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Volume 20, Issue 5
Displaying 1-17 of 17 articles from this issue
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Isao TAKEMURA1971 Volume 20 Issue 5 Pages 531-534
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe author had previously pointed out a linear relationship betweeen logarithmic relative retention value of isothermal gas chromatography and relative retention value of programmed temperature gas chromatography, and discussed on some factors determining the gradient of the linearity.
This paper was subjected to the comparisons of the retention values on polar and nonpolar liquid phases using Apiezon L, Silicone SE-31, polydiethyleneglycol-succinate and Carbowax 20M coated on 60/80 Celite 545. The linear relationship was acertained in every case, but the linearities on nonpolar liquids were more distinct than those on polar liquids. And the nonpolar solutes with low by deviated from the linearities on polar liquids. These results could be easily explained with the general liquid phase theory.View full abstractDownload PDF (546K) -
Keiichi FURUYA, Kazuyoshi FUJIMURA, Chikao TSURUMI1971 Volume 20 Issue 5 Pages 535-541
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA spectrophotometric method for the determination of tantalum, based on ion exchange extractions of the associated ions in high alloy steels using high molecular weight amine-benzene solution (Amberlite LA-2), is described.
The behaviors of the tested ions are investigated for the various extractants, hydrofluoric acid-hydrochloric acid solutions (Table I, Fig. 2, and Fig. 3).
The main procedure of the recommendation for the determination is as follows:
Dissolve 1g of high alloy steel with aqua regia and hydrofluoric acid and dilute the solution to 100ml. Shake an aliquot of the solution with 50ml of 1F HF-0.1F HCl and 25ml of Amberlite LA-2-benzene solution. The organic layer is shaken with 50ml of 0.5F HF-3F HCl and 50ml of 0.5F HF-0.5F HCl, successively, to eliminate interfering ions.
Back-extract tantalum in the aqueous phase with 1F NH4F-4F NH4Cl. Add 0.5ml of 1.5F NH4OH, 10ml of (NH4)2SO4 (0.45g/ml) and 3ml of H2SO4 (1:1), 7.5ml of Malachite Green solution (0.2%). Extract the complex with 25ml of benzene after standing for 5min. After 7min, the absorbancy at 630mμ is measured.
A synthesized and three steel samples were analyzed.View full abstractDownload PDF (1009K) -
Giichi SAITO, Katsuko SUGIMOTO, Ken HAGINO1971 Volume 20 Issue 5 Pages 542-549
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the presence of concentrated sulfuric acid, the heat of dilution of sulfuric acid has a great influence on the reaction of nitrate with brucine producing soluble yellow compounds. So that, in an ice-water bath, sulfuric acid has been added to the reaction contents in a vessel which is afterwards heated for 40 minutes at 60°C. This color reaction proceeds gradually also at a room temperature, so the contents are cooled in a running water after heating followed by the measurement of the absorbance at 405mμ. Beer's law holds in a concentration region 0.052.5 ppm of NO-3 -N and a minute quantity of nitrate ion can be determined with satisfactory reproducibility. In the case of nitrite, the color develops also in the presence of perchloric acid or hydrochloric acid, but, for obtaining the linear relationship, the coexistence of moderate amounts of sulfuric acid and perchloric acid is indispensable whereby Beer's law holds for 0.28.0 ppm NO-2 -N.
Determination of a minute quantity of nitrate ion in the presence of nitrite is also studied.
Nitrate and/or nitrite ion in natural waters could be determined with satisfactory results by the proposed method.View full abstractDownload PDF (1175K) -
Isamu TSUBAKI, Tsutomu NAKANISHI1971 Volume 20 Issue 5 Pages 549-551
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSChloride, bromide and iodide were oxidized respectively by fusion with vanadium (V) oxide to liberate gases of halogens identifiable by their colors. Bromide and iodide were oxidized to halogens by fusion with sodium hydrogen sulfate, and only iodide was oxidized to iodine by fusion with boric acid. By combining these three tests, a halide was identified solely by dry method.View full abstractDownload PDF (434K) -
Takatoshi KONO1971 Volume 20 Issue 5 Pages 552-557
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDetermination of tin was done by atomic absorption spectroscopy combined with MIBK extraction, and measuring conditions for air-acetylene flame method and nitrous oxide-acetylene flame method were examined.
