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Volume 17, Issue 11
Displaying 1-21 of 21 articles from this issue
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Nobusuke MASUDA, Meisetsu KAJIWARA1968 Volume 17 Issue 11 Pages 1353-1358
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGlyoxime was synthesized from glyoxal and hydroxylamine hydrochloride, and its reaction with various metal ions has been studied. It readily formed yellow complexes with cobalt, copper, nickel and ferric ions in an alkaline solution, which except of cobalt were decolorized by an addition of EDTA.
The cobalt complex was stable over the pH range 8.09.5, its wavelength of maximum adsorption being 285290 mμ.
The molar extinction coefficient at this wavelength was 15, 000, indicating high sensitivity in spectrophotometric determination of cobalt. Beer's law was obeyed for 04 ppm of Co. The Composition of the complex ion was shown as [CoCl2(HCNO)4]3- by the molar ratio method. Cobalt was precisely determined even in the presence of copper, nickel and ferric ions by masking them with EDTA.View full abstractDownload PDF (877K) -
Takako SHINODA, Hisae ENOKIDO, Yo-ichiro MASHIKO1968 Volume 17 Issue 11 Pages 1358-1363
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSeveral experimental methods were examined for the synthesis and preparation of highly pure neopentane. The results indicated that, for the purification, a combined use of a "spinning band" type fractional distillation column of 3 m height and 180 theoretical plates and of Molecular Sieve 5A adsorption column was the most effective.
The amount of impurity in a refined specimen of neopentane was measured by means of an adiabatic calorimeter, designed and constructed in the authors' laboratory. It showed the purity to be 99.9968 mol%, the triple point temperature and pressure 256.750°K and 268.47±0.13 torr., and the heat of fusion 740.0±0.3 cal/mole.
The heat capacity of neopentane was measured between 190°K and 260°K on the same specimen, and the detailed shape of the heat capacity curve was determined in order to study the premelting phenomenon of neopentane. Despite of its high purity, Cp in the region just below the melting point increased unexpectedly with temperature. This anomaly, excluding the premelting induced by impurities, was interpreted as an effect of formation of vacancies in the solid. The enthalpy of formation of the vacancies was estimated to be 3240±220 cal/mole from the analysis of the heat capacity curve.View full abstractDownload PDF (1000K) -
Emiko SUDO, Morimasa SAITO, Hiroyuki INOUE1968 Volume 17 Issue 11 Pages 1364-1369
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSOxygen in ferrosilicon alloys (Si content 6090%) was determined by vacuum fusion method. Powdered samples were used for avoiding the influence of segregation, and various baths were compared for complete extraction of gases. Among the methods examined including carbon chip method, iron-nickel bath, platinum bath, copper bath, and various metal baths mixed with carbon chip, that using carbon chip with tin and nickel foil gave the highest extractability.
The established procedure was as follows. Carbon chips of 1016 mesh and tin were put in a crucible. After degasification, about 0.1 g of sample wrapped in nickel foil was thrown into the crucible at 11001200°C (furnace temperature). The temperature was quickly raised to 1750°C, and the gas was extracted for 4 min. The values by this method agreed fairly well with those obtained by the fast neutron activation analysis. The variation coefficient was less than 10%.View full abstractDownload PDF (1110K) -
Emiko SUDO, Morimasa SAITO, Minoru CHIBA, Akira HASHIMOTO1968 Volume 17 Issue 11 Pages 1369-1373
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of oxygen (0.0041.2%) in metallic beryllium by vacuum fusion method was studied. Comparison of various bath methods indicated that platinum bath, platinum-tin bath, copper bath and nickel-tin bath gave inaccurate results with incomplete extraction. By carbon chip-tin-nickel foil method where by samples were thrown in a crucible at 1300°C and the temperature raised stepwise to 1450°C, 1650°C, 1750°C, the extraction of gas was made much higher, and the results of determination were in good agreement with those by fast neutron activation method and iodine-methanol method. The coefficient of variation was about 10%.View full abstractDownload PDF (638K) -
Kingo HISANO, Kiyoshi OYAMA1968 Volume 17 Issue 11 Pages 1373-1377
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSX-ray fluorescence analysis by the method of borax fusion was applied to the determination of tantalum in tin slag treated. In order to analyze rapidly, the fused borax bead was employed without crushing. Sodium fluoride was added to melt the samples clearly, and sodium sulfate was added to prevent the borax bead from cracking. Lanthanum oxide was added to eliminate the effects of diverse elements. The measuring time was shortened exceedingly by this method.View full abstractDownload PDF (642K) -
Koichi KATOH1968 Volume 17 Issue 11 Pages 1377-1384
