All issues
Volume 9, Issue 4
Displaying 1-25 of 25 articles from this issue
- |<
- <
- 1
- >
- >|
-
Michio MASHIMA1960 Volume 9 Issue 4 Pages 269-271
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSο-Aminobenzaldehyde-ethylenediimine and nickel in alkaline solution above pH 9.6 gave quantitative formation of red precipitate. This is soluble in benzene and can be extracted from the aqueous layer. This fact was applied on the colorimetric determination of nickel. The maximum absorption of benzene layer was at 486 mμ and the presence of an excess of reagent had no disturbing influence. The standard estimation curve prepared by application of this wave length followed the Beer's law within this experimental range. An aqueous sodium hydroxide alkaline solution containing tartaric acid had no disturbing influence by the presence of large amount of iron in the determination of nickel. The limit for determination was 0.2γ/ ml. The presence of large amount of sodium salt other than sodium acetate, aluminum, chromium, cadmium, manganese, zinc and antimony salts gave no disturbing influence for analysis of nickel.View full abstractDownload PDF (335K) -
Michio MASHIMA1960 Volume 9 Issue 4 Pages 272-275
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSο-Aminobenzaldehyde-ethylenediimine was used as a reagent for colorimetric determination of copper and nickel in iron and steel. The result indicated that copper can be estimated by extracting it with 0.01% reagent in benzene from ammonia alkaline solution not containing large amount of ammonium salt or from sodium hydroxide alkaline solution containing tartaric acid. The presence of nickel can be corrected. Nickel in sodium hydroxide alkaline solution containing tartaric acid can be precipitated by use of 0.1% alcoholic solution of the reagent and estimated by extracting with benzene. The presence of copper can be corrected. Also, the estimation of copper in the presence of iron has been tried. Copper is precipitated in sodium hydroxide alkaline solution containing tartaric acid, filtered, and weighed as oxide after ignition.View full abstractDownload PDF (500K) -
Mutsumi IHIDA1960 Volume 9 Issue 4 Pages 276-281
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn order to determine minor content of aluminum in steel accurately by the intermittent arc excitation using the Littrow type quartz spectrograph, the author examined the conditions as arc current, arc gap, exposure time and the rate of interruption and then found recommendable analytical conditions.
Of those four factors, the arc current had the largest effect on the results of analysis, and the arc gap and the exposure time followed, and the rate of interuption had only slightest effect.
By the comparison of analytical lines of aluminum, it was concluded that those of 3092.71Å or 3082.16Å were sometimes convenient for the simultaneous determination with other elements but the line 3961.53Å was better for the dermination of exceedingly minor content (<0.01%) of aluminum.View full abstractDownload PDF (807K) -
Susumu TAKAMOTO1960 Volume 9 Issue 4 Pages 281-284
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSSodium is precipitated as an antimonate when other cations are masked with a mixed solution of ethylenediaminetetraacetate and dihydroxyethylglycine. The following cations can be masked at pH 11: copper, nickel, cobalt, iron (II), iron (III), manganese, lead, tin (II), aluminum, mercury (II), cadmium, zinc, barium, strontium, calcium, magnesium and lithium. If iron (III), mercury (II), manganese and magnesium are absent, even chromium (III) and tin (IV) can be masked at higher pH. 0.3mg of sodium in 1ml sample solution is generally detectable, but if a large excess of free masking reagent or a large amount of potassium or ammonium salt is present, sensitivity of the analysis decreases because of the super-saturation of sodium antimonate.View full abstractDownload PDF (546K) -
Shigeo WAKAMATSU1960 Volume 9 Issue 4 Pages 284-288
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSLight absorbancy method of determination of Vanadium (V) by use of α-pyridyl-β-azonaphthol (PAN) has been investigated. A solution of Vanadium (V) of pH 3.04.0 reacts with PAN and gives a coloration having the maximum absorption at 560mμ. The coloration is unstable and discolors immediately. However, an addition of 10ml of 20% (NH4)2S2O8 solution to 50 ml of the solution gives a stable coloration. The complex Vanadium (V) -PAN salt, similarly as in PAN complex salt of Cu, Ni, U, etc., is difficulty soluble, but an addition of 10ml acetone to 50ml solution gives no formation of precipitate.
