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Volume 16, Issue 6
Displaying 1-24 of 24 articles from this issue
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Microdetermination of N-methyl group. IKiyoshi NAKAMURA, Yuzo UTSUI, Tadao MAEDA1967 Volume 16 Issue 6 Pages 535-539
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThere needed some investigations on the microdetermination of N-methyl group, since several compounds do not give methyl iodide quantitatively under the usual conditions for decomposition of N-methyl compounds in hydroiodic acid.
The authors tried to find the best conditions for the quantitative formation of methyl iodide in two ways as follows, and established a method applicable to a routine analysis in microdetermination of N-methyl group, by adopting volumetric finish for methyl iodide.
(1) The catalytic effect of metals on the formation of methyl iodide was investigated, and aluminum was proved to be the best, giving quantitative results.
(2) The heat response of the reaction was investigated under the controlled temperature, by using an electric heating device with a heater inserted in a brass block.View full abstractDownload PDF (802K) -
Microdetermination of N-methyl group. IIKiyoshi NAKAMURA, Yuzo UTSUI, Tadao MAEDA1967 Volume 16 Issue 6 Pages 540-546
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe authors had given, in their previous paper, the optimum conditions for the decomposition of N-methyl compounds into methyl iodide in hydroiodic acid in the microdetermination of N-methyl group with volumetric finish.
In this paper, more sophisticated methods with gravimetric finishes using solid absorbents were investigated in place of the volumetric finish.
Measurement of the weight increase of the heated silver granules caused by the absorbed iodine, which had been given after the combustion of methyl iodide, was prefered to give satisfactory results in a routine analysis, while that of the molecular sieve 13-X resulted by the absorbed methyl iodide required a further investigation concerning significantly high(+) error with certain compounds.View full abstractDownload PDF (940K) -
Spectrophotometric determination of bismuth and thallium (III)Tsutomu MATSUO, Junichi SHIDA, Toshitsugu SASAKI1967 Volume 16 Issue 6 Pages 546-551
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSOptimum conditions for the determination of bismuth and thallium(III) by an extraction of the reaction product of zephiramine and iodo-complex of bismuth or thallium(III) into dichloroethane was investigated.
Determination of bismuth. The pH of the aqueous solution of 10 ml of M/100 zephiramine solution added with 5 ml of a freshly prepared 0.3 M potassium iodide solution was adjusted to 5. Succeeding extraction after 10 minutes was recommended for the determination of 1080 μg of bismuth. Maximum absorptions were found at 360 mμ and at 490 mμ, but the latter wavelength was preferable for the determination.
Determination of thallium(III). The same conditions as above except for the pH 6 of the aqueous layer were recommended for the determination of 1060 μg of thallium. The absorption maximum of dichloroethane solution was at 395 mμ, and the mole ratio of the complex was 1:1.
Copper interfered seriously with the determination of both elements.View full abstractDownload PDF (897K) -
Hiroshi MATSUO, Shokichi CHAKI1967 Volume 16 Issue 6 Pages 551-555
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSZephiramine reacts with complex molybdenum thiocyanate ion to form yellowish orange precipitate. The precipitate is extracted with chloroform. The extract is stable for at least 2 days and has two absorption maxima at 320 mμ and 460 mμ. The mole ratio of molybdenum to zephiramine in the extracted compound is 1 : 2. Beer's law holds for the chloroform extract when molybdenum-thiocyanate-zephiramine is extracted into 10.0 ml of chloroform from 25.0 ml of the sample solution containing 0.5×10-5 M5.0×10-5 M molybdenum. Many ions except bismuth, copper, iron, iodate, periodate, chromate, tungstate and permanganate do not interfere with the determination in their amounts equal to that of molybdenum.View full abstractDownload PDF (736K) -
Kenji YASUDA, Kyozo NAKASHIMA1967 Volume 16 Issue 6 Pages 556-560
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA rapid, sensitive and selective color reaction for detecting acylanilides on thin layer chromatography has be presented. The reaction involves nitrosation of acylanilides by gaseous mixture of nitrogen oxides and hydrogen chloride, and succeeding intramolecular rearrangement of the derived nitroso compounds, followed by coupling with α-naphthylamine to produce azo dyes. It reveald 0.05 μg formanilide and 0.01μg p-nitroformanilide.
