All issues
Volume 18, Issue 3
Displaying 1-23 of 23 articles from this issue
- |<
- <
- 1
- >
- >|
-
Kiyoko TAKAMURA, Yumiko HAYAKAWA1969 Volume 18 Issue 3 Pages 309-314
Published: March 05, 1969
Released on J-STAGE: February 15, 2010
JOURNAL FREE ACCESSMost quinones give some polarographic reduction waves in both the aqueous and the non-aqueous media. The influence of some proton donative species on the polarographic behavior of quinones was discussed previously, in which the presence of small concentration of acid in the solution caused a diffusion controlled prewave to the reduction wave of quinones. The probable expression of the electrode reaction for the prewave is,
Q+2HA+2e_??_H2Q+2A-
The prewave height was proportional to the concentration of the acid added, and the half-wave potential varied with the acidity of added species.
The present paper dealt with the analytical application of those facts to the determination of minute quantity of acid. The method was applied to the free acid contained in some commercial reagents as an impurity. For example, the contents of free sulfuric acid in potassium sulfate and free salicylic acid in sodium salicylate were determined from the polarograms of p-benzoquinone obtained in aqueous solutions containing each salt as a supporting electrolyte. The content of free acetic acid in crude ethyl acetate was also determined from the prewave recorded with the solution of methyl-p-benzoquinone using ethyl acetate itself as a solvent.
The results were accurate to within 1.4% error for 10-310-4M and 5% for 10-5M of acid. This method might be applicable to the determination and the detection of small amount of free acid in the crude reagent as low as ppm range.View full abstractDownload PDF (1045K) -
Katu TANAKA1969 Volume 18 Issue 3 Pages 315-319
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSExtractabilities of selenium (IV) into benzene from hydrobromic acid or HBr-containing hydrochloric, sulfuric or perchloric acid and of tellurium (IV) into nitrobenzene from HBr-containing sulfuric or perchloric acid have been given. Under equal volumes of phases, selenium (IV) of 0.01M in aqueous phase is extracted to the extent of greater than 90% from 0.87N HBr-9.6N HCl, and greater than 99% from the following media: 1.0N HBr->14.0N H2SO4, 0.5N HBr->16.3N H2SO4, 0.2N HBr->16.3N H2SO4, 0.5N HBr->6.6N HClO4 and 0.2N HBr->7.5N HClO4. Tellurium (IV) does not come into benzene but does into nitrobenzene to the extent of greater than 99% from the following media: 0.1N HBr->18.6N H2SO4, 0.05N HBr->17.5N H2SO4, and 0.05N HBr->7.4N HClO4. The extractability of both elements, especially of tellurium (IV), decreases with the increase in hydrobromic acid concentration owing to the formation of their acid bromocomplexes. Influences of some other cations on the extraction of selenium (IV) and tellurium (IV) were also examined.View full abstractDownload PDF (910K) -
Katu TANAKA, Nobuyuki TAKAGI, Hiroshi TSUZIMURA1969 Volume 18 Issue 3 Pages 319-324
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new technique for determining selenium in iron and steels has been established, which involves the extractive separation of selenium by benzene and the iodometric microtitration with starch as an indicator. The recommended procedure is as follows. Dissolve 1g of sample in nitric acid or that combined with hydrochloric acid, and heat to gentle fumes with 20ml of perchloric acid. Transfer the residue into a separatory funnel with 20ml of concentrated hydrochloric acid. Add about 30ml of benzene and 1ml of hydrobromic acid (d=1.48), and then shake for 1min. Discard the aqueous layer and wash inside of the funnel once by shaking with a mixture of 5ml of concentrated hydrochloric acid, 5ml of 60% perchloric acid and 0.20.3ml of hydrobromic acid. Discard the washings. Back-extract selenium (IV) successively with 15ml of 2% sodium nitrite, 10ml of extremely dilute sodium hydroxide solution and finally with 10ml of water. Boil the combined extracts for a few min. in the presence of 5ml of 85% phosphoric acid and 0.3g of urea. Cool to about 20°C and expel dissolved oxygen by treating with 1g of sodium bicarbonate. Titrate iodometrically with 0.01N thiosulfate solution.
