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Volume 31, Issue 7
Displaying 1-20 of 20 articles from this issue
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Toru NOZAKI, Makoto TAKAHASHI, Tagako KANEKO, Kazuki MATSUOKA, Keiko O ...1982 Volume 31 Issue 7 Pages 353-356
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSIon flotation of the platinum metals and gold (III) in hydrochloric acid solutions was investigated with cationic surfactants, cetylpyridinium chloride, tetradecyldimethylbenzylammonium chloride, and cetyltrimethylammonium chloride. A (0.023) M hydrochloric acid solution (12 ml) containing (1.196.9) μg/ml of metal and (1.672.14) × 10-3 M surfactant was subjected to flotation in a 2.7 (diameter) × 20 cm cell for 20 min with nitrogen bubbles. Platinum (II), palladium (II), and gold (III) were separated from the solution in (9498) % yield, while only a few percent separation was achieved with rhodium (III), iridium (III), and ruthenium (III) at the acid concentration above 0.4 M. The separations of Pt (II), Pd (II), and Au (III) from Rh (III), Ir (III), and Ru (III) were fairly good at the acid concentration of 1.0 M. The relation between n (the mean number of the coordinated chloride ligand) and the concentration of hydrochloric acid was obtained by the mole ratio method. The existence of the species such as PtCl3-, PtCl42-, PdCl3-, PdCl42-, PdCl53-, and AuCl4- was ascertained.View full abstractDownload PDF (707K) -
Tadao SAKAI, Noriko OHNO, Takashi WAKISAKA, Yoshinori KIDANI1982 Volume 31 Issue 7 Pages 356-361
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA simple determination method of histamine in urine by solvent extraction and atomic absorption spectrophotometry has been proposed. The method is due to the formation of histamine-Cu (I) cationic chelate compounds and the extraction of the ion-associate complex with picrate into nitromethane. Histamine can be determined indirectly by the estimation of copper in nitromethane phase. The interference by various compounds was examined. Some inorganic substances, such as sodium chloride, potassium chloride, magnesium chloride, ammonium chloride, sodium nitrate, sodium carbonate of 100 fold molar excess over histamine and calcium chloride, potassium iodide and zinc sulfate of (510) fold molar ratio to the amine had no influences on the absorbance. Iron (II), cobalt, and nickel salts gave an interference, but that of nickel could be depressed by addition of tartrate. Of biogenic amines and amino acid, serotonine and histidine gave a strong interference, but it was depressed by adding iron (III) ions. Catecholamines such as adrenaline, noradrenaline, and dopamine did not interfere less than 5 fold molar ratio to 2× 10-5 M histamine. Calibration curve is prepared as follows; To a (15) ml histamine solution (5 × 10-4 M) placed in a 50 ml calibrated flask, 2 ml of CuCl2 solution (5 × 10-3 M) and 1 ml of 0.7 M hydroxylamine hydrochloride solution were added, and it let standing for a few minute. After addition of 5 ml buffer solution (pH 7.0) and 6 ml of 2.5 × 10-2 M picrate solution, the mixture is diluted with water and mixed thoroughly. After the solution has been transferred into a separatory funnel, it is shaken with nitromethane for 5 min. The copper in the organic phase diluted with ethanol is determined by atomic absorption spectrophotometry. The concentration range from 5 × 10-6 M (0.92μg/ml) to 3 × 10-5 M (5.52μg/ml) of histamine in sample solutions could be determined accurately. The coefficient of variation was about 2 %. This method can be applied to the determination of histamine in animal tissues and urine without separation and purification using ion exchange method.View full abstractDownload PDF (1223K) -
Katsushige TAKAMI, Kazunobu OHKAWA, Yoshio KUGE, Masao NAKAMOTO1982 Volume 31 Issue 7 Pages 362-367
