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Volume 12, Issue 12
Displaying 1-27 of 27 articles from this issue
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Eisaku KIMURA1963 Volume 12 Issue 12 Pages 1129-1134
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn apparatus for automatic connection and disconnection of absorption tubes with spherical or plane joint has been presented for micro elementary analysis. This enables a through-out hand-off operation from connection till weighing and gives following advantages : (1) elimination of wiping errors, (2) less heat- and atmospheric influence by the adoption of an elongated connection and a protecting chamber of absorption tube, and (3) little fear of breaking tubes in the conventional hand-operations.
The apparatus consists of five parts, u. e. a driving motor with an eccentric cam, a transmission mechanism by utilization of levers, a transportation mechanism with a guiding plate sliding on two rails, an absorption tube operator with a special tube stand, and a controlling circuit. The transportation mechanism is equipped with a special delayed-operation device to increase the safety in removing and carrying absorption tubes.
The proper position of absorption tube is kept by a variable position adjustor equipped on the tube stand. The apparatus is equipped with a calculator of an approximate life of manganese dioxide and also a direct-reading indicator of measuring numbers. The time required for either removing or carrying of absorption tube is only 3 sec.View full abstractDownload PDF (3788K) -
Eisaku KIMURA1963 Volume 12 Issue 12 Pages 1135-1139
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTwo new contact type absorption tubes convenient for connection are presented. The one is made of whole glass and the other is made of a glaas or metal tube with a metal cap with needle pipe on the inner surface. These are further divided into a plane contact type and a ball contact type. The ball types have higher connecting efficiencies. While, the plane types are operated without any obstacle in the analytical procedure.
These tubese have been made for the automatic operation, but they can be hand-operated simply by a lever. They can be connected or disconnected without a wiping operation and the errors therefrom can be eliminated. Each tube has twice capacity of absorbent compared with that of conventional type.View full abstractDownload PDF (1051K) -
Motosuke FURUYA, Masatoshi TAJIRI1963 Volume 12 Issue 12 Pages 1139-1144
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe precipitation of phosphoric acid with thorium ion has been applied on the separation of phosphoric acid.
The sample solution containing phosphoric acid is treated with 20 ml of nitric acid-hydrochloric acid mixture (1+1+2), and diluted to 50 ml with water. About 20ml of 50% ammonium acetate was added for adjusting pH of the solution to 2.03.5. It is then treated with 1.53ml of M/50 thorium nitrate solution against 1 mg P and boiled for about 3 min. to complete the precipitation. It is cooled, the precipitate being filtered and washed with 1% ammonium acetate solution. The recovery of phosphoric acid precipitate adsorbed a little amount of thorium and could not be used for the gravimetric determination of phosphorus.
The method is suitable for removing of phosphoric acid in the determination of magnesium and calcium by EDTA titration and for separation of a large amount of phosphoric acid from copper, nickel and zinc.View full abstractDownload PDF (1273K) -
Hiroshi ASAOKA1963 Volume 12 Issue 12 Pages 1144-1149
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe reaction of cyanide ion with manganese (III) triethanolamine complex in alkaline solution was studied by polarography and spectrophotometry in visible and ultraviolet region.
Manganese (III) triethanolamine complex (green) is reduced gradually to manganese(II) triethanol-amine complex (colourless) in the presence of a large quantity of cyanide ion in alkaline solution, and the latter is again oxidized to the former by air when it is bubbled through the solution soon after the reduction. But if the reduced colourless solution is allowed to stand, the oxidizability of bivalent manganese diminishes with the lapse of time. It seems that manganese(II) triethanol-amne complex changes gradually to a new complex coordinating with cyanide ion, which is incapable of being oxidized to manganese (III) triethanolamine complex.
Provided that the concentration of cyanide ion is less than ca. 0.02 M, the reduction of manganese in this case proceeds very slowly and the effect is negligible for the determinaiion of manganese.View full abstractDownload PDF (1058K) -
Kozo MOMOKI, Jun SEKINO1963 Volume 12 Issue 12 Pages 1149-1153
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSEDTA titration of lead in solution of pH 5 containing small amount of iron(III) has usually been thought as not being affected by iron(III) provided that Cu-PAN is used as an indicator. From the results of similar titration using XO indicator, however, the present authors doubted of this concept, and assumed that positive errors would be caused by the presence of iron(III) for percentages of lead obtained in EDTA titration of such solutions even with Cu-PAN indicator. This assumption came from their general observation that iron(III) had so slower chelate formation rate against its so larger chelate formation constants, and was verified, in this paper, by small but definite positive errors found for the first time in this titration system. These positive errors were supposed to have the same origin as in the titration of solutions containing iron(III) only, as both showed similar dependance on the quantities of iron (III) present. On the other hand, errors were larger than, and thought to have somewhat different mechanism from, the case of XO-EDTA titration.
