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Volume 15, Issue 3
Displaying 1-16 of 16 articles from this issue
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The behaviour of acid-base indicators in mixed solvents. IIIKoichi KATOH1966 Volume 15 Issue 3 Pages 241-246
Published: March 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe absorption spectra of sulfophthaleins in mixed solvents were relatively independent of the organic solvent, but azoes showed larger dependence. In this experiment, alcohols and acetone were used as water-soluble solvents. The influences seemed to have some relation to basicity of the mixed solvents and the type acidic or basic of indicators. In acidic solution, absorption spectra of B.C.G. were independent of the composition of solvent.
On the other hand, on the absorption spectrum of D. Y. in acidic solution, a valley appeared near the peak of the spectrum with increasing concentration of organic solvent. In basic solution, however, absorption at 450 mμ decreased and a shoulder at 410 mμ developed. Other azo indicators such as M.R., p-M.R. behaved similarly. Absorption spectra of D.Y. in 80% methanol, ethanol and iso-propanol indicated that the wavelengths of acidic peaks did not vary with the solvent, while the alkaline peaks shifted to shorter wavelengths as the alcohols became higher. Molecular structures of B.C.G. and D.Y. at their transformation ranges were also described.View full abstractDownload PDF (941K) -
Ikuo ATSUYA1966 Volume 15 Issue 3 Pages 247-251
Published: March 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAtomic absorption spectroscopic determination of copper in aluminum alloys and steels was established, whereby a quite linear calibration line was obtained for 040 μg Cu/ml in 0.30.7N hydrochloric acid solution in the presence of aluminum (0.050.3g/25 ml) and iron (0.10.5g/25 ml). When the diethyldithiocarbamate-MIBK extract was applied to the analysis for micro amount of copper, the sensitivity of the method was ten-fold multiplied, and the 0.003% Cu in aluminum metal could be determined.
The conditions recommended were: wavelength 3247Å, hollow cathode lamp current 30 mA, slit width 0.025 mm, air pressure 1.5 kg/cm2, and acetylene pressure 0.5 kg/cm2 for aqueous solution and 0.3 kg/cm2 for MIBK solution with the water cooling of the burner.View full abstractDownload PDF (882K) -
Ohiko KAMMORI, Tomoo TAKAHARI1966 Volume 15 Issue 3 Pages 251-256
Published: March 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of 0.1 to 10 micrograms of tungsten in pure iron by spectrophotometric method is described. The sensitivity was increased by extracting thiocyanate with n-butyl acetate after reducing tungsten (VI) with titanium trichloride. The method for removal of molybdenum and other interfering elements is proposed.
One tenth g. of the sample is decomposed with the mixture of 5ml of hydrochloric acid and 5 ml of hydrofluoric acid solution (1:9). The solution is heated gently after the addition of 4 ml of hydroxylamine hydrochloride solution (25%). Four ml of hydrofluoric acid solution (1:9) and 4 ml of potassium thiocyanate solution (25%) are added and molybdenum is removed by extracting its thiocyanate with 20 ml of n-butyl acetate. The aqueous layer is evaporated to dryness. The residue is dissolved in 6 ml of sodium hydroxide solution (10%), acidified with 10 ml of hydrochloric acid, and reduced with 3 ml of titanium trichloride with gentle heating. This solution is shaken with 5 ml of n-butyl acetate for about 3 min. after 4 ml of potassium thiocyanate solution (25%) is added. The organic layer is washed twice with an oxalic acid (2%)-1.2 N hydrochloric acid solution in order to remove titanium and other interfering elements. Tungsten is determined from the absorbance at 420 mμ by using a 50 mm cell.
The time required for an analysis is about 2 hrs. Each of the 21 elements contained usually in pure iron is permitted to exist to at least 20 times as much as tungsten.View full abstractDownload PDF (980K) -
Eiji NIKI, Hideko SIRAI, Takero KYOYA1966 Volume 15 Issue 3 Pages 257-263
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAs a method to improve the square wave ac bridge polarograph, the authors have combined the gate circuit with the syncronized rectifier and have obtained a high S/N ratio.
The linearity of the analytical curves is excellent, and the probable errors are below ±0.5%. The minimum concentration for quantitative analyses of lead and cadmium ions in dilute phosphoric acid is 2×10-7M.