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSTotal nitrogen and phosphorus in river water and industrial wastewater were successfully determined as nitrate and phosphate by ion chromatography after digestion with peroxodisulfate in an alkaline medium. A 20 ml of sample, where total nitrogen content should be less than 0.1 mg, was taken into a digestion tube and mixed with 3 ml of 3.2 % (w/v) potassium peroxodisulfate solution and 1.5 ml of 1 N sodium hydroxide solution. After digesting at 120°C for 30 min in an autoclave, the sample was acidified by adding 1.5 ml of an AG 50W-12X ion exchange resin and then passed through a Chelex 100 column with 0.05 N sodium hydroxide eluent, to eliminate interfering ions such as calcium, magnesium, and other heavy metals. A 100 μl aliquot of the eluate was analyzed by ion chromatography equiped with a Dionex anion separator column (25 cm × 4 mm i. d.) by using 1.5 mM sodium carbonate-5 mM sodium bicarbonate solution as a mobile phase. Nitrate and phosphate were separated effectively without the interference by high concentration of sulfate produced from the decomposition of peroxodisulfate. The identification of NO3- and PO43- was made by retention time, and the quantitation was performed by peakheight. The detection limits for nitrogen and phosphorus were 0.007 mg/l and 0.017 mg/l, respectively.View full abstractDownload PDF (1196K) -
Hiroshi UCHIKAWA, Rikihisa FURUTA, Yasuo MIHARA1982 Volume 31 Issue 7 Pages 367-372
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTrace mercury in coals and cokes was determined by using a flameless atomic absorption instrument equipped with a heating vaporization device, a double gold trap, and a non-dispersive double beam detector (N. D. B.) (RIGAKU Mercury/SP). The additive in the mercury vaporization process and the related operational conditions were studied. Another detector which allowed a simultaneous background calibration (S. B. C.) using a deuterium lamp was employed in series after the N. D. B. detector to check the effect of additives on the interfering background vapors. The optimum conditions were determined by the analysis of NBS 1632 a bituminous coal standard sample {certified value, Hg (0.13±0.03) ppm}. The analed value for NBS 1632 a was 136μg/g (R. S. D. 3 %), regardless of the nature of the detectors and additives (aluminum oxide, magnesium oxide-aluminum oxide, magnesium oxide-sodium carbonate-aluminum oxide, calcium oxide-sodium carbonate-aluminum oxide). In the analysis of high sulfur oil coke, high background absorptions resulted when the additives free from sodium carbonate were used; the N. D. B. detector gave incorrect (higher) values for these determinations. The addition of sodium carbonate removed the interference. The high sulfur oil coke was also successfully analyzed after low temperature ashing followed by the aluminum oxide treatment.View full abstractDownload PDF (1116K) -
Shin-ichiro OKAWA, Bunshiro KOMINAMI, Akira KAWASE1982 Volume 31 Issue 7 Pages 373-377
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESS10-(2-Benzothiazolylazo)-9-phenanthrol (TAP) reacts with cobalt in an aqueous solution in the presence of non-ionic surfaceactive agent, Triton X-100, to form a soluble complex. The optimum conditions for the spectrophotometric determination of cobalt and the removal of the interference from diverse ions were studied. The absorption maximum of the cobalt-TAP complex, that of the reagent blank and the isosbestic point at pH 6.7±0.3 were at 560 nm, 480 nm, and 508 nm, respectively. The absorbance of the complex was constant in the pH range from 6.2 to 7.2. Beer's law was valid up to 15.0 μg/25 ml of cobalt and the apparent molar absorption coefficient was about 5.0 × 104 dm3 mol-1 cm-1. The binding ratio of cobalt and TAP in the complex was 1 : 2. The proposed procedure is as follows: To a sample solution containing 10μg of cobalt in a 100 ml beaker, add 5 ml of sodium acetate and borate buffer (pH 7) and 1 ml of Triton X-100 (0.2 g/ml) solution. Then, control the total volume from 15 ml to 20 ml with water, and adjust to pH 6.7±0.3 with 0.1 M sodium hydoxide or 0.1 M hydrochloric