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Volume 14, Issue 5
Displaying 1-20 of 20 articles from this issue
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Yusuke UJIHIRA1965 Volume 14 Issue 5 Pages 399-403
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe carrier precipitation of microgram quantities of gold, silver, mercury, palladium, copper, cobalt and zinc were investigated using dithizone as a collector. A single precipitation of dithizone gathered gold, silver, mercury, palladium and copper completely from diluted nitric hydrochloric, or sulfuric acid solution.
Cobalt and zinc were collected almost quantitatively at pH 89. The presence of complexing agents, however, decreased the carrier precipitation of these elements. The metal chelates extracted well into dithizone-CCl4 (or -CHCl3) were always carried down efficiently with 5 mg of dithizone.
The percent of recovery vs. pH relationship was quite similar as was observed for solvent extraction. The precipitates of dithizone were readily decomposed by the ignition or the wet ashing with nitric and perchloric acids. The information derived from these experiments were applied to the separation and determination of trace gold in copper, iron, lead, manganese, nickel and zinc.View full abstractDownload PDF (857K) -
Toshio SAWADA, Sakae KATO1965 Volume 14 Issue 5 Pages 404-409
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe mechanism and the rate of dissolution of zirconium in hydrofluoric acid and in fluoboric acid at two temperatures of 9°C and 100°C have been studied for the purpose of effective dissolution of samples in various analytical procedures.
In both systems, the rate of dissolution of zirconium is first-order with respect to hydrofluoric acid, and respective activation energies for the dissolution are 5.8 kcal (9100°C). Evidence confirms the same mechanism of the dissolution of zirconium in both systems, and the steady-state in the dissolution is probablythe rate of diffusion of hydrofluoric acid to the surface according to the rate equation with Fick's law.
The difference between hydrofluoric acid and fluoboric acid on the rate of dissolution of zirconium is understood from each magnitude of their HF concentration calculated from the acid ionization constant of hydrofluoric acid and the hydrolysis constant of fluoboric acid. A rather small effect of sulfuric acid on the dissolution of zirconium in both systems can also be deduced. from the very small acid ionization of hydrofluoric acid together with the larger formation constant of fluoride complex of zirconium than that of its sulfate.
The mixtures of hydrofluoric- and sulfuric acid or of fluoboric- and sulfuric acid are probably useful as reagents for the complete dissolution of the samples of zirconium and zirconium-base alloys in many analytical procedures.View full abstractDownload PDF (1057K) -
Kingo MIZUNO1965 Volume 14 Issue 5 Pages 410-414
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple and reliable microdetermination of extremely small amounts of gallium in red mud, in which large amounts of aluminum and iron were generally present as interfering elements in the conventional methods of analyses, has been described.
The Ga3+ can be separately extracted by isopropylether from 7M HCl solution, in which 1030 μg of gallium is accompanied with 1020 mg of Al3+, Fe3+ and other smaller quantities of foreign metal ions, after the solution has been treated with titanium trichloride as a reducing agent. The isopropylether is then evaporated on a water bath and a few drops of 10% HNO3 and 10 ml of water are added to dissolve the residue completely.
A small amount of a masking agent containing NaF and Na2B4O7 is then added to eliminate the last traces of Al3+ and Ti3+, and ascorbic acid to reduce the Fe3+ completely. The solution is adjusted to pH 2 by NaOH solution and an excess of 10-4M EDTA is added. Back titration with 10-4M Bi(NO3)3 is successively carried out on the boiled solution in which xylenol orange is used as an indicator.
Thousand times of Al3+ and Fe3+ as well as 100 times of As5+, Ge3+, In3+, MoO42-, and Mn2+ as large as the amount of Ga3+ do not practically interfere. Nitric acid must be avoided in preparing the solution, since it destroyes titanium trichlorideView full abstractDownload PDF (984K) -
Application of a high molecular weight amine to analytical chemistry. IVToshio SUZUKI, Takeshi SOTOBAYASHI1965 Volume 14 Issue 5 Pages 414-419
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThallium (III) could be completely extracted from lower acidity (0.10.5N hydrobromic or hydrochloric acid solution) with xylene or benzene solution of a high molecular weight secondary amine (Amberlite LA-1).