The series resistance of polarographic cell in the bridge changed the ratio of faradaic current and capacitive current in the period of open gate. The maximum amount of the series resistance was calculated by the sensitivity of automatic balancing.View full abstractDownload PDF (2632K) -
Haruo TSUJI1966 Volume 15 Issue 3 Pages 263-268
Published: March 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNitrogen and phosphorus contents in various compounds were determined by means of 13N [14N (n, 2n), T1/2=10 min.] and 28Al[31P (n, α), T1/2=2.3 min.] radioactivities, which were produced by 14 MeV neutron irradiation. The sample of 25 g was packed in a polyethylene rabbit capsule and an inner standard (copper plate for nitrogen analysis and quartz for phosphorus analysis) was attached on the cup of the rabbit capsule. It was irradiated with 14 MeV neutrons by T-d reactions with a Cockroft-Walton type accerelator, and then the radioactivity was measured by a well type NaI scintilation detector connected with a single channel pulse height analyzer. Five min. irradiation and 0.51 MeV photopeak counting was adopted for the nitrogen analysis. And 2.5 min. irradiation and total gamma-rays higher than 1.40 MeV were adopted for phosphorus analysis. The radioactivity produced in each sample was normalized with an inner standard.
By this method, nitrogen and phosphorus content in various compounds, particuraly organic compounds can be determined rapidly and nondestructively with an error less than 5 per cent. When the neutron flux could be elevated to 1.0×107 n per cm2 per sec. the limit of detection may be about 10 mg for nitrogen and 7 mg for phosphorus, equivalent to 0.2 % of N and 0.15% of P with each 5 g sample.View full abstractDownload PDF (1029K) -
Application of coutrolled potential coulometry to the automatic recording of liquid chromatography. IIYoshinori TAKATA, Giichi MUTO1966 Volume 15 Issue 3 Pages 269-274
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe coulometric detector of liquid chromatography presented in the first report was improved for micro detection, by which was detected less than 10-10 equivalents of copper ion. More than 99.7 per cent of dissolved oxygen was eliminated by an electrolytic impurity eliminator with controlled potential and the interference was removed. Ultramicro quantities of samples were given by an electrolytic sample supplier, by which was taken as lower as 1 mμg of copper(II) ion.View full abstractDownload PDF (1159K) -
Hiroyuki INOUE, Yukio NURISHI, Kenjiro HAYASHI, Yasumitsu UZUMASA1966 Volume 15 Issue 3 Pages 275-279
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe effects of coexistent anions on the sedimentation volume of agglomerate or precipitate and the apparant solubility products of ferric hydroxide were studied.
The volume of coagulated ferric hydroxide sol increases in the order of NO-3, Cl-, and SO42- (Table I).
In the precipitation of iron by using the urea method from homogeneous solution (initial pH 0.71.2), the sedimentation volume of the precipitate increases in the same order mentioned above (Table II, B), but the presence of small amounts of sulfate gives a dense precipitate (Table II, B No. 7, 8). If the sample solution has the initial pH range 2.02.5, with the probable occurrence of the olation, the volume of precipitate increases in the order of SO42-, Cl-, and NO-3 (Table II, A).
The evidence thus obtained supports the assumption that the volume of precipitate depends on the size of olated compoumds of iron (i. e. primary colloidal particles) and the size is controlled by the apparent solubility of the ferric hydroxide and the buffer effect of the sulfate on the coordination rate of hydroxyl ion for ferric iron.
The effect of anions on the sedimentation volume of the aluminum precipitate may be explained in the same manner. For some organic acids, however, their action as a pH buffer is also to be considered.View full abstractDownload PDF (974K) -
Analytical studies on pesticides by infrared spectroscopy. VNaobumi OI, Isao UMEDA1966 Volume 15 Issue 3 Pages 280-283
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSAn infrared spectrophotometric method has been developed for the determination of Phthalthrin isomers. The amounts of trans-isomer and cis-isomer were determined by their absorbances at 1148 cm-1 and 1070 cm-1 respectively, with the base line technique in carbon disulfide solution. On the other hand, the total Phthalthrin content could be determined by use of the isoabsorption point of two isomers at 1132 cm-1. The impurities do not interfere at these analytical wave numbers. And the results of both the infrared spectrophotometric method and thin layer chromatographic separation-ultraviolet spectrophotometric method were in excellent agreement on technical Phthalthrin samples.View full abstractDownload PDF (507K) -
Analytical studies on pesticides by infrared spectroscopy. IVNaobumi OI, Hiroshi TAKEDA1966 Volume 15 Issue 3 Pages 284-285
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple infrared spectrophotometric method has been developed for the rapid determination of Dimethoate (O, O-dimethyl-S-[N-methylcarbamoyl-methyl]-dithiophosphate) in some formulations. The amount of Dimethoate was determined by its absorbance at 12.0 μ in acetonitrile solution without interference of thermal degradation impurities by the use of a suitable base line. The results obtained by analysing standard mixed samples indicated that the method gave good recovery, and the results of both the infrared spectrophotometric method, and the thinlayer chromatographic separation-bromimetric method were in excellent agreement for some unknown samples of formulations.View full abstractDownload PDF (308K) -
Naobumi OI, Isao UMEDA1966 Volume 15 Issue 3 Pages 285-287
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple method for the determination of the new insecticide, N-(3, 4, 5, 6-tetrahydrophthalimido)-methyl-dl-cis-trans-chrysanthemate (Phthalthrin), in technical products, and in some formulations has been developed using thinlayer chromatographic separation, and spectrophotometry. A sample solution was applied to silica gel plate, and developed with chloroform-ether (19+1). After elution with chloroform, Phthalthrin was determined by its absorbance at 282mμ.View full abstractDownload PDF (559K) -
Ohiko KAMMORI, Hirofumi SHIRAI, Satoshi OKUBO1966 Volume 15 Issue 3 Pages 288-290
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSFor the determination of microamounts of copper (010μg) in pure iron, the bathocuproine photometric method is applied. The procedure is as follows.
