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Volume 6, Issue 12
Displaying 1-13 of 13 articles from this issue
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Shigeru YOKOSUKA1957 Volume 6 Issue 12 Pages 753-761
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn order to elucidate the cause of abnormal deposition in the electrolysis of ammoniac solution, the time and temperature of electrolysis were varied for electrolysis at the current density of 2amp/dm2, 1amp/dm2, 0.2amp/dm2, and 0.1amp/dm2, and the relation among current density, the temperature and time of electrolysis, and abnormal deposition have been investigated, The electrolysis at high temperature caused an abnormal over-deposition due to co-deposition of platinum, although there were some variations in its extent due to the difference of current density and the amount of sample. The platinum deposition is related to the amount of residual nickel ion in the electrolyte, and the rate of increased deposition is related to the current density. Electrolysis at low temperature caused abnormal over-deposition due to the adsorption of hydrogen gas, except the case of 0.1amp/dm2, and the amount of over deposition is shown to have close relation-ship with current density and the amount of sample. Based on the above findings, a suitable condition of electrolysis for electrolytic determination of nickel without accompanying the abnormal over-deposition is shown.
In order to investigate the behaviors of co-existing elements in the electrolysis of nickel under the condition specified in the preceeding report, the electrolysis were carried out in the presence of various amounts of elements, such as Cu, Pb, Bi, Sb, As, Sn, Cd, Fe, Al, Cr, Mn, Zn, and Mg. Then the state of electro-deposition and the amounts of co-existing elements was examined. Procedures for removing those elements which gave unfavorable effect on the electrolytic deposition of nickel have been investigated by applying such methods, as the removing of the whole elements of group II, removing of all Fe, Mn, etc. In these oparations the loss of Ni was examined. By selecting the best method from the results of this and preceeding reports, determinations of 20 samples of high quality nickels (Ni + Co> 99.95%. and Ni + Co < 99.94%) have been carried out with the result of 0.005% of standard deviation of error in case of the former and 0.01% in the case of the latter.View full abstractDownload PDF (1780K) -
Masaichiro MASUI, Sumiko FUJIOKA1957 Volume 6 Issue 12 Pages 762-764
Published: December 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe result of investigation of detection of N-alkylhydroxylamines formed from electrolysis of nitroparaffins at fixed potential indicated that these can be derived to a sensitive coloration by oxidation with iodine solution in neutral, acid or alkaline solution and by combination of Griess reaction just the same as in hydroxylamine, without hydrolyzing these by boiling with mineral acid. The sensitivities are indicated in Tab. 2. N-alkylhydroxylamines are prepared mainly by electrolysis at fixed potential under the specified conditions as indicated in Tab. 1. N-methylhydroxylamine prepared by synthesis was included for comparison. The coloration by the hydroxamic acid was fairly strong but that of oxime was rather weak ; in either case, the sensitivity was better by boiling with hydrochloric acid. Nitroparaffins and hydrazine did not show any coloration;therefore, these gave no disturbing influence. The distinction from hydroxylamine (NH2OH)was difficult.View full abstractDownload PDF (650K) -
Shun ARAKI, Naoharu YAMAGUCHI1957 Volume 6 Issue 12 Pages 764-767
Published: December 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMass spectrometric study was investigated about chlorine, hydrochloric acid, vinyl chloride and vinyliden chloride etc., and the results are as follows : (1) Mass spectrum of chlorine is replica of that of hydrochloric acid and has poor reproducibility about pattern and sensitivity, therefore its detection as well as determination is very difficult. (2) Detection of chloric acid free from chlorine is possible but determination is difficult because of its poor reproducibility of sensitivity. (3) Spectra of vinyl chloride and vinyliden chloride have good reproducibility. Four computing methods were tried about five synthetic mixtures and results were in good accordance with each other.View full abstractDownload PDF (653K) -
Spectrochemical analysis with the universal source unit. VKazuo YASUDA1957 Volume 6 Issue 12 Pages 768-774
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn continuance of the preceeding report, spectrographic analysis of high purity zinc has been investigated by applying controlled discharge of the universal source unit. This method has not only more merits of simplicity and rapidity than the solution method in the preparation of sample and excitation since the metal samples is used as an self electrode, but it does not require the skill and the cost for analysis is less. In this experiment, the consumption of zinc electrode by the sparking as well as the accumulation of zinc oxide has been investigated. For the quantitative determination of lead, 3 kinds of line pair with or without graphite counter electrode, were tested by various methods. The results indicated that the sensitivity of 0.0001% Pb was attained with good accuracy by use of a strong arc-like discharge of the universal source unit.View full abstractDownload PDF (1227K) -
Studies on the rapid-routine analyses of the iron pickling liquor. IVKimio MUKAEWAKI1957 Volume 6 Issue 12 Pages 775-779
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSWith a view to controlling the iron pickling liquor, the author undertook previously an investigation of the rapid-routine analyses of free acid, iron, chromium, hydrofluoric acid and ferric nitrate in the hydrofluoric-nitric acid pickling liqulor, making some observations, at the same time, on the state of the solution of iron, in the hydrofluoric-nitric acid pickling liquor, and revealed in the previous report that the descaling capacity depended upon the concentration of nitric acid in the pickling liquor.