From the above result, the sample solution {0.0050.3 mg Vanadium (V)} is treated with 3ml of 60% HClO4, 10ml of 20% (NH4)2S2O8, 10ml of 99.5% acetone and 5ml of 50% ammonium acetate, adjusted to pH 3.03.5 (affected by Mn in case of pH 4.0), this is treated with 3ml of 0.05% PAN-CH3OH, made up to 50ml with water, let stand for 5min, light absorbancy at 560 mμ is measured, making the blank test at the same time and Vanadium is determined from the estimating line.
In this method, the presence of Cu, Fe, Ni, Cr, Co, Bi, U, In, etc. gives disturbing influence. The author determined Vanadium in iron and steel by this method; in the case, the disturbing components were removed by the magnetic mercury cathodic method and a small amount of residual Fe could be masked by EDTA.View full abstractDownload PDF (731K) -
Syntheses of derivatives of dithizone and their application to analytical chemistry. IIIShinsuke TAKEI1960 Volume 9 Issue 4 Pages 288-294
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe title reagent is synthesized by the Bamberger method and its fundamental properties in carbontetrachloride solution have been investigated. The reagent solution showed only one maximum absorption at 685mμ and there was no absorption at near 450mμ of enol-form. The maximum absorption of metal complex solution was shifted to a longer wave length side than that of the dithizone complex. Ag+ and Cd2+ complexes were insoluble in carbontetrachloride. The reagent had lower reactivity to Zn2+, Cd2+, Pb2+, and Bi3+ than that of dithizone and showed selectivity of reaction towards Ag+, Hg2+, and Cu2+. Molecular extinction coefficient of the reagent, Hg2+ comlex and Cu2+ complex solutions at their maximum absorption wave lengths have been estimated and the values of 49.9× 103, 51.5× 103, and 66.3× 103, respectively, was obtained. The extraction cofficient (log K) of Hg2+ complex was 22.14.View full abstractDownload PDF (997K) -
Synthesis of derivatives of dithizone and their application to analytical chemistry. IVShinsuke TAKEI1960 Volume 9 Issue 4 Pages 294-298
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe title reagent, when used on the quantitative determination of Hg2+, suffered practically from no disturbing influence of Zn2+, Cd2+, Pb2+, etc. and showed higher sensitivity than ο, ο'-dimethyldithizone [di (ο-tolyl) thiocarbazone]. Although there was some difficulties in removing the disturbing influence of Cu2+ and Bi3+, it could be used satisfactory as a reagent to Hg2+ superior than dithizone. For the quantitative ditermination of Cu2+, it can be used as a reagent superior than dithizone in its sensitivity and selectivity. A large amount of co-existing metal ions such as Zn2+ and Cd2+ caused the lowering of the rate of extraction of Cu2+, the rate of the lowering depending on the kind of the salt. In comparison with ο, ο'-dimethyldithizone, it showed a slight lowering of the selectivity, but it can be used conveniently on account of the difficulty in the formation of enol-form salt.View full abstractDownload PDF (709K) -
Ken SAITO, Daido ISHII, Tsugio TAKEUCHI1960 Volume 9 Issue 4 Pages 299-305
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSpectrophotometric determination of 20.05ppm of cadmium in uranium metal by dithizone-carbon tetrachloride method was studied. Copper in uranium metal was removed by dithizonecarbon tetrachloride extraction from the sample solution at pH 12. Nickel was rejected by dimethylglyoxime-chloroform extraction. After hydroxylamine hydrochloride and a large amount of concentrated ammonia water were added to the solution, cadmium was extracted with dithizone-carbon tetrachloride. Uranium and iron etc. remained in the water layer, and were separated from cadmium. Lead and zinc etc. were removed by washing the carbon tetrachloride layer with sodium hydroxide solution. By the back extraction with dilute hydrochloric acid, the oxidized product of dithizone was removed being retained in the carbon tetrachloride layer. Then cadmium was extracted from 1N sodium hydroxide solution with dithizone-carbon tetrachloride, and determined by measuring the absorbancy of the extract at 520mμ.
Using 115mCd as a tracer, the recovery of cadmium was followed throughout the procedures of the method.View full abstractDownload PDF (1172K) -
Hiroshi AWAYA1960 Volume 9 Issue 4 Pages 305-309
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSDithizonate extraction method seems to have many merits than other methods, for the quantitative determination of small amount of mercury. However, for the perfect dithizonate extraction, all mercury must have the form of mercuric salt. The author studied to know the conditions of the oxidation of mercury, and found that, on the quantitative determination of mercury in the field of electrolytic caustic soda industry by the mercury cell process, the samples to be analyzed could be oxidized enough by an addition of HCl-KClO3.
