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Volume 10, Issue 5
Displaying 1-26 of 26 articles from this issue
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Studies on the analytical methods of trace impurities in high purity substances. XIMasuo MIYAMOTO1961 Volume 10 Issue 5 Pages 433-438
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of Si in high purity copper has been achieved by the molybdenum-blue method. It is able to determine a minimum content of 0.5μg in about 3 hours.
Sample is decomposed by nitric acid and hydrofluoric acid, and ammonium molybdate is added to make Si to silico-molybdate after masking of F- by boric acid and adjusting of solution to pH1.2. The silico-molybdate is extracted with isoamylalcohol from the solution made 3N with H2SO4, and back-extracted, with weakly basic aqueous buffer solution, and then reduced to molybdenum-blue by ferrous sulfate and stannous chloride. The content of Si is determined from the spectrophotometrical measurement at 800mμ.View full abstractDownload PDF (954K) -
Studies on the analytical methods of trace impurities in high purity substances. XIIMasuo MIYAMOTO1961 Volume 10 Issue 5 Pages 438-443
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn analytical method of Sn in high purity copper by A. C. polarography has been established, which is able to determine as little as 0.1ppm.
To the solution of sample dissolved in HNO3, manganese sulfate and potassium permanganate are added, and Sn is coprecipitated with manganese dioxide by boiling the solution. The precipitate is fused with ferrous sulfate by sodium peroxide and leached by water. On the leach liquor, as it is free from interfering ions, Sn is determined by A. C. polarography, after the addition of hydrochloric acid and gelatin.View full abstractDownload PDF (1055K) -
Takashi ASHIZAWA1961 Volume 10 Issue 5 Pages 443-448
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe extraction of mercury as its dithizone complex into carbontetrachloride has been investigated for a wide range of reagent concentrations and from various acid solutions. By utilizing the alumina column chromatographic method in which chloroform is used as eluant to separate mercury dithizonate from the other dithizonates and an excess of dithizone, it was possible to get essentially complete separations of microgram quantities of mercury from 1g of copper. In that procedure the mercury dithizonate was not retained on alumina column while the elements extracted from acid solution were strongly adsorbed on alumina column. Optimum conditions for separation of 0.110μg mercury were as follows : column, 0.7×5cm; alumina, 100/325 mesh and 10% moisture content; eluant, chloroform, effluent less than 2ml. The absorbance was measured at 490mμ against a water blank. For 1μg and 5μg mercury, the coefficients of variation were 9.2% and 5.1% at 5% risk, respectively. The method is extremely rapid (about 10 minutes) and adaptable to small scale procedures.View full abstractDownload PDF (876K) -
Takashi ASHIZAWA1961 Volume 10 Issue 5 Pages 449-453
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe work reported is an outgrowth of a study in extending the applicability of the chromatographic adsorption analysis of metal chelates to trace analysis. Palladium dithizonate has been separated on an activated alumina column. After chromatographic separation from interfering elements, palladium dithizonate of green color was determined photometrically at 640 mμ. With about 10 μg palladium, a complete extraction with dithizone was carried out in wide range of dithizone concentrations and from 1 to 6N hydrochloric or sulfuric acid. Palladium separations effected with 0.7 × 5cm columns of alumina, 100/325 mesh, 10 % moisture content, and using chloroform as an eluant. The effluent was diluted to 2 ml when palladium was less than 1μg. In the proposed method, copper, bismuth, mercury and platinum had no interferences. About 0.01% of palladium could be rapidly determined from 1 mg of platinum metal sample in 30 minutes. Palladium contents found by the proposed method were 0.014% and 0.0094% in platinum wire and plate, respectively. For 0.2μg of palladium, the coefficient of variation was 15%.View full abstractDownload PDF (732K) -
Keiichiro HOZUMI, Kingo MIZUNO1961 Volume 10 Issue 5 Pages 453-456
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGravimetric methods have been currently applied to the determination of organic phosphorus, but they require several hours of standing for complete precipitation of ammonium phosphomolybdate and further complications are needed for separating the precipitate and desiccating it until it shows constant weight.