More than 99% of tin was extracted with MIBK from the mixed acid 3.5N HCl, 7N H2SO4 solution without an interference from 1000ppm iron. By the aid of MIBK extraction, the determination of 20ppm of tin in aqueous solution was sensitized threefold. The sensitivity by the use of N2O-acetylene flame was 0.5μg/ml/1% and nine times as high as that by the conventional procedure, provided that 1.8kg/cm2 (5l/min) of N2O and 0.5kg/cm2 (4l/min) of acetylene were used and the beam was 7mm higher than the burner top.
The method was applied to the determination of tin in aluminum alloy, zinc die cast and cast iron.View full abstractDownload PDF (921K) -
Studies on analysis of rare earths. IIIMatsuji SATO, Susumu KODAMA, Norihisa MORI1971 Volume 20 Issue 5 Pages 557-561
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSStoichiometric reduction of europium (III) to europium (II) was achieved by liquid zinc amalgam in hydrochloric acid solution, and two titrimetric methods were proposed. Method I (conventional procedure) titrated Eu (II) with ferric chloride solution, and method II (standard procedure) replaced Eu (II) with Fe (II) and titrated it with potassium dichromate solution. The recommended procedures are as follows.
Dissolve a sample containing 100200mg of Eu2O3 in 10ml of hydrochloric acid (1:1). Transfer the solution with 50ml of water into a reductor (modified by the authors) whose amalgam receiver is filled with deoxigenated water, and add 15ml of zinc amalgam. Shake the reductor vigorously for 5min. to reduce europium (III), and replace amalgam with water. (Method I) Add ammonium thiocyanate and titrate with 0.05N ferric chloride standard solution. (Method II) Add 15ml of deoxygenated solution of ca. 0.1N ferric chloride and 5ml of phosphoric acid (1:1) to replace europium (II) with iron (II). Add diphenylamine-p-sulfonic acid and titrate with 0.05N potassium dichromate standard solution.
In the method I, the ferric chloride solution was to be standardized against europium oxide before the analysis, because the titration factor of the ferric chloride standard solution was the sum of oxidizing power of iron (III) and dissolved oxygen. By the method II was carried out a reliable determination of europium because the influence of dissolved oxygen was negligibly small.
Coefficients of variation for the method I and the method II for 80% contents of europium oxide were 0.17% and 0.11%, respectively.View full abstractDownload PDF (915K) -
Analytical studies on pesticides and related compounds. IVAtsushi MURANO1971 Volume 20 Issue 5 Pages 561-565
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAnalytical methcd for the determination of o-sec-butylphenyl N-methylcarbamate (BPMC) by thin layer chromatographic separation and bromometric titration has been developed. A sample solution of BPMC was applied to a silica gel plate and developed with n-hexane-ethylacctate-formic acid (80:20:1). The portion of silica gel corresponding to the Rf-value of BPMC was scraped from the plate and transferred to a 500ml iodine flask. BPMC was hydrolyzed to o-sec-butylphenol (OSBP) with potassium hydroxide solution, acidified with acetic acid and hydrochloric acid and brominated under cooling with ice. The excess bromine was replaced by iodine by addition of potassium iodide and titrated with 0.02N sodium thiosulfate solution. OSBP and bromine reacted in sulfuric acid solution to form 2-sec-butyl-4, 6-dibromophenol (IIa). In hydrochloric acid solution, Br of IIa was further replaced by Cl and majority of IIa was changed to IIb, IIc and IId, but it did not interfere with the determination of BPMC because the equivalent amount of bromine consumed did not vary. The results obtained for standard and technical samples of BPMC were accurate, precise and in excellent agreement with those obtained by TLC-UV method already reported.View full abstractDownload PDF (768K) -
Analytical studies on pesticides and related compounds. VAtsushi MURANO, Masayuki NAGASE, Setsuo YAMANE1971 Volume 20 Issue 5 Pages 565-569
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAnalytical methods have been developed for thedetermination of Salithion (2-methoxy-4H-1, 3, 2- benzoxyphosphorin-2-sulfide) by using thin layer chromatography and gas chromatography. An acetone solution of Salithion was applied to silica gel plate, developed with n-hexane-benzene (1+1), eluted with methanol and heated for 15minutes at 4555°C with added sodium hydroxide solution. Saligenin produced was then colored with potassium ferricyanide and 4-aminoantipyrine at pH 8.2 and spectrophotometrically determined from its absorbance at 505mμ.
