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Volume 13, Issue 10
Displaying 1-29 of 29 articles from this issue
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Study on polarographic analysis of iron and steels. VIRokuro KAJIYAMA, Masao KAWAHATA1964 Volume 13 Issue 10 Pages 951-956
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNiobium gives polarographic waves in a slightly acidic solution in the presence of EDTA. Sulfates or acetates are recommended as the indifferent electrolyte, whereas tartrates or citrates remarkably reduce the wave height and the wave disappears in the presence of oxalates.
Although the characteristic two-step waves of niobium in an ammonium acetate-sulfuric acid buffer solution appear in the a. c. polarogram with two clear peaks at -0.80, -1.33V (vs. Hg pool), the second wave in the d. c. polarogram is not so well-defined due to the influence by the hydrogen wave, and the first is used for the determination. The amount of niobium and the wave height are linearly correlated over the range of 110 mg Nb/100 ml. Niobium is separated from matrix metals by the fuming treatment with perchloric acid followed by the hydrolysis. It is dissolved in KOH solution, and EDTA and the buffer are added to it to obtain the electrolytic solution. The polarogram is taken after gentle heating and ripening of the solution, and the amount of niobium is determined.
The method was applied to the determination of 0.52% niobium in stainless steels, and satisfactory results were obtained.View full abstractDownload PDF (975K) -
Yoshiaki MARUYAMA1964 Volume 13 Issue 10 Pages 956-960
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIon exchange separation of Rb and Cs was studied by the batch and the column methods using 86Rb and 137Cs as radioactive tracers. The cation exchanger Diaion SK #1 was chosen, and 0.5N, 0.75N HCl were used for the eluant. The distribution coefficients Kd were determined by the batch method. The apparent Kd were invariable when Rb or Cs carrier increased from trace quantities to about 5 mg, and decreased thereafter.
The separation factors α also were determined by the batch method. Their values of KdRb KdCs and α were 43.0, 56.6 and 1.32 in the 0.5N HCl, and were 25.9, 33.5 and 1.29 in the 0.75N HCl respectively. The elution curves were taken for Rb and Cs by the column method. The distribution coefficients Kd and separation factors α calculated from the column experiments coincided with those by the batch method.
Also 0.15N NH4 acetate solution was used to elute Rb and Cs, but the separation was less effective than the elution by HCl.
At last 0.1N Ba(OH)2 solution was used for the treatment of a large amount of material, and about 300 mg crude Rb (containing Cs) was purified experimentally.View full abstractDownload PDF (817K) -
Eiji FUTAMURA, Haruo SHIMADA, Nobuo OBA1964 Volume 13 Issue 10 Pages 961-966
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNonmetallic inclusions on the sandmark of steels can nowadays be extracted mechanically by means of ultrasonic jackhammer. The authors established the methods of chemical analysis of the inclusions above. The methods consist of the colorimetric procedures for the determinations of silica, alumina, iron, manganese and chromium. The exployment of the microchemical techniques makes these methods possible to be applied to the sample of 100 μg or less.
The reagents used in this case are ammonium molybdate for Si, Chromazurol S for Al, nitroso R salt for Fe, formaldoxime for Mn and diphenylcarbazide for Cr. When 100 μg of the sample is used, the minimum percentage of the components to give good results is about five.View full abstractDownload PDF (1283K) -
Teru YUASA, Kazuko KAMIYA1964 Volume 13 Issue 10 Pages 966-970
Published: 1964
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the identification of organic chemicals in vulcanized rubber, sixteen kinds of common antioxidants and nine accelerators were examined by silicagel thin layer chromatography.
The acetone solutions of antioxidants and accelerators were spotted and developed with organic solvents and Rf-values of them were measured. It was possible, even when their chemicals were mixed, to certify them from Rf-values and characteristic colors of chromatogram with the mixture of chloroform and carbon tetrachloride (1 : 1) as developing solvent.
The color reaction of the accelerators were developed with copper sulfate-platinum reagent. and, for amine type and phenolic type antioxidants, diazonium salt of sulfanilic acid and Tollen's reagent were respectively used.
