All issues
Volume 11, Issue 4
Displaying 1-23 of 23 articles from this issue
- |<
- <
- 1
- >
- >|
-
Iodine-azide reaction and its application to quantitative micro-analysis. VIII.Shin SUZUKI, Tetsumasa ISHIDA1962 Volume 11 Issue 4 Pages 377-384
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSWhen iodine-azide was added to the insufficiently buffered thiourea solution, the pH was lowered showing a distinct shift. The cause of this phenomenon was persued and the results indicated that this was not due to the absorption of carbon dioxide by the solution nor to the dilution by the additional solution, but to the chemical reaction itself between thiourea and iodine-azide. The more extensive studies led to the conclusion that the pH lowering was attributable to iodine, not to sodium azide in the reagent.
The studies were furthermore extended, where by several kinds of thiourea solutions, in which thiourea concentration and pH were the same but the sorts and amounts of buffering agents contained were different each others, were prepared and variations of pH of these solutions with the addition of iodine-azide or the related solutions were estimated.
The results were summarized in several graphs, which indicated that even though the pH of thiourea solutions were all the same before the titration, the pH change during or after the titration were not always same, depending on how the pH of thiourea solution was initially adjusted. Accordingly, the notice must be taken of this point, if this method would be about to be applied for analysis of thiourea under the fixed condition of pH.View full abstractDownload PDF (1359K) -
Influence of titrating speed of iodine-azide solution upon the results of the iodine-azide titrationIodine-azide reaction and its application to quantitative micro-analysis. XIShin SUZUKI1962 Volume 11 Issue 4 Pages 384-388
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSSince the iodine-azide reaction was considered as one of catalytic reactions, the titrating speed by iodine-azide was assumed to influence with the result of the analysis using this reaction. The detailed experiment was performed on thiourea and iodine-azide, and the result indicated that as far as the titrating speed was quite large, the linearity was maintained between the titer of iodine-azide solution and thiourea content.
However, if the titrating speed was too low, the calibration curve deviated from the linear relation. A general equation of titrating curve indicating the relation was derived from the theoretical base.View full abstractDownload PDF (769K) -
Kimio MUKAEWAKI1962 Volume 11 Issue 4 Pages 388-393
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn absorptiometric aluminon method for the determination of beryllium in iron and steel has been presented by separating beryllium from ironetc. with sodium hydroxide solution and hydrogen peroxide mixture and masking the interfering elements as aluminum etc. with EDTA.
The recommended procedure is as follows : Weigh 2g sample into a 500ml flask, dissolve with 20ml of a mixed acid (HCl 1+HNO3 1) and successively with 30ml of perchloric acid, evaporate to fumes of perchloric acid, oxidize chromium to dichromate, allow to cool down to room temperature, and add approximately 50ml of water to dilute to the mark. Pipet 120ml from this solution into the mixture of 30ml of hot sodium hydroxide solution (25%) and 5ml of hydrogen peroxide (3%), transfer the solution to a 100ml. Volumetric flask after boiling for 3 min., dilute to the mark, and filter with a dried filter. Pipet 50ml from the filtrate into a 100ml beaker, just neutralize it with hydrochloric acid (1+1) and add excessive 0.25ml.
Transfer the solution to a 100ml volumetric flask, cool, add 3ml of EDTA solution (2.5%) and 15ml of aluminon-buffer solution (0.1%) with 1ml of gum arabic, and immerse the whole in boiling water for 4 min. Cool down to room temperature, dilute to the mark with water, and measure the absorbance with filter S 53. A blank test using the pure iron is followed by the same procedure. Calculate the difference of the absorbances and determine the amount of beryllium from the calibration curve.
The time required for an analysis was about 2530 min.
In addition, as compared with the aluminon method, the Eriochrome cyanine R method and the Qinalizarin method improved by the author, Eriochrome cyanine R method was found to be better than the others on the rapidity and sensitivity, although this method required more or less skill to control pH of the solution. The aluminon method was found to have an advantage in the simplicity of operation and the lower blank absorbance.View full abstractDownload PDF (1020K) -
Polarographic study of chloranil and its related compounds. III.Yasuhisa MIZUNOYA1962 Volume 11 Issue 4 Pages 393-395
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe author had revealed in the preceding study that chloranil was determined satisfactorily by the polarography in 50% alcohol solution at pH 3.4 using N/10 potassium nitrate as a supporting electrolyte. The principle was applied for the determination of salicylic acid which can be oxidized quantitatively to chloranil.
