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Volume 4, Issue 9
Displaying 1-17 of 17 articles from this issue
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The Limit of Determination of Impurities in Raw Materials for Organic SynthesesHITOSHI KAMADA, SHIGEYUKI TANAKA, SHOJI HAYASHIBARA1955 Volume 4 Issue 9 Pages 545-546
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the detection of quality of raw materials to be used for organic syntheses by infrared absorption spectrum, the optimum intensity of compensating light on compensation method was studied. The result of using Baird Infrared Spectrophotometer indicated that concentration of compensation liquid or cell thickness just to allow the transmission of 3040% of the compensation light was the most effective in the determination of the minimum impurities. Based on the above result, the limits of determination of 20 kinds of impurities in raw materials were determined and found that this method was far superior than heretofore known methods.View full abstractDownload PDF (443K) -
Separation of Hydration Isomers of Chromic Chloride and Chromic SulfateMASAFUMI MAKI1955 Volume 4 Issue 9 Pages 547-549
Published: November 05, 1955
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSHydration reaction according to the following general equation, such as
[MY1Xm](k-m)++n·H2O→[MY1Xm-n(H2O)n](k-m+n)+
where M is a central metal having a valency k, causes change of electrical charges of the complexsalt as above, therefore, mutual separation of these hydrated products in order of their electrical charges is considered to be possible [M.Maki: Japan Analyst, 4, 217, 512(1955)]; For example, experimental proofs of separation of three isomers of CrCl3·6H2O into [Cr(H2O)6]Cl3, [Cr(H2O)5Cl]Cl2·H2O and [Cr(H2O)4Cl2]Cl·2H2O, and the separation of purple and green coloured chromic sulfate are madein order of their electrical charges as expected. The main constituent of green coloured chromic sulfate obtained by boiling of purple coloured chromic sulfate with water is considered to be [Cr(SO4)]1+, furthermore, both chromic chloride and chromic sulfate caused hydrolysis beside the hydration when boiled with water and several of their hydrolysis products are separated.View full abstractDownload PDF (556K) -
Studies on the Chemical Analysis of the Rare Earth Elements. XSEIZO MISUMI1955 Volume 4 Issue 9 Pages 549-552
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the fractional separation of Pr, the fraction of Pr containing Nd is tested under fusion by electrolytic oxidation method. The result indicates that the separation s simple under a certain condition, especially when the content of Pr oxide is over 50%, the precipitate is consisted of higher oxides of Pr of high purity. In this method, the sample of Pr oxide containing Nd is converted into hydroxide fused in KOH containing a definite amount of water and the higher oxides of Pr are precipitated by electrolytic oxidation together with a small amount of hydrated oxide of Nd as a solid solution, in which the purity of higher oxide of Pr is over 95%. Thus, a crude Pr fraction containing Nd obtained by usual fractional crystallization can easily be separated and concentrated by repeating several times of this method and the coefficient of concentration is superior in comparison with the other methods. The determination of active oxygen in Pr higher oxides is made by iodimetry, and the determinations of Pr and Nd in each fraction are made by spectrophotometric method.View full abstractDownload PDF (927K) -
SHIZO HIRANO, MORIJI KUROBE1955 Volume 4 Issue 9 Pages 552-554
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor rapid determination of total sulfur in pyrite, the sample mixed with sodium peroxide is fused, the product is extracted with water, made up to a known volume with water, a part of which is used for ion exchanging with H-type exchange resin for formation of sulfuric acid and this is titrated with a standard alkali, using a mixed indicator at pH 5.4. By use of this method, the total sulfur in pyrite is determined within 2 hours and the result showed good agreement with that of the total sulfur determined by fusion and gravimetric method.View full abstractDownload PDF (747K) -
TSUGIO TAKEUCHI, ETSUO NAKAMURA1955 Volume 4 Issue 9 Pages 555-557
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new method for rapid quantitative analysis of cellulose in viscose has been developed. The method is to regenerate cellulose in viscose by use of ammonium chloride and hydrochloric acid, the regenerated cellulose is separated by centrifuging, taken up in sulfuric acid, oxidized with an excess of potassium dichromate solution and the excess of the dichromate is back titrated with the standard ferrous ammonium sulfate solution with the use of barium salt of diphenylamine as an internal indicator. The time required for the analysis by this method is about one hour while it requires about hours by usual quantitative method.View full abstractDownload PDF (690K) -