The above method was applied to identify organic chemicals in vulcanized rubber, then the samples were extracted with acetone at room temperature. The results for the known vulcanized rubbers were satisfied, but from the sample using thiazole type accelerators, not only each chemicals, but also zinc salt of 2-mercapto-benzothiazole was identified and also zinc dimethyl dithiocarbamate was found from the sample containing thiuram type accelerators.
The decrease of antioxidant contents by oxidation (100°C, test tube method) of vulcanized sample could be confirmed from the density of color.
The proposed method is rapid, simple and sensitive.View full abstractDownload PDF (924K) -
Photometric titration based on the distimulus colorimetry. IMitsuo ITO, Sôichirô MUSHA1964 Volume 13 Issue 10 Pages 971-975
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA photometric titration of two-color mixture modifying the complementary distimulus colorimetry is proposed.
An instrument available for this purpose is described, and its application to acid-base titration is discussed. The optical system consists essentially of two phototubes and two interference filters. Each interference filter in the front of the phototubes give a primary stimulus, and the meter current in an amplifier indicates the value corresponding to the resultant stimulus. Titration of weak acid with standard sodium hydroxide solution was carried out by measuring x, the ratio of one stimulus to the resultant stimulus.
The shape of titration curve was analogous to that obtained in the conventional photometric titration. When the dissociation constant of an acid is much larger than that of an indicator, it has been found as the result of analysis based on the principle of complementary tristimulus colorimetry that the end point locates at a half jump of x.
Titration of weak acids of pK from 2.2 to 5.5 gave satisfactory results with coefficient of variation less than 0.32%, which is approximately equal to that for pH titration with a glass electrode. The pK of several acid-base indicators were determined from an x-pH diagram.View full abstractDownload PDF (739K) -
Studies on inorganic thin layer chromatography. IIIKoji KAWANABE, Shoji TAKITANI, Motoichi MIYAZAKI, Zenzo TAMURA1964 Volume 13 Issue 10 Pages 976-981
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe separation and identification of 20 common anions were examined on a plate of HCl-treated silica gel containing 5% of soluble starch using 3 kinds of developing solvents.
The separation of CNS-, I-, Br-, Cl-, Fe(CN)63-, Fe(CN)64-, ClO3-, BrO3-, IO3-and NO3- by acetone-H2O (10:1), F-, NO2-, S2O32-, SO42-, CrO42-, PO43-, AsO43- and AsO33- by methanol-n-butanol-H2O (3:1:1), C2O42-and BO22- by n-butanol saturated with 2N HNO3 were successfully carried out.
An improved developing chamber of turning type has been made for the effective saturation of solvent vapour.View full abstractDownload PDF (1132K) -
Shichibei KOZAWA, Shigeru KIMURA, Takashi KIDA, Teiji NAKAGAWAL, Shige ...1964 Volume 13 Issue 10 Pages 981-988
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new spectrophotometer is constructed for the measurements in the wavelength region of far ultraviolet to near infrared, that is, from 183 mμ to 1200 mμ. For the measurements in the far ultraviolet region, the monochromator can be effectively flashed by nitrogen gas. If flashed, the stray level is less than 0.1% in the wavelength of 185 mμ. A null method with a potentiometer is adopted in the photometric circuit.
Transistors are used for the power supply of light sources. By these devices, the whole set becomes compact, the accuracy is increased and the reproducibility of less than 0.1% can be obtained for measured values. The results of the measurements of ammonia vapor and methyl ethyl ketone vapor show very good resolution in far ultraviolet region and certify the measurability of the apparatus below to 183 mμ.View full abstractDownload PDF (1320K) -
Narito YOKOUCHI, Hitoshi TAMURA1964 Volume 13 Issue 10 Pages 988-993
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDEHQ was nitrated by a mixed acid (HNO3 : HClO4-1 : 1) and determined polarographically, utilizing the reduction of nitro group. 1.05.0× 10-3 mole DEHQ in 5 ml methanol solution was nitrated quantitatively by 4 ml mixed acid in 10 min.at 40°C. The dinitration did not occur in the condition. DEHQ was nitrated in a water-methanol solution in a milder condition than that for its nitration in methanol.