Selenium more than 0.01% in ordinary iron, stainless steels and heat resisting steels was determined successfully. The relative errors were -3% and ±5% for, respectively, 1% and 0.10.01% of selenium.View full abstractDownload PDF (1210K) -
Tamotsu TANAKA, Kazuo YAMASAKI1969 Volume 18 Issue 3 Pages 324-328
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTo the silicate samples like glasses or rocks were added sodium carbonate and the diluent consisting of germanium dioxide and the twice amount of graphite powder, in the ratios 1 : 1 : 2 or 1 : 1 : 40. The thoroughly mixed sample was put into a carbon electrode and excited by the d.c. arc of 200 volts and 8 amperes. The spectra recorded photographically were processed by the usual methods. The line of germanium at 3067.0 or 2829.0Å was used as the internal standard, the latter being used for samples containing larger amounts of iron. The elements Ag, Al, Bi, Ca, Co, Cu, Fe, Mg, Mn, Ni, Pb, Sb, Sn and Ti can be determined with the relative deviation of about 10%, and Si of about 5%. The concentration ranges applicable are Ag 0.001Ti 0.6% as listed in Table I, and those of major components, SiO2 and PbO are ca. 15100% and 1075%, respectively. The purpose of the present investigation is the application of spectrographic methods to the study of ancient glasses.View full abstractDownload PDF (807K) -
Yoshizo HORIUCHI, Tsunemi KAWAMOTO1969 Volume 18 Issue 3 Pages 329-332
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA gravimetric method of determining zinc with 2-(ο-hydroxyphenyl)-benzoxazole has been studied.
Add ammonium tartrate as masking reagent to a sample solution containing zinc, and adjust pH of the solution to 12.513 with sodium hydroxide solution.Add the precipitant to the solution in excess 20 to 40% over the stoichiometric amounts for zinc, heat for 30 minutes at 7080°C, filter and dry the pale yellow precipitate for 3 to 4 hours at 150160°C, and weigh as Zn (C13H8O2N)2.
By the present procedure, 1 to 50 mg of zinc could be determined rapidly with good precision as well as the oxine method. The effect of diverse ions on the determination of zinc was also examined. Ni, Co, Cd, Cu, and Pd interfered remarkably with the determination forming their complex salts.
The method has been successfully applied to the determination of zinc in brass.View full abstractDownload PDF (624K) -
Ohiko KAMMORI, Minoru SASAKI, Tomoo TAKAHARI, Shoji MUROTA1969 Volume 18 Issue 3 Pages 333-338
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe optimum conditions for determining carbon contents in various carbides were investigated by using an electron probe microanalyzer. Though the profiles of Cr Kα and Ni Lα lines overlapped partly with C Kα, the interferences could be eliminated by the use of a pulse height analyzer. The chemical shifts of C Kα lines were measured for several carbides. The accelerating voltages which give the maximum X-ray intensities of C Kα lines were 15, 10, 9.5, 9, 5.2, 2.7 and 2.5 for graphite, diamond, TiC, VC, Cr3C2, Mo2C, TaC, and WC, respectively. The X-ray intensities of these carbides were almost proportional to the carbon contents. The absorption corrections for SiC and B4C were calculated by Philibert's and modified Philibert's equations. The applicability of those equations was discussed.View full abstractDownload PDF (1046K) -
Yoshitaka YOICHI, Akira SANO, Akio OGINO1969 Volume 18 Issue 3 Pages 339-345
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSColorimetric determination of N-acetyl-N-phenyl glycine dimethylamide with p-dimethylaminocinnamaldehyde has been scrutinized to be applied to the determination of N-acetyl-N-phenyl glycine dimethylamide in mixed pharmaceutical preparations.
N-Acetyl-N-phenyl glycine dimethylamide was treated with sulfuric acid to form N-phenyl glycine dimethylamide which reacted with p-dimethylaminocinnamaldehyde and gave reddish yellow color. This color reaction was applied to the determination of small amounts ofN-phenyl glycine dimethylamide(416μg/ml).
Its sensitivity was very high, the molar absorptivity being 2.14×105.
The absorbance measured at 510 mμ against the reagent blank obeyed Beer's law over 416 μg/ml of N-phenyl glycine dimethylamide.