Alternatively, gas chromatographic determination of Salithion was performed on a gas chromatograph equipped with a hydrogen flame ionization detector. The operating condition was as follows. Column: 1.5m×3mm made of pyrex; column package:6080 mesh, acid-washed, silane-treated Chromosorb W coated with 2% LAC-2R-446; column temperature: 165°C; carrier gas: nitrogen 25ml/min; and internal standard: benzylbenzoate.
The analytical results by both methods agreed on technical products of Salithion. Standard deviations for TLC method and GC method were 0.32% and 0.80%, respectively. The latter was more simple and rapid.View full abstractDownload PDF (732K) -
Shigeru TAGUCHI, Mitsuhiko TAGA, Hitoshi YOSHIDA, Seiichiro HIKIME1971 Volume 20 Issue 5 Pages 570-574
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSHydrolysis of urea with urease was applied to the precipitation of Mn (II)-oxinate from homogeneous solution and the optimum conditions for the quantitative precipitation of the oxinate were determined.
To the solution containing 650mg of manganese (II) were added 100mg of ascorbic acid, 1ml of 10% citric acid, 50ml of 20% urea solution and an alcoholic solution of oxine in 20% excess. The pH of the solution was adjusted to 5.0 with ammonia water and then 0.3mg of urease was added to the solution. The mixture was kept at 35°C for 610hours in a thermostatic water bath. The precipitate formed was filtered, washed, dried at 170°C for one hour, and weighed as Mn (C9H6ON)2.
It was found that urease was co-precipitated almost completely with manganese oxinate. Manganese was determined with satisfactory result by deducting the weight of urease used from the weight of the precipitate.View full abstractDownload PDF (1031K) -
Tsunenobu SHIGEMATSU, Yasuharu NISHIKAWA, Keizo HIRAKI, Shiro GODA, Yo ...1971 Volume 20 Issue 5 Pages 575-581
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCerium in sea-water was determined by the Ce (IV)-Ce (III) fluorometric method.
Into 20l of sea-water were added 100ml of conc. HCl and 50mg (30mg, 10mg, 10mg) of Fe3+ as FeCl3 solution, and pH of the solution was adjusted to 99.5. After standing overnight, the precipitate was filtered and dissolved in 40ml of 6N HCl. Fe3+ was extracted with 40ml of MIBK, and the aqueous phase was evaporated to dryness with 3ml of 70% HClO4. The residue was treated with 10ml of 0.002N HClO4, poured on the column (HDEHPPVC column) and eluted with 0.3N perchloric acid solution (flow rate: 1ml/min). The cerium fraction of the eluant (50100ml) was decomposed with HClO4 and evaporated again to dryness. The residue was dissolved with HClO4 to make the final perchloric acid concentration 0.7N. The solution was transfered to a 25ml volumetric flask with 500μg of Ti3+, and was diluted to the volume with water. The fluorescence intensity of the solution was measured at 350nm with excitation at 255nm. In this procedure, the recovery of cerium was about 90%.
Cerium in sea-water collected at offshore of Dorinzawa, Tokyo and Shirahama, Wakayama was found to be 25×10-3μg/l.View full abstractDownload PDF (1047K) -
Setsu KOBAYASHI, Takuji KANNO1971 Volume 20 Issue 5 Pages 582-589
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA study was made on the spectrometric determination of micro-amount of titanium, zirconium and hafnium by the spark-in-spray method, in which the sample solution were atomized into the spark gap between carbon electrodes. The atomizer used was of a flame photometer.