Further, the author studied, in this report, on the rapid volumetric analyses of nitrate and nitrite in the hydrofluoric-nitric acid pickling liquor. Nitrate in the presence of iron, chromium, hydrofluoric acid was reduced with ferrous sulfate in the strong sulfuric acid in the atmosphere of carbon dioxide, and the excess of ferrous sulfate was titrated with potassium permanganate solution. Furthermore, the corrosion of glass-ware due to the hydrofluoric acid by this method was prevented by means of adding boric acid.
This method was applied to the solution containing 312% NO3, and the determination could be carried out in about 15 min. within ±2% relative errors. Nitrite was titrated directly with the potassium permanganate solution in the weak sulfuric acid, warming to about 40°C near the end point. The time required for the analysis was about 3 min. and the NO2 contents was about 0.20.3 % in the pickling liquor.View full abstractDownload PDF (1034K) -
Electrochromatography. XIXMasafumi MAKI1957 Volume 6 Issue 12 Pages 779-782
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS(1) A filter paper is saturated with an electrolyte composed of 0.05 M citric acid and 0.05 M NaCl and adjusted pH to 2.65 or 2.95 with NH4OH. The paper is spotted with the solution of a rare earth mixture separated from monazite sand by the usual chemical method, and direct current of a definite potential is applied for a definite time through both ends of the paper for the separation of Th, Y, Pr, Nd, Ce, and La on the paper.
(2) Each paper saturated with 0.05 M citric acid-0. 05 M NaCl-NH4OH (pH 2.9) is spotted with various amounts of the standard rare earth sample of Nd3+ or Ce3+, and these are electrochromatographed for a definite time at the same time. Then they are colored with a 0.16 % of alcoholic solution of oxine, and the spots are cut out, extracted with dilute nitric acid, and titrated with M/1000 EDTA using Eriochrome Black T. The result indicated that the amount of Nd3+ or Ce3+ on the spot and the amount of EDTA required for titration were in a linear relationship. Therefore, the quantitative determination of rare earths is possible by this method.
(3) This method is applied for the quantitative determination of the rare earth components of monazite sand separated on the filter paper by the method (1). That is, the rare earths of monazite sand separtated on the filter paper are divided first into two portions of Y +Pr +Nd +and Ce +La; these are cut off and determined by the method (2). The results indicated that the molar ratio of the rare earth metals in these two portions was 40 : 60 (±3 %). Accordingly, a simple quantitative determimation of rare earths in monazite sand is possible by this method.View full abstractDownload PDF (754K) -
Colorimetric determination of tetracyclines with the use of Th (IV)-reagent. IITakeichi SAKAGUCHI, Kiyomi TAGUCHI, Akira SUZUKI1957 Volume 6 Issue 12 Pages 782-787
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSWe have already reported on the new colorimetric determination of chlortetracycline based upon Th (IV)-chelate compound. Oxytetracycline, which can make stable chelate with Th(IV) in the same way, can be determined by this method.
Its chelate shows maximum absorption at 390 mμ and molecular extinction coefficient of 23, 300, and also stable range of pH (3.64.4), which enables us to perform sensitive colorimetric determination of oxytetracycline.
The isolation of oxytetracycline from biological fluids is carried out by Th(IV)-butanol extraction method. We have satisfying results on the determination in urine.
The range of 220 γ/ml of oxytetracycline can be determined by this method. In biological solutions such as urine and culture fluid except blood, this method will be able to give the reliable results. It can also be applied to various dosage forms of oxytetracycline.View full abstractDownload PDF (1007K) -
Colorimetric determination of tetracyclines with the use of Th(IV)-reagent. IIITakeichi SAKAGUCHI, Kiyomi TAGUCHI1957 Volume 6 Issue 12 Pages 787-790
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe same method, as that used to chlortetracycline and oxytetracycline, is applied to the colorimetric determination of tetracycline with the use of Th(IV)-reagent.
Tetracycline-Th(IV)-chelate compound has the highest molecular extinction coefficient of three tetracycilnes. Its maximum absorption shows at 395mμ. This method can be applied to the determination in urine, capsule and any other dosage forms of tetracycline. In this case, Th(IV)-butanol extraction method is applicable.View full abstractDownload PDF (578K) -
[in Japanese], [in Japanese]1957 Volume 6 Issue 12 Pages 791-792
Published: December 05, 1957
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (324K) -
[in Japanese], [in Japanese]1957 Volume 6 Issue 12 Pages 792-793
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS -
[in Japanese]1957 Volume 6 Issue 12 Pages 793-794
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS -
[in Japanese]1957 Volume 6 Issue 12 Pages 795-805
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS -
[in Japanese]1957 Volume 6 Issue 12 Pages 806-815
Published: December 05, 1957
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS
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