All issues
Volume 15, Issue 7
Displaying 1-26 of 26 articles from this issue
- |<
- <
- 1
- >
- >|
-
Nobuhiko ISHIBASHI, Hitoshi KOHARA, Makoto FUKUDA1966 Volume 15 Issue 7 Pages 637-642
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe radiometric titration of trace amounts of cobalt with EDTA has been investigated. After known amounts of EDTA are added to a series of aliquots of the sample solution containing 60Co, the free metal ion is separated from the EDTA complex by the chelating resin or cation-exchange resin. The radioactivity of the supernatant solution that contains the complex is measured to determine the end point of the titration. The optimum pH and the lowest determinable concentration of this trace analysis are discussed. The experimental results show that 10-6 or 10-7M of cobalt can be determined. The titration of both ferric and cobaltous ions in the mixture is possible.
The mixture of cobaltous and zinc ions is analysed by a replacement titration. After adding EDTA equivalent to the total amount of the both ions and 65Zn as an indicator, the Co(II)-EDTA complex is oxidized to the Co(III) complex. Finally Zn-EDTA complex is titrated with the Fe(III) standard solution. Zinc in the EDTA complex is replaced by ferric ion and separated from the cobalt(III) and iron(III) complexes using a cation-exchange resin. The end point of the titration is determined from the radioactivity of 65Zn in the supernatant solution.View full abstractDownload PDF (924K) -
Hitoshi KOHARA, Nobuhiko ISHIBASHI1966 Volume 15 Issue 7 Pages 642-646
Published: July 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe complex formation of a portion of cobalt present in an analysing sample and the paper chromatographic separation of the complex from excess free cobalt have been investigated for the radioisotopic dilution analysis of the trace amount of cobalt. Beta-nitroso-a-naphthol as the complexing reagent and acetone-isoamyl alcohol mixed solvent (4 : 1) as the developer were shown to be effective for the separation. The recommended procedures are as follows. To the standard cobalt solution containing 60Co as the tracer, the complexing reagent is added less than corresponds to the stoichiometric ratio of the complex. After the formation of complex, the solution is chromatographed by the assending method. The analysing solution, to which a suitable amount of the radioactive standard solution has been added, is treated in the same way as the standard. The amount of cobalt in the analysing solution is obtained by comparing the activity of the separated complex from the standard solution with that from the analysing one. The effects of ferric, cupric and nickel ions are relatively small, and the determination of 10μg/l of cobalt is possible by this dilution analysis.View full abstractDownload PDF (904K) -
Analysis of aminopropylon. IJunji KOIZUMI, Yoshitaka YOICHI, Teisaburo TAKEMOTO1966 Volume 15 Issue 7 Pages 647-652
Published: July 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe authors presented a specific method for colorimetric assay of aminopropylon. The hydrolyzate of aminopropylon forms a soluble reddish-violet pigment with ninhydrin in acidic aqueous solution even at room temperature. The pigment in solution has twoabsorption peaks at 414416mμ and at 536mμ, respectively.
The peak at 536mμ is not influenced by reagent blank absorption, so that it is used as an assay wavelength. Aminopropylon existing with other compounds such as ephedrine-hydrochloride, sulupyrin (J.P.), and quinine-sulfate can be determined with good accuracy.View full abstractDownload PDF (952K) -
Analysis of aminopropylon. IIJunji KOIZUMI, Yoshitaka YOICHI, Masakazu UENO1966 Volume 15 Issue 7 Pages 652-656
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe authors have reported in the previous papers (Analysis of aminopropylon. I.) the spectrophotometricassay of aminopropylon. The method was not satisfactory in removing interferences by noscapine (J.P.), phenacetin (J.P.) and acetaminophene. In order to remove these interferences, and to determine the aminopropylon existing with antifebrile, anodyne, antihistamine etc., the authors adopted a method with 0.1N HCl-chloroform extract treatment whereby most of them were extracted into chloroform and aminopropylon remained in 0.1N HCl layer.
Aminopropylon in antifebrile, anodyne, antihistaminne etc. was determined with good accuracy.View full abstractDownload PDF (850K) -
Masami MURANO, Shigeru MIYAZAKI1966 Volume 15 Issue 7 Pages 657-661
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTin in metals (ferrous metal, copper alloy, zinc metal, aluminum and zinc alloy die castings, lead metal and hard lead) was determined by an extraction-spectrophotometric method with gallein. Tin-gallein complex was formed in a weak acidic solution (I. 0.15NHCl in general and II. 0.05N HCl in case of higher sensitivity required). It was extracted into iso-amylalcohol after standing and washed by a solution containing suitable substane. Its absorbance (I. 575mμ or II. 500mμ) is measured. Interferences of diverse elements were removed as follows; antimony, tungsten and zirconium were masked with tartaric acid, iron and vanadium were reduced with ascorbic acid, and molybdenum and titanium were washed out with a solution containing hydrogen peroxide. The reproducibility of the method represented as relative standard deviation were 2.0% for carbon steel with 0.08% tin, and 0.6% for brass casting with 0.14% tin. The accuracies were good except for lead metal with tin content below 0.01%.