The author recommended a method in which the chloranil derived from salicylic acid by potassium chlorate-hydrochloric acid oxidation was extracted with ether and was determined by the polarographic method. This offers an easy and accurate means for the determination of salicylic acid.
The method was applied practically to the determination of salicylic acid in 4% acetic acid solution (vinegar).View full abstractDownload PDF (548K) -
Polarographic study of chloranil and its related compounds. IVYasuhisa MIZUNOYA1962 Volume 11 Issue 4 Pages 395-396
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSPentachlorophenol was oxidized to chloranil with potassium chlorate and hydrochloric acid as in the cases of phenol and salicylic acid as in the preceding studies. But chloranil was quantitatively obtained as a stable end product from pentachlorophenol by the oxidation with nitric acid instead of potassium chlorate and hydrochloric acid.
The author recommended a method in which the chloranil derived from pentachlorophenol by nitric acid oxidation was extracted with ether and was determined by the polarography in 50% alcohol solution at pH 3.4 using N/10 potassium nitrate as a supporting electrolyte.View full abstractDownload PDF (323K) -
Sublimatographic separation of mixed system. I.Kiyoshi YOSHIMURA1962 Volume 11 Issue 4 Pages 397-400
Published: April 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSV. C. P. in sublimatography was studied to establish the sublimatographic separation of mixed systems. When sublimed vapor condensed and crystallized on the wall of a glass tube with temperature gradient, a certain critical point of condensation had been obtained. The ratio γ=Ph/Pc, where Ph was the pressure of vapor phase and Pc. was the saturated vapor pressure at the critical point temperature had a significance and showed a characteristic value for each substance.
The mean values of γ for mercuric chloride, mercuric bromide, mercuric iodide, stannic iodide, arsenic trioxide and phosphorus pentoxide were 1.50, 1.40, 1.72, 1.42, 1.79 and 1.99, respectively.View full abstractDownload PDF (683K) -
Sublimatographic separation of mixed system. II.Kiyoshi YOSHIMURA1962 Volume 11 Issue 4 Pages 400-406
Published: April 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSIn order to examine the effect of vapor flow on the V. C. P. in sublimatography, fundamental experiments were carried out on two methods (effusion method and direct method).
The relation between the vapor flowF (mol/sec) in the glass tube with temperature gradient and the V. C. P. was studied and an empirical formula (γPs)n=k' · F was obtained, where γ was Ph/Ps with Ph : pressure of vapor phase and Ps : saturated vapor pressure at the temperature of V. C. P., and F was a value concerning with the heating temperature of the substance th.
From the relations, it is evident that V. C. P. depends upon th, and under a fixed condition, the position where the substance condenses in the tube with temperature gradient is determined by th.
The possibility of separation of any mixture will be presumable from the th-V. C. P. curve for each component in the mixture.View full abstractDownload PDF (1024K) -
Generalized method for determination of nonmetallic elements in inorganic materials. I.Nakaaki ODA, Masaji KUBO1962 Volume 11 Issue 4 Pages 406-411
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA generalized method for the determination ofC, H, N, S, and X (halogen) in inorganic compounds has been investigated, whereby the authors aimed to estimate these nonmetallic elements simultaneously under the same procedure.
Based on the surveying of the present methods of elementary analysis anddetailed investigation thereof, the authors selected and constructed a procedure in which the samplewas incinerated at high temperature in the presence of decomposition catalysts and the volatilized nonmetallic elements were converted into their weighing forms and estimated (Table I, II).
An apparatus for the decomposition and the determination was presented (Fig. 1).View full abstractDownload PDF (1229K) -
Generalized method for determination of nonmetallic elements in inorganic materials. II.Nakaaki ODA, Masaji KUBO1962 Volume 11 Issue 4 Pages 411-415
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe generalized method for determination of C, H, N, S and X presented in the preceding report was applied for many inorganic compounds and their mixtures, and satisfactory results were obtained except for several alkaline earth sulfates.
Based on the further investigations on the conditions for decomposition and determination, the authors recommended a method as follows : For the determination of C, H, S and X, the sample (3050 mg) was heated at 1000°C (or at 1300°C provided that the sample contained alkaline earth sulfate) with an addition of 500 mg WO3 in the current of oxygen, and the C, H, S, and X were converted into CO2, H2O, SO3, and X2, respectively, by use of a platinum catalyst, and each of them was determined by gravimetry. The N in sample was converted into N2 in the presence of CuO-Cu under CO2 current, and determined directly by gas volumetric method.
