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Volume 14, Issue 10
Displaying 1-26 of 26 articles from this issue
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Yoshikazu YASUMORI, Masao IKAWA, Yasuhiro NOZAWA1965 Volume 14 Issue 10 Pages 871-874
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe results of Karl Fischer titration by coulometry with an electrolytic cell with a long. connecting chamber are described.
The obtained values agreed with the theoretical ones within 0.52.0% errors for the watercontent of more than 80 μg. Although the reproducibility in the repetition of measurements was good in the earlier determinations, the later results were too high. The amount of electrolytic current did not affect the result, but for a slight tendency to give a little higher result with increasing electrolytic current.View full abstractDownload PDF (565K) -
Preparation of samples for quantometry by means of powder metallurgical method. IAkira IKEHATA, Yoshikazu SUZUKI, Sougo SAYAMA, Teiichi MATSUMAE1965 Volume 14 Issue 10 Pages 874-880
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPowder metallurgical method was applied to the preparation of powdered samples for quantovac, whereby the analytical sample was mixed with electrolytic iron powder and sintered after its press molding. The surface texture of samples varied remarkably with the sintering conditions and this gave a remarkable influence on the spectrum line intensities of base iron. The high voltage spark excitation for the sample prepared by 1 hr. sintering at 350°C in air gave stable line intensities.
The method was applied to the analysis of coal ash, and satisfactory calibration curves were obtained for SiO2, Al2O3, and MgO. The precision of the method was 2.1% for SiO2 (contents in ashes 43.480.5%), 3.2% for Al2O3 (9.321.0%), and 0.5% for MgO (0.59.6%).View full abstractDownload PDF (965K) -
Toshiharu MURAKAMI1965 Volume 14 Issue 10 Pages 880-886
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of potassium in sea water and marine salt based on its precipitation with an excess of sodium tetraphenylborate and the subsequent titration of the excess after filtration with a standard solution of benzalkonium chloride using titan yellow or calmagite as an indicator was performed. The titration using titan yellow indicator must be carried out, in the presence of a large amount of magnesium, by masking magnesium ion with EDTA solution. The optimum pH range for calmagite indicator becames narrower in the presence of an appreciable amount of magnesium.
Pontachrome Azure Blue B, Sunchromine Blue FBG and Chrome Azurol S can serve as indicators and the suitable pH ranges for them were 35 in the presence of sodium chloride or magnesium chloride. Aqueous solutions of these dyes (0.2%) were stable for at least 3 months and were employed successfully as indicators for the determination of potassium in sea water and marine salt. Sunchromine Blue FBG and Chrome Azurol S were better for use than Pontachrome Azure Blue B, since the titration was performed even in the presence of small amount of perchloric acid or phosphoric acid.View full abstractDownload PDF (1132K) -
Takeshi ISHII, Sôichirô MUSHA1965 Volume 14 Issue 10 Pages 886-891
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn alternating current polarographic method for determining vanadium present in petroleum as porphyrin complex is described.
The proposed method was applied to the determination of vanadium in petroleum as follows: Vanadium in 10 ml of sample is extracted by shaking for 10 min. with 20 ml of 2F potasium thiocyanate-0.45F sulfuric acid in a separating funnel. The extract is diluted to 25 ml in a volumetric flask with new solution. The alternating current polarogram in the region of applied potential from 0.0 to-0.8 volt vs. SCE without deaeration is recorded, and vanadium is determined by a standard addition method.
Three determinations on Santa Maria Valley, Kuwait and North Texas Petroleum of the samples gave the average of 1.38 ppm, 2.72 ppm and 0.90 ppm with 1.82%, 1.24% and 2.78% of coefficient of variation, respectively. The present method is more rapid than the conventional one and the time required is 30 min. per sample.View full abstractDownload PDF (767K) -
Yatsuka ONO, Takeichi SAKAGUCHI1965 Volume 14 Issue 10 Pages 891-895
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe flexibility of adenosine triphosphate (ATP) with gradually decomposing structures has led to a study of the thin layer chromatography in the microgram region per 0.01 ml and the development of a method of separation for multipreparations containing amino acids, α-ketogulutaric acid and sugar.