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFluorescence spectra of uranine and dichlorofluorescein were measured in water-methanol, water-ethanol, and water-acetone mixed solvents at various acidities, and the ranges of the fluorescent color change were followed by their fluorescent spectra. The color change range of uranine in water solution is pH 3.05.0, but is shifted to pH 5.27.5 in 40% ethanol, and to pH 6.78.4 in 80% ethanol. Dichlorofluorescein showed a similar behaviour to the case of uranine. In the higher pH range, fluorescent intensities became smaller and the peak wavelengths of their fluorescent spectra showed a red shift. In order to find the cause of this red shift, the absorption and fluorescent spectra were measured on the same sample. A wide absorption band appeared in the higher pH range. It overlapped on the fluorescent spectrum, and resulted in the decrease of intensity and the red shift of the fluorescent spectra.View full abstractDownload PDF (932K) -
Fumio YAMAUCHI, Yoshihisa OTAKA1968 Volume 17 Issue 11 Pages 1384-1387
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDissolution of alumina with a mixture of orthophosphoric acid and sulfuric acid was applied to the determination of sodium. From 0.1 to 0.2 g of alumina containing 0.051.5% Na2O is boiled with a mixture of 2.0 ml of 85% H3PO4 and 3.5 ml of conc. H2SO4 in a test tube of transparent quartz for about 10 min., until completely dissolved. The solution is diluted with water to 50 ml, and the flame intensity is measured at 589 mμ. The procedure is more rapid and accurate than the conventional boric acid sintering method and autoclaving method.View full abstractDownload PDF (612K) -
Research on the X-ray luminescence method. INaohisa SASAKI1968 Volume 17 Issue 11 Pages 1387-1395
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn X-ray luminescence spectrometer has been developed for measuring the X-ray-excited emission spectra. The apparatus is assembled with X-ray excitation units of an X-ray spectrometer (Rigaku Denki Model K-3 with Machlett OEG-50 tube tungsten target) and a spectrophotometer (Hitachi Model 139 with QPD-53 recorder). A single convex lens ( f 35 mm) is used at the connection part. The X-ray source gives no interference with emission spectra, because X-rays are not reflected, and hence the apparatus can be easily assembled. Discoloration of lens due to X-ray radiation has not appeared even after a year. Emission intensity and sensitivity as functions of X-ray tube and spectrophotometer conditions are studied. Rare earths in yttrium oxide are determined with sensitive results.View full abstractDownload PDF (952K) -
Yai SHIOBARA1968 Volume 17 Issue 11 Pages 1396-1400
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSeparation of rhenium (VII), tungsten (VI) and molybdenum (VI) can be effected chromatography on a silica gel-coated polyester film. A sample solution is applied on Eastman Chromagram Silica Gel Sheet 6060, 100μ thick, and developed by the ascending technique simply using a solution of either acid or salt as the developing solvent. Among the solvents studied 1.01.8N hydrochloric acid is found to give the most favourable resolution of the three elements, yielding discrete spots with the least tailing.
Development with 1.0N thiocyanic acid, 1.01.8N malonic or acetic acid also affords a good separation of rhenium and tungsten/or molybdenum. Ammonium thiocyanate solution 1.01.8N is suited to resolve molybdenum and tungsten as well as rhenium and tungsten. In all the solvent systems studied Rf values are in the order rhenium>molybdenum≤tungsten. The methods described can successfully be applied to the detection of rhenium in rhenium-tungsten alloys.View full abstractDownload PDF (728K) -
Hitoshi KOHARA, Nobuhiko ISHIBASHI, Kazumi FUKAMACHI1968 Volume 17 Issue 11 Pages 1400-1406
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of beryllium by using complexation on the micelle surface has been investigated. Quaternary ammonium salt promotes the protolytic dissociation on hydroxyl group Eriochrome Cyanine R, and gives the higher order complex {molar ratio of Be (II) to ligand 1 to 2} with its absorption maximum shifted to longer wavelengths. In the presence of the quaternary ammonium salt of the concentration sufficient for micelle formation, the complex has an absorption maximum at 595 mμ with a constant absorbance in the pH range from 6.7 to 7.2. The relation between the absorbance of the complex and the concentration of beryllium is linear over the range of 0.0180.055 μg/ml, but it does not hold for the lower beryllium concentration. The effects of diverse ions are also examined. This method is the most sensitive among the spectrophotometric methods for beryllium with organic reagents.View full abstractDownload PDF (922K) -
Toshiaki NOMURA, Sumio KOMATSU1968 Volume 17 Issue 11 Pages 1406-1411
Published: November 05, 1968
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSThiocyanate ion reacted with mercury (II)-methylthymolblue (Hg-MTB or HgMe4-) to form a mixed ligand complex [HgMe(SCN)]5-(blue) and with mercury (II) ethylenediaminetetraacetate (Hg-EDTA or HgY2-) [HgY(SCN)]3- (colorless). The former reacted further with an excessive amount of thiocyanate ion into mercury(II)thiocyanate and H2Me4-(yellow) as follows.