The error in the proposed method for each element was within±0.5%, and the lower limit of determination was around 1%.View full abstractDownload PDF (924K) -
Gaschromatographic determination of carbonyl compounds by pyrolysis of 2, 4-dinitrophenylhydrazones.Sueo NISHI1962 Volume 11 Issue 4 Pages 415-420
Published: April 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSC2C6 Carbonyl compounds were regenerated quantitatively from 2, 4-dinitrophenylhydrazones by heating with dicarbonic acids. The regeneration reaction was carried out in a glass tube attached to gaschromatography unit (see Fig. 1), and the liberated carbonyl compounds were carried directly into the column. Among dicarbonic acids studied, ο-phthalic acid, α-ketoglutaric acid, glutaric acid etc. had an excellent property in liberating carbonyl compounds on heating with 2, 4-dinitrophenylhydrazones.
However, α-ketoglutaric acid and glutaric acid produced volatile products on heating alone at 250°C, and disturbed base line (see Fig. 2). On the other hand, ο-phthalic acid produced no volatile material except water, which could be eliminated by fixing on calcium chloride, and regenerated carbonyl compounds in good yield from 2, 4-dinitrophenylhydrazones.
The ratio of ο-phthalic acid to the hydrazones should be more than 10 (see Fig. 3). Carbonyls were completly recovered in the case of n-butyraldehyde and methylethylketone. Formaldehyde was detected but not determined quantitatively. Aqueous solutions of carbonyl compounds (concentrations less than 1%) were analyzed quantitatively by this technique in good accuracy (see Table V).View full abstractDownload PDF (1101K) -
Determination of trace of impurities in uranium metal. XVIII.Iwao FUJISHIMA, Tsugio TAKEUCHI1962 Volume 11 Issue 4 Pages 420-425
Published: April 05, 1962
Released on J-STAGE: January 15, 2010
JOURNAL FREE ACCESSA method suitable for the routine determination of total carbon in uranium metal, titanium metal and steel has been presented, in which 90 μg to 500 μg of carbon is determined within 8 minutes.
The precisions attained by the following method are 2.2 μg, 4.9 μg, 4.7 μg, 4.7 μg and 7.4 μg in terms of standard deviation based on 93 μg, 190μg, 286Pμg, 385μg and 484μg of carbon, respectively.
The sample is burnt in an oxygen stream and the resulting CO2is absorbed in an absorber, containing 100mlof an absorbing solution and finely powdered BaCO3under vigorous agitation. The absorbing solution consists of 1-liter of N/1200 Ba(OH)2 and 1ml of iso-amyl alcohol as the surfactant.
The CO2absorbed is determined by using a high-frequency submersion type condenser electrode and a 30 mega-cycle oscillator.
The apparatus has been described and illustrated.
Analytical results on uranium metal, titanium metal and steels are given.View full abstractDownload PDF (1105K) -
Studies on polarography with organic solvent extraction method. I.Michihiro ISHIBASHI1962 Volume 11 Issue 4 Pages 426-431
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSMicro-determination of metals by diethyldithiocarbamate-chloroform extraction with subsequent polarography was investigated. The extraction of Tl (I), Tl (III), Pb, Cd, and Bi was examined in the presence of the masking agents such as EDTA or KCN and buffering agents such as Na-tartrate, Na-citrate, Na-phosphate or glycine. The metals were extracted from the solution of pH 213, the chloroform extracts were evaporated with mineral acid to syrup or to dryness, but not to carbonization of organic substances, and the metals in the residual solution were determined polarographically after the addition of suitable supporting electrolytes.
The masking effects of EDTA on the extraction of Tl (III) and Bi were not recognized and pH range for the quantitative extraction of them were 213. On the contrary, the masking effects of EDTA on the extraction of Tl (I), Cd and Pb were obvious, while the pH range for the quantitative extraction of them were considerably restricted as follows ; Tl (I) between Cd between and Pb between 45.
By the use of EDTA solutions containing the buffering agents, the pH range for the quantitative extraction of Tl(I) and Cd, was the same as those in case of the absence of buffering agents, or varied within pH 1.5. Meanwhile the reco-veries of Pb were lowered to 5075 per cent of the amounts added, even at its optimum pH value of 4, probably owing to the multiple effects. of EDTA and Na-citrate or Na-tartrate.View full abstractDownload PDF (863K) -
Kiyosi FUKUI, Hideo NAGATOMI, Saburo MURATA1962 Volume 11 Issue 4 Pages 432-434
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSIn order to determine fatty acids directly by gas-liquid chromatography, stearic acid and sebacic acid have been used conventionally as the column material.