The oxidized solution was adjusted to pH 4.65.2, and EDTA solution and hydroxylamine hydrochloride were added to reduce the excess of the chlorine delivered from HCl-KClO3. Then (mercuric) mercury in the solution could be extracted by dithizone-carbon tetrachloride.View full abstractDownload PDF (740K) -
Kakuma NAGASAWA, Yosihiko KASIDA, Yasumasa KIDO1960 Volume 9 Issue 4 Pages 310-316
Published: April 05, 1960
Released on J-STAGE: May 25, 2010
JOURNAL FREE ACCESSThe ashes of the livers of fishes caught in the Pacific Ocean in 1958 were analyzed for their radio contamination by the ion exchange and precipitation methods. As a result, some radio nuclides, 59Fe, 65Zn, 115mCd and 90Sr+90Y were identified with the measurements of their halflives, absorptions and energies. The maximum concentrations of the elements determined were 59Fe of 4.0 × 10-3 μc, 65Zn of 4.0 × 10-1μc, 115mCd of 6.3 × 10-3 μc, and 90Sr+90Y of 2.5 × 10-5 μc.View full abstractDownload PDF (756K) -
Toru NOZAKI, Kan MANABE1960 Volume 9 Issue 4 Pages 316-319
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAn indirect colorimetric method of Li, Na and K was studied. Using Amberlite IR-120 (H type, 4.1 ml in water, 2.5 cm in height), Li, Na were eluted separately with the eluant of 10% (volume) CH3OH-0.2N HCl, and then K was done with 0.5N HCl by the method of H. Okuno et al. Being these effluents evaporated up on a sand bath, excess HC1 was expelled out perfectly. After the residues were dissolved with water, color was developed with the addition of Hg (SCN)2 and iron alum by the method of I. Iwasaki et al. Indirectly 30500γ of Na was determined with error in less than 10%. For small amounts in less than 100γ of K error exceeds sometimes 10%. More than 20γ of Li may be determined. This method was applied to the determination of Na and K in river water. Being 50ml of the water evaporated up with dil.HCl, the residue was dissolved with 23 ml of conc.HCl. The resulting solution was passed through a column of Dowex 1-X8 resin (10 ml), followed washing with 10.5N HCl, and the 14 ml of the effluent was evaporated up. After dissolution with 5ml of water and 1 drop of 2N HCl, the resulting solution was analyzed by this method. The result showed good agreement with that of flame photometric determination.View full abstractDownload PDF (625K) -
Spectrophotometric studies on organometallic complexes used in analytical chemistry. IXTakuji KANNO1960 Volume 9 Issue 4 Pages 319-324
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThorium forms two sorts of yellow colored chelates with quercetinsulfornic acid which were easily soluble in water, and one of them formed at about pH 5.0 has been used in the spectrophotometric determination of minute amounts of thorium in this paper. The chelate had an absorption maximum at around 438mμ. When the concentration of quersetinsulfonic acid was above 4.8×10-4M, the absorbancies of the chelate were definite at 435mμ in the range of pH 5.0 to 6.5. However, at pH above 5.5, the absorption of quercetinsulfonic acid increased rapidly with increasing of pH. Therefore, the optimum pH for the determination of thorium must be defined in the range of pH 5.0 to 5.5. In these conditions, the Beer's law obeyed in the concentration range from 1.0γTh/ ml to 6.76γ Th/ml, in the wavelengths between 435mμ and 460mμ, and the molar absorption coefficient was calculated as 33, 100 at 435mμ.
It was found with the Job's method of continuous variations that one chelate which had an absorption maximum at about 412mμ was formed with one molecule of thorium and quercetinsulfonic acid respectively, and another which had an absorption maximum at about 438mμ was formed with one molecule of thorium and two molecules of quercetinsulfonic acid.View full abstractDownload PDF (969K) -
Eiji NIKI, Kazuo MASATO1960 Volume 9 Issue 4 Pages 324-328
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe determination of total and free carbon in metal carbides and their cermets is inevitable for testing the manufacturing process and the qualities of the products.
Total carbon content was determined by a combustion method with liquid nitrogen trap; that is, carbon dioxide produced by combustion of sample was coudensed in a trap cooled by liquid nitrogen, and the gas-volume of the collected carbon dioxide was measured with a gas-burette, after removing the liquid nitrogen and warmed up to room-temperature.