An exposure to bromine gas as a preliminary treatment was found to be effective to increase the sensitivity for some anilides.
Mono- and di-substituted anilines gave yellow coloration by the nitrosation, but did not change their color even by the coupling. Aniline and acylanilides gave the same coloration, but the both compounds were distinguished by a tratment with a benzene solution of dimethylaminobenzaldehyde which gave yellow Schiff's base with the former but virtually no color with the latter. The Schiff's base was changed into the diazonium compound by the nitrosation process, and then it was also detected as the azo compounds.
Some attempts to select suitable solvent mixture for the TLC of acylanilides were also made. A solvent mixture of either benzene-pyridine (7:3) or cyclohexane-pyridine (7:3) was successful in separating various anilides and amines. Acylanilides involving electronegative substituents in their nucleus had a tendency to give lower Rf values in these solvent mixtures.View full abstractDownload PDF (803K) -
Kazuo YONEDA, Kunihiko KIGOSHI1967 Volume 16 Issue 6 Pages 561-565
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn experimental procedure is given for measurement of tritium by proportional beta counting on the ethane gas prepared from hydrogen and acetylene. The results of studies on the method of preparation of palladium catalyzer and memory effect are reported in detail. Residual counting rate after the preparation and the measurement of high level tritium (106 T. U.), i. e. memory effect, is usually within 1% of initial counting rate, but is reduced to less than 0.01% by the change of catalyzer and repeated flushing of counting gas in he counter. Using a counter of 1l volume with shielding by anticoincidence counter, the proportional counting of ethane gas gives good and stable counting characteristics with 1 cpm for 92 T. U. under the filling of 1 atm. C2H6.View full abstractDownload PDF (801K) -
Tetsuo TOYOGUCHI, Hiroshi SHIMIZU1967 Volume 16 Issue 6 Pages 565-569
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAlthough the fire assay method is widely accepted as the international umpire method for the determination of gold in ores, the author has presented a new method of its determination by the atomic absorption spectroscopy.
The ore sample was treated with aqua regia and filtered from silica. Gold in the filtrate was coprecipitated with tellurium and isolated from other ions. The precipitate containing gold was dissolved in aqua, regia and determined by the atomic absorption spectroscopy.
From a study of interferences, it was proposed that the coprecipitation of gold with tellurium was a very effective means for its isolation and concentration, and for the elimination of matrix elements. An addition of ethanol to the gold solution increased the sensitivity of the atomic absorption spectroscopy, and was applied to the determination of lean gold.
The standard deviation of the results by the proposed method was 0.20.6 g/t for ores with 230 g/t gold.View full abstractDownload PDF (706K) -
Akira KAWASE1967 Volume 16 Issue 6 Pages 569-576
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSVarious PAN analogues with pyridine-, nitropyridine-, or methylquinoline rings were synthesized. To study analytical properties of these compounds, their acid dissociation constants, extractability of metal chelates, and their stability constants and compositions were compared. These compounds, compared with PAN, showed greater shifts of wavelengths of maximum absorbance by chelation, and are recommendable as extractive-spectrophotometric reagents. Several of their chelates have very high molar extinction coefficients, especially those of 4'-methyl-α-QAN- and 5'-nitro-α-PAN chelates amounting to 8×104.View full abstractDownload PDF (1287K) -
Yoshizo HORIUCHI, Hiroshi NISHIDA1967 Volume 16 Issue 6 Pages 576-582
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNickel and cobalt were determined spectrophotometrically (567 mμ) with Chromazurol S (abbreviated to CAS below) at pH 9.7. Beer's law held for 0.06 to 1 ppm of nickel and 0.08 to 2.4 ppm of cobalt in 5.32×10-4M CAS. Apparent molar extinction coefficients of nickel and cobalt complexes were 3.93×104 and 1.96×104, respectively. Sulfate, phosphate, tartrate, oxalate, EDTA, hydrogen peroxide, ammonium, beryllium, aluminum, iron(III), chromium(III), gallium, tin(IV), and zirconium interfered.
