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Volume 20, Issue 4
Displaying 1-24 of 24 articles from this issue
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Kikuo WAKINO, Mitihiro MURATA, Masayuki OMATU1971 Volume 20 Issue 4 Pages 395-398
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn JIS method of iron determination ( JIS M 8212) iron(III) is reduced by stannous chloride the excess of which is then oxidized by mercuric chloride.
A method was proposed to avoid the pollution of the drainage with mercury especially in the analyses of many samples. Iron(III) in a hydrochloric acid solution out of contact with air was reduced to iron(II) by dissolving aluminum foil at about 98°C and resulted iron(II) was titrated with 0.1N standard. potassium dichromate solution using sodium diphenylaminesulfonate as an indicator. The method was more rapid than a method proposed by Reigel and Schwartz.
The analytical result for iron dioxide by this method coincided with that by the JIS method and the standard deviation (σ) was 0.100.
The analytical result for Ba-ferrite was also given.View full abstractDownload PDF (682K) -
Masao TAKAHASHI1971 Volume 20 Issue 4 Pages 399-405
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA dry-inert atmosphere drybox system for handling sodium metal without any contamination of oxygen and water in air has been designed and constructed. This system maintains a working atmosphere of argon containing less than 1 ppm each of oxygen and water. It consists of a stainless steel drybox which has three pairs of butyl rubber gloves and an atmosphere purifier, using NaK as the purifying medium. A spiral blower circulates the gas from the drybox through the purifier and back to the drybox at a flow rate of approximately 1 m3/min. A subsystem of pressureactivated switches and solenoid valves maintains the drybox at a slightly positive pressure. Surface of sodium metal in the system remains bright for a period of up to 8 hours.View full abstractDownload PDF (1240K) -
Masami AKATSUKA, Hirotaro AMAMOTO, Setsuyo YOSHINAGA1971 Volume 20 Issue 4 Pages 406-410
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSColorimetric determination of α-naphthyl thiourea, benzaldehyde thiosemicarbazone and thioacetazone was done by applying the purple color formed by the reaction of 3-chloro-1, 2-naphthoquinone with those compounds in potassium carbonate or hydroxide solution. The optimum condition for the determination were decided and a procedure was established. Less than 80 μg/ml of those compounds could be determined. The determination of α-naphthyl thiourea was scarcely influenced by the presence of other antirodents as sodium fluoroacetate and warfarin.View full abstractDownload PDF (681K) -
Hiroshi NISHIDA1971 Volume 20 Issue 4 Pages 410-415
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe acid dissociation constants of Chromazurol S (CAS, H4L) in the presence of 5.42×10-3M zephiramine (tetradecyldimethylbenzylammonium chloride, ZCl) and 0.1M ammonium chloride were pK2'=0.3, pK3'=4.0 and pK4'=12.3 at 25°C. The presence of zephiramine enhanced the acid dissociations of carboxyl groups in CAS but it decreased that of hydroxyl group.
Iron (III) with an excess CAS mainly formed a 1 : 1 complex (FeHL) at pH below 3, but formed in the presence of zephiramine a 1 : 2 complex [Fe(HLZ)2-] with an absorption maximum at 634 mμ increasing the photometric sensitivity.
