VHisao FUKAMAUCHI, Ryuko ENOHARA, Mitsuko UEHARA, Satoko TERUI, Yoshiko ...1959 Volume 8 Issue 6 Pages 353-356
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWhen Sb (V) is added to a mixture of fluotitanic acid and hydrogen peroxide, titanium ions, corresponding to the more stable fluoantimonic acid formed, are released, and converted to teh colored substance pertitanic acid by the action of the hydrogen peroxide present. As the color intensity is proportional to the concentration of Sb (V), a straight standard line is obtained in a certain range of Sb (V) quantity. As a reagent, a 2.5N HCl solution of mol-ratio, Na2TiF6: NaF: H2O2=1:4:1, and of 0.1M concentration with respect to titanium, was found to be suitable. Good results were obtained when the color reaction was carried out in a 2.5N HCl solution. Since the color reaction takes place almost instantaneously at ordinary temperatures, and the color being stable, this method is suited to the colorimetric determination of Sb (V) of more than micro-quantity. All reaction apparatuses, reagent vessels, and colorimetric cells used were made of plastic.View full abstractDownload PDF (683K) -
Separation of concomitant ions by means of anion exchange resinMutsuaki SHINAGAWA, Toshifumi MURATA, Hiroshi OKASHITA1959 Volume 8 Issue 6 Pages 356-361
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA column of Amberlite IRA-400 has been used for the separation of uranyl from titanium (IV), nickel, iron (III), copper (II), tin (IV), bismuth, antimony, chromium, cobalt, cadmium, arsenite, permanganate, and vanadate, and it was proven successfuly. Perchloric acid or hydrochloric acid served as the eluent as well as the supporting electrolyte in the polarographic analyses. The presence of molybdate caused serious interference in the polarographic determination of uranyl, especially in the case of perchloric acid eluate. However, if the sample solution had been treated with hydroxylamine-sulfuric acid before the column separation, up to 3×10-4M and 5×10-4M of molybdate became innocuous in perchloric acid eluate and hydrochloric acid eluate respectively. In the presence of a great deal of iron (III), 25270 times as much as uranyl, the perchloric acid eluate gave better results than the hydrochloric acid eluate.
The recovery of uranyl in the eluate is almost complete within the range of polarographically effective concentration of uranyl in the case of perchloric acid eluate, while it is poor when dilute in the case of hydrochloric acid eluate. The practical analyses of a synthesized sample and of uranium ore from Ningyo-Pass were satisfactory. The results were compared with those of colorimetric analyses.View full abstractDownload PDF (1212K) -
Yoshikazu YASUMORL1959 Volume 8 Issue 6 Pages 361-366
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe momentary changes of the Faradaic and non-Faradaic currents in square wave polarography are theoretically discussed and an instrument for square wave polarography, in which the potential of the square wave and the gating signal were obtained with the timing circuit of the decatrons, is described. As the result of studying the Cd-waves with various positions of gating, it was ascertained that the non-Faradaic current disappears almost within 1/2000 sec; on the other hand, for the Faradaic current to disappear takes at least 1/400 sec. The polarograms were studied, which had been obtained by applying the square waves whose upper and lower edges had various slopes with the change of time constant of the condenser-coupling in the square wave-generating amplifier. There was an optimum slope where the non-Faradaic current did not interfere with the Faradaic current. After the above studies, the determination of 2×10-7M Cd became possible.View full abstractDownload PDF (1076K) -
Toshio NAKAI, Seishi YAJIMA, Isao FUJII, Minoru OKADA1959 Volume 8 Issue 6 Pages 367-372
Published: June 05, 1959
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn order to detect and determine with the minimum chemical procedure, the various kinds of impurities in silicon for semiconductors, neutron activation analysis, which includes neutron irradiation, ion-exchange chromatography, and gamma spectrometry has been investigated.
In gamma-spectrometry two or more kinds of radionuclides can be determined without chemical separation, if their γ-energy values are for enough apart from each other that they can be desolved by a spectrometer. Therefore, the separation procedure is considerably simplified, and so, any error caused by the separation can be avoided. Since the photopeaks of copper, antimony, cadmium, and arsenic are in the narrow range of 0.51 to 0.57 MeV, which is little more than the resolution power of the spectrometer used, these elements, in their chlorocomplex, are separated from each other by anion exchange resin chromatography.
Samples of silicon were irradiated by neutron having a flux of 2×1011n/cm2· sec in a JRR-1 reactor.
The method possesses a sensitivity of 4×10-3, 3×10-3, 1×10-3, 2×10-2, 1×10-1, 3×10-3, 3×10-3μg and 4μg for arsenic, copper, antimony, cadmium, zinc, sodium, gallium, and iron, respectively.View full abstractDownload PDF (1223K) -
Shigeo WAKAMATSU1959 Volume 8 Issue 6 Pages 372-377
Published: June 05, 1959
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSThere are a few instances of estimating Fe+3 by utilization of absorption at 300mμ of ferric sulfate complex, but there is no instance of its application to the quantitative determination of S and SO4. The author has investigated a rapid and simple determination of S and SO4 by measuring the absorption at 380mμ of ferric sulfate complex, and has obtained the absorption curve of the complex salt. Using a wave length of 380mμ the determination of S and SO4 without any disturbing influence from the presence of a large excess of iron perchlorate was possible. The influence on the light absorbancy of iron, of perchloric acid and of the temperature of the solution were also determined: the error of light absorbancy of 2mg iron and 1ml perchloric acid using a solution of 0.3g iron and 30ml perchloric acid was 0.4%; and the error produced by a change in temperature was approx. 0.8%/1°C. The standard curve for estimation was derived and is presented. This method is suitable for determination of 0.430mg of S. Various interfering substances are listed in a table; among them, the interference of Cr6+ could be avoided by reduction with H2O2. That of Cl- and of NO3- could be avoided by white fuming temperature treatment, but this was accompanied by a partial volatilization of SO4, and data to indicate this tendency are given.