Titration of Ammonium, Sodium and Potassium Sulfate by Use of Sodium Rhodizonate Test PaperTOMOYUKI MUKOYAMA1955 Volume 4 Issue 9 Pages 558-563
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSulfate in macro-quantities was rapidly determined by titrating its hot solution with a standard 0.3N BaCl2 solution, using preservable Na rhodizonate test paper as an external indicator. The standard BaCl2 solution may be standardized either by the usual gravimetric method or by the volumetric method of using (NH4)2SO4 solution prepared by neutralizing a know volume of a standard 0.3N H2SO4 with NH4OH. The spot test upon a Na rhodizonate test paper for Ba++ was sensitively done by touching a very small quantity of the sample solution several times on the same spot, using a glass rod with a fine tip (diam. 1-2mm.). The procedure is carried out as follows: 0.4-0.5g sample of (NH4)2SO4, Na2SO4 or K2SO4 (or their bisulfate) was taken into a 300-ml conical beaker, diluted to about 100ml with hot water (or the sample solution was neutralized with NH4OH or CH3 CO2H against methyl red, if necessary), heated at 90-100°C and titrated immediately at a moderate speed with 0.3N BaCl2 until near the expected end point, then titrated dropwise with thorough stirring until the pink spot or ring was just appeared upon the Na rhodizonate test paper. When the solution became cool, it should be reheated for the titration and the end point should be determined at above 60°C. In the back-titration method, the excess of 0.3N BaCl2 was added and back-titrated with the standard 0.3N (NH4)2SO4 until the pink spot upon the test paper was just disappeared. The effect of the presence of various substances were studied in the present procedure. For technical use, determination of sulfate such as (NH4)2SO4 in fertilizer was satisfactory carried out. The present method of determination for sulfate in macro-quantities can be carried out within 10minutes without using any organic solvent, or special and expensive apparatus.View full abstractDownload PDF (1322K) -
ISAMU TSUBAKI, SHIGEO HARA1955 Volume 4 Issue 9 Pages 563-565
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSXXI. Fe+++ is reduced to Fe++ by the U++++, the Fe++ turns pink by the alkaline solution of dimethylglyoxime and this reaction is applied for detection of U; the limit of detection is 0.98γ.
XXII. Since carbonic acid has a property of discoloring brown color of uranyl-ferrocyanide, this.is applied for detection of carbonic acid ;the limit of detection is 0.4γ.
XXIII. A solution of metallic Se in KCN is acidified to give red precipitate of Se. The limit of detection of Se by this reaction is 10γ.
XXIV. Cinchonine.. KI solution gives white precipitate by the addition of Cd. The limit of detection of Cd by this method is 0.7γ.
XXV, Cinchonine.. Bi(NO3)3 solution gives white precipitate on addition of Br-. The limit of detection of Br- by this method is 5γ.
XXVI. A solution of V++ reduces Ge salt and gives colloidal precipitate. The limit of detectionof Ge by this reaction 5γ.
XXVII. The F of titanium fluorides in hydrogen peroxide solutionis liberated by the addition ofBe to give yellow pertitanic acid and this is applied for detection of Be; the limit of detection is 3γ.View full abstractDownload PDF (645K) -
SHIZO HIRANO, MORIJI KUROBE, FUMIO ITO1955 Volume 4 Issue 9 Pages 565-568
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe determination of total sulfur in insoluble substances, such as cements, pigments and rubberproducts, has been made by gravimetric method by decomposing them with acid and precipitating as -barium sulfate; however, this method has a defect of requiring too long a time. Experiments were carried out by the authors to determine the total sulfur by use of ion exchange resin. Sample (0.1-0.5g) in 5 g fusion mixture (Na2O2+ Na2CO3) is fused in a nickel crucible, the product is extracted with water, transferred into a 200-ml measuring flask and made up to the mark with water, 50ml of which is pipetted out, treated with H-type Amberlite IR-120 AG in a separatory funnel until the evolution of CO2 gas ceased, then the solution is passed through a column of H-type Amberlite IR-120 AG, the sulfuric acid in the effluent is titrated with the standard sodium hydroxide solution and the equivalent amount of sulfur is calculated. The time required for this method is 1.5hours and the result agreed well with that of gravimetric method.View full abstractDownload PDF (921K) -
TSUGIO TAKEUCHI, MOTOHISA FURUSAWA, YUJI TAKAYAMA1955 Volume 4 Issue 9 Pages 568-571
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPhenol is used as one of polymerization inhibitors in the preparation of methyl methacrylate monomer and the determination of the phenol in methyl methacrylate monomer can be made by either one of the two following methods.
