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Volume 18, Issue 4
Displaying 1-24 of 24 articles from this issue
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Jihei IWATA1969 Volume 18 Issue 4 Pages 431-434
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA diazo reagent prepared by diazotization of sulfanilamide was applied to the rapid determination of total bilirubin in serum as azobilirubin with colorimetry, and the condition of determination was optimized.
The absorption maximum of the colored solution obtained by the recommended standard procedure was at 545mμ. The method has advantages in faster color development and higher absorbance than Evelyn-Malloy's method, which uses the diazo reagent prepared by diazotization of sulfanilic acid and is now in general use in clinical laboratories.View full abstractDownload PDF (552K) -
Yoshihito SUZUKI, Daido ISHII, Tsugio TAKEUCHI1969 Volume 18 Issue 4 Pages 434-438
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSGas-chromatography of α- and β-naphthol as trimethylsilyl ether derivatives was investigated.Alpha-and β-naphthol were converted with HMDS to silyl ether derivatives under trimethylchlorosilane as a catalyst and determined by gas-chromatography.
The conversion of parent naphthol to the trimethylsilyl ethers and the separation of each compound were excellent.
The resolution factor was 1.88 for α- and β-naphthol and the column efficiency was 2550 theoretical plates for α-naphthol. The condition for optimum separation was as follows; column, 10%-SDGP on Celite 545 (80100); column length, 2m; i.d. 4mm; temperature 160°C; and flow rate of carrier gas, nitrogen, 20ml/min.View full abstractDownload PDF (730K) -
Hisahiko EINAGA, Hajime ISHII1969 Volume 18 Issue 4 Pages 439-446
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSNickel (II) was found to be extracted with α-benzoinoxime into chloroform from a slightly alkaline aqueous solution showing an absorption in the near ultraviolet region and it was applied to the determination of traces of nickel. A general procedure established is as follows.
To a solution containing less than 50 μg of nickel add an alcoholic solution of α-benzoinoxime, adjust the pH to about 9 with borate buffer, extract nickel-(II) as an α-benzoinoxime complex into chloroform, and obtain the absorbance of the organic phase at 330 mμ.
Nickel (II) is extracted quantitatively with α-benzoinoxime at pH 8.210.7 into chloroform, and gives an absorption spectrum in near ultraviolet region. The complex extracted has a composition of 1 to 2 (metal to ligand). Beer's law is obeyed, the molar extinction coefficient at 330 mμ being 7.0 × 103. Copper (II), cobalt (II), manganese (II), zinc (II), lead(II), and cadmium (II) interfere with the determination, but the interference from the last four elements can be eliminated by masking them as tartrate.
The method established was applied successfully to the determination of traces of nickel in high purity beryllium oxide by combining it with an ion exchange separation method.View full abstractDownload PDF (1281K) -
Difference quantitative determination. III.Bunzo TAMURA, Ikuyo FURUYAMA, Kazuyuki MORIURA, Sumio KATAYAMA1969 Volume 18 Issue 4 Pages 446-454
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the previous paper, the absorbance ratio method was developed and was applied to quantitative determination of various drugs, reagents and food additives.
In this paper, factors influencing on the precision and accuracy of determination in this method were investigated to keep the deviation of the assay values within 0.1%. As the results, it was found that, as for the absorbance measurements(Table I), |dr/dx|value, differentiation of the absorbance ratio by the reciprocal of neutralization grade, must be more than 35, and as for the addition of volumetric standard solution (Table II), the determination is carried out precisely in case a whole pipet is used. In the determination of quinine ethylcarbonate and aminopyrine using this method, the influences of wavelength(Table III), of indicator lot (Tables VIII and XIII), of indicator concentration (Table IX), of sample concentration (Table X)and of time exposed (Table XI) on the assay value are negligible, and the influence of solvent concentration (Tables IV and V)is also negligible provided the solvent concentration is exactly adjusted. The lnfluence of temperature (Tables VI, VII and XII and Fig.1) is also negligible in case suitable range of x values is used. lf the assay value is calibrated for temperature by formula (1) and Fig. 1, the other range of x values can also be used. The similar results were obtained on the other substances tested.
It was confirmed from the results of several investigations (Tables XIV, XV and XVI)that the x-r working curves are accurately prepared.