Spectral line pairs, Ti II 3349.035Å/La II 3949.106 Å, Zr II 3391.975Å/La II 3949.106Å and Hf II 2641.406Å/Al II 2669.166Å were used respectively for the determination of titanium, zirconium and hafnium.
The most sensitive line for hafnium, Hf II 3134.719 Å was inavailable for the determination of hafnium in the solution containing zirconium, because it overlapped on the broad slope of the line, Zr II 3133.475Å.
The detection limits and the coefficients of variation are as follows: 0.03μg Ti/ml and 4.6% for 0.4μg Ti/ml level, 0.06μg Zr/ml and 3.2% for 20μg Zr/ml level, and 6μg Hf/ml and 4.4% for 33μg Hf/ml level.
The method was applied successfully to the determination of titanium in steel and hafnium in zircon.View full abstractDownload PDF (1154K) -
Shoji MOTOMIZU1971 Volume 20 Issue 5 Pages 590-595
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe extraction of cobalt into organic solvents was studied by using 6-nitroso-3-dimethylaminophenol (I), α-nitroso-βnaphthol(II), 1-nitroso-2-hydroxy-3- naphthoic acid (III) and 1-nitrosc-2, 7-dihydroxynaphthalene (IV).
The reagents (I), (III) and (IV) were suitable for the extraction with the solvents having relatively high dielectric constant, while the reagent (II) was suitable for that with the solvents having lower dielectric constant. When cobalt and the reagent (III) were shaken with a non-polar solvent, red precipitate appeared on the boundary of organic and aqueous phases. It was extracted into the organic phase (benzene, toluene, chloroform etc.) by an addition of quaternary ammonium salts, such as zephiramine.
The optimum pHs for the extractions were 6.8, 4.5 and 5.5 for the reagents (I), (II), (III) and (IV), respectively.
The calibration curves at their maximum absorption wave-lengths followed Beer's law. The apparent molar absorptivity of the complex(I) in the organic phase was the highest and the value was about 5×104, which was 1.52times those of other reagents. Consideration of the other factors including shaking times and the stabilities of the reagent and the complex also showed that the reagent (I) was the most useful. In this case, 1, 2-dichloroethane was recommended as the extracting solvent.View full abstractDownload PDF (835K) -
Determination of oxide inclusion in copper-base alloys. VIwao TSUKAHARA1971 Volume 20 Issue 5 Pages 596-601
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTwo methods, methanolic bromine method and acid decomposition method, for the determination of nickel oxide inclusion in Cu-Ni alloy have been presented. The effects of decomposition temperature, decomposition time etc. on the recovery of nickel oxide have been studied. The oxygen content calculated from the content of the inclusion was compared with that determined by vacuum fusion method, and the structure of nickel oxide inclusion isolated as the decomposition residue was discussed. The recommended procedures are as follows.
(1) Methanolic bromine method: 25g of Cu-Ni alloy is dissolved with methanolic bromine (150ml of methanol+15ml of bromine) in a decomposition flask at 3035°C for about 20hr. The solution is filtered through a filter paper. The residue is washed with methanol, ignited in a platinum crucible and fused with 58 g of potassium pyrosulfate. The melt is leached with water. The solution is made up to 100ml with water, and to its aliquot containing 5 100μg of Ni is added 10ml of 30% ammonium citrate solution. The pH is adjusted to 8.59.5 with ammonia. It is transferred into a separatory funnel, and 1.0ml of 1% dimethylglyoxime solution is added. The solution is shaken vigorously with 10.0ml of chloroform for 1min. The absorbance of the chloroform layer at 375mμ is measured against pure chloroform. The amount of Ni is determined by referring to the calibration curve.