Thallium extracted in the organic phase was hardly stripped with the conventional stripping agents, but it was stripped quantitatively into the aqueous phase without hydrolysis of thallium (III) by EDTA in a buffer solution (pH 10).
The extracting determination of thallium was carried out as follows.
Milligram amount of thallium was extracted with a 5% LA-1 xylene solution and stripped from the organic phase with a buffer solution containing a definite excess of EDTA. The stripped solution was adjusted to pH 5 and backtitrated with 0.01M Th4+ standard solution using Xylenol Orange as an indicator.
Microgram of thallium was extracted with a 0.1% LA-1 benzene solution, stripped into the aqueous phase with the same way, and determined photometrically by Malachite Green at 635 mμ.
Many other metals such as Zn, Cu, Fe, Co, Ni, etc. had shown very low extractabilities under these conditions, and thallium was separated quantitatively from these metals.View full abstractDownload PDF (998K) -
Application of a high molecular weight amine to analytical chemistry. VToshio SUZUKI, Takeshi SOTOBAYASHI1965 Volume 14 Issue 5 Pages 420-423
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSExtraction of iodides of metal ions such as Cu, Cd, Bi, Pb, In, Fe (III), Zn and Ga with a high molecular weight amine is described. A definite quantity of each metal standard solution was placed in a separatory funnel, potassium iodide and sulfuric acid (nitric acid was used in the extraction of Pb alone) were added to form the metal iodide, and the solution was shaken vigorously for about one minute with 10% vol. xylene solution of Amberlite LA-1. Relations between extractabilities of those metal ions and concentrations of sulfuric acid and potassium iodide were examined.
Results in Fig. 15 indicated that the extraction rates of Cu, Cd, Bi, Pb, and In were higher than those from hydrobromic acid solution, exceeding 99% under optimum conditions. But Fe (III), Ga and Zn were scarcely extracted.View full abstractDownload PDF (640K) -
Shizuya MAEKAWA, Takanori SUZUKI1965 Volume 14 Issue 5 Pages 424-433
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe influence of nonmetallic inclusions on the quantitative spectral analysis of silicon, manganese and aluminum in ladle steel samples and rolled steels has been studied.
The results are: (1) In ladle samples solidified rapidly, nonmetallic inclusions are distributed finely and homogeneously, thus, little variations of analytical values are obtained. (2) Significant relations are recognized between the deviation of analytical results and the cleanness of steels. (3) In rolled steels, the variation of analytical values is reduced if the spark surface is selected perpendicularly to the rolling direction.View full abstractDownload PDF (1566K) -
Shizuya MAEKAWA, Kiyotoshi KATO1965 Volume 14 Issue 5 Pages 433-437
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA photometric method for the determination of molybdenum with sodium thiocyanate and ascorbic acid in perchloric or sulphuric acid medium has been studied. The new method has two merits compared with standard stannous chloride reduction method; the sensitivity is higher by about thirty per cent, and the color is stable for at least 4 hours regardless of molybdenum concentration. This fact can be explained, by the milder reducing force of ascorbic acid than that of stannous chloride which suppresses the reduction from molybdenum (V) thiocyanate to colorless molybdenum (III) thiocyanate. The method is suitable for the analyses of samples with high molybdenum content and also for the routine works for treating a mumber of samples at a time.View full abstractDownload PDF (926K) -
Polarographic study of artificial food colors. IYasuhisa MIZUNOYA, Takako KITA1965 Volume 14 Issue 5 Pages 437-443
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe polarographic behaviors of eight watersoluble azo compounds used as artificial food colors-Food Orange No. 1 (Orange I), Food Red No. 101 (Ponceau R), Food Red No. 1 (Ponceau 3R), Food Yellow No. 5 (Sunset Yellow FCF), Food Red No. 4 (Ponceau SX), Food Red No. 2 (Amaranth), Food Red No. 102 (New Coccine)and Food Yellow No. 4 (Tartrazine)-were studied in buffered solutions at pH 1.014.0, with 0.1M tetramethylammonium chloride as a supporting electrolyte. All these dyes gave well defined waves in acidic medium, which corresponded with two electrons reduction except for Food Red No. 102.