Randerath's method was examined. An empirical function of the area of the spot varies in position and shape as the amount of ATP and the thickness of the layer of DEAE-cellulose changes, and it was found that the spot of 15 μg/ 0.01 ml in the case of 0.5mm layer and the spot of 20 μg/0.01ml in 1 mm layer was the best.
The method was applied successfully to a separation of the preparation of ATP containing ADP and AMP with widely varying distributions.
The results indicate that this method can be applied with confidence to the separation of ATP, amino acids, a-ketogulutaric acids and sugar.View full abstractDownload PDF (661K) -
Nobukazu OKAMOTO, Akimitsu KOBAYASHI, Masao KAJIKAWA, Keishi HASEGAWA1965 Volume 14 Issue 10 Pages 896-902
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChemical structural analysis can be done on the fine structure of X-ray K absorption spectrum of a compound which is expected to be closely related to its chemical structure and valence state.
High resolution and precision are required to obtain the fine structure and the double crystal spectrometer has been widely applied.
In this paper, the use of a single crystal spectrometer (Topaz single crystal) is discussed and it is applied to obtain the fine structures of X-ray CoK absorption spectra in various cobalt compounds.
The main edges and the first absorption amplitude are almost indifferent in every case, but compounds of high covalent bond character gave the first absorption amplitude slightly displaced towards the higher energy sides.
By using the fact, the form of cobalt in hydrofining catalysts is identified to be cobalt aluminum oxide.
Another result suggests that fine structure depends on immediate surroudings of the cobalt atom.View full abstractDownload PDF (897K) -
Yasumitsu UZUMASA, Kenjiro HAYASHI, Yukio NURISHI1965 Volume 14 Issue 10 Pages 902-908
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new method for precipitation of aluminum hydroxide from homogeneous alkaline solution with ethylenechlorhydrine was proposed. In this method, aluminum ion is generated at a slow rate to produce the precipitate of hydroxide, and it precipitates as a dense, readily filterable form. The influence of various anions on the character of the precipitate and the amount of coprecipitated anions was determined in varied conditions. The influence of various anions on the volume of coagulated precipitate of aluminum hydroxide sol was also studied.
The results of the experiments gave the following conclusions.
(1) The volume of precipitate (after 24 hr.) is affected by the size of primary particle of the precipitate, which is determined by the rate of hydrolysis of ethylenechlorhydrine. The influence of anion on the volume of precipitate is smaller in this method than in the urea method.
(2) The volume of precipitate increases in the order of NO3-, Cl-, and SO42-
(3) An anion used as the coagulant is adsorbed on the primary particle of aluminum hydroxide, and the amount of coprecipitated anion is given by the following equation.
logM=K+alog[A]+bph where M is the amount of an anion coprecipitated, [A] is the concentration of the anion added in the solution, and a, b and K are constants.View full abstractDownload PDF (1017K) -
Masao MARUYAMA, Hiroko SAKAGUCHI1965 Volume 14 Issue 10 Pages 908-912
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFundamental experiments were performed for the determination of nitrobenzene in aniline by the use of an electron capture detector. A Wilkens' Detector containing 250 mC tritium as a radiation source and a glass column packed with Carbowax 6000 5%/C-22 (5060 mesh, KOH, treated) were employed.
The mutual separation of aniline and nitrobenzene was complete under the following condition : the column temperature, 100°C : carrier gas flow rate, 40 ml /min. : whereby the calibration line for nitrobenzene was linear over the range of 2 × 10-101.5 × 10-7g. As little as 2 × 10-5% of nitrobenzene in aniline can be determined.View full abstractDownload PDF (788K) -
Sueo NISHI1965 Volume 14 Issue 10 Pages 912-916
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBenzenesulfonates including their alkyl (C1C4) derivatives and naphthalenesulfonates were desulfonated by heating them in phosphoric acid. Resulting aromatic hydrocarbons were trapped into cold solvent, and estimated by gas chromatography (using internal standard technique).
Desulfonation of benzenedisulfonate required 90 min. at 270°C, and benzenesulfonate required 60 min. at 250°C. But the other sulfonates were desulfonated rapidly before the temperature reached 250°C.