In the authors studies however, an innegligible evaporating loss of these acids from column was observed. This caused the gradual changes in retention time and separation effect and made these acids unsuitable for the purpose.
The authors tried to use the high-boiling and low-melting behenic acid as a column material. G. Raupp's column packing with 85 parts dioctyl sebacate and 15 parts sebacic acid on 3 times quantity of celite 545, was modified, and the column packed with 1 part dioctyl sebacate and 1 part behenic acid on 3 times quantity of celite 545 was recommended. The column temperature was maintained at 150°C, and the flow rate of carrier gas (He) was adjusted to 40 ml/min.
The mixture of water, formic acid, acetic acid, n-propionic acid, iso-butyric acid, n-butyric acid, iso-valeric acid, crotonic acid, n-valeric acid and n-capronic acid was separated into each component completely, and no evaporating loss of behenic acid from column was observed after 70 hours.View full abstractDownload PDF (434K) -
Wataru FUNASAKA, Tsuguo KOJIMA, Genji TAKESHIMA, Jitsumi KIMOTO1962 Volume 11 Issue 4 Pages 434-437
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSAn anion exchange chromatographic procedure has been presented for the determination of small concentrations of trimesic acid(TMA), p-toluic acid(PTA), and p-carboxyl benzyl alcohol (PCBA) in terephthalic acid(TPA).
In the separation of TMA and TPA, the sample is placed on an Amberlite IR-45 (R-Cl, 100200 mesh) column of 175 mm in length and 8 mm in diameter, and the elution is carried out with a methanolic solution of NaCl containing5030% water.
PTA, PCBA, and TPA are separated from each other by the stepwise elution with a methanolic solution of NaCl containing 3070% water. The acids in each effluent are determined by u. v. spectrophotometry.
From 0.8 to 2% of TMA or PTA in TPA can be determined by this method within a deviation of 0.1%.View full abstractDownload PDF (637K) -
Application of ethylenediaminetetraacetic acid to the determination of metal.IShigehiko HAYASHI1962 Volume 11 Issue 4 Pages 438-442
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSThe optimum pH giving the quantitative reduction of molybdenum with zinc amalgam in the presence of EDTA and tartrate was sought, and it was found that molybdenum could be reduced quantitatively to the tervalent state at pH 4.0 and 5.0 by shaking with the reagent for 2 min. After an addition of sodium hydroxide solution to the reduced solution, molybdenum was determined by titration with a standard potassium ferricyanide solution using indigocarmine as an indicator.View full abstractDownload PDF (893K) -
Studies on the polarographic analysis. XXXXITaitiro FUJINAGA, Kazuyoshi HAGIWARA1962 Volume 11 Issue 4 Pages 442-447
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSA series of supporting electrolytes was examined Table I Determination of Mn in Fe alumfor the determination of trace amount of manganese by the square-wave polarography, whereby triethanolamine in alkaline media was found the most adequate. From the result of fundamental experiments, the following procedure has been recommended : to a sample solution containing 1.122 μg of Mn is added triethanolamine and potassium hydraxide until their final concentrations in the electrolysis solntion reach 0.2M and 0.5M, respectively.
Air is passed through the solution heated in a boiling water-bath for about twenty minutes. The solution of manganese ions oxidized to +3 state produces a sharp reproducible wave at a peak potential of -0.5 volt vs. S. C. E. in the square-wave polarogram.
A linear relationship hold over the concentration range from 2×10-5 to 1×10-6M of manganese in the solution.
Only copper ion when present more than 1×10-5M intereferes with the determination.
The present method was applied to the determination of a trace amaunt of manganese (of the arder af 0.005%) in reagent grade ferric alum and a satisfactory agreement was obtained with the value by the spectrophotometric method.View full abstractDownload PDF (726K) -
[in Japanese], [in Japanese], [in Japanese]1962 Volume 11 Issue 4 Pages 448-449
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese]1962 Volume 11 Issue 4 Pages 449-451
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (489K) -
[in Japanese], [in Japanese]1962 Volume 11 Issue 4 Pages 451-453
Published: April 05, 1962
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese], [in Japanese]1962 Volume 11 Issue 4 Pages 453-454
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese]1962 Volume 11 Issue 4 Pages 454-458
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese], [in Japanese]1962 Volume 11 Issue 4 Pages 459-472
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (2679K) -
[in Japanese]1962 Volume 11 Issue 4 Pages 473-480
Published: April 05, 1962
Released on J-STAGE: May 29, 2009
JOURNAL FREE ACCESSDownload PDF (7576K)
- |<
- <
- 1
- >
- >|