Nitro-DEHQ gives a wave, of which half wave potential was -0.17 V vs. S. C. E. at pH 2.0 in phosphate buffer.
Comparison of the wave height to that of nitrophenol indicates that the polarographic reduction proceeded to the amine. The concentration of gelatin as a maximum suppressor give a larger influence on the wave height. Although hydroquinone and its monomethyl ether interfere, . DEHQ can be separated from them by a preliminary ether extraction at pH 12.0.
The method was applied to the determination of DEHQ in methyl-metacrylate in which 0.1% DEHQ was determined within an error -5%.View full abstractDownload PDF (753K) -
Masami MURANO, Shigeru MIYAZAKI1964 Volume 13 Issue 10 Pages 994-1000
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTin forms a red colored complex with gallein in a weakly acidic solution. The proposed method for determination of tin involves the extraction of the complex with iso-amylalcohol and measurement of the absorbance of the extract. Influence of various factors on the absorbance including the acidity of the solution, the concentration of gallein and coexisting salts, the color stability, and the velocity of the complex formation have been studied.
The recommended procedure : a sample solution containing 050μg of tin is taken into a 50 ml volumetric flask and acidity of the solution is adjusted with 1N hydrochloric acid so that it reaches 0.15N by the final dilution. After an addition of 2 ml of 0.1% gallein solution, it is diluted to the mark with water and is allowed to stand for at least 15 minutes. The solution is extracted with 10 ml of iso-amylalcohol and the extract is taken into a 1 cm cell through a dry filter paper. The absorbance is measured at 575 mμ against the blank.
When higher sensitivity is needed, the acidity is adjusted to 0.05N and the absorbance is measured at 500 mμ within 30 minutes.
A large amount of sulphate decreases the absorbance of the reagent although chloride or nitrate increases it.
Molybdenum, tungsten, titanium, germanium, zirconium, iron (III), vanadium (V), antimony (III), and cerium (IV) interfere with this method.View full abstractDownload PDF (1020K) -
Tsuneo SHIMIZU, Kyoichi HOSOHARA1964 Volume 13 Issue 10 Pages 1000-1005
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method has been proposed for the simultaneous determination of tantalum and niobium in ammonium oxalate-pyrosulfate medium using tiron as a color reagent.
For the simultaneous determination of tantalum and niobium the absorbance at 420 mμ is first measured at pH 4.9. Then an aliquot of the colored solution is taken, adjusted to pH 7.5 and diluted to a definite volume, being the absorbance measured at 450 mp. The value thus obtained corresponds to the absorbance for niobium. The contribution of niobium to the absorbance at 420 mμ can be estimated by an analytical curve constructed previously in the same condition. The net absorbance of tantalum is obtained as a difference between first and second readings of absorbance at 420 mμ.
Satisfactory results are obtained with the simultaneous determination of 0.5 to 2.0 mg Ta and up to 2.7 mg Nb in 25 ml of the sample solution.View full abstractDownload PDF (777K) -
Sadao HAYASHI, Chiyoko NAKANO, Takuhiko MOTOYAMA1964 Volume 13 Issue 10 Pages 1005-1011
Published: 1964
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPolyvinyl acetate turns to red-brown or red-violet by reaction with iodine-potassium iodide, and this specific reaction is utilized for the detection of polyvinyl acetate blended with other polymers. Copolymers of vinyl acetate with other monomers exhibit less coloration with iodine, probably because of shorter chains of vinyl acetate units in those polymers.
Identifications of copolymers and blend polymers of vinyl acetate-methylacrylate system were studied by their color reactions with iodine on emulsified polymers, as well as by their sorption of iodine and the swelling of polymer films.View full abstractDownload PDF (1073K) -
Takashi ASHIZAWA, Kikuo NAGASAWA, Kanji HARUYAMA1964 Volume 13 Issue 10 Pages 1011-1016
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe cause of abnormality in the dithizone extraction of trace of bismuth from an acidic solution was clarified. A minimum extractability appeared at pH 4 in the presence of citric acid and at pH 6 in the presence of halogen ions.