acid. Add 0.8 ml of 10-3 M TAP-dioxane accurately, and heat the solution on a boiling water bath for about 10 min and cool. Transfer the solution into a 25 ml volumetric flask and dilute it until the mark with water. Measure the absorbance at 560 nm against the reagent blank or water. The determination gives a positive error in the presence of nickel (II), copper (II), zinc (II), palladium (II) or cadmium (II), and gives a negative error in the presence of ions, which precipitate at pH 6.7 ± 0.3. In order to remove the interference the precipitation method, the masking method, and the solvent extraction method based on cobalt β-nitroso-α-naphthol complex were studied, and good results were obtained. Cobalt in metallic iron was determined successfully by this method.View full abstractDownload PDF (801K) -
Toshiyasu MATSUOKA, Toshiyuki MITSUI1982 Volume 31 Issue 7 Pages 377-381
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSTropaeoline OO or calcon forms an ion-association complex with nicotine at pH 4.14.8 which can be extracted into dichloromethane. The concentration of the nicotine can be determined by measuring the absorbance of the extracts at 408 nm or 540 nm(tropaeoline OO), or 530 nm (calcon). Calibration curve obeyed Beer's law over the range of 01.1×10-4 M (408 nm), 07.4×10-5 M (540 nm), and 01.7 × 10-4 M (530 nm), respectively. The procedures for the determination are as follows. In a 10 ml test tube, place 1 ml of the sample solution containing less than 1.6 × 10-4 M of nicotine, 1 ml of reagent solution containing 2.9× 10-3M of tropaeoline OO or 1.1 × 10-2 M calcon, 2 ml of Briiton-Robinson buffer solution (pH 4.35), and 5 ml of dichloromethane. Shake the solution for 2 min mechanically and allow to stand for 15 min. Measure the absorbance at 408 nm (tropaeoline OO) or 530 nm (calcon) with 1 cm glass cells. When tropaeoline OO is used, take 2 ml of the dichloromethane layer, add 0.5 ml of methanol solution of 10 % hydrochloric acid and measure the absorbance at 540 nm using 1 cm glass cells. The proposed method is much simpler and can be done more rapidly than gas chromatography, and it is useful for the determination of trace amounts of nicotine. No detectable interference for the determination of nicotine occured with any other compounds, such as glucose, glycine, and glycerol. Interference of Ca2+, Mg2+, Fe3+, Co2+, and Cu2+ were eliminated by adding 1 ml of 5.8 × 10-2 M EDTA solution.View full abstractDownload PDF (863K) -
Tsutomu MASUJIMA, Hideo IMIAI, Hisanobu YOSHIDA, Katsuya WADA, Takuji ...1982 Volume 31 Issue 7 Pages 381-385
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSA combined dying-photoacoustic spectroscopic method (PAS) was developed for the microdetermination of proteins (albumin, lysozyme, melittin, insulin, and pepsin), glycoproteins (mucin, transferrin, immunoglobulin, and hyaluronic acid), and nucleic acid (DNA). The dyes were allowed to be bound to these biopolymers; amino black, alcian blue, and toluidine blue to proteins, glycoproteins, and nucleic acid, respectively. The precipitates of these biopolymer-dye complexes were trapped on a membrane filter and the desiccated filter was directly submitted to the PAS measurement with the He-Ne laser as a light source. The linear ranges of the determination in the combined method were (0.150.8) μg for albumin, (0.050.8) μg for lysozyme and melittin, (0.11.0) μg for insulin, (0.75.5) μg for pepsin, (0.10.8) μg or (0.62.2) μg for mucin, (0.12.1) μg for transferrin, (0.11.0) μg for immunoglobulin, (0.21.1) μg for hyaluronic acid, and (0.130.33) μg for DNA.View full abstractDownload PDF (1033K) -
Toshinori TANAKA, Tetsuo YAMADA, Takashi JOHNOKUCHI, Junro YAMADA, Kaz ...1982 Volume 31 Issue 7 Pages 385-390
Published: July 05, 1982
Released on J-STAGE: February 16, 2010