(2) Acid decomposition method: 25g of Cu-Ni alloy is decomposed with 50ml of HNO3 (1+1) in a 200ml beaker at 35°C or below. The solution is filtered through a filter paper. The residue is washed with water and treated in accordance with the above mentioned procedure (1).View full abstractDownload PDF (951K) -
Tetsuo MATSUMURA, Mitio TAKAHISA, Muneharu TAKIZAWA, Satoshi KITAMURA1971 Volume 20 Issue 5 Pages 601-606
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSParallel examinations were done on the fluorescent X-ray spectrometric determination of iron and manganese in button ingots and forged blocks of titanium metal to know the effect of metallurgical history on X-ray measurement, the limit of detection and the range of inner- and inter-laboratory errors. By using the working curves established, the standard deviations of the analytical values were 0.003% and 0.0007%, respectively, for 0.0050.329% of iron and 0.0010.075% of manganese. The lower limits of detectionof iron and manganese were, respectively, 0.0026% and 0.0007%. The precision and accuracy of the result were higher than, or at least comparable to, those of the conventional chemical analysis. Discussions were given on the influence of Cr on X-ray intensities of MnKα line and also on the effect of metallurgical history of the specimens.View full abstractDownload PDF (933K) -
Kazuyoshi MATSUNAGA1971 Volume 20 Issue 5 Pages 606-610
Published: May 05, 1971
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and rapid method was presented for the colorimetric determination of sodium cyclohexyl sulfamate (sodium cyclamate) in food products.
Sodium cyclamate was found to give cyclohexylamine by the reaction with dimethylsulfoxide in an H2SO4-acidic medium and the reaction was applied to its determination as follows.
Three milliliters of dimethylsulfoxide and 0.5ml of 0.5N sulfuric acid were added to the test solution, and the mixture was heated in boiling water for 60 minutes. After beeing cooled, it was neutralized with sodium hydroxide. It was then brought to pH 12.0 with a buffer solution and shaken with chloroform. The extract was washed with Kolthoff's buffer solution (12.0), and ethanol and quinhydrone were added. The mixture was warmed, and its absorbancy was read at 495mμ.
The standard deviation of the result was 15.5ppm and the coefficient of variation was 2.5%.View full abstractDownload PDF (627K) -
Tsunetoshi KAITO, Kazuhiko SAGARA1971 Volume 20 Issue 5 Pages 610-614
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn ultraviolet spectrophotometric method has been proposed for the determination of dl-methylephedrineHCl (MEP) in pharmaceutical preparations. MEP is quantitatively oxidized with K3Fe(CN)6 in an alkaline solution to benzaldehyde having an absorption maximum at 241nm. The oxidation product represents an increase in sensitivity of approximately 68 fold over the absorbance obtained by the ultraviolet determination of MEP.
In this method, MEP is determined without aninfluence of cphedrine-HCl 3times against it at 25°Cand 10times at 20°C. The analytical procedure is as follows.
Transfer 2ml of the test solution containing 120mg of MEP into a centrifuge tube. Add 2ml of 3% K3Fe(CN)6 solution and 3ml of pH 10 buffer solution (0.05M Na2CO3-0.05M Na2B4O7), and stand for 60minutes at 25°C. Add 1ml of 20% HCl and 20mlof n-hexane and shake for 1minute. Separate the n-hexane layer. Determine the absorbance of the n-hexane extract at 241nm (AT) against the reagent blank. At the same time, determine the absorbance of the standard solution (AS). Calculate the amount of MEP by AT /As. The influences of other compounds are examined, among which acetaminophen, acetanilide, phenacetin, ethoxybenzamide, aspirin, sulpyrin etc. interfered considerably. In order to remove these ingredients, the test solution is prepared as follows.
Transfer 40ml of the sample solution containing 6mg MEP into a column of cation exchange resin (Amberlite CG50 NH4 type, 5cm×1cm i. d.) and pour 150ml of water. Then elute MEP with 90ml of 0.1N HCl and after adjusting pH to 10 with 2N NaOH solution, make up exactly to 100ml with water.View full abstractDownload PDF (758K) -
[in Japanese], [in Japanese]1971 Volume 20 Issue 5 Pages 615-628
Published: May 05, 1971
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2305K)
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