Alkylbenzenesulfonates of which alkyls contain more than 3 carbon atoms charred at 200°C in phosphoric acid and decreased the yield of hydrocarbon. However, the charring was prevented by the addition of tin metal into phosphoric acid. The sulfuric acid formed was reduced to hydrogen sulfide during desulfonation, and the yield of alkylbenzene was quantitative.
Tertiary-butyl benzenesulfonate was dealkylated partially to give some quantities of benzene.
The desulfonation technique is widely useful as an analytical method of aromatic sulfonates.View full abstractDownload PDF (851K) -
Sueo Nisui1965 Volume 14 Issue 10 Pages 917-920
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method involving alkali fusion of alkylaryl sulfonates followed by gas chromatography of resulting phenol has been developed.
The lower homologues of alkylaryl sulfonates are identified simply by comparing the elution time with corresponding standard phenols, and higher homologues are also identified from the relation between their carbon number and elution time of resultants. The method is applied to the classification of alkylbenzene sulfonates for detergent whereby their alkali fusion products give characteristic gas chromatographic patterns comparable to those of original alkylbenzenes.View full abstractDownload PDF (423K) -
Sinko GOTO, Fujio ITO1965 Volume 14 Issue 10 Pages 921-926
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA specific method for the determination of microgram quantities of pentachloronitrobenzene (PCNB) contaminated with the other nitrobenzenes was investigated. The recommended method for the analysis of soil samples is as follows.
The sample containing 20150 μg of PCNB was extracted with ether by batch procedure. After the evaporation of the ether, the residue was dissolved in acidic ethanol and boiled under refluxing with zinc dust to reduce nitrobenzenes to corresponding anilines. The high chlorinated anilines such as pentachloroaniline, tetrachloroaniline and trichloroaniline was partitioned into low boiling petroleum ether from diluted ethanol solution. The petroleum ether solution was condensed to about 0.5 ml on a water bath held at about 50°C and the condensed solution was applied to an thin layer plate with 1 mm thickness made of alumina powder containing 10% of water. The plate was developed using a 95+5 mixture of n-hexane and ethyl acetate as a solvent. After drying for 5 minutes the band of pentachloroaniline (Rf 0.5) was scraped from the plate and collected into a centrifuge tube and was mixed with 15 ml of a 1+3+4 mixture of hydrochloric acid, acetic acid and water. After the centrifuge, 10 ml of the supernatant was pippeted into a test tube. Pentachloroaniline in the solution was diazotized by adding sodium nitrite solution and after the removal of excess nitrous ion with ammonium sulfamate, the diazonium compound was coupled with N-(1-naphthyl) ethylenediamine dihydrochloride. The resulting brown color was subjected to the spectrophotometric measurement. The calibration curve had to be prepared by treating standard PCNB dissolved in ether solution in just the same manner as the extract of sample treated, because about 50% of PCNB and pentachloroaniline was lost as vapor during the evaporation of solvents and the chromatography.
The results of recovery test were tabulated in. Table VI.View full abstractDownload PDF (912K) -
Masayoshi YAMAO1965 Volume 14 Issue 10 Pages 926-930
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe behavior of formaldehyde on various polyethyleneglycol columns in gas chromatography was studied, and following results were obtained.
1. Retention time of formaldehyde shortens as the amount of hydroxyl group in liquid phase decreases.
2. Temperature dependence of retention time of formaldehyde is affected largely by the amount of hydroxyl group in liquid phase.
3. Relative sharpness of formaldehyde peak increases as the amount of hydroxyl group in liquid phase decreases.
Therefore, when samples containing formaldehyde are analyzed by gas chromatography, overlaps of other peaks on formaldehyde peak can be avoided by adjusting the amount of hydroxyl group in liquid phase.
In the case of a glycerin column, the relative retention time of formaldehyde differed from that in the report of Stevens (2), and the difference was discussed.View full abstractDownload PDF (686K) -
Tsugio TAKEUCHI, Yoshio SHIJO1965 Volume 14 Issue 10 Pages 930-934
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS4-(2-Pyridylazo)-resorcin (PAR) reacts sensitively with iron (III) to form a water-soluble red complex in the presence of nitrilo-triacetic acid (NTA). The complex gives a fixed value of absorbance at pH 8.0 to 9.3, and its maximum absorbance lies at 536 mμ. The sensitivity is extremely high, since its molar extinction coefficient 6.04×104 is 6 and 3 times as much as those of 1, 10-phenanthrolin complex and bathophenanthrolin complex, respectively.