The combustion-temperature of the specimen is 1200°C for titanium carbide, and 1400°C for TiC-Ni cermet without any flux. If the specimen of the cermet can be powdered finely under 200 mesh, the combustion-temperature can be decreased down to 1200°C.
The precision of the method is about 0.5%, and is adequate for a rapid analysis of total carbon content of the named specimens.
Free carbon content was determined as follows:-Powdered specimen was dissolved with a solution of 10cc nitric acid (d. 1.4) and 20cc sulfuric acid (1:1). The solution was heated up to 130°C until the specimen could be dissolved completely, then added 100cc cold water, and filtered with glass wool. After being washed the residue on the glass wool was dried at 105°C. By combustion of the residue with the glass wool, the carbon dioxide produced was captured in a cold trap, and measued with a manometer; from this value free carbon content was calculated.
The result was in good agreement with the other method, and the precision of the method in the case of 0.1% free carbon is about 0.01%.
This method of separation of free carbon from combined carbide-carbon by nitric and sulfuric acid is more convenient than that by hydro-fluoric and nitric acid; the glass wool for filtering is more useful than the asbestos.View full abstractDownload PDF (853K) -
Nakaaki ODA, Masaji KUBO, Tadahiko YAMAGISHI1960 Volume 9 Issue 4 Pages 329-333
Published: April 05, 1960
Released on J-STAGE: May 07, 2010
JOURNAL FREE ACCESSA dry method of simultaneous determination of carbon and hydrogen in titanium tetrachloride has been established. The merits of an appratus (Fig. 1) devised are mentioned as follows: (1) A sampling vessel of a new type is devised for a complete avoidance of atmospheric contamination. (2) A trap (Table I and II) is set to prevent low boiling substances for escaping out of the system during the exchanging of atmospheres. (3) By inserting a quartz spiral, a complete oxidation of sample is made possible without any disturbance. (4) To remove a large amount of chlorine evolved during the oxidation of sample, a silver wire is employed.
By using the apparatus, analytical conditions of standard titanium tetrachloride with additions of various known amounts of compounds containing carbon and hydrogen have been investigated. In the process of the method, 0.5 ml sample is placed on a boat, vaporized for 10 min in the atmosphere of oxygen and oxidized by heating at 11001200°C. After the gas generated by combustion of the sample is driven out for 20min, the content of carbon and hydrogen are determined by microgravimetric method. This method can be applied for analysis of total carbon and total hydrogen in titanium tetrachloride with 100 % recovery. Its accuracy was within 9% in terms of variation coefficient for both carbon and hydrogen (Table III) and the lower limit of determination was 0.001%.View full abstractDownload PDF (988K) -
Problems on the quantitative analysis of silicate glass : Especially on the effect of heat-treatmentChujo MATSUMOTO1960 Volume 9 Issue 4 Pages 334-339
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe change of intensity of the spectral lines by heat-treatment in the quantitative analysis of silicate glass was investigated. The effects of heat-treatment at the various temperature ranges were found on the intensity of lines, on the ratio of analytical line pair and on the ratio of fixed line pair. Plate glass, borosilicate glass and high silica glass were used as the samples in this experiment, and the results obtained were as follows;
1) The effect of heat-treatment was found on Na+ as the network modifier for the quenched and annealed sample having a composition of plate glass.
2) The change of intensity of the lines by heat-treatment for sodium borosilicate glass was found for Si4+, B4+, 3+ as network former and Na+ as network modifier.
3) The intensity of lines were compared for porous glass and shrunk glass was also observed, and the ratio of excitation for Si in shrunk glass was found to be larger than that in porous glass.View full abstractDownload PDF (1516K) -
Shigeru YOKOSUKA, Humiki MORIKAWA1960 Volume 9 Issue 4 Pages 340-344
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSElectrolysis of Co in ammonia alkaline solution gives usually the deposition of Co oxide on the cathode and the quantitative electrodeposition of metallic Co is difficult.
This abnormal excessive deposition cannot be suppressed by means of reducing agents such as hydrazine sulfate. It was found by the authors that when sodium pyrophosphate-NH4OH solution or ammonium carbonate-NH4OH solution was used as an electrolyte, there was no great error due to an excessive deposition of Co oxide and the quantitative electrodeposition of metallic Co was obtained within an error of 0.01%. The constituent of electrolyte and the conditions for the electrolysis were as follows:
CoSO4 (1g as Co equivalent).
10g (NH4)2SO4.
10g sodium pyrophosphate or 10g ammonium carbonate.
NH4OH enough to dissolve the precipitate and then 05ml in excess.