The pigment produced in this reaction was isolated as a perchloric acid salt, and its structure and the mechanism of this color reaction were revealed.View full abstractDownload PDF (980K) -
Isamu AOKI, Masatake HORI, Hideo MATSUMARU1969 Volume 18 Issue 3 Pages 346-348
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDetermination of idonic and gluconic acid was carried out chromatographically by the use of Dowex 1, X-8 column (Cl- type, 400 mesh minus, 9 × 200 mm) and the borate buffer (pH 7.35) as the eluent. The eluate from the column was made to react with periodate reagent and the absorbance was determined automatically by an Auto Analyzer (Technicon). Some other sugar acids could be determined in this condition by the same manner.View full abstractDownload PDF (553K) -
Soichiro MUSHA, Masami NUKADA, Toshimasa OKANO, Shintaro FUDANO, Masar ...1969 Volume 18 Issue 3 Pages 349-353
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSMethods for standardization of sulfur dioxide gas used for the calibration of a measuring apparatus were studied.
Sulfonal, which is used as a standard substance for the organic elementary analysis, was used as a primary standard substance, and the following two standardization methods were studied.
(1) Sulfur oxides evolved by the combustion of sulfonal was absorbed in a hydrogen peroxide solution, and the sulfuric acid produced was determined by coulo metric titration.
(2) Sulfur oxides evolved by the combustion of sulfonal was caught on the silver gauze as silver sulfate, and was converted into hydrogen sulfide by the reduc tion with hydrogen.
The resulting hydrogen sulfide was absorbed in a zinc acetate solution.
Methylene Blue was produced in the usual way and its concentration was determined by spectrophotometry.
The latter method (Takeuchi's Method*) is recommended because it is more accurate and precise.
*T. Takeuchi, et al.: Mikrochim. Ichnoanal. Acta, 1965, 635.View full abstractDownload PDF (923K) -
Yuroku YAMAMOTO, Takahiro KUMAMARU, Yasuhisa HAYASHI, Mitsue OTSUCHI1969 Volume 18 Issue 3 Pages 354-359
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new spectrophotometric method is proposed for the determination of salicylic acid. The method is based on solvent extraction of the ion-pair formed between tris(1, 10-phenanthroline)iron(II) and the anion of salicylic acid into nitrobenzene.
The color intensity of the organic phase (516 mμ) is proportional to the initial amount of the salicylic acid in aqueous phase.
The constant extraction is obtained when the cationic metal chelate concentration is 3.2 × 10-3M in the aqueous solution buffered at pH 5.5 to 9.5.
The calibration curve is constructed as follows.
To 5 ml of 0.3 M phosphate buffer solution (pH 6) and 8 ml of tris(1, 10-phenanthroline)iron(II) solution (1.0 × 10-2 M) are added varying amounts of the standard salicylic acid solution (2.0 × 10-4M, 05 ml). It is diluted to 25 ml with water, and is shaken for 2 min. with 10 ml of nitrobenzene. The absorbance of the organic phase is measured at 516 mμ against the reagent blank.
A linear relationship is obtained over the range of 8 × 10-6 to 4 × 10-5M of salicylic acid in aqueous solution.
The effect of diverse organic compounds such as preservatives, sweetening agents and others on this method was investigated.
The proposed method was applied to the determination of salicylic acid in commercial Japanese Sake and the results were in good agreement with those by official UV method.View full abstractDownload PDF (1007K) -
Yuroku YAMAMOTO, Takahiro KUMAMARU, Yasuhisa HAYASHI, Yuzuru OTANI1969 Volume 18 Issue 3 Pages 359-363
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new application of atomic absorption spectrophotometry is reported for the determination of nitrate. Nitrate ion is extracted into MIBK as the ion-pair formed between bis(neocuproine)copper(I) and nitrate ion; the copper concentration in the extract is then determined by atomic absorption method in an air-acetylene flame at the 3247Å copper line. Optimum conditions are described. The absorbance of the extract showed a linear relationship to the concentration of nitrate initially present in the aqueous solution over the range of 10-5 to 7 × 10-5M. The effect of diverse anions on the nitrate extraction, the composition of the extracted species and the extraction percentage were also investigated.View full abstractDownload PDF (845K) -
Hisao OSAWA1969 Volume 18 Issue 3 Pages 364-370
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe relations between vaporized amounts, vaporization behavior and spectral line intensity of copper in graphite powder have been examined with graphite electrodes under varying arc discharge conditions and buffer concentrations.
Standard samples were prepared with highly purified graphite powder, 10 ppm of copper as cupric oxide and various amounts of lithium fluoride as a spectrographic buffer substance. The element was excited by the d.c. arc discharge, and the concentration of copper remaining in graphite powder after the discharge was measured by the neutron activation analysis.