The formation of the complex concluded in 8.56×10-4MCAS and 5.42×10-3M zephiramine at pH 3 and Beer's law held for 0.044 ppm of iron (III) with molar absorptivity at 634 mμ 1.5×105.View full abstractDownload PDF (829K) -
Akira NONAKA1971 Volume 20 Issue 4 Pages 416-421
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA G-S chromatography was applied to the analyses of hydrocarbons (C5C9 normal alkanes, petroleum fractions, and benzene and its derivatives) using water vapor as the carrier gas and activated alumina as the stationary phase (Fig. 1). By using a steam carrier, these samples were eluted quite rapidly at comparatively low temperatures (120220°C) even with a column of activated alumina (Figs. 25). Samples were injected in the form of extremely diluted aqueous emulsions but the water in the sample had not influenced on the chromatograms. The retention, volumes increased with the rise of the column temperature up to 180°C and then began to decrease (Fig. 6). This anomaly in the retention volume temperature dependence was explained by a mechanism different from that of ordinary G-S chromatography ; i. e., the sample molecules were adsorbed and were migrating on the multi-molecular water film which was formed on the adsorbent as speculated in the B. E. T. theory of physical adsorption.View full abstractDownload PDF (829K) -
Akira NONAKA1971 Volume 20 Issue 4 Pages 422-427
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGas chromatographic separation of high-boiling hydrocarbons was carried out using steam carrier and stationary solid such as diatomaceous firebrick powder (e.g., Chromosorb P AW, 30/60 mesh, Johns-Manville). Polynuclear aromatic hydrocarbons (naphthalene and its derivatives, anthracene, crysene and triphenylene) and polyphenyls (biphenyl, terphenyl and quaterphenyl) as the sample were made into the form of a 0.1%10ppm aqueous suspension by milling to fine powder and dispersing into water (Figs. 15). The water in the sample did not affect the efficiencies of the, column and the detector (hydrogen flame ionization). The elution was very rapid, even at a much lower column temperature than the boiling-point of the sample material : e. g., p-quaterphenyl was eluted in only 3 minutes at 260°C (Fig. 6). This rapid elution was explained by a temporary modulation of the stationary phase by adsorption of the steam carrier on its surface. The values of NTP were comparatively small (Table IV) but were large enough for the chromatographic separation of the samples in this experiment.View full abstractDownload PDF (1006K) -
Non-aqueous solvent column chromatography. IWataru FUNASAKA, Teiichi ANDO, Kazumi FUJIMURA, Toshihiko HANAI1971 Volume 20 Issue 4 Pages 427-430
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe relationship between the structure and the chromatographic behavior of a variety of mono-and di-substituted benzenes on an anion-exchange resin was investigated in anhydrous ethanol. It has been found that the distribution coefficients (Kd') depend on the kind and the position of the substituents and that the degree of adsorption is, at least partially, related with the electron-withdrawing property of the substituents. The experimental data suggest that the adsorption occurs by the formation of either a chargetransfer complex or a hydrogen bonding between the sample and the anion of the resin. By using an anion-exchange resin (Cl-form) and ethanol as eluting agent, ο-, m-and p-nitroanilines, ο-and m-chloroanilines as well as ο-and p-nitrophenols could be separated satisfactorily.View full abstractDownload PDF (420K) -
Application to the state analysis of ethoxo-aluminum complexesTakao YOTSUYANAGI, Shigeo YOKOYAMA, Yasuo KUDO, Kazuo AOMURA1971 Volume 20 Issue 4 Pages 431-438
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn order to establish a new method for the determination of mononuclear and polynuclear aluminum species in absolute ethanol solution, a spectrophotometric study was made on the reaction of pyrocathechol-4-sulfonate (PCS) with aluminum in ethanol. PCS reacted with aluminum in ethanol solution to form a stable ethanol-soluble complex with molar ratio of Al to PCS 1: 2 in apparent pH range from 8 to 11. This complex showed two absorption peaks at 255mμ and 298 mμ. The maximum absorbance at 298mμ was obtained at apparent pH 9.5. The molar absorptivity was 1.56×104 at 298 mμ, and the sensitivity of determination at apparent pH 9.0 was 0.0019 μg Al/cm2. The color intensity did not change for more than 10 hours. A reaction rate study showed that a partially neutralized aluminum chloride solution in absolute ethanol contained three different kinds of aluminum species : one of them reacted instantaneously with PCS and the other two followed apparently the first and 0-th order reaction kinetics. The concentrations of these species could be determined by graphical means.View full abstractDownload PDF (1327K) -
Kazuo SHIOZAKI, Kiyoshi FUKUI, Toyokichi KITAGAWA1971 Volume 20 Issue 4 Pages 438-443
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSα-Tocopheryl acetate (TAG), gives a reproducible diffusion controlled wave of one electron anodic oxidation at +1.33 V vs. SCE in acetonitrile using glassy carbon as indicator electrode and lithium perchlorate as supporting electrolyte. The peak current is proportional to the concentration of TAC up to 1000 mg/l. Under the same condition, α-tocopherol (TOC) shows an anodic oxidation wave, peak potential at +0.68 V vs. SCE. The mixture of TAC and TOC can be thus determined simultaneously without any other separating technique. Water does not interfere if its amount is less than 0.3%. TAC in commercially available vitamin E products can be determined by this method with standard deviation 0.45.View full abstractDownload PDF (878K) -