[HgMe(SCN)]5-+SCN-+2H+→Hg(SCN)2+H2Me4-
When a solution containing thiocyanate ion and a small amount of HgMe4- was titrated with Hg-EDTA standard solution, the excess amount of thiocyanate ion was consumed with HgY2-, and then, at the end point, mercury(II) thiocyanate reacted with HgY2- and H2Me4- by the equation below, resulting in the development of blue color of [HgMe(SCN)]5-.
Hg (SCN)2+H2Me4-+HgY2-→[HgMe(SCN)]5-+[HgY(SCN)]3-+2H+
Thiocyanate ion was thus determined directly by a titration with Hg-EDTA by employing Hg-MTB as an indicator.View full abstractDownload PDF (804K) -
Kazuyoshi TAKIYAMA, Eiko KOZUKI1968 Volume 17 Issue 11 Pages 1412-1416
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSBismuth 8-hydroxyquinolate was precipitated from a homogeneous solution using 8-acetoxyquinoline, and the conditions for precipitation, the effects of diverse ions and the morphological properties of particles were examined.
Bismuth 8-hydroxyquinolate precipitated quantitatively in the range of pH 6.0 to 11.0. One to 35 mg of bismuth was determined successfully with 8-acetoxyquinoline of 8 times that equivalent to 20 mg of bismuth. A small quantity of lead coprecipitated with bismuth 8-hydroxyquinolate, but magnesium and calcium did not. The particles formed were much larger than those by the conventional method and were easily filterable.View full abstractDownload PDF (2678K) -
Studies on correlations between thin-layer chromatography and column chromatography. IShoji TAKITANI, Masao SUZUKI1968 Volume 17 Issue 11 Pages 1416-1424
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe transferability from thin-layer chromatography to dry column chromatography together with the utilization of the gradient front development by demixing of developer for the separation were investigated, by using several pigments as well as 2, 4-dinitrophenyl derivatives of several amino acids and amines as model samples.
To obtain a comparable result of separation by the both methods, at least, the same adsorbent and an identical developing temperature were required. The utilization of the gradient front procedure was effective for good separation, shortening of time and decreasing of adsorbent volume. It was found, on the other hand, that the position of the sample at the beginning was an important factor for good separation.View full abstractDownload PDF (1273K) -
Studies on the sulfur-containing chelating agents. XIXHisashi TANAKA, Yukio SUGIURA, Akira YOKOYAMA1968 Volume 17 Issue 11 Pages 1424-1427
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new radioisotope dilution method was developed for the determination of trace amount of mercuric chloride and phenylmercuric chloride. Penicillamine was used as the chelating agent, and paper chromatography was applied for the separation. A known amount of radioactive mercury (203Hg) and a substoichiometric amount of penicillamine are added to the sample solution, and the resulted solution is chromatographed on filter paper, by using the mixture of isopropyl alcohol-conc. ammonium hydroxide solution-water (7:1:2) as the developer. Standard solution containing radioisotope is treated in exactly the same manner. The separation of the chelate and unreacting mercury compound was satisfactory. Radioactivity of the spot of the chelate obtained on the respective chromatogram from the sample and the standard solution is measured, and the amount of mercury compound can be calculated from the values of activity. Determination of the amount down to 10-6g could be possible, 10-5M of penicillamine and 10-5M of mercuric chloride-203Hg or 10-5M of phenylmercuric chloride-203Hg being used within the range of pH value 610. The influence of nickel, iron, copper, zinc and cobalt was not serious.View full abstractDownload PDF (634K) -
Studies on the sulfur-containing chelating agents. XXHisashi TANAKA, Nobuko NAKANISHI, Yukio SUGIURA, Akira YOKOYAMA1968 Volume 17 Issue 11 Pages 1428-1432
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn an attempt to develop the application of thio-β-diketones as analytical reagent, the determination of mercury compound by thiodibenzoylmethane was investigated. Thio-β-diketones including thiodibenzoylmethane were prepared by an advantageous method of synthesis. Thiodibenzoylmethane was chosen among the various kinds of thio-β-diketones prepared, because of its easiness of preparation and its high stability. Radioisotope dilution method using thiodibenzoylmethane as the extractant was stisfactory for the determination of the amount down to 10-7 g of mercury. A known amount of radioactive mercury (203Hg) and a substoichiometric amount of thiodibenzoylmethane were added to the sample solution, and the chelate formed was extracted into chloroform at pH 4.
