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Volume 14, Issue 7
Displaying 1-21 of 21 articles from this issue
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Masao KAWAHATA, Rokuro KAJIYAMA1965 Volume 14 Issue 7 Pages 583-586
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid indirect determination of a comparatively large amount of silver in Cu-Ag, or Cu-Ag-Au alloys was examined, which involves the shaking of the silver solution with Cu-diethyldithiocarbamate with successive polarographic determination of the liberated copper.
The sample was acid-digested, and the silver was separated as the AgCl precipitate. This was dissolved in ammonia, and was shaken in a separatory funnel into ethyl acetate solution of Cu-diethyldithiocarbamate to liberate equivalent amount of copper. The aqueous layer was transferred into a beaker and adjusted to pH 3.2 with EDTA solution and ammonium acetate buffer solution. The polarogram of -0.15 to -0.75V was obtained to determine the amount of copper from which was indirectly estimated the amount of silver. The half-wave potential of Cu-EDTA was -0.23V (vs. S. C. E.), and the sensitivity of the determination was 0.3 mg Ag /100 ml for the wave height of 10 mm. Five to 30% of silver was determined rapidly with satisfactory resultsView full abstractDownload PDF (744K) -
Tetsuyasu HATTORI, Satoshi KAWAI, Michinori NISHIUMI1965 Volume 14 Issue 7 Pages 586-592
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSimultaneous determination of the main components in antipyretics was done by the highsensitive gas chromatography. The employed column was 3.5% SE-30, and the temperature 205°C. Since the -OH or -NH2 containing components often show remarkable tailings and are labile to be readily decomposed, their acetates as stable derivatives were selected to be subjected to the gas chromatography. The reaction was quantitative, and the standard deviation for each component was not more than 2.7% (n=6). Several compounds difficultly determined by the conventional method such as methylephedrine and guaiacol glycerine ether were easily determined by this means. The inner standard method was employed and the peak magnitude was measured by peak height method.View full abstractDownload PDF (1064K) -
Ikuo ATSUYA1965 Volume 14 Issue 7 Pages 592-597
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of iron by atomic absorption spectroscopy was applied to the analysis of aluminum metals and alloys.
The optimum conditions for the determination were, the wavelength 248 mμ, the current of the hollow cathode lamp for Fe 30 mA, the slit width 0.11 mm, air pressure 1.5 kg/cm2, acetylene pressure 0.5 kg/cm2. In the case of the atomizing after an extraction with MIBK, the optimum acetylene pressure was 0.3 kg/cm2 with water cooling of the burner. The presence of alloying elements and acids did not interfere except nickel, the interference from which varied with the anions present.
A rapid method for the determination of 0.05 10% of iron in aluminum metals and alloys without any separation of main elements was established. Also as little as 0.00050.1% of iron in high purity aluminum was determined after the extractive concentration of Fe with MIBK.View full abstractDownload PDF (986K) -
Studies on inorganic thin layer chromatography. VShoji TAKITANI, Masao Suzuki, Nobuko FUJITA, Kazuko HOZUMI1965 Volume 14 Issue 7 Pages 597-601
Published: July 05, 1965
Released on J-STAGE: February 15, 2010
JOURNAL FREE ACCESSSome 20 common metallic ions were separated and identified by the thin layer electrophoresis using thin layer plate of purified silica gel and starch. Fundamental experiments were at first carried out using citric acid as an electrolyte solution. The relation between the migration distance and the concentration of citric acid as well as with the applied voltage and also the relation between the position of the original point and the migration distance as well as its direction were examined. The electrophoresis was carried out for 20 min. with 1200 V/30 cm, using 0.15M citric acid as the electrolyte and setting the spot at 10 cm from the center of the thin plate toward the anode. Na+, Li+, Ca2+, Mg2+, Ba2+, Sr2+, Cu2+, Ni2+, Co2+, Fe3+, Pb2+, Zn2+, Cr3+, Mn2+, Al3+, Cd2+, Bi3+, Sn4+, Sb3+, As3+, Ag+, and Hg2+ were separated, and identified by respective detecting reagents.View full abstractDownload PDF (851K) -
Shigeru SUZUKI, Takeshi KAJIWARA1965 Volume 14 Issue 7 Pages 602-605
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the case of analysis of phosphorus in low carbon-ferrochromium containing about 15% of silicon, the results obtained by alkali-fusion method always show lower values than those obtained by nitric-hydrofluoric acid-decomposition method.
The reason for this was studied and attributed to the exceedingly low recovery of phosphate with ferric hydroxide from a solution containing a large amount of silicate. The recovery is lowered with increasing amount of silicate present and with decreasing amount of ferric hydroxide.
It seems that there is a linear relation between the amount of coexistent silicate and the minimum amount of ferric hydroxide required for the quantitative recovery of a definite amount of phosphate.View full abstractDownload PDF (628K) -
Studies on rhodanine derivatives as analytical reagent. IYahyoe KINOSHITA, Hisashi KOIKE, Kaoru OHASHI1965 Volume 14 Issue 7 Pages 606-610
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAbsorption spectra of a number of methyl derivatives of rhodanine indicated that hydrogen in 3-position of rhodanine molecule dissociated although that in 5-position did not. The silver ion added to each rhodanine derivative in the acidic medium only weakened the absorbancy as a whole and any shift in the absorption maximum was not observed, hence the effect could not be applied to the determination of silver.However, the addition of silver to the solution of methylrhodanines remarkably lowered the pH of the solution, which seemed to indicate an acceleration of the dissociation of H atom in 3- or 5-position of rhodanines by the formation of silver complex.