Although chelatometric titration of magnesium in magnesium ammonium phosphate precipitated. by magnesia mixture was recommended by several workers, a further simplification has been achieved by the authors with the following procedure : 35mg of organic samples are put in a small glass test tube before the addition of 45drops of reaction mixture (H2SO4+HNO3+HClO4), and decomposed for 1520 minutes. The digested mixture is transfused completely with 20ml water into a 50ml beaker, and neutralized with ammonia. Add 5.00 or 10.00ml of 0.005M MgSO4, condense the solution to 510ml, adjust to pH10 with 2ml ammonia buffer solution and stand for 30 minutes. After the same volume of methanol is added to avoid the hydrolysis of precipitate, the residual magnesium ion in liquid phase is quickly titrated with 0.005M EDTA, using a drop of Eriochrome black T as an indicator.View full abstractDownload PDF (678K) -
Studies on flame photometry by organic solvents extraction method. IVHidehiro GOTÔ, Emiko SUDÔ1961 Volume 10 Issue 5 Pages 456-462
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMicro-determination of metals by flame photometric method was studied in which metals were changed into their oxine complex and the extracted complex with organic solvent was excited in the oxygen-hydrogen flame and measurements of the intensities of titanium, gallium and indium were made by using respectively the band head at 518mμ, the line at 417.2mμ and the line at 451.1mμ.
The for conditions determination were examined in each case using the following solvents, methyl isobutyl ketone, amyl acetate, ethyl acetate and chloroform, and it was confirmed that the sensitivity could be increased 515 time than in the case of aqueous solution by selecting optimum gaseous pressure for each solvent.View full abstractDownload PDF (935K) -
Studies on flame photometry by organic solvents extraction method. VHidehiro GOTÔ, Emiko SUDÔ1961 Volume 10 Issue 5 Pages 463-467
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe oxine complex of nickel and cobalt was extracted with organic solvent, such as methyl isobutyl ketone, amyl acetate, ethyl acetate or chloroform, the extract was excited in the oxygen hydrogen flame, and the line intensities of nickel and cobalt were measured at 352.4mμ and 352.7mμ, respectively.
The intensities of flame under various conditions have been investigated for each solvent, and the sensitivity for nickel and cobalt was found to be 1030 times higher than that achieved by the flame photometry with aqueous solution.View full abstractDownload PDF (577K) -
Chemical analysis of chromium. VTadashi YANAGIHARA, Nobuhisa MATANO, Akira KAWASE, Haruno OGAWA1961 Volume 10 Issue 5 Pages 467-472
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe determination of phosphorus in high-purity chromium has been investigated and a procedure was recommended as follows.
The chromium metal was dissolved in aqua regia and perchloric acid and converted to chromic acid. It was diluted with water, and, after the addition of aluminum salt as a carrier, made ammoniac to precipitate phsophorus. 50 mg aluminum was sufficient (Fig. 4) and did not interfere with the color reaction (Table I). The phosphorus collected was determined colorimetrically with molybdenum blue method. The interference of chromium, tungsten, molybdenum, etc., has been criticizeá. The interfering elements such as silicon, arsenic, germanium, etc., was removed by adding dropwise hydrochloric acid and hydrobromic acid while heating the solution with perchloric acid. A large amount of iron interfered ( Table II) even after the reduction with sulfite. An analysis of electrolytic high-purity chromium from chromic acid or an analysis of com. electrolytic chromium of 99.99% purity from chromium-alum found 2.2 and 10.1ppm of phosphorus, respectively. The result of recovery tests was practically satisfiable.View full abstractDownload PDF (921K) -
Satoshi KAWAI, Sakae TAKEUCHI1961 Volume 10 Issue 5 Pages 473-478
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGas chromatographic method was applied for analyses of JP saponated cresol solutions and creosotes, and the following results were obtained.