As reported in the previous paper, the standard deviation (n=6) for all substances tested were within 0.1%2).View full abstractDownload PDF (1631K) -
Yoshihiko SHIUCHI, Yoshiko MIYAZAKI1969 Volume 18 Issue 4 Pages 455-458
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIn the presence of alkali hydroxide, 1-(2-phenyl-2-cyclohexyl 1, 3-oxolan-4-methyl)-1-methyl piperidium iodide(I) reacted with potassium β-naphthoquinone sulfonate solution. The chloroform extract of the reaction product had an absorption maximum at 466 mμ and was stable for 24 hours. The relation between the absorbance at this wavelength and the concentration of (I) from 5μg/ml to 100μg/ml was linear and quantitative determination of (I) was possible. This substance in aqueous solution was very stable against heat at pH 3.5. Ultraviolet rays gave only slight decrease of absorbance when the concentration of (I) was greater than 0.2%.View full abstractDownload PDF (615K) -
Tsugio TAKEUCHI, Yoshihito SUZUKI, Yutaka YAMAZAKI1969 Volume 18 Issue 4 Pages 459-463
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA thin-layer chromatographic separation of metallic ions (Cr, Mn, Fe, Co, Ni, and Cu) is described.
(1) Glass plates coated with Kieselguhr G in 0.25mm thick were used. Kieselguhr G was pretreated with HCl.
(2) Two step development procedure was used. The solvent systems were acetone-6N HCl (100: 3, v/v) for 1st step, and acetone-MIBK-6N HCl-acetic acid (45: 55: 3: 2, v/v/v/v) for 2nd step.
(3) Visualization of chromatogram was carried out by spraying of 0.5% oxine solution. Mean Rf values were as follows: Fe 0.97, Cu 0.78, Co 0.51, Mn 0.42, Cr 0.26, and Ni 0.04. Spots are well-separated.View full abstractDownload PDF (745K) -
Akira KAWASE1969 Volume 18 Issue 4 Pages 463-469
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPAN analogues with a phenanthrene or an acenaphthylene ring were synthesized, and their analytical characteristics including acid dissociation constants, color reactions with metal ions, and structures, extractabilities and formation constants of their metal chelates were compared with those of PAN.
That with phenanthrene ring showed similar properties with PAN and was recommended as an extractive spectrophotometric reagent as it had greater formation constants of metal chelates than PAN.
That with acenaphthylene ring had smaller formation constants, and reacted with only fewer number of metals.View full abstractDownload PDF (1196K) -
Yoshio SHIJO, Tsugio TAKEUCHI1969 Volume 18 Issue 4 Pages 469-473
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSChromazurol S reacts with thorium to form a blue association complex in aqueous pyridine in the presence of cetyltrimethylammonium chloride (CTMAC). The absorption maximum at 631mμ of the complex is almost independent on reagent concentration and pH of the solution, and the agbsorbance is nearly constant at pH 5.66.1. The sensitivity is very high, the molar absorptivity being 1.74×105 for 0.78μg Th/ml solution. Beer's law is not obeyed, but calibration line is linear for 0.150.8μg/ml Th. The complex is assumed to have 1:4 (Th: CAS) composition. V, Mo, Zr, W, Cu, Au, Cr, U, As, Sn, Ga, Bi, Hf, Ti, Al, Be, and Fe interfere seriously.
The recommended procedure for obtaining calibration line is as follows. To a solution containing 440μg Th in a 100ml beaker is added 1.7 ml of 2M nitric acid, and it is made to about 25ml with water. One milliliter of 0.5% CTMAC is added and agitated. Five milliliters of 0.02% CAS is added quietly by dipping the tip of a pipet into the liquid on the vessel wall, and then similarly 5ml of 4M pyridine. After allowing to stand for 5min., the solution is transferred into a volumetric flask and made up to 50ml with water. The absorbance at 631mμ is measured after 10min. The pH of the final solution is 5.9.View full abstractDownload PDF (740K) -
Rapid analysis by centrifuge. I.Susumu TAKAMOTO, Kazuko KIMURA1969 Volume 18 Issue 4 Pages 473-477
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSLead sulfate was rapidly separated with minimized loss by the use of centrifuging technique.
Two milliliters of sample solution containing 120 mg of lead was taken in a centrifugal tube. To it were added 0.5 ml of concentrated sulfuric acid and a few drops of non-ionic detergent, and the mixture was centrifuged at a speed of 4000 rpm. After washing three times with ammonium sulfate solution (or diluted sulfuric acid) the precipitate was dissolved in ammonium acetate solution, and then the lead was titrated with EDTA by use of Xylenol Orange indicator and acetate buffer solution.