The temperature of electrolysis at 4560°C.
Current density at 0.25 amp/dm2.
Time required for electrolysis is about 20 hrs.
The interferences of coexisting elements, errors produced by dissolution and deposition of Pt as the electrode were discussed.View full abstractDownload PDF (840K) -
Studies on 2-(2-hydroxy-5-methoxypheylazo)-4-methylthiazole as an analytical reagent. VTadasi YANAGIHARA, Nobuhisa MATANO, Akira KAWASE1960 Volume 9 Issue 4 Pages 344-348
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS2-(2-Hydroxy-5-methoxyphenylazo)-4-methylthiazole reacts with ferrous ion and forms waterinsoluble violet-colored chelate compound. This is soluble in organic solvents, such as isoamylalcohol, benzene and chloro-form, and these solutions have violet color. The isoamyl-alcohol solution has absorption maxima at 777, 559, and 391 mμ (Fig. 1). The absorption at 777 mμ is convenient for detirmination of iron. The iron chelate at pH 5. 57.0 can be extracted completely by isoamyl-alcohol as indicated in Fig. 2, and the sensitivity is found to be 0.004γ/cm2. The abosorption curves of isoamyl-alcohol extract of the reagent-ferrous iron system are all close to around 513 mμ, indicating the formation of only one kind of chelate (Fig. 5). From the results of continuous variation method (Fig. 3) and slope ratio method, the chelate is found to consist from iron and reagent in the ratio of 1: 2 (Fig 4). The disturbance by the presence of copper, nickel and cobalt is found to be great and phosphoric acid showed also disturbing influence but tartaric acid had no disturbing influence.View full abstractDownload PDF (646K) -
Application of infrared absorption spectroscopy to the examination of drugs and their preparations. VIIITakuma OBA1960 Volume 9 Issue 4 Pages 348-351
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe propellent and the synergist in insecitcidal aerosols are collected separately and their identifications have been attempeted by use of the infrared absorption spectrum method. For the measurement of the spectra, the propellent is placed in a gas cell having the length of 10 cm, and the synergist is estimated by placing it between two NaCl plates with a lead spacer of the thickness of 0.03mm, and the results are confirmed by comparing them with the IR absorption spectrum of each standard substance. This method has a merit of rapid estimation of all constituents with the use of a small amount of sample wihthout breaking the aerosol container. The results of estimation of 11 kinds of commercial samples indicated that 4 kinds of them showed difference in composition from those indicated on their labers.View full abstractDownload PDF (496K) -
Tsutomu MOMOSE, Yo UEDA, Yoshiko MUKAI1960 Volume 9 Issue 4 Pages 352-354
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSSodium amide reacts with various organic and inorganic compounds by heating and gives sodium cyanide. Therefore, detection of carbon is possible by the detection of cyanide ion as Prussian blue. In this reaction, the heating is made under a definite condition with the addition of sodium chloride and zinc dust in order not to lose sodium cyanide once formed and to give the limit of detection of 4075γ of carbon. The limit of detection of several representative compounds is shown in Table I; various compounds which showed positive reaction are indicated in Table II; and the effect of coexisting substances is given in Table III.View full abstractDownload PDF (416K) -
Determination of boron in metallic uraniumTakayoshi YOSHIMORI, Tsugio TAKEUCHI1960 Volume 9 Issue 4 Pages 354-359
Published: April 05, 1960
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn order to determine less than 1γ of boron, several methods using curcumin were compared. As the method proposed by Luke and that by Silverman and others were fairly suitable, they were criticized in detail. The former method was greatly affected by the presence of sodium salt and by the water, and it could not be recommendable in the present case. On the latter method, several improvements were successfully tried for determining boron in the range of 0-1γ. The results were adapted for the estimation of boron in metallic uranium. Uranium was preliminarily separated by the cation-exchange resin, and boron was determined by the improved Silverman's method with satisfactory results.View full abstractDownload PDF (740K) -
[in Japanese], [in Japanese], [in Japanese]1960 Volume 9 Issue 4 Pages 360
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1960 Volume 9 Issue 4 Pages 360a-363
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (488K) -
[in Japanese], [in Japanese]1960 Volume 9 Issue 4 Pages 363-365
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESS -
[in Japanese]1960 Volume 9 Issue 4 Pages 366-373
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1075K) -
[in Japanese]1960 Volume 9 Issue 4 Pages 374-380
Published: April 05, 1960
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (931K)
- |<
- <
- 1
- >
- >|