For the tests on JP saponated cresol solutions:
a) They contained m- and p-cresols as main components and ο-cresol, phenol, 1, 2, 6-xylenol and 1, 2, 4- xylenol as impurities. b) Fractional distillation specified in the JP method of determination of m-cresol, therefore, was thought to have little effect practically.
For the tests on JP creosotes : a) They contained usually 3648% guaiacol and 1628% creosol as the main constituents and 1929% cresol, 715% phenol, 14% xylenol. b) The items 3 and 4 in the "purity test" in JP for bidding the presence of cresol and phenol should be practically revised. Gas chromatographic method for analyses of saponated cresol solutions and creosotes was found to be useful.View full abstractDownload PDF (925K) -
Iwaji IWASAKI, Akira KISHIOKA, Yukito YOSHIDA1961 Volume 10 Issue 5 Pages 479-482
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt was found that this method has some defects in its reproducibility, and that they are caused chiefly by the influence of varying temperature and the color fading by light. To avoid these defects the solution was heated for a definite time in boiling water and was protected from the strong light after the reaction has been completed. Such a procedure brought us far better results.
It was found that by using the mixed solution (1:1) of HCl (12N) and H2O2 (0.3%), elementary selenium could be changed very easily into selenious acid in a short time with high reproducibility. This method was very convenient and the experimental errors were within ±4.2% in the range of 6.0γ60.0γ of elementary selenium.View full abstractDownload PDF (739K) -
Studies on the separation of anions with anion exchange resin. IKiyoshi TAKIURA, Yoshio TAKINO1961 Volume 10 Issue 5 Pages 483-488
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe progress of ion exchange reaction of a OH-type resin (Dowex 2) gives a continuous increase in the concentration of OH ion and a proportional increase in conductivity of the solution, and constant OH ion concentration and conductivity are reached on the equilibrium point of exchange reaction. Accordingly, an estimation of the rate of increase in conductivity should give an exchange velocity. According to the experiment of the authors, the ion exchange reaction took place as soon as the resin was immersed and an equilibrium was reached within 5 minutes. The concentration of OH ion could be sought by a simple calculation from the value of conductivity at the equilibrium stages; further-more, calculation of selective coefficient (anion exchange equilibrium constant), KAnionOH (25°C), was made. The results were :
BO2-<F-<AsO2-<IO3-<BrO3-<Cl-<(OH)-<CN-<NO2-<NO3-<ClO3-<Br-<I-<NCS-.
The procedure of this method is more simple than the conventional titrimetric methods, the range of application is wide and there is a merit of being able to confirm the point just reaching the equilibrium.View full abstractDownload PDF (924K) -
Studies on the separation of anions with anion exchange resin. IIKiyoshi TAKIURA, Yoshio TAKINO1961 Volume 10 Issue 5 Pages 488-493
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSBy application of differences in selective coefficient at 25±1°C of monovalent common anions against the OH-type basic resin (Dowex 2), those were separated into four groups consisting of group I of BO2-, F-, IO3- and AsO2-, group II of BrO3-, Cl-, CN-, and NO2-, group III of NO3-, ClO3-, and Br-, and group IV of I- and NCS-. In order to confirm the correctness of this system of separation, the group-separation by column operation has been attempted and it was found that the ions in group I, II, III, and IV were liberated in the order named by use of 0.1, 0.51.0, and 25N NaOH and 2.55M NaNO3. Individual anions in group I (0.1 meq. BO2-, 0.1meq. F-, 0.025 meq. IO3-, and 0.025 meq. AsO2-) were liberated in the order named and separated completely by use of 10ml of the resin and 200ml 0.1N NaOH at the flow rate of 0.5ml/min.View full abstractDownload PDF (874K) -
Studies on the separation of anions with anion exchange resin. IIIKiyoshi TAKIURA, Yoshio TAKINO1961 Volume 10 Issue 5 Pages 493-497
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn continuance of the preceeding report, mutual separation of anions within a group has been investigated for group II (BrO3-, Cl-, CN-, and NO2- ), group III (NO3-, ClO3-, and Br- ), and group IV (I- and NCS-). By using 0.1meq. of each ion for 10 cc (11.7 meq.) of OH-type resin, separations of BrO3- and NO2-, and of Cl- and NO2- in group II were possible by using 1N NaOH as an eluant, while the separations of Cl-and CN-, Cl- and BrO3-, CN- and BrO3-, and CN- and NO2- were incomplete or impossible. Separation of ClO3- and Br- in group III was succesfully done by use of 5N NaOH, while the separation of NO3- and Br- failed, and the complete separation of I- and NCS- in group IV was made quite easily by use of 2.5M NaNO3.