Nickel and cobalt with CAS formed a 1:1 blue chelate in the range below 3.5×10-4M CAS and a 1:2 blue chelate in the range above 4×10-4M CAS. Both the complexes had an absorption maximum at 567 mμ.View full abstractDownload PDF (978K) -
Iwao TSUKAHARA1967 Volume 16 Issue 6 Pages 583-589
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe proposed method for determination of tantalum involves the extraction of the colored brilliant green fluorotantalate from a tartaric acid medium by benzene, and the measurement of absorbance of the extract.
Various influencing factors such as pH, concentrations of hydrofluoric acid and brilliant green, concentration of tartaric acid, phase ratio, diverse ions, etc. have been studied, and the optimum conditions for the estimation of tantalum have been determined.
The recomended procedure: (1) When the sample contains more than 0.1% tantalum, 0.1 g of sample is taken in a platinum dish and decomposed with 5 ml of hydrofluoric acid, followed by a few drops of nitric acid. The solution is heated with 1.0 ml of sulfuric acid and evaporated to fumes to expel hydrofluoric and nitric acids. The residue separated out is dissolved with 50 ml of 20% tartaric acid solution by heating on a hot water bath, and the pH is adjusted to 1.751.80 with ammonia. It is then made up to 100 ml with water. An aliquot less than 3.0 ml of this solution is taken into a 100 ml separatory funnel, and added with a definite volume of buffer solution (10% tartaric acid adjusted the pH to 1.751.80 with ammonia) required to make the final volume of the aqueous phase 30 ml. To this are added, successively, 5.0 ml of 0.1% brilliant green solution, 4.0 ml of hydrofluoric acid (1.0 N), and 10.0 ml of benzene.
The funnel is shaken vigorously for 2 minutes, and the two layers are allowed to separate by standing for 23 minutes. Immediately after the drainage of the aqueous layer, the absorbance of the benzene layer is measured at 640 mμ in a 1 cm cell against benzene.
(2) When the sample contains less than 0.1% tantalum, 0.51.0 g of sample is decomposed according to procedure (1). The solution is evaporated to fumes with 8.0 ml of sulfuric acid cooled and added with 4.0 ml of hydrofluoric acid (7.0 N). It is poured into a 100 ml-separatory funnel and the total volume is adjusted to 40 ml with water. After cooling, it is shaken vigorously with 20 ml of hexone for 2 minutes. The combined hexone extract from successive two extractions is evaporated with 20 ml of water, 2.5 ml of hydrofluoric acid and 1.0 ml of sulfuric acid to white fume of sulfuric acid, and then tantalum is determined by the procedure (1).View full abstractDownload PDF (928K) -
Ryoei ISHIDA, Takeo SAWAGUCHI1967 Volume 16 Issue 6 Pages 590-595
Published: June 05, 1967
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCupric ion reacts with Chromazurol S to form two sorts of colored complexes according to pH value of the medium. It was estimated that one had a 1 : 1 molar ratio of copper and Chromazurol S, with its absorption maximum at 600 mμ, in a nearly neutral medium; and the other had a 1 : 2 ratio, with its absorption maximum at about 550 mμ, in a slightly acidic medium.
The color of the former is more intense, and it was applied to the determination of copper.