A shaker with eccentric motion was very useful in every procedure. It was especially effective for preventing bumping during the rapid evaporation of hydrochloric or nitric acid under diminished pressure. Co-precipitation of nickel or mercury (II) could be avoided by a re-precipitation, but bismuth (III) precipitated during evaporation and interfered with the titration of lead.View full abstractDownload PDF (848K) -
Takao YOTSUYANAGI, Katsumi GOTO, Masaichi NAGAYAMA, Kazuo AOMURA1969 Volume 18 Issue 4 Pages 477-481
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS4-(2-Pyridylazo)-resorcin (PAR) reacts with manganese to form a water soluble red complex. The complex has an absorption maximum at 500 mμ and the absorbance is constant over the pH range from 9.7 to 10.7. The molar extinction coefficient of the complex is found to be 7.8×104.
Majority of interfering metals in service water can be masked in the following succesive procedure : (1)Preliminary addition of L-ascorbic acid, thiourea, potassium sodium tartrate and ammonium fluoride to the sample solution. (2) Addition of PAR and ammonium buffer solution (pH=10). (3) Addition of sodium diethyldithiocarbamate and potassium cyanide after the development of color due to the formation of PAR complexes of manganese, iron(II), cobalt and nickel. The addition of EDTA, afterwords, leads to the selective decomposition of the manganese-PAR complex so that manganese can be determined by the decrease of absorbance. The sensitivity of the determination is claimed to be 0.00077μg Mn/cm2. This is seven times as high as that of the formaldoxime method.
The PAR method proposed in this paper can be applied to the determination of trace amounts of manganese in service water and in industrial water.View full abstractDownload PDF (807K) -
Hisao OSAWA1969 Volume 18 Issue 4 Pages 482-488
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe relations between the vaporized amounts, vaporization behavior and spectral line intensity of europium in graphite powder have been examined with graphite electrodes under varying arc discharge conditions and buffer concentrations.
Standard samples were prepared with highly purified graphite powder, 216 ppm of europium as europium oxide and various concentration of sodium fluoride as a spectrographic buffer substance. The element was excited by d. c. arc discharge, and the concentration of europium remaining in graphite powder after the discharge was measured by the neutron activation analysis.
It was revealed that the vaporized amounts were increased and the temperature of anode was raised with an increase of the arc current. The spectral line intensity of Eu 2813.9Ådepended on the vaporized amounts in the argon atmosphere. Under the conditions involving arc current 4.95.0A, electrode gap 3 mm, discharge time 60 sec., and NaF concentration 1.02.0%, the vaporized amounts were 7.78×10-8g/mg sample at the anode crater in the air and 3.89×10-8g/mg sample in argon atmosphere. Under the same anode temperature, the vaporized amounts behavior of europium showed little difference in the air and in argon atmosphere, but the line intensity of Eu 2813.9Å was higher in the latter.
In spite of the difference in boiling point of europium and sodium, the vaporization behaviors of the two elements in a spectrographic buffer of sodium fluoride were closely related. The vaporized amounts of europium in the sample without NaF did not depend on the discharge time, both in the air and in argon atmosphere.View full abstractDownload PDF (1297K) -
Tsutomu MATSUO, Junichi SHIDA, Kenji KUDO1969 Volume 18 Issue 4 Pages 488-491
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSAnalytical conditions for the potentiometric determination of hypophosphite and phosphite in their mixture have been optimized. Hypophosphite is oxidized to phosphate through phosphite by vanadate in presence of silver salt, but phosphite is not oxidized to phosphate in absence of silver. Hypophosphite alone is determined by adding an excess of 0.1N solution of ammonium vanadate to a sample solution containing sulfuric acid followed by boiling for 23 min., and titrating the remaining vanadate with 0.1N Mohr's salt. Simultaneously, 2 ml of 5% silver sulfate solution in concentrated sulfuric acid and a definite excess of 0.1N vanadate solution were added to an equal volume of the sample solution, and boiled for 23 min. The sum of hypophosphite and phosphite is obtained by titrating unreacted vanadate with 0.1N Mohr's salt.View full abstractDownload PDF (609K) -
Tamotsu TANAKA, Chuzo IIDA1969 Volume 18 Issue 4 Pages 492-496
Published: April 05, 1969
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSFrom 0.5 to 1.0g of sample was decomposed with mixture of HF and HNO3. After having been converted to the chlorides, the residue was dissolved into 60 ml of 8N HCl and the solution was shaken with isopropyl ether to remove iron(III). The solution was evaporated to dryness and the residue was again dissolved in 20 ml of water. Heavy metals including lead in the solution were extracted into carbon tetrachloride as dithizonates from which only lead was stripped into 20ml of 0.02N HCl. The solution was subjected to atomic absorption measurement.