The time required for a single determination was about 30 minutesView full abstractDownload PDF (866K) -
Application of a high molecular weight amine to analytical chemistry. VIToshio SUZUKI1966 Volume 15 Issue 7 Pages 662-666
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the liquid-liquid extraction from a potassium iodide-sulfuric acid solution with 10 vol.% Amberlite LA-1 in xylene, indium shows its preferential behavior to be extracted in the organic phase, but gallium is hardly transfered from the aqueous phase. Hence indium could be separated from gallium, and the latter remaining in the aqueous phase could be titrated withan EDTA solution by using Cu-PAN as an indicator after the solution was adjusted to pH 3.03.5. On the other hand, indium in the organic phase was backextracted with a buffer solution of pH 3.8 consisting of acetic acid and sodium acetate, and titrated with an EDTA solution after, the pH of the solution was adjusted at 3.8. The procedure could be applied to practical samples such as indium-gallium alloys with satisfactory results.View full abstractDownload PDF (786K) -
Application of a high molecular weight amine to analytical chemistry. VIIToshio SUZUKI1966 Volume 15 Issue 7 Pages 666-671
Published: July 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe extraction of bismuth with high molecular weight amines from its mixed solution of hydrobromic and nitric acids rather than from its hydrobromic acid solution was readily achieved. For example, bismuth could be completely extracted from hydrobromic (0.05M) and nitric acids with a 5 vol.% solution of trin-octylamine or tris(2-ethyl hexyl)amine in xylene without the interference of turbidity. Zinc, tin(IV), indium and lead extracted from hydrobromic acid were removed from the organic phase when nitric acid was present in the aqueous phase. Cadmium was extracted in the organic phase together with bismuth under these conditions, but the former was removed from the organic phase by washing with a 0.5M nitric acid solution. The bismuth was hardly stripped with common agents such as nitric acid, but it was stripped quantitatively into aqueous phase of EDTA buffered to pH 3.03.8. After the stripping of bismuth, a conventional EDTA back-titration, with Xylenol Orange as an indicator was successfully utilized to determine the bismuth.View full abstractDownload PDF (977K) -
Ikuo ATSUYA1966 Volume 15 Issue 7 Pages 672-677
Published: July 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAtomic absorption spectrometric investigation of manganese was carried out and a method was applied to the determination of manganese in iron and steels, aluminum alloys and ferror alloys.
The optimum conditions for the determination of manganese were the wavelength 2795 Å, the currentof hollow cathode lamp for manganese 60mA, the slit width 0.05mm, air pressure 1.5kg/cm2 and acetylene pressure 0.5kg/cm2.
Influences of coexisting elements and acids were also examined. The alloying elements and acids except a large amount of molybdenum did not interfere.
A rapid method for the determination of manganese in iron and steels, aluminum alloys and ferro alloys without any preliminary separation of main elements was established. The method is very accurate and highly reproducible.View full abstractDownload PDF (972K) -
Eiji NIKI, Atsushi SAWATARI1966 Volume 15 Issue 7 Pages 677-683
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the purpose of discussing the performance andthe application of the continuous analyser with the feed back elements, the stability of the continuous titrator with proportional plus integral actions was analysed by the automatic control theory. According to the stability analysis, the conditions for the more stable system were concluded as follows; the larger integral time, the smaller controller sensitivity, the smaller time constants of detector and of titration cell parts and the smaller dead time of the system. The theoretical results were compared with the ex perimental ones. From the experimental data on the response, the authors obtained the response really without fluctuation in the neighborhood of the theoretical region. In the other regions, however, the response showed some fluctuation.View full abstractDownload PDF (1053K) -
Koichi TONOSAKI, Makoto OTOMO, Koichi TANAKA1966 Volume 15 Issue 7 Pages 683-686
Published: July 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChromium (III) reacts with an excess of Xylenol Orange (XO) to form two complexes, the absorption maxima of which are found at wavelengths 527mμp and 510mμ, respectively. The former, which was used to the spectrophotometric determination of chromium, gives the maximum absorbance in the pH range from 1.9 to 2.2. Under the conditions investigated, Beer's law is obeyed up to about 30μg of chromium in 25ml. The sensitivity of the reaction is 0.002μg Cr per cm2. Among the anions tested, chelating agents such as NTA and EDTA interfere seriously wiht the determination.
