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Volume 17, Issue 3
Displaying 1-21 of 21 articles from this issue
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Kazuo YASUDA1968 Volume 17 Issue 3 Pages 289-300
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe linearity of working curves for silver, copper, strontium and calcium were studied with the Fabry-Perot interferometer together with theoretical calculation in the atomic absorption spectrophotometry. The theoretical calculation was based on the facts that the atomic vapor temperature of the hollow cathode lamp is within the range of 1200°K to 1300°K and the self-absorption of the resonance emission line from the lamp is between 0% and 22%. By assuming that the profile of the emission line is symmetrical and the central wavelength of the line is not shifted, the following results were deduced from the observations that a broadening of the resonance absorption line of the flame is 1.62 times that of the resonance emission line from the lamp, the profile of the absorption line is asymmetrical, and also that the central wavelength is shifted.
The working curve for silver shows a good linearity, which is due to the small ratios of both half-width and broadening of the emission line from the lamp to those of the absorption line of the flame. With these ratios much greater, the working curve for calcium has an inferior linearity. The working curve for strontium has a very small linear range and bends gradually, which is attributed to a great shift of the central wavelength of the absorption line. The working curves for copper and calcium give a cliff in their high absorbance region, accounted for their large ratio of the half-width of the emission line to the absorption line, and small shift of the central wavelength of the absorption line.View full abstractDownload PDF (1499K) -
Kimitaka SATO, Naoharu YAMAGUCHI, Ohiko KAMMORI1968 Volume 17 Issue 3 Pages 301-306
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSWhen the analysis of surface-treated steel was done by means of infrared absorption, it was quite often that the spectra could not be obtained even in the attenuated total reflectance (ATR) method. It was found that this fail of measurement depended on the thickness of the surface layer, and the lower limit of its thickness was examined on practical specimens. The following equation showing the relationship between the thickness d and wavelength λ was derived from interference spectra:
d=λ1λ2/4 (λ1-λ2) ·1/√n22-n12sin2θ1
in which n1 and n2 are refractive indice for different media, and θ1 is incident angle.
The result indicated that the thickness less than 20μ was inapplicable for a measurement in ATR method. The thickness of surface layer available for measurements by ATR method was estimated to be greater than 2025μ, taking simultaneously into consideration the depth of a layer into which light oozes out from boundary face.View full abstractDownload PDF (825K) -
Toyozo UNO, Masayasu YAMAMOTO1968 Volume 17 Issue 3 Pages 306-310
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMethods for the detection of amines and the colorimetric determination of aromatic secondary amines are described.
The color reaction of amines with quinonedichlorodiimide (QDCI) can be used for their qualitative test. Namely, when the sample amine and QDCI in ethanol are heated for 20 minutes at 80°C, aliphatic amines give a yellow color for primary and secondary amines but no color for tertiary amines. Aromatic primary amines give a reddish brown color, while the secondary amines form characteristic green color. This color reaction is applied to the quantitative determination of small amounts (110 μg/5 ml or 20 μg/5ml) of aromatic secondary amines. Ethanol solutions of the sample amine and QDCI are added to the potassium biphthalate buffer solution. After heating the mixture for 15 minutes in boiling water and allowing to stand for 25 minutes at room temperature, the absorbance is measured at 689 mμ.
This method for aromatic secondary amines is not interfered from other amines except some aniline derivertives such as m-toluidine which have no substituent in para position and have an electron-donor group either in ortho or meta position to the amino group.View full abstractDownload PDF (753K) -
Analytical studies on fatty acids. ISadayoshi KOSUGE, Masaji FURUTA, Okitatsu YAMAGUCHI1968 Volume 17 Issue 3 Pages 310-314
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSp-Hydroxyphenacyl esters of fatty acids were prepared as derivatives for separation and identification of fatty acids. p-Hydroxyphenacyl bromide used for their preparation was synthesized according to King-Ostrum's method, which involves selective bromination of ketones with copper (II) bromide.