The apparatus used was Hitachi Spectrophotometer 139 with a long path flame adaptor of Vycor tube (0.9cm inside diameter, 40 cm long) and Beckman burner (4020) for air-hydrogen flame.
The spectrum line employed was 2170Å
The absorbance was sensitive to the gas pressures and 1.10kg/cm2 for air and 0.10kg/cm2 for H2 were decided as optima. No enhancement of the absorbance was found with organic solvents tested. Apparent absorption was examined with solutions of major components of the silicates.
The working curve from 0.1 to 1.0 ppm was almost straight and the sensitivity was 0.008 ppm, about 100 times more sensitive than those with a slot burner. Noise in measurements was much smaller with 0.02N HCl solution than with organic solvents.
The accuracy and recovery by the use of the NBS standards and various kinds of standard rock samples were satisfactory for practical purposes.
The results obtained agreed well with those by other methods.View full abstractDownload PDF (868K) -
Takashi ISHII, Sôichirô MUSHA1969 Volume 18 Issue 4 Pages 496-500
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the alternating current polarographic determination of lead in commercial soft solder after dissolving the sample in acetylacetone was established. Calibrating solutions can be prepared by dissolving commercially available lead metal of special grade (purity 99.999%) in acetylacetone.
After passing nitrogen gas for 15 min., the alternating current polarogram from 0.0 to -0.7 volt vs. mercury pool anode is recorded, and lead is determined by referring to a calibration curve.
The method is rapid and has accuracies nearly comparable to those attained by the conventional ashing method followed by JIS.View full abstractDownload PDF (837K) -
Emiko SUDO, Haruno OKOCHI1969 Volume 18 Issue 4 Pages 501-506
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSExaminations were done on the square wave polarographic determination of microamounts of chromium in iron, steel and other metals, and the following method was established.
One half gram of sample is dissolved in hydrochloric acid, and iron etc. are oxidized with nitric acid. EDTA for masking matrix and interfering elements and 1mg of Be are added, and beryllium hydroxide is precipitated by adding ammonia water dropwise. The precipitate is filtered, washed throughly with water, and dissolved with 25 ml of 0.1M KCl-0.1N HCl solution into a 25 ml volumetric flask. The polarogram is taken, without deaeration, from -0.70 to -1.30V vs. Hg pool. Tin, niobium and tantalum interfered. The lower limit of determination was 0.0005%.View full abstractDownload PDF (918K) -
Emiko SUDO, Haruno OKOCHI1969 Volume 18 Issue 4 Pages 507-512
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSExaminations were done on. the square wave polarographic determination of arsenic in iron and steel, and a method was established as follows.
One gram of sample is dissolved in mixed acid (nitric and sulfuric), and evaporated by heating to fumes of sulfuric acid. After cooilng, it is made up to 100ml with 9.5N hydrochloric acid. A 10ml aliquot is taken in a separatory funnel. Iron and arsenic are reduced by potassium iodide and ascorbic acid, and extracted with chloroform. The organic layer is washed with 9.5N hydrochloric acid, and arsenic is back-extracted into hydrazine sulfate solution. The arsenic is once oxidized, and is again reduced after concentration by evaporation. After an addition of 2N hydrochloric acid as supporting electrolyte, the polarogram is taken over the range from -0.40V to -0.65V vs. Hg pool. As large as 100 μg of Pb, 100 μg of Te and 300 μg of Se did not interfere. The lower limit of determination was 0.001%.View full abstractDownload PDF (959K) -
Katsuji SATO1969 Volume 18 Issue 4 Pages 513-515
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSIn the determination of manganese by the persulfate oxidation-volumetry without an addition of sodium chloride, it is a merit to be titrated with arsenite solution to a clear end point. But it has been reported that manganese (VII) is not completely reduced to manganese (II) by sodium arsenite, and it is necessary to standardize the sodium arsenite solution against the standard steels that have approximately the same manganese contents as samples to be analyzed.
This treatment is inconvenient for analysis of lots of samples that have different amounts of manganese. By the investigation with an attempt to avoide the above cumbersome treatment, a linear correlation was found between the amounts of manganese and the titration volumes of sodium arsenite solution.
Manganese contents were thus calculated from either regression equation or a linear regression line with consistently good results agreeing with those by JIS absorptiometry.View full abstractDownload PDF (437K) -
Shizo HIRANO, Hiroshi FUJINUMA, Yoshihiko YOSHIDA, Yukitoshi MAKITA1969 Volume 18 Issue 4 Pages 516-519
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for determining traces of fluoride in tantalum metal powder using pyrolytic separation and alizarin complexone extraction spectrophotometry has been established.