JOURNAL FREE ACCESSThe determination of trace amounts of fourteen rare earth elements in high-purity yttrium oxide was developed by inductively coupled plasma-atomic emission spectroscopy (ICP). A commercial high-purity yttrium oxide (99.9999 %) was used as a base material and standard solutions were prepared to add other rare earth elements to it. The sample was dissolved in hydrochloric acid to contain 1 g sample/100 ml and measured by ICP. The intensities of spectral lines of all measured elements decreased with an increase of concentrations of yttrium oxide and hydrochloric acid. Thus the suppression effect was easily minimized by keeping the same concentrations of yttrium oxide and hydrochloric acid both in sample solutions and in standard solutions. The operating conditions were as follows; R. F. power was 1.0 kW, Argon gas flow rates for a coolant and for plasma were 14 l/min and 1 l/min, respectively, and sample uptake rate was 4.7 ml/min. The detection limits were 0.2 ppm for Lu, Yb, 0.5 ppm for La, Dy, Eu, Er, 1 ppm for Ho, Tm, 2 ppm for Pr, Nd, Gd, Tb, and 3 ppm for Sm, Ce. The coefficients of variation for all measured elements were less than 2 %. Actually, trace amounts of rare earth elements in two commercial yttrium oxides were determined and the results obtained by this methed were in good agreement with ones by spark source mass spectrometry.View full abstractDownload PDF (930K) -
Seiichiro HIGUCHI, Hideki SHIMADA, Shigeyuki TANAKA1982 Volume 31 Issue 7 Pages 390-396
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe resonance Raman spectra have been measured for the azo dye derivatives of 42 kinds phenols, and the results have been examined in view of the selectivity of spectral patterns. The derivatization method is based on the coupling reaction of phenols with the diazonium ion produced from p-nitroaniline. The derivatives exhibit broad bands in visible region, having the absorption maxima in (470510) nm, which, therefore, fulfil the resonance Raman condition when Ar ion laser is used as an excitation source. The resultant spectra are examined in terms of the position, the kind, and the number of substituents. In the case of monosubstituted phenols, it has been made clear that the spectra corresponding to ortho-, meta-, and para-substituted phenols are distinctly different in their patterns and that the results indicate the sufficient selectivity in the resonance Raman spectrometry for the analysis of this type of isomers. On the other hand, provided that the positions of substituents are the same, the spectra have been found to be all similar regardless of the kinds of substituents, that is, the difference of substituents does not contribute to the manifestation of selectivity. Finally, it has been proved that, in the case of polysubstituted phenols, the spectra exhibit the inherency in each individual compound rather than the type of compounds. Thus, the numbers of substituents induce the obvious selectivity in resonance Raman spectra of colored derivatives of phenols.View full abstractDownload PDF (1366K) -
Shu TAHARA, Syotaro OKA1982 Volume 31 Issue 7 Pages 396-401
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe selectivity of anion-selective electrodes is improved by introducing a small amount of cation-exchange group on the surface of the sensory membrane, where a sufficient amount of anion-exchange group being fixed. This phenomenon occurred markedly for smaller diffusion coefficient anions and also for multivalent anions. The log Kpotj-i plot against the product of the diffusion coefficient and the hydration entropy of the interfering foreign ions was very close to a linear form. The plot for the membrane with a small amount of cation-exchange group showed a steeper line than that for the membrane without the cation-exchange group. The phenomenon, will be explained by assuming that the fixed cation-exchange group hamper the movements of the smaller diffusion coefficient anions in the developing process of Donnan equilibria at the phase boundary between the membrane and solution, so that the anions, that is, the interfering foreign anions, are considerably prevented from approaching to the surface of membrane and less contributive to the formation of Donnan potential. The very similar and symmetrical phenomenon was also observed for the cation-selective electrodes.View full abstractDownload PDF (1101K) -