The p-hydroxyphenacyl esters of C2C20 saturated fatty acids and aromatic acids were obtained as colorless needles using p-hydroxyphenacyl bromide. It was found that the p-hydroxyphenacyl bromide serves as a useful reagent for the identification of saturated fatty acids and some aromatic acids. Properties of p-hydroxyphenacyl esters have also been investigated.View full abstractDownload PDF (786K) -
Tohru WAINAI, Yohichi SUZUKI1968 Volume 17 Issue 3 Pages 315-319
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTo obtain a convenient method for determining ο-, m-and p-cresols in their mixture, the NMR technique was investigated. The mixtures of cresol isomers in methanol and water were found to give NMR spectra including three methyl peaks sufficiently resolved for the determination of each component. The best resolution of these peaks was obtained in the mixture of 11 mole% cresols, 22 mole% methanol and 67 mole % water, and they were in the order of p-, m-and ο-cresols from intense field. The hights of three peaks were proportional to the amounts of respective cresols, and the standard deviation was smaller than 2.4%. The method was applied satisfactorily to the determination of ο-, m-, and p-cresols in metacresylic acid.View full abstractDownload PDF (647K) -
Katsuaki FUKUDA, Atsushi MIZUIKE1968 Volume 17 Issue 3 Pages 319-322
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new rapid method has been proposed for the concentration of microgram or submicrogram quantities of silver in acid solutions.
A solution of p-dimethylaminobenzilidenerhodanine in ethanolic nitric acid is added to a smaple solution to give a small quantity of precipitate. The precipitate involving silver is then floated to the surface, by bubbling air into the solution through a disc of sintered glass after an addition of sodium n-dodecylbenzenesulfonate solutions. As little as 0.021 μg of silver is concentrated, with yields greater than 95%, from 100500 ml of 0.11 M nitric acid solution within 5 min. In case of 1 μg of silver and 0.5 g of copper in a solution, the concentration factor of silver with respect to copper is approximately 103. The method offers the following merits compared with the usual p-dimethylaminobenzilidenerhodanine coprecipitation method : rapidity, applicability to higher acidity, and a smaller quantity of the reagent required. It is successfully applied to the photometric determination of a few ppm of silver in high purity copper.View full abstractDownload PDF (694K) -
Yoshio SHIJO, Tsugio TAKEUCHI1968 Volume 17 Issue 3 Pages 323-327
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSEriochromecyanine R reacts with Al in the presence of cetyltrimethylammonium chloride to form a blue ternary chelate. Its absorption maximum is at 587mμ, the absorbance being constant at pH 5.36.3 The sensitivity was very high, the molar extinction coefficient being 1.17×105. The absorbance obeys Beer's law over 0.010.08μg Al/ml. V, Zr, Cu, Fe, Cr, Ga, Bi, Ta, Ti, Pt, Ge, Be, Th, and U interfere remarkably.
The recommended procedure for obtaining the calibration curve is as follows. About 25ml of the neutral solution containing 0.54μg Al is transfered to a 100ml beaker. To this solution are added 2ml of 0.5M acetic acid and 1ml of 0.5% cetyltrimethylammonium chloride solution. Further, 10ml of 0.02% Eriochromecyanine R solution and 5ml of 4M ammonium acetate solution are added quietly. After five minutes, the mixture is transfered in to a 50ml volumetric flask and is diluted to 50ml with water. The absorbance of the solution is measured at 587mμ against a reagent blank.View full abstractDownload PDF (643K) -
Atsuko ITO, Keihei UENO1968 Volume 17 Issue 3 Pages 327-332
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSChelometric titration of various metal ions with TTHA (Triethylenetetraminehexaacetic acid) can be performed in quite similar way as that with EDTA. The color changes of indicators are, however, sluggish in general, and some of them give end points hardly distinguishable.
As suggested by Pribil, the mixture of metal ions which react with TTHA in the ratio of 1 : 1 and 2 : 1 (metal : ligand), respectively, may be titrated selectively. In the mixture of calcium and magnesium taken as the first case, however, it was unsuccessful to find an optimum condition which was common for both ions. Among the other combinations of metal ions such as the mixtures of calcium with nickel, zinc and cadmium, the mixtures of cerium with lead, zinc and mercury, and the mixtures of lanthanum with lead, zinc and cobalt, a satisfiable result was obtained only in the mixture of lanthanum and mercury.
In order to evaluate the TTHA titration, the theoretical titration curves of calcium and magnesium were derived by calculations using the equilibrium data of 1 : 1, 2 : 1 and 3 : 1 complexes, as well as monohydrogen and di-hydrogen complexes. Somewhat sluggish color change of the indicator near the end point is explained by the increase of pM at the earlier stage of titration.View full abstractDownload PDF (869K) -
Amperometric argentometry of a mixture of iodide and iodate utilizing the difference in solubilitiesSôichirô MUSHA, Sanae IKEDA, Girô NISHIDA1968 Volume 17 Issue 3 Pages 332-338
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSShort-circuit amperometric titrations of a mixture of iodide and iodate with silver nitrate solutions using a rotating platinum wire electrode (1000 rpm) have been investigated at zero applied potential with an S. C. E. or a merucry-mercuric iodide electrode.