The dissociated hydrogen ion was determined potentiometrically or conductometrically, from which could be indirectly determined the amount of silver.View full abstractDownload PDF (789K) -
Studies on rhodanine derivatives as analytical reagent. IIYahyoe KINOSHITA, Hisashi KOIKE, Kaoru OHASHI, Masaaki MATSUO1965 Volume 14 Issue 7 Pages 610-614
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of silver by 5-(2, 6-dimethyl-4-pyranylidene)-rhodanine (P. R.) was investigated. The silver complex of this reagent has one of the absorption maxima at 330 mμ. P. R. as the analytical reagent has a number of advantages including smaller reagent blank at 330 mp and comparatively larger solubility in water than the conventional rhodanine reagent. The P. R. reagent was added to a solution containing silver ion (540μg/ml), the mixture was diluted to a definite volume with a buffer solution of pH 1.73, and the absorbance at 330mμ was measured against the P. R. reagent blank. The color obeyed Beer's law in the above concentration range. Metal ions other than Hg2+ and Fe3+ did not interfere, and the silver was determined accurately within 2% error. The color did not change with time and the mole ratio of the complex was determined as 1 : 1 by the continuous variation method.View full abstractDownload PDF (777K) -
Yutaka ASAHI, Fumiko KASAHARA1965 Volume 14 Issue 7 Pages 614-618
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for the determination of idonate and gluconate in the reduction product of calcium 5-ketogluconate has been developed. Idonate and gluconate form complexes with molybdate and borate to give a change in their optical rotation and other physical properties. For the determination, optical rotatory power was measured under the following two conditions : (A) In 0.35M diammonium molybdate with 18% acetic acid, 0.010.05M idonate gives [M]25°D-577° (M-1m-1) and 0.010.15M gluconate gives 748°, (B) In 0.05M borax, 0.010.25M idonate gives [M]25°D 38.6 and 0.010.15M gluconate gives 58.8°. The determination takes only 10 min. for a sample. The accuracy was about 1%.View full abstractDownload PDF (904K) -
Yutaka ASAHI, Fumiko KASAHARA1965 Volume 14 Issue 7 Pages 619-622
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBoth idonic acid and gluconic acid consume 4 moles of periodate in acid solutions. This reaction is used for a simple determination of their sum. Periodate gives two steps of reduction waves : the first wave by the reduction of periodate to iodate and the second wave by the reduction of iodate to iodide. The reaction rate of periodate with idonic acid or gluconic acid was followed polarographically in various conditions. The rate constant of the reaction of 10 mM periodate with 1 mM sample at pH 6.8 and 15°C was 1.09 (min-1) for idonic acid and 0.65 for gluconic acid. The difference is used for the determination of each acid.View full abstractDownload PDF (747K) -
Tsugio TAKEUCHI, Sadao MORI1965 Volume 14 Issue 7 Pages 622-630
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCommercial F&M C.H.N. Analyzer (Model 180) is an instrument for determination of elements C, H and N at one operation by gas chromatography. Many factors influencing on precision and accuracy of the determination by this analyzer were examined statistically. Day's difference of precision and bias of means were small at the same condition, although the calibration curve must be checked each time when reduced copper was renewed. The life of reduced copper was estimable from the values of standard deviation. Precision of C, N analysis was improved by preparing respective calibration curves for group types or homologues.Considering the blank values of Ag2O, the lower limit of determination was estimated as follows; C 5%, H 0.5%, N 3.5%.View full abstractDownload PDF (1539K) -
Studies on the Hydroxy Derivatives of Chromone as Analytical Reagents. IAkira MURATA, Tetsuo SUZUKI, Takushi ITO1965 Volume 14 Issue 7 Pages 630-636
Published: July 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS5-Hydroxychromone (I), yellow crystals, mp. 125.5127.5°C, was prepared by treating 2, 6-dihydroxyacetophenone with ethyl formate and metallic sodium. The acid dissociation constant of (I) was estimated by the spectrophotometric method to be pka=10.75. The reactions of (I) with a number of metallic ions at various pH were examined. Twelve ions formed complexes; those of Cu2+, Be2+, Al3+, Sn4+, Ti4+, Bi3+, U6+, Fe3+, and Pd2+ were extractable into organic solvents and those of Th4+, Co2+, and Ni2+ were not. The compound (I) may be used as a sensitive reagent for the photometric determination of Cu2+, Be2+, Al3+, Ti4+, Fe3+, and Pd2+. The beryllium complex fluoresced strongly under ultraviolet radiation in both aqueous and organic solutions, and beryllium can be determined by the fluorometric method. The absorption spectra of the complexes and the effects of pH on the extraction of these complexes were shown.View full abstractDownload PDF (1042K) -
Satoru EGASHIRA, Hitoshi NAKASUKA, Yasumasa TAKEYAMA1965 Volume 14 Issue 7 Pages 636-640
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the ion exchange chromatography of weak acids such as carboxylic acids, a theoretical relation between the distribution coefficient, Kd and pH of the eluent was proposed. The relation was represented by equations (5) and (8), and its adequacy was proved experimentally.
The equation (8) is almost equivalent to Beukenkamp's equation, but differs in the existence of the first term, α0χ0, which represents the participation of the adsorption of undissociated molecules.
A remarkable difference was observed in the chromatographic behaviors of cis and trans isomers of unsaturated dicarboxylic acids, e.g.fumaric acid and maleic acid or mesaconic acid and citraconic acid.View full abstractDownload PDF (693K) -
[in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 641-643
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 643-645
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 7 Pages 645-646
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 647-649
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 649-650
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 650-652
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 7 Pages 652-655
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 7 Pages 656-660
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 7 Pages 661-671
Published: July 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS
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