From the results of the fundamental experiments in the preceeding and this reports, an attempt was made on ion exchange chromatography of 11 kinds of monovalent ions throughout the groups in which a complete systematic separation was obtained for 10 anions, namely, BO2-, F-, AsO2-, IO3-, BrO3-, NO2-, Br-, ClO3-, I-, and NCS-.View full abstractDownload PDF (780K) -
Akira MURATA, Takashi UJIHARA1961 Volume 10 Issue 5 Pages 497-501
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSKojic acid (5-hydroxy-2-hydroxymethyl-1, 4-pyrone)reacts with microgram quantities of Au(III) in a neutral or slightly acidic solution to give an intense blue-green fluorescence in ultra-violet radiation. The fluorescence intensity is strong and unchanged in the range of pH5.7 to 6.8, and increases by the addition of 0.5 to 2.5g of NaCl. About 30 minutes are required for the full development of fluorescence. It fades by an exposure to light, especially to ultra-violet radiation, although it is stable in the dark for at least 24 hours.
The recommended procedure is as follows : To a sample solution containing 2 to 50μg of Au, add 5ml of 20% NaCl, 2.5ml of the buffer solution (mixture of phosphoric acid and potassium hydroxide, pH 6.7, concentration of PO43-1mol/l), and 5ml of 2% kojic acid solution. Dilute to 50ml with water, stand for about 30 minutes in a dark box, and measure the total fluorescence intensity (>470mp) against 0.4μg/ ml sodium fluorescein solution. The influence of some cations has been examined. Te(IV) up to 2mg does not interfere, and it can be used as a coprecipitant for the isolation of Au from the other interfering cations.View full abstractDownload PDF (836K) -
Masao KAWAHATA, Heiichi MOCHIZUKI, Takeshi MISAKI1961 Volume 10 Issue 5 Pages 502-508
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of a micro amount of titanium coprecipitated with niobium has been investigated, in which titanium is dissolved in sulfuric acid and developed a coloration. with hydroquinone.
The light absorbancy of sulfuric acid solution of hydroquinone complexes of niobium, tungsten, and titanium was changed with the concentration of sulfuric acid and this was measured at different wavelengths. The solution made up to 100ml with hydroquinone-sulfuric acid solution hardly showed the sign of complex formation and the light absorbancy at wavelength longer than 400mμ was very slight for niobium and tungsten, when 30ml and 35ml (or more) of water had been added previously to their solution, respectively.
On the other hand, the light absorbancy of titanium complex at 480mμ gave practically no. change even with addition of 040ml water, but it was affected at the other wavelengths.
Above condition for determination of titanium in niobium thus established had no influence by the presence of 3mg niobium and 1.5mg tungsten, above which they showed disturbing influence.