Masking of iron (III) for the determination of lead without further separation process was successful by a successive titration method based on the one developed by the authors for the case of XO-EDTA system. After the solution containing lead and small amount of iron (III) was titrated at pH 2.5 for iron (III) using sulfosalicylic acid indicator, the solution was then adjusted to pH 5 and titrated for lead using Cu-PAN indicator.
This method was applied successfully to the determination of lead in lead slag, showing quite a practical but excellent nature, as the separation process of lead sulfate precipitate was able to be minimized yet it rather maximized precision and accuracy of the titration.View full abstractDownload PDF (1089K) -
Hiroshi ONISHI1963 Volume 12 Issue 12 Pages 1153-1155
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method is described for the determination of both thorium and zirconium with arsenazo III. In 3N hydrochloric acid containing oxalic acid, thorium alone forms a colored complex with the reagent. The absorbance is measured at 665 mμ. In 9N hydrochloric acid containing gelatin, both thorium and zirconium form colored complexes. The absorbance of the 9N hydrochloric acid solution at 665 mμ is equal to the sum of the absorbances of the thorium and zirconium complexes.
Therefore, zirconium can be determined by difference. Satisfactory results were obtained with 530 μg of thorium and 510 μg of zirconium in a volume of 25 ml or with weight ratios of Th/Zr ranging from 0.5 to 6.View full abstractDownload PDF (594K) -
Studies on inorganic thin layer chromatography. IShoji TAKITANI, Michiko FUKAZAWA, Hitoshi HASEGAWA1963 Volume 12 Issue 12 Pages 1156-1161
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe separation and identification of 24 common metal ions have been made on a plate of 0.3mm thickness with HCl-treated silica gel containing 5% of soluble starch using 3 kinds of developing solvent.
An improvement of the developing chamber has been also made by consideration on the saturation of solvent. In the recommended procedure Ni, Co, Cu, Fe, Pb, Mn, Cr and (As) were separated first by acetone-3N HCl (99 : 1) and it was followed by the separation of Ba, Sr, Ca, Mg, Al, NH4, Na, K and Li by methanol-n- butanol-35% HCl (80 : 10 : 10).
Sb, As, (Cu), Cd, Sn, Bi, Zn and Hg were separated lastly by n-butanol-benzene-1N HNO3- 1N HCl (50 : 46 : 2.6 : 1.4). The relation between composition of developing solvent and Rf values of ions as well as the mutual separation of the same elements (As, Sn, Fe, Sb, Hg etc.) with different ionic valencies has been investigated.View full abstractDownload PDF (1265K) -
Wataru FUNASAKA, Teiichi ANDO, Hiroshi OGIRI1963 Volume 12 Issue 12 Pages 1161-1169
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn thorium nitrate titration of fluoride with Alizarin S indicator, a formate buffer has been applied for adjusting pH of the titrand in order to reduce the remarkable interference from traces of oxidizing agents. Detailed investigations have also been made upon the conditions of titration in the presence of large amounts of sodium nitrate or chloride (as in the analysis of fluorine in organic compounds).
The results are summarized as follows:
(1) The end-point can be detected with satis-factory precision (σ=2.54.5μg F) by the aid of a color standard solution.
(2) Interference from carbonate ion can be easily eliminated by using an appropriate indicator for neutralization.
(3) Interference from oxidizing agents is reduced markedly owing to the reducing action of the formate buffer.
(4) Fluoride over the range of 190 μg to 3 mg can be titrated directly with 0.01N thorium nitrate solution with satisfactory accuracy and reproducibility.
(5)Composition of the buffer solution to be used must be altered depending on the amount of co-existing sodium nitrate or chloride.View full abstractDownload PDF (1793K) -
Wataru FUNASAKA, Tsuguo KOJIMA, Kazumi FUJIMURA, Sue KUSHIDA1963 Volume 12 Issue 12 Pages 1170-1174
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA salting-out chromatography using a weakacid cation exchange resin and an aqueous salt solution as adsorbent and developer has been applied to separations of naphthalene-1, 5- and -1, 6-disulfonic acids and also of naphthalene-2, 6- and 2, 7-disulfonic acids.
In order to obtain the most suitable column size and developer for the separation of these isomers, distribution coefficients (Kd) of the acids between Amberlite CG-50 of 100200 mesh and calcium-, magnesium- and zinc chloride solutions were measured. As the result, Kd was found to be varied by changing the nature of salt and also the concentration and the pH value of its solution. When the acids were eluted with 2M calcium chloride of pH 2.0 or 4.0, through the columns of 11 mmφ×214 mm and 10 mmφx230 mm packed with the same resins of 200400 mesh, the separations of isomers were complete.
The acids in eluants were determined spectrophotometrically with good results.