Two methods were proposed of which one (I) is based on the difference in solubilities of silver iodide and silver iodate in an aqueous solution, and the other (II) is based on the difference in their solubilities in a dilute ammoniacal solution.
(I). Suspended silver iodide does not cathodically depolarize the rotating platinum electrode due to its low solubility, while silver iodate readily gives rise to a cathodic current because of its much greater solubility in an aqueous solution at the potential of S. C. E. Iodide in a neutral supporting electrolyte such as potassium nitrate, ammonium acetate or sodium acetate can therefore be titrated with silver nitrate at room temperature (ca. 20°C) in the presence of iodate. Iodate can then be titrated in the presence of 0.02% gelatin after cooling the solution below 5°C, or by adding organic solvent such as ethanol (3040 vol.%) at room temperature to decrease the solubiltity of silver iodate. The possible determining ranges of concentration were 0.0010.01F for iodide and 0.0020.01F for iodate. The relative errors were about ±2%.
(II). Silver iodate dissolves in a dilute (0.1 F) ammonia water, while silver iodide essentially does not. Iodide in the presence of iodate can therefore be titrated in a dilute ammoniacal solution by amperometry with a rotating platinum electrode and silver nitrate solution at the potential of mercuric iodide electrode, using the indicator current of silver ammonium complex. The total amount of iodide and iodate is determined by titration in a neutral supporting electrolyte below 5°C, in the presence of 0.02% gelatin and 3040 vol.% ethanol at the potential of S.C.E. The determining range of concentration of iodide in the presence of iodate was 0.00010.01 F. The relative errors for 0.0010.01 F iodide were about ±0.5%. The total amount of iodide and iodate in the concentration range of 0.0020.02 F was determined with the error of about ±1%.View full abstractDownload PDF (1220K) -
Emiko SUDO, Haruno OKOCHI1968 Volume 17 Issue 3 Pages 338-344
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of microamounts of manganese has been investigated by means of square wave polarography, and an established procedure is given as follows.
A half gram of sample is dissolved in perchloric acid. Triethanolamine and sodium hydroxide are then added until their final concentrations in the electrolysis solution reach 0.58 M and 2.0 M, respectively, in the case of iron and steel samples, and 0.62 M, and 1.8 M, respectively, in the case of aluminum sample. After the aeration under the room temperature for about 25 min., the square wave polarograms from-0.1 to-0.5 V vs. Hg pool are recorded. As large as 500 μg of copper and cobalt do not interfere.
The lower limits of the determinatins are 0.001% manganese in iron and steel, and 0.002% manganese in aluminum.View full abstractDownload PDF (908K) -
Hiroshi ONISHI, Hitoshi NAGAI1968 Volume 17 Issue 3 Pages 345-348
Published: March 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA spectrophotometric method is described for the determination of less than 40μg of boron. To a sample solution are added 4ml of 1N sulfuric acid and 1.5ml of 0.5% hydrofluoric acid, and the solution is diluted to 20ml with water. After allowing the solution to stand overnight, 0.5ml of 0.1% Rhodamine B solution is added, and Rhodamine B tetrafluoroborate is extracted with 10.0ml of n-butyl acetate. The organic phase is separated and centrifuged, and its absorbance is measured in a 1cm cell at 555mμ.
The sensitivity of the method is 0.009μg B/cm2 for an absorbance of 0.001, and an apparent molar abscrptivity is 1.2×103 at 555mμ. Among foreign ions examined, perchlorate and thiocyanate interfered seriously, and 1mg of thorium or zirconium caused low results.View full abstractDownload PDF (381K) -
Toshikazu EZAWA, Motoshi KITAMURA1968 Volume 17 Issue 3 Pages 349-353
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn carrying out the determination of phosphate in serum phospholipids by molydbenum blue spectrophotometry, the authors happened to meet an “impure” sodium molybdate of G. R. grade, which involved about 0.05% of tungsten {W (VI)}. Using this impure reagent, the color development of molybdenum blue was remarkably retarded with a shift of maximum absorption wavelengths. The magnitude of this influence varied with standard phosphate solution and with the lipid extract from serum samples, hence it resulted in maximum 30% negative errors.