One tenth gram of sample is dissolved in 10ml of hydrochloric acid (1 : 1) with a few drops of hydrogen peroxide (30%). After 15ml of ammonium citrate solution (20%) is added, the pH of the solution is adjusted to about 6 with ammonia water. Two ml of hydroxylamine solution (10%), and 2ml of bathocuproine alcohol solution (0.1%) are added. After standing for 5 minutes, the solution is shaken with 5.00ml of chloroform for about 2 minutes. Copper is determined by measuring the absorbance of the organic layer at 477mμ against chloroform.
Twenty micrograms of each element of Al, As, B, Ca, Ce, Co, Cr, Nb, Ni, Mg, Mn, Mo, P, Pb, Si, Sn, Ta, Ti, V, W, and Zn do not interfere.View full abstractDownload PDF (405K) -
Ohiko KAMMORI, Akihiro ONO1966 Volume 15 Issue 3 Pages 290-293
Published: March 05, 1966
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFor the determination of microamounts of selenium (010 μg) in pure iron, the extraction procedure was studied to separate selenium from iron as follows.
One tenth gram of sample is dissolved in 3 ml of HNO3 (1+1) and 1 ml of HClO4 (60%) and evaporated to white fumes. The solution is placed into a separatory funnel with 20 ml of the mixed acid (HCl 3, HNO3 2, H2O 4) and shaken vigorously with 20 ml of methylisobutylketone for about one minute. The lower layer is separated to a beaker and heated to white fumes after adding 2 ml of HClO4. Thirty ml of water, 3 ml of formic acid (2.5 M) and 5 ml of EDTA solution (5%) are added and the pH of the solution is adjusted to 2.32.7 with NH4OH (1+1). After 2 ml of 3, 3'-diaminobenzidine solution (0.5%) is added, the solution is boiled for about half a minute. After cooling, the pH is adjusted from 6 to 7 with NH4OH (1 +1), the solution is immediately placed into a separatory funnel and shaken with 5.00 ml of toluene for about one minute. Selenium is determined by measuring absorbance of the organic layer at 420 mμ against toluene.
Twenty micrograms each of Al, As, B, Ca, Ce, Co, Cr, Cu, Mg, Mn, Mo, Nb, Ni, P, Pb, Si, Sn, Ta, Ti, V, W, and Zn do not interfere. From 0.01 to 10 μg of selenium in pure iron was determined within about half an hour.View full abstractDownload PDF (682K) -
Masatsugu MATSUMOTO, Michihiko MIYAZAKI1966 Volume 15 Issue 3 Pages 294-296
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA rapid and simple technique to determine D-ribonolactone, by converting it to hydroxamic acid with hydroxylamine, and comparing the color produced upon the addition of ferric chloride to the converted solution, was studied. By measuring the absorbance at 510mμ, D-ribonolactone of a concentration smaller than 600μg/ml was determined with good accuracy. Effects of coexistence of salts (NH4)2SO4, Na2SO4, NH4Cl, (NH4) H2PO4, NH4NO3, and H3BO3 were examined.View full abstractDownload PDF (303K) -
[in Japanese], [in Japanese]1966 Volume 15 Issue 3 Pages 297-301
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1031K) -
[in Japanese]1966 Volume 15 Issue 3 Pages 302-308
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (1159K) -
[in Japanese], [in Japanese]1966 Volume 15 Issue 3 Pages 309-311
Published: March 05, 1966
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (470K)
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