The tendency was increased in the chloroform solution than in the carbontetrachloride solution. Although the pH 2.53.5 had been hitherto considered as the optimum condition for the extraction of bismuth, the authors recommended the extraction from the solution adjusted to pH 1.5 by nitric acid and ammonia in the presence of acetate ion, whereby trace bismuth could be separated completely even from 1 g of lead. Phosphate and sulfate also disturbed the extraction.
An optimum condition was determined for the extraction with 10 ml of dithizone (1 × 10-3M)carbontetrachloride from 50 ml of aqueous solution of pH 1.5. 210Pb in a uranium are from Ningyo-Toge mine was preliminarily separated by the precipitation as lead sulfate using a large amount of lead carrier, the daughter 210Bi was extracted by the proposed method, and the β-activity was measured for the determination of 210Pb. The amount of 210Pb was only 75% of that expected from the radiation equilibrium.View full abstractDownload PDF (927K) -
Polarographic determination of impurities in semiconductor materials.I.Susumu KAKUMOTO1964 Volume 13 Issue 10 Pages 1016-1023
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the square-wave polarographic determination of copper and lead in high purity tellurium for the semiconductor material, a large amount of tellurium was removed preliminarily with MIBK extraction.
64Cu was applied for detecting slight extractability of copper with MIBK, and nitric acid was added to the aqueous phase to prevent the extraction of trace of copper.
The sample was decomposed with aqua regia, evaporated to dryness and evaporated again with hydrochloric acid. The residue was dissolved in. 20ml of 6N or 7N hydrochloric acid-0.5N nitric acid solution and the extraction was repeated a few times using 20ml each of MIBK.
Nitric acid was supplied, during the extraction, . to maintain its concentration in the aqueous, phase within the range of 0.50.8N. The aqueous. phase was evaporated with nitric acid and sulfuric acid (6+1) to the disappearance of acid fumes. The residue was dissolved in a definite amount of 1M sulfuric acid or 2M phosphoric acid, and the square-wave polarogram was recorded over the range of -0.0-1.0V (vs. Hg pool).
The proposed method was applied to various tellurium samples with purity above 99.99% and satisfactory results were obtained.View full abstractDownload PDF (1469K) -
Fumio AOKI, Hideo TOMIOKA1964 Volume 13 Issue 10 Pages 1024-1029
Published: 1964
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn absorptiometric method for the determination of minute amounts of iron(III) by the solvent extraction of N-benzoylphenylhydroxylamine-iron complex from weakly acidic media has been studied.
Extracting agents such as carbon tetrachloride, chloroform, n-butyl alcohol etc. have been tested, among which carbon tetrachloride has proved to give highest and uniform absorbance over the pH range of the aqueous solution from 1.8 to 6.
Tin, vanadium, titanium, molybdenum and tungsten interfere with the determination of iron by this reagent but they have been found not to interfere when hydrogen peroxide and tartaric acid are added prior to the extraction.
The molar extinction coefficient at 440 mμ is 5.07× 103 and the sensitivity is 0.011 μg/cm2 in Sandell's expression.
The outline of the method is as follows :
To the sample solution, which contains 5 to 150 μg of iron (III), are added 5 ml of hydrogen peroxide, 1 g of tartaric acid and water to bring the volume to about 30ml. This solution is adjusted to pH 2.53 with 30% sodium acetate and water is added to bring the volume to 50 ml. Iron is extracted with 10 ml of 0.2% N-benzoylphenylhydroxylamine in carbon tetrachloride.
Absorbance of the extract is measured at 440 mμ.
The reagent enabled us to perform the successive determinations of iron and vanadium in crude oils and fuel oils.View full abstractDownload PDF (1078K) -
[in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1030-1032
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1032-1035
Published: 1964
Released on J-STAGE: February 16, 2010
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[in Japanese]1964 Volume 13 Issue 10 Pages 1035-1037
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1037-1040
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1040-1042
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1042-1043
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1044-1045
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1046-1051
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1051-1053
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1054-1056
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1056
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1060-1064
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1065-1080
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1964 Volume 13 Issue 10 Pages 1081-1087
Published: 1964
Released on J-STAGE: June 30, 2009
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[in Japanese]1964 Volume 13 Issue 10 Pages 1088-1093
Published: 1964
Released on J-STAGE: June 30, 2009
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