Tsutomu FUKASAWA, Masaaki IWATSUKI, Hiraku ASAKAWA1971 Volume 20 Issue 4 Pages 444-450
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSimple and rapid methods have been developed for the determination of 0.04 to 1 ppm of iron in water and 5 to 50 ppm of iron in aluminum in alkaline media. For the determination of iron in water, all the iron in the sample is reduced to ferrous state with 0.5% hydrazine sulfate solution, and if acidic, the sample is neutralized with a diluted sodium hydroxide solution. For the determination of iron in aluminum, 0.51.5g of sample is dissolved in 10 ml of 20% sodium hydroxide per 1 g of the sample and a solution of hydrazine sulfate is added. An adequate amount of 0.3M sodium sulfide is added and the absorbance of the colored solution, after standing for 45 or 60 min., is measured at 430 mμ against water. A blank is run through the entire procedure. The time required for a determination is about 60 or 100 min. for water or aluminum, respectively. The detail of the experiments and also a discussion on the colored compound are given.View full abstractDownload PDF (986K) -
Masaaki KATAYAMA, Yoshitaka MASUDA, Toshikazu TARUTANI, Seizo MISUMI1971 Volume 20 Issue 4 Pages 451-456
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSWhen the metal DTPA complex solution is passed through in the cation exchange resin at the constant pH, the complex anion is not adsorbed on the resin, and only the dissociated metal cation is exchanged on it. So we investigated the possibility of the separation and the concentration by the relation between the exchanged adsorption volume of the metal ions and pH experimentally.
First the adsorption of some metal-DTPA complexes {M=La(III), Y(III), Sm(III), Yb(III), Zn(II), Ni(II), Fe(II), Th(IV), Cu(II)} was studied about pH and the flow rate using the sodium type of cation exchange resin (Dowex 50-X4, 50100 mesh). As these complex anions exhibited the adsorption over the pH range 4 to 1, the separation and the concentration were possible. It was confirmed that the separation of between Th (IV) and Yb (III) (pH=1.65), between Sm (III) and Cu (II) (pH=1.90) was possible applying the results above.
As DPTA ligand produced the ionic species as H2Y3- HY4- and Y5- mainly by the variation of pH in the area of this studied solution, we considered the reaction between some metals and them. Especially the metal hydrogen DTPA complex must be considered in the complexation of the transition metal. It was found that the distribution coefficient Kd, depended on its stability constant.View full abstractDownload PDF (830K) -
Hideo NAGAI, Akira UTSUNOMIYA1971 Volume 20 Issue 4 Pages 457-460
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSChloroform-containing alcohols, -ketones, -phenol, -carbon tetrachloride, -hydrochloric acid and -acetic acid have been widely used as the developer of paperchromatography of familiar and less familiar metal ions. Rare earth elements, however, have not yet been separated with those developers containing chloroform. One hundred ml of chloroform, 150 ml of methyl carbitol and 50 ml of 0.2M acetic acid-0.2M sodium acetate buffer (pH=ca. 4) were shaken well and to the separated lower layer was added 7.5 g of oxine. The developer thus prepared was used throughout this study. A mixture of La, Ce, Nd, Sm, Eu and Tb could be separated by one development. There was considerable evidence to support the migration of cations in the form of positively charged complexes coordinated with one or two oxine molecules.View full abstractDownload PDF (544K) -
Kanji ISHIKAWA, Yoshio YUSA, Yuzuru ASANO, Katsuyuki AKASAKI1971 Volume 20 Issue 4 Pages 461-466
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn analytical method has been established for separation and determination of residues of some N-methylcarbamate insecticides in rice grain. The clean-up procedures consisted of distribution between n-hexane and acetonitrile and of alumina column chromatography. The eluates were fractionated into two groups; the first contained 2-isopropylphenyl-, 2-sec-butylphenyl-, 3-tolyl- and 3, 5-xylyl-N-methylcarbamates, while the second involved phenyl-, 2- isopropoxyphenyl- and 1-naphthyl-N-methylcarbamates. These carbamates were hydrolyzed to corresponding phenols, which were then coupled with 4-nitrobenzenediazonium ion to produce colored compounds. These compounds were separated by TLC on alkalized silica gel G with a mixture of n-hexane and ethyl acetate (1:1) as the developer. Interferences were almost removed by this procedure, and the recoveries of 0.1 ppm N-methylcarbamates, except 1-naphthyl-N-methylcarbamate, were 6080%.View full abstractDownload PDF (922K) -
Keiichiro HOZUMI, Naoshige AKIMOTO1971 Volume 20 Issue 4 Pages 467-473
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn electro-analytical study on the dynamic property of the fluoride-selective electrode has been carried out for the microdetermination of fluorine by means of direct potentiometric measurement of the fluoride activity in a sample solution. The electrode potential responded to the fluoride activity down to 10-4M with extremely fine traceability to the Nernstian slope and the potential was equilibrated within a few minutes after dipping the electrode into the solution. The reproducibility of the electrode potential was practically invariable for the concentration down to 10-4M and a fluoride concentration ranging 10-310-4M was the most preferable for 1001000 μg of fluorine because it made possible to make up the test solution to a convenient volume, 100 ml.