Tabulated results of the estimation of S and SO4 in practical samples by this method are also presented: these results were obtained, by in one case, fusion of the sample in Na2O2, dissolving it in hot water, filtering and using a portion of the filtrate. This was treated with 30ml iron perchlorate (containing 0.3g Fe3+ and 30ml HClO4), and made up to 50ml with water, after which the light absorbancy at 380mμ was estimated. In another case, the results were obtained by dissolving the sample in water, adding 30ml iron perchlorate solution, and then treating it as above. The time required for analysis was 1030 min.View full abstractDownload PDF (1297K) -
Manganimetry. IIIMasayoshi ISHIBASHI, Tsunenobu SHIGEMATSU, Shozo SHIBATA1959 Volume 8 Issue 6 Pages 377-379
Published: June 05, 1959
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSQuantitative determination of a small amount (0.22mg) of iron in the presence of arsenic, antimony, and tin with manganic pyrophosphate was carried out. The sample solution of iron (II) containing various amounts of co-existing ions and sulfuric acid (1: 1) or conc hydrochloric acid was made up to 25ml and titrated with a standard solution of manganic pyrophophate using diphenylamine as an indicator.
The results indicated that the presence arsenic in an amount of less than 24 times that of iron caused no interference, and the maximum error of estimation was 4% with an average error of 0.4%. The presence of tin less than 20 times the iron caused no interfernce. Increasing the tin up to 24 times gave 6.5% error for 0.45mg iron. The presence of antimony up to 20 times the iron did not interfere either, and up to 25 times was possible with the addition of 3% tartaric acid solution.View full abstractDownload PDF (478K) -
Manganimetry. IVMasayoshi ISHIBASHI, Tsunenobu SHIGEMATSU, Shozo SHIBATA1959 Volume 8 Issue 6 Pages 380-382
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSQuantitative determination of several organic acids using manganic pyrophosphate has been investigated. A sample with an excess of manganic pyrophospate was heated for 15min on a water bath, then the excess of the oxidizing agent was determined. The results indicated that oxalic acid was oxidized into water and carbon dioxide; and malonic, tartaric, citric, and salicylic acids were found experimentally to consume 4.34, 6.64, 8.60, and 11.60 equivalent weights of oxygen, respectively. The determination of these acids using these values gave good results. Acetic acid and formic acid were not oxidized by this method.View full abstractDownload PDF (522K) -
Hiroshi HAMAGUCHI, Nagao IKEDA, Toshi KAWASHIMA1959 Volume 8 Issue 6 Pages 382-387
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn electrolytic method for preparing carrier-free lanthanum-140 has been devised. The radiochemical examinations of the activity electrode-posited on a copper disk or a platinum net cathode from nitrate, sulfate, and perchlorate media indicate that, while electrolysis from nitrate media is not desirable because of the poor yield and purity of the lanthanum-140, that from sulfate and perchlorate media leads to better yield and purity.
The recommended procedure is the following: Prepare 0.01M NH4Cl04-0.01M Ca(Cl04) 2 solution containing the 140Ba-140La equilibrium mixture in perchlorate form, adjust the pH to 2.53.5 with perchloric acid or ammonia, and electrolyse at 6 volts with platinum net cathode against platinum spiral anode for a given time.
The radiochemical purity of lanthanum-140 separated as above is higher than 99.9 per cent.View full abstractDownload PDF (1004K) -
Studies on organic microanalysis. VMinoru FUKUDA1959 Volume 8 Issue 6 Pages 387-390
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSLiquid wash-reagents for alkyl iodide have been used heretofore, but the use of these reagents has been accompanied by various inconveniences; also, the wash-effect was not in all cases sufficient.
The author recommends the use of a superior solid wash-reagent containing soda lime which is prepared as follows:
A mixture of 60 parts of grade A sodium hydroxide, 3 parts distilled water, 20 parts commercial soda lime, and a slight amount of nickel monoxide, is fused in a nickel dish, cooled, ground, and sieved to collect the 12mm portion.
This wash-reagent was tested in every aspect, and satisfactory results were obtained.View full abstractDownload PDF (827K) -
Studies on organic microanalysis. VIMinoru FUKUDA1959 Volume 8 Issue 6 Pages 390-393
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the determination of the alkoxyl groups by hydrolysis employing the usual method, there are some instances of insufficient reaction with hydriodic acid.
Improving Kirsten's method and introducing the "Combustion Method"8), the author obtained satisfactory results. The sample and reagent were placed in a flask (Fig. 1 ) and the flask was stoppered (Fig. 1 ) with application of rather strong springs. The mixture was then heated by suspending the flask in boiling water for hydrolysis. The stopper was released after the hydrolysis, and the flask connected to a distillation apparatus (Fig. 1) for distillation of the alkyl iodide produced by hydrolysis.
Also, a sample boat (Fig. 2) was devised in order to prevent the bumping during the distillation of the reaction product in the flask.View full abstractDownload PDF (875K) -
[in Japanese]1959 Volume 8 Issue 6 Pages 394-395
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1959 Volume 8 Issue 6 Pages 395-397
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1959 Volume 8 Issue 6 Pages 398-403
Published: June 05, 1959
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1136K) -
1959 Volume 8 Issue 6 Pages 418a
Published: 1959
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (148K) -
1959 Volume 8 Issue 6 Pages 418b
Published: 1959
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (148K)
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