The lower limit of determination of titanium by this method was 0.01mg/100ml.View full abstractDownload PDF (909K) -
Seiichiro HIKIME, Hitoshi YOSHIDA, Masahiro YAMAMOTO1961 Volume 10 Issue 5 Pages 508-513
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDiscoloration of yellowish brown color of copper complex with bis(2-hydroxyethyl)-dithiocarbamate occurred by adding mercury(II) to the solution. It was found that the discoloraion was applicable to the determination of mercury, and the conditions for the determination were investigated. Add copper solution and EDTA solution to the sample solution, adjust the pH to 4.5, and add the alcoholic copper bis-(2-hydroxyethyl)dithiocarbamate. Absorbance of the solution was measured at 432mμ (or using a filter 440mμ), the amount mercury was determined from the decrease of the absorbance. The calibration curves at these wavelengths showed good linearities, and the sensitivities of the recommended procedures were 0.016γHg/cm2, and 0.019γHg/cm2 respectively. By the method presented, 10200γ/20ml of mercury was determined rapidly in the coexistence of Br-, Cl-, C2O42-, PO43-, SCN-, and many metallic ions, while Fe3+, Cu2+, I-, and CN- interfered. It was suggested, moreover, that there were two kinds of the copper complex with bis (2-hydroxyethyl) dithiocarbamate each having an absorption maximum at 432mμ or 383mp, and the former changed to the latter by adding cupric ion or mercuric ion to the solution, while the change from the former to the latter was impeded by the addition of EDTA.View full abstractDownload PDF (908K) -
Syotaro OKA1961 Volume 10 Issue 5 Pages 513-518
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn automatic titrator has been developed for continuous measuring and controlling of the manufacturing processes in chemical industry.
This titrimetric analyzer performs a batchtype-analysis which eliminates some of the inaccuracies and sample flow-control problems usually associated with the continuous sampling. The sequence of operation is controlled by a multiple switch programmer and a number of valves and relays. The instrument introduces precisely a definite volume of solution to be analyzed into a titration cell by means of a automatic pipette. The titration cell has an indicator electrode for detection of equilibrium point, the solution in the cell is agitated by a magnetic stirrer. The addition of the titrant is automatically stopped when the potential of the indicator electrode has reached its equilibrium value. The titrant is added at a controlled flow rate while a valve in the titrantflow-line is opened. The titration device, of course, has an anticipator. The consumed volume of the titrant is then transposed to an electrical signal and measured by a pen-and-ink recorder. These operations are automatically repeated every 7.0 minutes.
Good selectivity and reproducibility over the wide field of electro-chemical analysis are important feature. The details of instrumentation and the results of basic experiment are described here.View full abstractDownload PDF (876K) -
Dichloroacetate (DADA) by the method of nitrosation. IIMasao MARUYAMA, Kazue HASEGAWA1961 Volume 10 Issue 5 Pages 518-522
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFundamental conditions for the spectrophotometric determination of di-iso-propylamine dichloroacetate by the method of nitrosation have been investigated. Glacial acetic acid and sodium nitrite solution are added to the sample solution at 4060°C, and di-iso-propylamine is nitrosated to N-nitroso-di-iso-propylamine. After cooling, the reacted solution is made strongly alkaline with an excess of potassium hydroxide solution and extracted with cyclohexane. By measuring the absorbancy at 235mμ of the extracted solution, DADA can be determined. Beer's law is obeyed in the range of 5200γ of DADA with high reproducibility.View full abstractDownload PDF (709K) -
[in Japanese]1961 Volume 10 Issue 5 Pages 523-524
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
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[in Japanese], [in Japanese]1961 Volume 10 Issue 5 Pages 524-526
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese]1961 Volume 10 Issue 5 Pages 526-528
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1961 Volume 10 Issue 5 Pages 528-529
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese]1961 Volume 10 Issue 5 Pages 529-531
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1961 Volume 10 Issue 5 Pages 532
Published: May 05, 1961
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1961 Volume 10 Issue 5 Pages 532a-533
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
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[in Japanese]1961 Volume 10 Issue 5 Pages 534-541
Published: May 05, 1961
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (1605K)
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