Kazuyuki AKIYAMA, Machiko NAGASHIMA, Chiyomi OKUMOTO, Kiyoshi TERASHIM ...1982 Volume 31 Issue 7 Pages 402-404
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple method for determining cyanide was applied for the preliminary test of waste water samples from metal plating process. A sample (1 ml) is acidified with sulfuric acid and let to stand overnight in a simple microdiffusion apparatus sealed with 3 M Scotch Acetate Film Tape 800. During this procedure, cleaned-up hydrogen cyanide is quantitatively taken up into 0.15 M sodium hydroxide solution (1 ml), which is subjected to cyanide ion-selective electrode analysis. Sulfurous ion and thiosulfuric ion slightly interfered. The present method (x) gave somewhat higher results than the official method (y) did in the analyses of 103 waste water samples (with and without addition of sodium cyanide). A correlation was observed between the results obtained by these two methods (y=0.64x+0.97, r=0.980).View full abstractDownload PDF (463K) -
Akinori ISOZAKI, Yoshio FUKUDA, Satori UTSUMI1982 Volume 31 Issue 7 Pages 404-406
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA sensitive method for the determination of ultramicro amounts of lead by electrothermal atomic absorption spectrometry was attemped. The method is based on the direct atomization of lead-adsorbed resin, that is, the resin is introduced directly as a “resin-suspention” into a carbon tube atomizer. To a 250 ml sample solution (pH : 4) containing less than 0.40μg of lead, 0.10 g of chelating resin (NH4+-form, below 400 mesh) is added, and mixture is stirred for 10 min. After separation of the resin from the aqueous phase through a membrane filter, 5.0 ml of resin-suspension is prepared by adding water to the resin. Then, 10 μl (resin:0.2 mg) of the suspension is injected into an atomizer. Lead-adsorbed resin is initially dried at ca. 300°C for 20 s, subsequently heated at ca. 900 °C for 90s in the atmosphere, and lead on the resin is atomized at ca.2100°C for 10 s in argon atmosphere (argon flow rate: 2 l/min). The calibration graph was linear up to 1.6 ppb of lead, and the relative standard deviation was 3.7 % at 0.8 ppb level of lead.View full abstractDownload PDF (479K) -
Fumihiko IKEDA, Hideyuki MATSUNAGA, Takao YOTSUYANAGI1982 Volume 31 Issue 7 Pages 407-409
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA new masking reagent, maleonitrildithiolate (MNT) ion, was proposed for the spectrophotometric deter-mination of Al(III) by 8-quinolinol extraction method. Meleonitrildithiolate ion reacts with various heavy metal ions to form water-soluble and stable anionic complexes, but hardly reacts with Al(III). As these MNT complexes were not extracted into chloroform, only Al(III) was able to be extracted into chloroform as a neutral 8-quinolinolato complex. Diverse heavy metal ions, such as 1900 fold amount (μg/cm3) of Cu (II) for 0.54 μg/cm3 of Al(III), 220 fold of Co (II), 210 fold of Ni(II) and 130 fold of Fe (II) for 2.16 μg/cm3 of Al(III) were quantitatively masked in the extraction of Al (III), by shaking for one minute using 60 mg of MNT (sodium salt) and 20 mg of L-ascorbic acid.View full abstractDownload PDF (517K) -
Toshio YAO, Masaru AKINO, Soichiro MUSHA1982 Volume 31 Issue 7 Pages 409-412