The amount of mercury was calculated from the activity of the chloroform phase. Interferences from other metal ions were practically negligible. Thiodibenzoylmethane forms extractable chelates in chloroform with cobalt, nickel, copper, zinc, cadmium and lead, but it can not be considered as an excellent reagent for the spectrophotometric method, because it has strong absorption in visible regions. Therefore, radioisotopic tracer technique is considered to be particularly effective for the application of thiodibenzoylmethane as well as of the other thio-β-diketones.View full abstractDownload PDF (712K) -
Shin TSUGE, Hajime ITO, Tsugio TAKEUCHI1968 Volume 17 Issue 11 Pages 1432-1436
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn analytical method for nylon 6-66 copolymers was investigated with pyrolysis-infrared absorption spectrometry.
The sample weighing 30 mg was pyrolyzed at 500°C under an inert atmosphere (Ar), and the degradation products were trapped in CCl4 cooled to 0°C in an ice-water bath. Then the infrared spectrum of the CCl4 solution was measured on the solution cell. Strong characteristic bands were observed at 2920 cm-1, 1750 cm-1, 1680 cm-1, and were assigned as, νasym (CH) of CH2 groups, ν(C=O) of cyclopentanone and ν(C=O) of ε-caprolactam (Amide I), respectively. Among the absorption ratios between them, A1680cm-1/A2920cm-1 was found to be best with respect to the precision. Determination of the composition of the copolymers was possible by using the calibration curve for the physical blends of the homopolymers. The relative standard deviation was 25%. The pyrolysis mechanism of polyamides was also discussed.View full abstractDownload PDF (790K) -
Yoshitaka YOICHI, Kazuo KAKEMI, Masakazu UENO1968 Volume 17 Issue 11 Pages 1437-1439
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA colorimetric method for the determination of 2-(1-piperidino)ethylbenzilate ethylbromide (I) based on its association with an organic dye has been established. Dyes which have optimum pH in the weakly acidic range are used in the phosphate-buffered solution. The procedure is as follows.
Twently milliliters of ethylenedichloride is put into a 40 ml glass-stoppered centrifuge tube. Four milliters of M/15 phosphate buffer solution of pH 6.4 (or of 5.0 in case of Iodophenol Blue), 2 ml of 0.1% Bromocresol Purple solution (or 0.1% Iodophenol Blue solution) and 2 ml of the sample solution containing 20140 μg of (I) are added. After the mechanical shaking for 10 min. and separation of layers by centrifuge, the water layer is discarded. A 10 ml aliquot of ethylenedichloride layer is transfered into another 40 ml centrifuge tube, and 10 ml of 0.1M sodium carbonate solution is added. After shaking for 2 min. and separation by centrifuge, the absorbance of the water layer is measured at 591 mμ (598 mμ in case of Iodophenol Blue solution) against a blank.View full abstractDownload PDF (480K) -
Tomitaro ISHIMORI, Kaoru UENO, Johkun AKATSU, Michio HOSHI1968 Volume 17 Issue 11 Pages 1439-1441
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIt is well known that the 235U content in uranium can be determined by comparing γ-activities from 235U and those from 234Th and 234m, 234Pa formed by the disintegration of 238U and in the radiochemical equilibria. Although this method looks convenient, it is not utilized widely, because about 8 months are necessary for attaining the equilibria after any chemical separation of uranium and thorium. In the present work, the above γ-spectrometric method was extended to uranium samples in which the equilibria are not yet attained. The proposed method determines 0.41% 235U at about 20 days after the purification of uranium from thorium. Values obtained agree well with those by the mass-spectrometry.View full abstractDownload PDF (415K) -
[in Japanese]1968 Volume 17 Issue 11 Pages 1442-1446
Published: November 05, 1968
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (861K) -
[in Japanese]1968 Volume 17 Issue 11 Pages 1446-1450
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (862K) -
[in Japanese]1968 Volume 17 Issue 11 Pages 1451-1467
Published: November 05, 1968
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (2821K)
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