It was shown that the vaporized amounts were increased and the temperature of anode was raised with an increase of the arc current. Under the conditions involving arc current 8.512.6A, electrode gap 3 mm, discharge time 60 sec., the vaporized amounts were 9×10-9g/mg sample on both anode and cathode craters in the air, and 5×10-9g/mg sample in argon atmosphere. The argon atmosphere gave, under the same vaporized amounts as in the air, a lower line intensity of Cu 3247.5Å. The ratio of Cobs. to Cstand. in the air, characterizing a vaporaization behavior of copper, depended mostly on the arc current and the discharge time. The vaporized amounts on both anode and cathode craters as well as the line intensity of Cu 3247.5Å were increased by an addition of lithium fluoride of a concentration from 0.5 to 2.0% to the sample under arc discharge.View full abstractDownload PDF (1204K) -
Naoharu YAMAGUCHI, Ryoichi SUZUKI, Ohiko KAMMORI1969 Volume 18 Issue 3 Pages 370-376
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSome basic techniques for the microprobe analysis by a mass spectrograph with high frequency spark source were investigated, in which platinum or tungsten wire (200μ in diameter) was used as the pointed counter electrode to plane sample. The craters on the surface of samples were 400500μ in diameter and 1020μ in depth for the exposure 1×10-10coulombs, and 300μ and 2μ, respectively, for the exposure 3×10-13 coulombs. The elements of 0.01% were detected by the former exposure and those of 1% by the latter. The size of crater depended on the repetition rate of pulse and the spark voltage. The ratio of ion intensities of sample to counter electrode changed in every discharge, and for the quantitative analysis the ion intensity of counter electrode had to be subtracted from the total ion intensity. By this reason, platinum having the wide range of abundance ratio of the isotopes was more suitable than tungsten as the counter electrode. The reproductivility of microprobe analysis with low alloy steel was 517% as coefficient of variation. The technique was applied for the analysis of inclusions in stainless steel samples.View full abstractDownload PDF (1768K) -
Shigeo WAKAMATSU1969 Volume 18 Issue 3 Pages 376-383
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA new simple and reliable method has been presented for the spectrophotometric determination of 0.01 to 4% of niobium in steel. The sample is decomposed with HCl, HNO3 and HClO4, and niobium is separated from common interfering elements such as iron, molybdenum, tungsten and vanadium by precipitation with phytin. The precipitate is decomposed with HNO3, HClO4, and H2SO4, and then determined photometrically by Sulfochlorophenol S method which is based on the reaction of niobium with Sulfochlorophenol S to form a blue complex. The method obeys Beer's law and is sensitive for niobium ranging from 4 to 40 μg. Zirconium is the only ion that inteferes seriously but can be masked with EDTA.View full abstractDownload PDF (1470K) -
Tsugio TAKEUCHI, Shin TSUGE, Hajime ITO1969 Volume 18 Issue 3 Pages 383-387
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA method for determining composition of ethylenepropylene copolymers(EPR) was developed by utilizing the infrared spectra of the CCl4 solution of the gaseous, liquid and waxlike decomposition products of EPR under an inert atmosphere (Ar).
The bands characterizing the composition of EPR are divided into two main classes : (1) δsym(CH) of CH3 at 1380 cm-1 and δasym (CH) of CH3+ δ(CH) of CH2 at 1470 cm-1 which are attributable to CH bending vibrations of CH2 and CH3, and (2) olefinic CH bending vibrations which appear in the region 1000850 cm-1. As to these characteristic bands was studied the pyrolysis-temperature dependence of the absorbance ratios between them as well as the reproducibility and precision of the determination.
Determination of the composition of EPR was possible within 3% of relative standard deviation for 30 mg of samples by using the pyrolysis temperature 750°C and the absorbance ratio A1380cm-1/A1470cm-1.View full abstractDownload PDF (854K) -
Tsugio TAKEUCHI, Mitsuru YAMAZAKI, Hideo HADA, Takashi YABUKI1969 Volume 18 Issue 3 Pages 387-391
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSWater was determined by Karl Fischer coulometric titration with dead-stop detection of end point by using a new stable circuit and an improved electrolytic cell.