The complex gives the maximum 600 mμ absorbance in the pH range from 6.5 to 6.9. The color development is almost instantaneous, and the absorbance remains constant for many hours at room temperature. The order of the addition of reagents has no effect upon the absorbance. Beer's law is followed within the range of copper concentrations from 0.7 to 2.5 μg/ml. The sensitivity of the color reaction as defined by Sandell is 0.003 μg/cm2 at 600 mμ. Polycarboxylate ions such as oxalate, tartrate, citrate, EDTA, etc. bleach the color of the complex, even by a very small amount. Cations such as Ce(III), Be(II), U(VI), Sc(III), Y(III), Sn(II), Fe(II, III) etc. interfere.View full abstractDownload PDF (864K) -
Hiroshi HASHITANI, Kazuo KATSUYAMA, Chiaki SAGAWA, Kenji MOTOJIMA1967 Volume 16 Issue 6 Pages 596-601
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of aluminum and manganese in a reactor material, Zircaloy-2 which contains 1.201.70% of tin, 0.070.20% of iron, 0.030.08% of nickel and 0.050.15% of chromium, has been established. The method can be used for determining down to 5 ppm of both aluminum and manganese in zirconium bearing materials.
Up to 2 g of the sample is dissolved with sulfuric acid and ammonium sulfate. Prior to the determination, zirconium is removed by extracting its cupferron chelate with chloroform. From 1 to 2 N sulfuric acid solution, not more than 400 mg of zirconium is extracted, while aluminum and manganese remain quantitatively in the aqueous solution. The extraction should be carried out twice to eliminate zirconium completely. Fifteen ml of 8% cupferron solution is used for each 100 mg of zirconium at the first extraction, and 3 ml of the same solution is used at the second extraction.
After removal of zirconium and decomposition of the residual cupferron, aluminum is determined by extracting its 8-hydroxyquinoline (oxine) complex from a solution (pH 5.0±0.2) containing cyanide, and by measuring the absorbance at 390 mμ. Chromium must have been removed by extracting from a solution of pH 5.0±0.2 as its 2-methyl oxine complex, before the aluminum determination.
Manganese is determined on another aliquot which has been treated with cupferron, by extracting its 2-methyl oxine complex and by measuring the absorbances at 395 and 580 mμ. Interferences from chromium, nickel and lead are eliminated by adding citrate, cyanide and EDTA as masking agents to the aqueous solution (pH 12±0.5).View full abstractDownload PDF (1136K) -
Koichi NISHIMURA, Teruo IMAI1967 Volume 16 Issue 6 Pages 602-605
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSCombination effects of diverse elements in the presence of lanthanum and barium were studied, and both lanthanum and barium were found to be suitable elements for supressing the interference from diverse elements. Procedures for atomic absorption spectrophotometric determination of magnesium in zinc base alloys and silicate minerals have been established and good results were obtained by using the proposed method. The determination limit was found to be 0.01 ppm, being the concentration corresponding to give 1% absorption.View full abstractDownload PDF (660K) -
Hitoshi YOSHIDA, Mitsuhiko TAGA, Seiichiro HIKIME1967 Volume 16 Issue 6 Pages 605-607
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSReactivity between several metallic ions and tetraethylthiurum disulfide, and extractability of the complexes with chloroform were studied.
An alcoholic solution of tetraethylthiurum disulfide was added to either hydrochloric acid solutions of various concentrations or ammonium citrate buffer solutions of various pH, containing metallic ions. After keeping the solutions at 40°C for 3 minutes, the complexes were extracted with chloroform, and the absorption spectra were measured. The distribution ratio of ions in organic and aqueous phases was also determined. The values for Te(IV), Fe, Ni, and Bi were 5.1×102, 1.6×10-3, 4.0×10-5, and 1.1×10-2, respectively, in 3 N hydrochloric acid solution. A separation factor of Te to the metallic ions was found to be greater than 104. Copper complex was extracted also with chloroform, and the value of the distribution ratio was smaller than 10.View full abstractDownload PDF (523K) -
Analyses of drugs and chemicals by infrared absorption spectroscopy. XVIIINaobumi OI, Keiichirc MIYAZAKI, Noboru SHIRAGA1967 Volume 16 Issue 6 Pages 607-610
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn examination was made on the general problems in the solvent extraction-infrared analysis of water soluble acids with amines and the findings obtained are:
(1) The amines used for the solvent extraction should not always be high molecular weight amine. It is extractable even with low molecular weight amine depending on the kinds of water soluble acids, and an excess of amines in organic layer is transfered to the water layer and therefore it will not interfere with the absorbance of the sample, accordingly it is considered to be convenient to the IR measurements.