(1), Phenol in the sample is acetylated with acetic anhydride and pyridine by heating for 5minutes at 100°C, the excess acetic anhydride is hydrolyzed and titrated with 0.3N NaOH, using amixed indicator consisting of cresol red and thymol blue.
(2). The sample is dissolved in 10ml water, 0.5ml diazotized p-nitroaniline reagent added, followed by addition of 0.3ml pyridine, allowed to stand for 15-30minutes at 0°C or for 8-20 minutes at 10°C, 2ml 2.5N NaOH added, the solution is diluted to 25ml and the optical density of the solution is measured by use of photoelectric colorimeter at 460mμ, after standing for 10 minutes; blank test of the reagents is carried out in the same way. Diazotized p-nitroaniline reagent is prepared daily bytreating a solution of 1g p-nitroaniline in 1 liter 0.5N H2SO4 with 0.3% NaNO2 solution until itbecomes colorless. In the first method, more than 1% of phenol in methyl methacrylate monomer canbe determined, while in the second method, more than 0.001% of phenol can be determined.View full abstractDownload PDF (799K) -
The Ultra-micro Detection of Boron with Filter PaperSATORU MUTO1955 Volume 4 Issue 9 Pages 572-574
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor detection of boron by spot test on filter paper, a paraffin ring is placed on the lifter paper for preventing the dispersion of the solution through the filter paper and for increasing the concentration of sample in unit area on the paper. The minimum limit of detection of boron by this method was 0.02γ in a solution containing boron only and the accuracy was increased 10 times more than those estimated without using the ring. This method seems to have a possibility to be applied on spot test other than boron. In boron test, oxalic and salicylic acids were the most effective in accelerating the color development of curcumin, in which oxalic acid made possible to detect 0.002γ boron (1:10, 000, 000).View full abstractDownload PDF (640K) -
TETSUO KATSURA1955 Volume 4 Issue 9 Pages 574-577
Published: November 05, 1955
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNitroso R salt has been applied for the determination of a small amount of cobalt in various samples. This report deals with the determination of cobalt in zinc electrolytic solution and the cobalt in precipitate produced during the process of purification of the electrolyte. For increasing the rapidity of estimation, a filter with wave length 562mμ. has been used and the result indicated that the determination of cobalt in electrolyte as high as 10% Zn and containing cobalt in the ratio of Co: Zn= 1:20, 000 was not disturbed by the presence of zinc; the effects of the addition of Cu++, Ni++, Fe++, Fe+++, Mn++ and Cd++ on the determination of Co were investigated and found that the presence of 100 time of Cu, 50times of Ni, 200times of Mn, 10times of Fe++, 200times of Fe+++ and 1000 times of Cd, respectively, than the weight of Co had no effect and good results were obtained for rapid and economical analyses.View full abstractDownload PDF (974K) -
[in Japanese], [in Japanese]1955 Volume 4 Issue 9 Pages 578-579
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1955 Volume 4 Issue 9 Pages 579-581
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese]1955 Volume 4 Issue 9 Pages 581-582
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
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[in Japanese]1955 Volume 4 Issue 9 Pages 582-583
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1955 Volume 4 Issue 9 Pages 584-591
Published: November 05, 1955
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese]1955 Volume 4 Issue 9 Pages 592-595
Published: November 05, 1955
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS
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