The complex has a composition of 1 to 1 in the metal-ligand ratio, and has the apparent formation constant of 3.7×103 at pH 1.7.View full abstractDownload PDF (649K) -
Eijiro KAMATA1966 Volume 15 Issue 7 Pages 687-688
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe mixture of succinic and lactic acids has been hardly isolated even with a longer column. In practice, in order to transfer the sample solution containing small amounts of the acids quantitatively onto a silica column (55cm long, 0.7cm dia.), the solution is mixed with one gram of silica gel which gives 6 cm of the sample column. The two acids are completely separated. by the development with an 18% tert-butanol-chloroform accompanied by a preliminary development with 10ml of 14% tert-butanol-chloroform. The effect of the preliminary development to give the clear-cut separation of the elution bands is attributed to the concentration gradient of tert-butanol occurring around each solvent front, namely, this concentration gradient is effective in constricting the individual chromatograms in the column.View full abstractDownload PDF (349K) -
Organic elemental analysis by the flask combustion method. IShigeki Ota1966 Volume 15 Issue 7 Pages 689-692
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAnalytical procedures could be very conveniently and rapidly performed by a method using a combustion flask with joint equipped with a measuring pipet, stopper cock, oxygen introduction pipe, washing pipe, washing effusive hole, platinum lead wire, platinum coil, and platinum, or quartz basket, etc.
In quantitative analysis with this apparatus, it is desired that the volume of absorption fluid be made as small as possible. For this purpose, the interior of the flask is washed with distilled water, which is then removed completely by shaking the flask several times, and thereafter placing an absorbent therein.
In the analysis of iodine, a satisfactory result was obtained by using sodium oxide in place of hydrogen peroxide. After sample combustion, the flask was allowed to stand, without shaking, in ice water for about 1 minute. The inner surface of the flask, cock, and basket could be rinsed automatically with the fluid aspirated by reduced pressure in the flask. Thus, titration could be performed without transferringthe fluid to other vessels. The titration was carried out with 0.005N Hg(NO3)2 for Cl, Br, and I; with 0.01N Th (NO3)4 for F; and with 0.01N Ba(CH3COO)2 for S. It took only 67 minutes to complete the analysis, excluding the time required for weighing the sample.View full abstractDownload PDF (703K) -
Hiroshi MATSUO, Shokichi CHAKI, Shigeki HARA1966 Volume 15 Issue 7 Pages 692-694
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSZephiramine reacts with iron thiocyanate complex ions to form a reddish-brown precipitate. The precipitate is extracted with chloroform, and the extract is stable for at least 2days after extraction, and shows an absorption maximum at 470mμ. The absorbance of the extract is invariable in the acidic region (pH1.20.2). Beer's law holds for the chloroform extract when iron-thiocyanate-zephiramine was extracted in 10.0ml chloroform from 25.0ml sample solution containing 0.5×10-6M 5.0×10-6M Fe(III). Metal ions, except for copper and bismuth, do not interfere with the determination.View full abstractDownload PDF (495K) -
Kazuichi AKIYAMA, Yukio KOBAYASHI1966 Volume 15 Issue 7 Pages 694-697
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe experiment deals with the determination of titanium in tantalum by chromotoropic acid method. Chromotoropic acid is dissolved in a sodium sulfitesolution to overcome instability under light. The final spectrophotometric determination is carried at pH 1.0to avoid interferences by diverse ions.
The proposed procedure is as follows. The metallic tantalum is changed to oxide by ignition, then fused with potassium pyrosulfate, and the melt is dissolved in a hot ammonium oxalate solution. The solution is cooled and diluted to about 70ml. Five ml of chromotoropic acid solution (made by dissolving 5g chromotoropic acid in 100ml of 5% sodium sulfite solution) is added. Then the pH of the solution is adjusted to 1.0±0.1. The solution is diluted to 100ml, and the absorbance at 480mμ is measured.
The lower limit of determination by this method is 20ppm of titanium in metallic tantalum.View full abstractDownload PDF (515K) -
[in Japanese], [in Japanese], [in Japanese]1966 Volume 15 Issue 7 Pages 698
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1966 Volume 15 Issue 7 Pages 699-710
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2346K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 711-727
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (3322K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 727-736
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1880K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 737-743
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1350K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 744-754
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2051K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 754-761
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1532K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 762-774
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1966 Volume 15 Issue 7 Pages 775-779
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1016K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 779-790
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2242K) -
[in Japanese], [in Japanese]1966 Volume 15 Issue 7 Pages 791-796
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (981K) -
[in Japanese]1966 Volume 15 Issue 7 Pages 797-804
Published: July 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1051K)
- |<
- <
- 1
- >
- >|