While many ions interfere, more than 10 metal ions are masked by the presence of NTA and an addition of CyDTA. Cobalt and nickel are masked by potassium cyanide. Cu, Ga, Ti, Hf, Cr, U, V, Sn, Ta, Au, Bi, and Zr interfere. The method is useful for the determination of ppb iron (III) in water.View full abstractDownload PDF (630K) -
Studies on the analytical application of onium compounds. XXIHiroshi MATSUO, Shokichi CHAKI, Shigeki HARA1965 Volume 14 Issue 10 Pages 935-938
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSZephiramine reacts with thiocyanatocobalt (II) complex ion to form bright blue precipitate. The precipitate is extracted with chloroform, and the extract is extremely stable and has an absorption maximum at 625 mμ. The mole ratio of cobalt and zephiramine in the extracted complex is 1 : 2. The formation of precipitate and the efficiency of chloroform extraction are not influenced by the pH in the acidic region. Beer's law is obeyed over the range of cobalt_ concentration 1.2 ppm to 12 ppm.
Many metal ions in their amounts comparable to that of cobalt do not interfere, but 0.1 ppm Fe and 0.8 ppm Cu do interfere.View full abstractDownload PDF (448K) -
Yasuo TAKAHASHI1965 Volume 14 Issue 10 Pages 939-945
Published: 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDumas and Kjeldahl procedures were applied to the determination of nitrogen in uranium nitrides.
Apparatus of semi-macro scale, including a nitrometer of 8ml capacity, was employed for Dumas procedure. Uranium nitride was decomposed with or without oxidizing agent between 600°C and 900°C, and volume of nitrogen evolved was measured. Good reproducibility was obtained by using Cu-oxide or decomposition product of AgMnO4 as oxidizing agent.
Various acids and catalysers were tested to digest uranium nitride by Kjeldahl procedure, and a combination of H2SO4 with Se, which was added in the form of H2SeO4, SeOCl2 or SeO2, was found to be most effective Co dissolve uranium nitride and convert its nitrogen to ammonia.
On uranium nitride composed of body centered cubic U2N3 phase, the analytical results of nitrogen determined by the modified Kjeldahl procedure agreed well with those determined by the modified Dumas procedure, but on uranium nitride composed of UN phase, the results obtained by the Kjeldahl were lower by about 5% than those obtained by the Dumas. It was concluded that Dumas procedure was preferred for routine analysis of nitrogen in uranium nitrides.View full abstractDownload PDF (856K) -
Minoru OTA1965 Volume 14 Issue 10 Pages 945-949
Published: 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the process of separation and identification of inorganic substances by thin-layer chromatography, especially in their developement and revelation, an interference is occasionally caused by a minute amount of iron contained in silica gel being used. A simple method was investigated to remove the iron from the silica gel prior to its use, but it was necessary at first to know the amount of iron initially contained in the silica gel. The iron contaminating the silica gel seems to be represented as two kinds; that merely retained on the surface of the gel and that occluded in the gel. And the former seems to affect the chromatographic process. The total amount of iron was determined spectrophotometrically as usual as ferric thiocyanate after the treatment of a sample gel with hydrofluoric acid. On the other hand, dipping a sample in a mixed solvent consisting of acetone, hydrochloric acid and methyl isobutylketone, the iron retained on the surface could be readily released into the solvent, since the silica gel treated by this solvent showed no effect of iron on the chromatographic process. Thus the amount of the iron retained on the surface could be estimated as 25% of the total iron by carrying out the photometric measurement of ferric thiocyanate obtained from the mixed solvent.View full abstractDownload PDF (591K) -
[in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 10 Pages 950-951
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 10 Pages 951-953
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 10 Pages 953-955
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 10 Pages 955-958
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 10 Pages 959-962
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 10 Pages 962-968
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 10 Pages 968-973
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese], [in Japane ...1965 Volume 14 Issue 10 Pages 974-988
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 10 Pages 989-992
Published: 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 10 Pages 993-997
Published: 1965
Released on J-STAGE: June 30, 2009
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