When the pH of solution became higher in the acidic range, the half-wave potentials shifted remarkably to negative, but the shifts were not so great in the alkaline side. Moreover, the second waves appeared at lower pH in the order of numbers (3, 2 and 1) of acid radicals in the dye molecules, and became irreversible as the pH became higher.
It could be concluded that the limiting currents of the azo compounds were diffusion currents, because the observed temperature coefficients in acidic solutions on the limiting currents from 15°C to 35°C ranged 1.32.2% per degree and the limiting currents were proportional to square roots of the bights of mercury reservoir.
The eight water-soluble azo compounds of the concentrations 10-310-4M could easily be determined polarographically in acidic solutions.View full abstractDownload PDF (1054K) -
Absorptiometric determination of microamounts of vanadium. IMasatoshi MIYAMOTO, Masatake KATAGIRI1965 Volume 14 Issue 5 Pages 443-449
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the extraction-spectrophotometric determination of microamounts of vanadium (V) by benzohydroxamic acid, a pH-buffer solution simultaneously acting as a masking agent for interfering metals was used, and the color reaction and the extraction were done in one step by shaking with an organic solvent containing the reagent in order to avoid the difficulties hitherto reported as to the stability of the complex in the aqueous phase, the stability of organic extractants, and the preparation of the aqueous reagent solution. The proposed reagent solution was stable at least for 2 months. A wider optimum pH range was given for the extraction.
Procedure : pH of a solution containing 2.8 to about 90 μg vanadium (V) is adjusted to 2.84.4 by adding 4.05.0 ml of a malonate buffer consisting of 5 parts of 0.5M malonic acid and 1 part of 0.5M sodium malonate after the solution is roughly neutralized against phenolphthalein or 2, 4-dinitrophenol. Dilute the solution to 25 ml and shake it for 3 min. with 5.00 ml of 0.1440.171% extracting reagent solution in 3-heptanol. Resulting organic layer is ready for the absorption measurement at 450 mμ with 1 cm cells against water. The color is stable for at least 2 days. Permissible amounts of common diverse ions including titanium (IV) are individually 2.0 mg at least. The amounts of Fe (III), Mo (VI), Pt (IV), or W (VI) should not exceed 1.0, 0.5, 1.25, or 0.001 mg, respectively. The addition of 0.02M sodium pyrophosphate improved the permissible amounts of Fe to 5 mg.View full abstractDownload PDF (1161K) -
Separation and determination of sulphate in large amount of phosphate by ion-exchange chromatographyNaosuke SHIRAISHI, Tomoyuki IBA, Seizi YOSHIKAWA, Tsutomu MORISHIGE1965 Volume 14 Issue 5 Pages 450-453
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of small quantity of sulphate in a large amount of phosphate was presented, in which the sulphate ion was separated by Cl-form anion exchange resins and determined by chelatometric titration.
A solution of sulphate with large quantity of phosphate was poured on a Diaion SA # 100 column. The column was at first treated with 0.1N HCl1-0.19N KCl solution for the elution of phosphate and successively with 2N KCl solution for the liberation of sulphate ion.
The results obtained by this method upon a definite amount of sulphate ion added to the mixed samples of various compositions are given in Table III. The separating determination by the method is quite accurate.View full abstractDownload PDF (669K) -
Yoshinori TAKATA, Giichi MUTO1965 Volume 14 Issue 5 Pages 453-457
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe controlled potential coulometric detector for the detection of electroactive materials in liquid chromatography was investigated.