A stepwise elution analysis changing the con-centration of developer from 2M to 0.5M with the programming temperature column chromatography was tried to accelerate the development of the latter peak, and it was found quite powerful.View full abstractDownload PDF (867K) -
Katu TANAKA, Nobuyuki TAKAGI1963 Volume 12 Issue 12 Pages 1175-1178
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAbsorptiometric determination of minute amounts of titanium with N-benzoylphenylhydroxylamine (BPA), based on the extraction of the complex from higher concentrations of hydrochloric acid into chloroform has been investigated.
An absorption maximum of the extract lies at 371 mμ, while the absorption of the reagent blank is very little at the point. Determination of titanium is as follows. Put the sample solution of above 9.6N of hydrochloric acid containing up to 100 μg of titanium into a separating funnel, extract with 10 m/ of 0.1% BPA-chloroform for 12 minutes and measure the absorbancy at 371 mμ or preferably at 380 mμ by reason of the lower absorbancy of the reagent blank as a reference.
The color is stable. Calibration curve obeys Beer's law. The molar absorption coefficient of titanium is 6, 600. Errors coming from variabilities of hydrochloric acid concentration and the ratio Vaq./ Vorg. are negligible. A little vanadium, molybdenum and large amounts of iron do not interfere in their lower valent state. Only niobium gives a yellow color to the organic phase.
Good results were obtained by the proposed method for more than 0.001% of titanium in several metal samples.View full abstractDownload PDF (713K) -
Toshihide SAITO, Yoshio OZASA, Masako HAJI, Goro KONDO1963 Volume 12 Issue 12 Pages 1179-1183
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of sodium dodecylbenzene-sulfonate (DBS) has been investigated by use of triphenylmethane type dyes such as Methyl Violet, Malachite Green and Brilliant Green.
DBS reacted with these reagents in glycine buffer solution and its benzene extract gave green coloration.
The effects of pH, concentrations of glycine buffer solution and the reagents, and temperature on the extraction and stability of the color as well as the effects of various solvents and coexisting salts have been investigated.
The result indicated that the absorption and concentration of DBS followed the Beer's law at the maximum absorption of 600 mμ in Methyl Violet, at 635 mμ in Malachite Green and at 645 mμ in Brilliant Green at the concentration of 30 μg/15 ml benzene.
The spectrophotometric determination of a trace amount of DBS by use of Brilliant Green was rapid and sensitive.View full abstractDownload PDF (808K) -
Nobuhiko IRITANI, Taketsune MIYAHARA1963 Volume 12 Issue 12 Pages 1183-1188
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA colorimetric determination of mercury (II) in aqueous solution using Hg (II) complex with Methylthymolblue (MTB) was presented. The characteristics of the complex at pH 6.0 were as follows : the constitution Hg : MTB=1 : 1, the apparent formation constant log K = 5.5, the maximum absorption wavelength λmax=630 mμ, and the molar absorption coefficient at 630 mμ, ε=1.01×104.
The proposed method for the determination was as follows : the sample solution containing 0.0250.750 mg Hg(II) is mixed with 5.0 ml of 10-4M MTB solution and 1 ml of hexamine-HNO3 buffer solution (pH 6.0), made up to 25 ml with water, and the absorbance of the mixed solution at 630 mμ is measured within 1030 minutes against the reagent blank in a 1 cm cell. The method was simple and accurate. Cu(II), Zn (II), Pb (II), Fe (III), Cl and citrate interfered, and the suppretion of their interferences was discussed.View full abstractDownload PDF (1011K) -
[in Japanese], [in Japanese]1963 Volume 12 Issue 12 Pages 1189-1191
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
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[in Japanese]1963 Volume 12 Issue 12 Pages 1191-1192
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1963 Volume 12 Issue 12 Pages 1192-1193
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
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[in Japanese], [in Japanese]1963 Volume 12 Issue 12 Pages 1194-1196
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
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[in Japanese]1963 Volume 12 Issue 12 Pages 1196-1198
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
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[in Japanese], [in Japanese], [in Japanese]1963 Volume 12 Issue 12 Pages 1199-1200
Published: December 05, 1963
Released on J-STAGE: June 30, 2009
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[in Japanese], Louis Gordon1963 Volume 12 Issue 12 Pages 1201-1207
Published: December 05, 1963
Released on J-STAGE: February 16, 2010
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1963 Volume 12 Issue 12 Pages 1224a
Published: 1963
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1963 Volume 12 Issue 12 Pages 1224b
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1963 Volume 12 Issue 12 Pages 1224c
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1963 Volume 12 Issue 12 Pages 1224d
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1963 Volume 12 Issue 12 Pages 1224e
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1963 Volume 12 Issue 12 Pages 1224f
Published: 1963
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1963 Volume 12 Issue 12 Pages 1224g
Published: 1963
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1963 Volume 12 Issue 12 Pages 1224h
Published: 1963
Released on J-STAGE: February 16, 2010
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