(2) To this method, the compensation method is applicable, and so it is found to be effectively applicable to the qualitative and quantitative analysis of small amount of impurities.
(3) Without any influence on the ratio of water content in samples, it is found to be usuful for analysis in measuring their spectra.View full abstractDownload PDF (713K) -
Isamu TSUBAKI1967 Volume 16 Issue 6 Pages 610-612
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMany papers on the analysis with reagents and instruments were recently published, however, few among them are applicable to the SiO2 determination and therefore the gravimetric method is now widely employed as one of the methods with high accuracy. However, the demerit of this gravimetric analysis is to take pretty long time for evaporation, drying and dehydration. In this study, the H3BO3 fusion instead of the Na2CO3 fusion usually employed, was carried out, followed by immediate HF treatment, and therefore SiO2 was determined in a shorter time. The originality in this study is this: as it is an acidic fusion and hence neither evaporation, drying nor dehydration is necessarly H3BO3 has a strong decomposition activity, and by HF it evaporates with SiO2. However, the HF treatment method requires the component other than SiO2 to be in the same form, before and after the weighing, accordingly this method is inapplicable to the analysis, especially when such components as Na2O, K2O, CaO and MgO are mainly consisted. This method was applicable to silicate sand whose SiO2 is more than 90% in this study.View full abstractDownload PDF (629K) -
Niro MATSUURA, Yoshimi KURIMURA, Keiichi KIYOKAWA1967 Volume 16 Issue 6 Pages 612-613
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA conventional method of ion-exchange chromatography has been modified effectively for separating ortho- and pyro-phosphates, which were contained as impurities in recrystallized tripoly-phosphate, by gradient elution with 500 ml of 2×10-3 N HCl, to which 0.6 M KCl is added continuously and mixed. The separation can be brought about at an elution volume of 100ml for orthophosphate, of 200 ml for pyrophosphate and of 300 to 350 ml for tripolyphosphate. In the course of pretreatment with molybdic acid for colorimetry, a faint yellow coloration is developed due to phosphomolybdate, if 10 ml of the fractionated aliquot contains a large amount of phosphate. One tenth portion of the yellow solution is then diluted to 10 ml for the subsequent colorimetry by the molybdenum blue method, in order to obtain an appropriate range of optical density. The use of 25 cm length of resin column allows to take some hundred milligrams of sample tripolyphosphate for the determination of the phosphates as impurities as low as 0.01%. For the analysis of higher condensed polyphosphate, an eluent of more concentrated KCl solution is employed, for instance 1 M or 2 M KCl gives better separation similarly to that observed with diluted eluent. A recovery of total phosphorous is more than 95% by colorimetry.View full abstractDownload PDF (349K) -
Keikichi MIYAHARA, Tomo TAKAOKA1967 Volume 16 Issue 6 Pages 614-615
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple device for making aluminum-boats used in micro-elementary analysis is described. A piece of aluminum-foil is placed on a polyurethane foam plate, block in the form of a boat is pressed against the foil and moved so as to knead the foil around the block.
It may be possible to prepare 100 boats in 20 minutes by this method including the time consumed in cutting the foil into the required size.View full abstractDownload PDF (380K) -
[in Japanese]1967 Volume 16 Issue 6 Pages 616-624
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese]1967 Volume 16 Issue 6 Pages 624-628
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese]1967 Volume 16 Issue 6 Pages 629-635
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese]1967 Volume 16 Issue 6 Pages 636-643
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese]1967 Volume 16 Issue 6 Pages 644-652
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1967 Volume 16 Issue 6 Pages 653-658
Published: June 05, 1967
Released on J-STAGE: June 30, 2009
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