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA method for the determination of pg ml-1 levels of inorganicmercury and organomercuric compounds in water has been developed. They were selectively preconcentrated by using two small sized quartz columns packed with 50 mg of silica gels with immobilized iminoacetate (SIIA) and dithiocarbamate (SIDT), respectively. The sample reservoir and the columns were connected with tygon tubing, and the sample (0.1 M HCl solution) was passed through the two columns at a flow rate of 10 ml min-1. The Hg (II) and organomercurys were respectively concentrated on the upper column (SIIA) and the lower column (SIDT). The columns were then inserted in the furnace of Hitachi Zeeman effect mercury analyzer 501, and the individual concentrations of Hg (II) and organomercurys were determined. Various foreign salts and metal ions did not interfere with the recovery of traces of Hg (II) and organomercurys. The proposed method was applied for the determination of Hg (II) and organomercurys at pg ml-1 concentration level in a synthetic sea water sample. The detection limit of this method was 10 pg ml-1 when 100 ml of sample solution was applied, with a relatively standard deviation of less than 4 %.View full abstractDownload PDF (744K) -
I.P. ALIMARIN, G.N. BILIMOVICH1982 Volume 31 Issue 7 Pages E213-E223
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe review is devoted to the developments of radioanalytical methods in USSR. Much attention is paid to applications of substoichiometry in isotope dilution and radioactivation analysis for determination of trace elements in high purity substances and for environmental analysisView full abstractDownload PDF (1567K) -
Yu KOMATSU, Yoshinori FUJIKI, Takayoshi SASAKI1982 Volume 31 Issue 7 Pages E225-E229
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe distribution equilibria of alkali metal ions between crystalline hydrous titanium dioxide fibers and aqueous solutions were measured at 298 K. The adsorption behavior of these ions was well explained by their ion-exchange with hydrogen-ions in the fibers. The distribution coefficients were determined and the effect of other alkali metal ions on the uptake of cesium(I) was measured.View full abstractDownload PDF (529K) -
Yuzi TAKAYAMA1982 Volume 31 Issue 7 Pages E231-E237
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSUsing methane as a marker gas, a methanol peak with FID gas chromatograph was measured to evaluate uncoated supports and capillaries. The amount of methanol injected was finely controlled, and quantitative results were obtained as to characters of supports and capillaries. The present method was compared with Grob's testing one for capillaries and it was concluded that the both gave the same results.View full abstractDownload PDF (514K) -
APPLICATION OF XANTHENE DERIVATIVES FOR ANALYTICAL CHEMISTRY. Part XXIItsuo MORI, Yoshikazu FUJITA, Kimiko SAKAGUCHI, Shoko KITANO1982 Volume 31 Issue 7 Pages E239-E242
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSA simple and sensitive spectrophotometric method for the determination of manganese(II) using o-hydroxyhydroquinonephthalein (On.Ph.) and tetradecyldimethylbenzylammonium chloride(zephiramine) was studied. The method could be used in the concentration range of 0-4.0 μg/10 ml of manganese(II), where the Sandell sensitivity was 0.00038 μg/cm2 at 535 nm, and was applied to the determination of manganese(II) in tap water and waste water.View full abstractDownload PDF (489K) -
Sadanobu INOUE, Suwaru HOSHI, Mitsuo SASAKI1982 Volume 31 Issue 7 Pages E243-E246
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSThe separation of diethyldithiocarbamate (DDTC) chelates of Hg(II), CH3Hg(I), C2H5Hg(I) and C6H5Hg(I) was done by reversed phase partition chromatography. The separation was accomplished within 20 min. The column was a 3.9 mm × 300 mm μ-Bondapak C18 column, and the eluent was 85 % (V/V) methanol-water mixture containing 10-4mol dm-3 of ethylenediamine tetraacetic acid (EDTA).View full abstractDownload PDF (423K) -
Sunao YAMADA, Koji KANO, Teiichiro OGAWA1982 Volume 31 Issue 7 Pages E247-E250
Published: July 05, 1982
Released on J-STAGE: June 30, 2009
JOURNAL FREE ACCESSLaser two-photon ionization technique has been applied for the trace determination of pyrene in a solution state. Analyzing the ion-electron current induced by two-photon ionization, 100 ngl-1 of pyrene in n-hexane has been detected.View full abstractDownload PDF (397K)
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