The method has been applied to the microdetermination of organic fluorine using oxygen flask combustion. A sample was burned in an oxygen flask conventionally using 10 ml of water as the absorption liquid. The liquid was transferred into a 100 ml volumetric flask with 50 ml of water. The ionic strength was adjusted by an addition of 100 ml of TISAB (buffer solution, Orion Research Inc., U. S. A.) by making up the final volume to 100 ml. The fluoride activity was then measured by a combination of the fluoride-selective electrode and a silver chloride reference electrode after 5 minutes of soaking in the test solution.
Analytical results using hard glass combustion flasks gave values approximately 8% relative lower than those by quartz combustion flasks. The possible interfering elements such as silicon, aluminum and calcium were detected by atomic absorption spectrometry while boron was detected by solvent extraction using Methylene Blue. The latter played the main role for giving above lower values because silicon, aluminum and calcium were detected in both hard glass and quartz flasks.View full abstractDownload PDF (1497K) -
Shizuya MAEKAWA, Kiyotoshi KATO1971 Volume 20 Issue 4 Pages 474-479
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid photometric method for the determination of 0.0010.1% of tin in iron and steel with salicylideneamino-2-thiophenol (SATP) has been established. The tin (II)-SATP complex was formed in a lactic acid medium at the pH range from 1.8 to 2.2, and the absorbance obeyed Beer's law up to 70 μg of tin. The complex was stable for at least 5 hours. The established method was as follows.
A half gram of sample was decomposed in a mixture of hydrochloric acid and hydrogen peroxide (30%) and boiled for 23 minutes. After cooling, it was diluted with water and the interfering iron (III) was masked by 5 ml of L-ascorbic acid solution (10%).The pH of the solution was adjusted to 1.82.2 with sodium hydroxide solution (10%) by using 2, 4-dinitrophenol as an indicator. To it were added 2 ml of lactic acid (20%), 2 ml of sodium thiosulfate solution (1%) and 5 ml of SATP solution (0.1%). It was allows to stand for 5 minutes, and shaken for 1 minute with 10.0 ml of benzene. The absorbance was measured at approximately 415 mμ against benzene.
The proposed method was very sensitive and simple, and the time required for an analysis was about 28 minutes.View full abstractDownload PDF (764K) -
Yosuke OHKURA, Kazuhiko MATSUMURA, Hiroshi HAMADA, Tsutomu MOMOSE1971 Volume 20 Issue 4 Pages 480-484
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDiazotized sulfamethizole was found to react sensitively and selectively with 2-oxogultaric acid to give a fairly stable red color in a sodium hydroxide solution in the presence of sodium sulfite and sodium hypophosphite. It was used as a new photometric reagent for the determination of the acid. The outline of the procedure was as follows.
To 1.0 ml of a test solution containing up to 50 μg/ml of 2-oxoglutaric acid add 1.0 ml of diazotized sulfamethizole solution (prepared by diazotizing 100 ml of 0.9% sulfamethizole solution in 6% hydrochloric acid with 10 ml of 2.5% sodium nitrite solution at 10°C) and 8 ml of an alkali reagent (8% sodium hydroxide, 1% sodium sulfite and 1.25% sodium hypophosphite as its monohydrate in water) by keeping the temperature of the solution at about 5°C, and mix. Warm the mixture at 37°C for 60 min, and then cool to room temperature. Measure the absorbance at 540 mμ against the reagent blank, and read the concentration of 2-oxoglutaric acid from a calibration curve, which is prepared by treating 2-oxoglutaric acid standard solutions (550 μg/ml) as described above. The calibration line is straight and passes zero. The absorbance given by 50 μg/ml of 2-oxoglutaric acid was 0.740.View full abstractDownload PDF (656K) -
Tsutomu TAKAHASHI1971 Volume 20 Issue 4 Pages 485-486
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSUsing electrodes of aluminum alloy, iron alloy and copper alloy, the relation of the composition of the electrode (in solid phase) and that deposited on anode surface after eroded by spark (in gaseous phase) were compared by using X-ray diffractive analysis.