A stable circuit for 5200mA constant-current applicable to non-aqueous solvent was presented, and optimum reagents for drying the electrolytic cell was selected.
An accurate and consistent end point was obtained by using the titration solvent containing formamide, pyridine, chloroform, methanol and commercial Karl Fischer reagent.
The relative error was less than 3% for methanol containing 2mg/ml of water.View full abstractDownload PDF (706K) -
Studies on analysis of pesticides by chromatography. I.Masato KOTAKEMORI, Takeo SAWADA, Humiyuki NISHIZAWA, Kenzo OBAYASHI1969 Volume 18 Issue 3 Pages 392-394
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGas chromatographic determination of sodium monofluoroacetate in aqueous rhodenticidal preparations has been presented.
Sodium monofluoroacetate was converted into the corresponding free acid by the method of ion exchange with Dowex W 50-8X, and the free acid solutions were immediately applied to gas chromatograph.
The apparatus used was a Model 700 gas chromatograph(F & M scientific Co.) equipped with a hydrogen flame detector and the 2 m, 3 mm, i.d. glass column packed with porous polymer beads, Porapak Q. The instrument was operated at a column temperature of 210°C and with a flow rate of 30 ml per minute of nitrogen.
By the internal standard method using n-butyric acid as the standard, the calibration line with peak height was linear and passed through the origin. The coefficient of variation was about 1%.View full abstractDownload PDF (493K) -
Satoshi MIZUKAMI, Koji DAIKATSU, Tadayoshi IEKI1969 Volume 18 Issue 3 Pages 394-396
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for measuring water in organic compounds at the microgram scale, based on quantitative electrolysis in a specially designed apparatus, has been developed.
A quartz sample protector containing 0.30.5 mg of sample weighed in a platinum boat is placed into the drying tube, and is heated at 100150°C under vacuum. Water vapor liberated from the sample is despersed in the diffusion chamber, and is introduced into the electrolytic cell in the stream of helium gas by the new technique of exchanged flow line. The method usually requires only 50 min. per sample, and the accuracy is within about ±0.5 per cent.View full abstractDownload PDF (502K) -
Nobuta HAYASHI, Shigeo INOUE, Keiji TAKEUCHI1969 Volume 18 Issue 3 Pages 397-398
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSurface structures of several kinds of diatomaceous earth supports, either washed with acids, coated with stationary liquids, or deteriorated in use, were observed under a scanning electron microscope.
C-22, Celite 545, Chromosorb-W and -P of commercially available diatomaceous earth supports were observed to have similar microstructures composed of fragmentary remains of diatomaceae.
On the other hand, Anakrom U and Gas Chrom S are composed of complete remains.
These observations provide useful informations on relations between surface structures of column packing materials and their performances.View full abstractDownload PDF (3114K) -
Taitiro FUJINAGA, Toru KUWAMOTO, Eiichiro NAKAYAMA, Masatada SATAKE1969 Volume 18 Issue 3 Pages 398-399
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA liquid-liquid extraction of metal chelate with a hot solution followed by a solid-liquid separation was successfully applied to the trace analysis of metals.
In the determination of traces of copper, the pH of the sample solution was adjusted to around 6.0, the solution was heated on a hot water bath, shaken vigorously after the addition of a pellet of oxine-diphenyl (0.05 g of oxine in 5.0 g diphenyl solution) to extract copper oxinate into the liquefied diphenyl layer, and allowed to stand still at room temperature. The solidified pellet was washed with water by decantation, dissolved and diluted to a definite volume with chloroform. An aliquot was then taken to an optical cell and the absorbancy at 410 mμ was measured to determine the amount of copper.
The Beers' law held with the amount of copper up to 150 μg in 50 ml of original solution. Fig. 1 shows the absorption spectrum of copper oxinate in diphenyl dissolved with chloroform.
The method could also be applied to the removal of interfering major components in trace analyses and to the decontamination of radioactive elements. The detailed results will be reported later.View full abstractDownload PDF (627K) -
[in Japanese], [in Japanese]1969 Volume 18 Issue 3 Pages 400-414
Published: March 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2196K) -
[in Japanese]1969 Volume 18 Issue 3 Pages 415-422
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (1250K) -
[in Japanese], [in Japanese]1969 Volume 18 Issue 3 Pages 423-427
Published: March 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDownload PDF (1157K)
- |<
- <
- 1
- >
- >|