An electrolytic cell was prepared in which electroactive materials were electrolyzed almost completely on passing through it with the elution flow rate of about 1 ml/min., with which was detected, for instance, Fe (III) eluted from an ion exchange column. The calibration curve of Fe (III) taken to the peak area agreed with the theoretical one.
This type of detector was proved to be useful for the automatic recording in liquid chromatography.View full abstractDownload PDF (731K) -
A theoretical consideration on the chelatometric titration using Xylenol Orange as a metal indicatorMakoto OTOMO1965 Volume 14 Issue 5 Pages 457-461
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe optimum conditions for the chelatometric titration of several metal cations with EDTA using Xylenol Orange as an indicator have been deduced from the theoretical consideration of the equilibria involved. A large difference in the stabilities between the Xylenol Orange and the EDTA complexes of cadmium (II), copper (II), zinc (II), indium (III) or some rare earths (III) offered a theoretical ground for the experimental conditions reported earlier for titrating these cations with EDTA : the optimum pH ranges for titration which were calculated from the theoretical data were in good agreement with those determined experimentally.
It was also found that manganese (II) and nickel (II) may theoretically be titrated under the suitable conditions, and that the titration of iron (III) may be impossible because of too little difference in the stabilities of the iron complexes of Xylenol Orange and EDTA.View full abstractDownload PDF (610K) -
Hiroshi ONISHI, Yukio TOITA1965 Volume 14 Issue 5 Pages 462-465
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSCerium or manganese can be determined with thenoyltrifluoroacetone in the presence of iron. In the first method, iron and cerium or manganese are extracted with 0.5M TTA in xylene from a 0.5M sulfuric acid-0.3M sodium bromate solution. The absorbances of the organic phase are measured at both 440 and 510 mμ. Iron and cerium or manganese can be determined by using the simultaneous spectrophotometric method. Fifty μg of cerium or manganese was determined within an error of 10% in the presence of 200 μg of iron, but the results for iron were not very accurate.
In the second method, phosphoric acid is used to mask iron. Manganese is extracted from the aqueous solution that is 2M in phosphoric acid and its absorbance is measured. Fifty μg of manganese was determined within an error of 6% in the presence of 400 μg of iron. Less than 10 μg of cerium also is masked by phosphoric acid.View full abstractDownload PDF (561K) -
some oxygenated compoundsMasahiko TSUCHIYA, Shinya MATSUHIRA, Hitoshi KAMADA1965 Volume 14 Issue 5 Pages 465-472
Published: May 05, 1965
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSMass spectrum is closely related with the structure of a compound. But it is not easy to determine the structure from its mass spectrum, because the behavior of molecule under electron bombardment is rather complicated and in many cases there are several compounds which show the similar mass spectra.
It can be said that when the energy of the bombarding electrons changed, the dissociation process of a given molecule may also change. We investigated the correlations between the structure of a compound and its mass spectrum at various energy bombardments, by using a CEC 21-103C mass spectrometer.
The formation of the large majority of ions under low energy (23 eV higher than its ionization potential) electron bombardment is through the simple cleavage of a weak bond. In some cases the rearrangement peak, such as the peak at m/e 61 in the spectrum of acetates, is the largest at low energy bombardment.
It is believed that very useful informations for correct interpretation of the mass spectra can be obtained by comparing the spectrum at low energy bombardment with that at ordinary measurement and the ionization efficiency curves are also useful.View full abstractDownload PDF (1031K) -
[in Japanese]1965 Volume 14 Issue 5 Pages 473-474
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese], [in Japanese], [in Japanese], [in Japanese]1965 Volume 14 Issue 5 Pages 474-476
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 5 Pages 477-479
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese], [in Japanese]1965 Volume 14 Issue 5 Pages 479-481
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 5 Pages 481-483
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
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[in Japanese]1965 Volume 14 Issue 5 Pages 484-488
Published: May 05, 1965
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS
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