The presence of tungsten in sodium molybdate and its unfavorable influence was acertained by emission spectroscopy and addition test of tungsten as WO42+, respectively.View full abstractDownload PDF (768K) -
Atsushi MIZUIKE, Shigeki KANO1968 Volume 17 Issue 3 Pages 354-355
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA technique with a simple apparatus has been applied to the concentration of dilute aqueous solutions based on the principle of normal freezing. A sample solution containing 0.03 to 5.0 μg of gold and 10-3 to 10-4N hydrochloric acid (or 2.0 μg of mercury and 10-3 to 10-4 N nitric acid) in 50 to 400 ml is frozen in a round bottom glass container by the use of a sodium chloride-ice or sodium nitrate-ice freezing mixture. The recoveries of gold and mercury were checked by tracer experiments using gold-198 and mercury-203 and found about 95% out of a few μg of gold and mercury, when concentration factors are 35 to 50. Investigations were made under several experimental conditions, such as stirring, temperature, etc., for the rapid formation of transparent ice, required for the perfect recovery.View full abstractDownload PDF (299K) -
Satoru EMURA, Nobuaki KONO1968 Volume 17 Issue 3 Pages 355-357
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid and accurate method is described for the determination of free alkali and aluminum in the sodium hydroxide solutions containing aluminate by alkalimetry.
In the proposed method, free alkali is titrated by standard acid solution after triethanolamine is added to mask aluminum ion. After it arrives at the equivalence point for free alkali, potassium fluolide is added to the solution and then the liberated alkali equivalent to aluminum is titrated with the same standard acid solutions.
More than 0.4 meq. of free alkali and 0.22.0 mmol of aluminum can be determined rapidly.View full abstractDownload PDF (382K) -
Naosuke SHIRAISHI, Seizi YOSHIKAWA, Tutomu MORISHIGE1968 Volume 17 Issue 3 Pages 358-360
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple method for the determination of manganese in Japanese acid clay with 4, 4'-tetramethyldiaminodiphenylmethane is described. The established method is as follows.
A half gram of crushed acid clay is put into a test tube of 10 ml capacity, and 5 ml of acetic acid-sodium acetate solution is added. It is shaken vigorously for one minute, and is filtered through a No. 5C filter paper. When a third volume is filtered, a drop is taken and spotted on the chromatographic paper. One drop of saturated potassium periodate is added, and after 2030 seconds to this are added two drops of 4, 4'-tetramethyldiaminodiphenylmethane in chloroform solution. After 2 minutes, the blue coloration is determined against the standard.
Although the resolution rate by acetic acid-sodium acetate solution is not high, the result is quite reproducible and only about five minutes is enough for the determination without any special equipment.View full abstractDownload PDF (517K) -
Naosuke SHIRAISHI, Tutomu MORISHIGE, Seizi YOSHIKAWA1968 Volume 17 Issue 3 Pages 360-363
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the determination of iron, titanium, aluminum and sulphate in soda lime glass by JIS, it takes several hours to follow the complicated procedures, therefore, a rapid determination method was studied.
Ratio of contents among iron, titanium and aluminum in ordinally soda lime glass is about 3 : 1 : 50. Therefore, iron and titanium are determined by the spectrophotometric method with 2-methyloxin. Aluminum is determined by the chelatometric titration after iron and titanium being removed with 2-methyloxin.
The determination of sulphate, being separated by cation exchange resins, is made by the chelatometric titration.
The results obtained by this method are found to be accurate and rapid.View full abstractDownload PDF (586K) -
Naobumi OI, Osamu NAKAZAWA, Eiji INABA1968 Volume 17 Issue 3 Pages 364-366
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIt was observed that Dimethoate {O, O-dimethyl-S- (N-methylcarbamoylmethyl) -pithiophosphate}, one of the organo-phosphoric insecticides, shows two absorptions at 3460 and 3430 cm-1, being assigned to NH stretching vibration of free molecule in dilute carbon tetrachloride solution. Changes of absorption intensity in various concentrations and of the absorption bands measured in a solvent mixture of both carbon tetrachloride and mesitylene were examined. In this connection, N-methylphenylmercaptoacetamide and N-methyl-β-phenylpropionamide, as related compounds, were also synthesized and their NH stretching vibrations in carbon tetrachloride were examined. The absorption3460 cm-1 is considered to be due completely to the free NH group, and that at 3430 cm-1 has been clarified to be caused by the stretching vibration fo the NH-group, intramolecular hydrogen bonding being formed such like N-H…S.View full abstractDownload PDF (355K) -
[in Japanese]1968 Volume 17 Issue 3 Pages 367-375
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese], [in Japanese], [in Japanese]1968 Volume 17 Issue 3 Pages 376-394
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese]1968 Volume 17 Issue 3 Pages 395-405
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
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[in Japanese]1968 Volume 17 Issue 3 Pages 406-413
Published: March 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1171K)
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