A half gram of sample is mixed with 1 g of uranium oxide (U3O8) by grinding, and the mixture is transferred into a porcelain boat. Pyrolysis is carried out under a stream of moist nitrogen (for 10 minutes) followed by moist oxygen (for 5 minutes) in a fused silica combustion tube (about 1100°C).
The volatilized fluoride is absorbed in 20ml of dilute sodium hydroxide solution. This solution is taken into a separatory funnel, and added with 20ml of combined lanthanum-alizarin complexone reagent solution.
Extraction is made with 10ml of 5vol% N, N-diethylaniline in iso-amyl alcohol by shaking for 3 minutes, and the two layers are allowed to separate by standing. After the drainage of the aqueous layer, the organic layer is washed with 50ml of acetate buffer solution. The absorbance of the organic layer is measured at 580 mμ using a reagent blank as a reference.View full abstractDownload PDF (850K) -
Atsushi MIZUIKE, Katsuaki FUKUDA, Junzo SUZUKI1969 Volume 18 Issue 4 Pages 519-521
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe concentration factor of a trace element with respect to a matrix element (usually 10 to 20 in the ion flotation technique) is much improved by the use of ethanol and multistage operation. Nitrogen is bubbled through a 200ml solution (pH 3 to 13) containing a trace element (Ag, Au, Co, Cu, Fe. 0.1 to 1.0 μg), a matrix element (Mg, Na, Zn. 0.5 to 3 g), a complexing agent (10-4M), benzalkonium chloride (10 ppm) and ethanol (4%), until the froth on the surface has ceased to grow. The froth containing the concentrated trace element is then taken out, destroyed by addition of 8 ml of ethanol, diluted to 200ml with water, and the flotation is repeated. The desired trace elements can be concentrated in greater than 90% yields with concentration factors of 30, 103 and 3×104 for single-, two- and three-stage separations, respectively. The time required for each stage is 8 to 10 min.View full abstractDownload PDF (589K) -
Tsutomu MATSUO, Junichi SHIDA, Masataka MOTOKI1969 Volume 18 Issue 4 Pages 521-523
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe oxygen bomb method was employed for the decomposition of three kinds of ABS resins for preparing sample solutions. Pellet sample was burnt as it was, and the powdered sample was after being pressed into tablets. Calcium, magnesium, sodium and potassium in resin were determined by atomic absorption spectrometry by using internal standard method. The contents of sodium and potassium were not much different among various resins (Na 210150 ppm, K 200125 ppm), but calcium and magnesiumn contents showed marked differences. The reproducibility of the results in five determinations on each element was not good. The maximum error was 50ppm, whereby the standard deviation was 12%.View full abstractDownload PDF (589K) -
Hiroshi ONISHI, Keiichi SEKINE1969 Volume 18 Issue 4 Pages 524-526
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSPrevious investigations have shown that uranium (IV) can be determined very sensitively with Arsenazo III in 6 to 7M hydrochloric acid solutions and that uranium (VI) can be determined sensitively with the same reagent at pH 2. The purpose of the present work was to establish the empirical formula of the uranium (VI and IV) -Arsenazo III complexes under the analytically useful conditions.
Results of the continuous variation (s) method and the polarographic method indicate that at pH 1.1 to 3.4 the complex is formed by one mole of uranium (VI) reacting with one mole of Arsenazo III. A result of the continuous variation (s) method indicates that in about 6 M hydrochloric acid solution the complex is formed by one mole of uranium (IV) reacting with two moles of Arsenazo III.View full abstractDownload PDF (464K) -
Tetsuo HASHIMOTO, Shiro IWATA1969 Volume 18 Issue 4 Pages 527-528
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new method for the detection of alpha radionuclides on the electromigrated paper has been proposed. The method is based on the alpha particle track detector with celluloid films. Alpha irradiated films are etched in NaOH solution and are compared with the autoradiographs on X-ray films, whereby the alpha nuclides could be easily distinguished from the beta and gamma nuclides. The authors could confirm the half life of the nuclide from measurements of the number of alpha tracks. The method is applicable to the chemical investigation of alpha nuclides, such as actinide elements.View full abstractDownload PDF (460K) -
[in Japanese], [in Japanese]1969 Volume 18 Issue 4 Pages 529-545
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2606K) -
[in Japanese]1969 Volume 18 Issue 4 Pages 546-558
Published: April 05, 1969
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSDownload PDF (2376K)
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