The result indicated that the both phase were similar in crystalization, intermetallic compound etc., and that the erosion process of the electrode was the explosive eruption of vapour jet from the cathode.View full abstractDownload PDF (238K) -
Hiroshi ASAOKA1971 Volume 20 Issue 4 Pages 487-489
Published: April 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSPolarographic behavior of titanium in hypophosphorus acid supporting electrolyte has been studied in the view of determination of titanium. Titanium gave a well-defined diffusion-controlled wave in this medium. The log(i/id-i) vs. voltage diagram was linear, and its slope corresponded closely to a reversible one electron reduction. The half-wave potential was-0.27 V vs. S. C. E. and id/C·m2/3 ·t1/6 was 1.43 at 25°C in 1.2M hypophosphorus acid. A linear relationship was obtained between the diffusion current and the concentration over the range of 2.2 ×10-33.7 × 10-4M. The precision of the calibration curve for titanium as the standard deviation was 1.77% for concentration of 0.75 × 10-3M and 3.79% for 0.75 × 10-4M. Antimony (III) and molybdenum (VI) gave cathodic waves and interfered with the titanium determination. The interference from iron and copper was easily eliminated by boiling the solution with hydrochloric acid and potassium thiocyanate. Hypophosphorus acid as supporting electrolyte was thus especially useful for determination of titanium in the presence of large quantities of iron and copper.View full abstractDownload PDF (392K) -
Takeshi ISHII, Sôichirô MUSHA1971 Volume 20 Issue 4 Pages 489-491
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the atomic absorption spectrophotometric determination of zinc in commercial vulcanizates was established.
Zinc in commercial vulcanizates can be determined by atomic absorption measurement after extracting the sample in ethyl acetoacetate (EAA).Calibrating solutions can be prepared by dissolving commercially available zinc metal of special grade (purity 99.999%) in EAA.
The recommended conditions were : wavelength 2138Å, hollow cathode lamp current 15 mA, slit width 300 μ, air pressure 1.0 kg/cm2, and hydrogen pressure 0.5 kg/cm2.
The method is rapid and has accuracies nearly comparable to those attained by the conventional ashing method.View full abstractDownload PDF (427K) -
Takeshi ISHII, Sôichirô MUSHA1971 Volume 20 Issue 4 Pages 491-493
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSGas chromatographic analysis of benzene and toluene in automobile exhaust gas was studied by using Yanagimoto Gas Chromatograph Model GCG-550. The operating conditions were :
Column : PEG · 6000 30%
Carrier gas : Helium
Column temperature : 84°C
Detector : F. I. D.
The method was rapid and simple, and the time required for an analysis was about 15 min.View full abstractDownload PDF (539K) -
Spectrochemical analysis of titanium and its alloy. IVTetsuo MATSUMURA, Naomi KOTANI, Takeshi GOTO1971 Volume 20 Issue 4 Pages 493-495
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the previous work, the authors presented a method for the correction of interelement effects by using the mass absorption coefficients, but the result on aluminum was not satisfactory because of the low reliability of the coefficient for aluminum and the disregard of the enhancement effect.
In this report, the method using the absorption parameters developed by Adachi and Ito for steel analysis was applied successfully to the fluorescent X-ray determination of aluminum in titanium-base alloys. Appropriate correction factors for the effects of interelements on aluminum determination were given.
In the analysis of titanium-base alloys with various alloying elements, the corrected results agreed closely with those obtained by chemical analysis.View full abstractDownload PDF (322K) -
[in Japanese]1971 Volume 20 Issue 4 Pages 496-504
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2048K) -
[in Japanese]1971 Volume 20 Issue 4 Pages 505-514
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1506K) -
[in Japanese]1971 Volume 20 Issue 4 Pages 515-521
Published: April 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1284K)
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