Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 3 , Issue 4
Showing 1-22 articles out of 22 articles from the selected issue
  • Irene S. FARKAS-CONN
    1987 Volume 3 Issue 4 Pages 283-284
    Published: 1987
    Released: July 27, 2007
    JOURNALS FREE ACCESS
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  • Daido ISHII
    1987 Volume 3 Issue 4 Pages 284
    Published: 1987
    Released: July 27, 2007
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  • Toru OZEKI, Hiroshi KIHARA, Seiichiro HIKIME, Shigero IKEDA
    1987 Volume 3 Issue 4 Pages 285-290
    Published: August 10, 1987
    Released: June 27, 2006
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    Conditions for uniquely separating the true spectra of individual components from the overlapped Raman spectra were examined by factor analysis. Whether the unique separation is possible or not depends upon the information contained in the data-set of the sample spectra. Unique solutions were obtained for two component Raman spectra under the following conditions. Case 1), two components each have a pure wavenumber and their pure samples exist; case 2), two components each have pure wavenumber; case 3), two pure samples exist; and case 4), one component has a pure wavenumber and its pure sample exists. Here, the pure wavenumber means the wavenumber at which only one component has a definite Raman intensity and the other components have zero intensities.
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  • Tomiyuki Maeda, Yasuaki Tanimoto, Nobuo Okazaki
    1987 Volume 3 Issue 4 Pages 291-295
    Published: August 10, 1987
    Released: June 27, 2006
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    A new micro-injection system for flame atomic absorption spectrometry has been devised. In this system, a small amount of sample, 20 to 100μl, is injected in the stream of a carrier solution through a sample inlet and thenfed into a nebulizer. Use of the carrier solution is found to be effective to minimize a sample volume and to reduce physical and chemical interferences. The carrier solution of water reduces the physical interference caused by the increased viscosity of sample solution which contained 5% albumin, and the carrier solution of 2000 ppm lanthanum suppresses the chemical interference caused by aluminum and phosphoric acid in the determination of magnesium and calcium. This method has been successfully applied to the determination of magnesium, calcium, copper and zinc in serum. The analytical results agreed well with those obtained by conventional flame atomic absorption, the relative standard deviation (RSD) being less than 5.1%
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  • Josef JANCA, Dana PRIBYLOVA, Cestmir KONAK, Blahoslav SEDLACEK
    1987 Volume 3 Issue 4 Pages 297-300
    Published: August 10, 1987
    Released: June 27, 2006
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    Fractions of polystyrene latex sample with very narrow particle size distribution obtained with the aid of micropreparative sedimentation field-flow fractionation (SFFF) were characterized by quasi-elastic light scattering. The measured values of the average particle size of individual fractions confirmed high resolving power of SFFF even for extremely difficult separations of samples with narrow polydispersity.
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  • Tsutomu NAGAOKA, Toshikazu FUKUNAGA, Takashi YOSHINO
    1987 Volume 3 Issue 4 Pages 301-304
    Published: August 10, 1987
    Released: June 27, 2006
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    A versatile microcomputer-controlled electrochemical system for data acquisition and analysis was constructed. The system is presently programmed for cyclic and normal pulse voltammetry, and can be used with other transient electrochemical techniques with a slight modification of the programme for data acquisition. The system can also be used with fast transient techniques; cyclic voltammograms were recorded at scanning rates of up to 1200V s-1. The response of the system was examined by monitoring of the fast electrochemical reactions of quinone/ semiquinone systems, and the collected data were analyzed by finite difference methods. The system could work with a microelectrode assembly, and the signal-to-noise ratio was high enough.
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  • Hiroshi KAWAGUCHI, Tomokazu TANAKA, Tetsunari NAKAMURA, Masafumi MORIS ...
    1987 Volume 3 Issue 4 Pages 305-308
    Published: August 10, 1987
    Released: June 27, 2006
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    Suppression of analyte signals by various concomitant elements was investigated. In addition to the ionization interference by easily ionizable elements reported previously, signal suppression by heavy matrix elements was found to be significant. The interference trend followed the order of atomic weight of the matrix elements, i.e., the larger the atomic weight, the severer the suppression effect. Ion scattering by collision with matrix atoms or ions in the course of ion traveling from the sampling orifice is proposed as the mechanism of the matrix effect.
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  • Koichi SAITOH, Satoshi TSUKAHARA, Nobuo SUZUKI
    1987 Volume 3 Issue 4 Pages 309-312
    Published: August 10, 1987
    Released: June 27, 2006
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    Metal chelate was equilibrated between 1cm3 of dodecane and 1cm3 of a water-methanol mixture in a shaking vessel at 25°C. After phase separation, a 10mm3 portion of each liquid phase was applied to high performance liquid chromatography. Partition coefficient (P) was determined simply as the ratio of the chromatographic peak areas measured at a mobile phase with the same solvent composition. The present method makes possible the accurate determination of P and the simultaneous determination of P for a mixture of two or more metal chelates. The P values of Cr(acac)3at XMeOH 0.40, 0.30 and 0.20, where XMeOH denotes mole fraction of methanol in the water-methanol mixture, are 3.28×10-2, 5.65×10-2and 1.00×10-1, respectively. Simultaneous determination of P of Cr(acac)3 and Pd(acac) 2 at XMeOH 0.30 was performed and Pvalues of 5.56×10-2 and 1.35 were obtained respectively. P values of mer- and fac-isomers of Cr(bzac)3 at XMeOH 0.60 were simultaneously determined as 7.38×10-1and 7.72×10-1respectively. The relative standard deviation of P values thus determined was less than 2% for most instances.
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  • Yuzo TAMARI, Rie HIRAI, Haruo TSUJI, Yuzuru KUSAKA
    1987 Volume 3 Issue 4 Pages 313-317
    Published: August 10, 1987
    Released: June 27, 2006
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    A new coprecipitation method for the fluorometry of selenium(IV) and selenium(VI) in groundwaters has been developed. Selenium(IV & I) were coprecipitated with zirconium(IV) hydroxide from 1l of roundwater at pH 8. Without aging, the precipitate was centrifuged nd then dissolved in hydrochloric acid. Selenium(IV) was determined y the usual fluorometry with 2, 3-diaminonaphthalene (DAN). From other portion of the same groundwater, selenium(IV) and selenium(VI) ere determined by the DAN fluorometry after reducing all the selenium o selenium(IV) by 6M hydrochloric acid treatment. The oncentration of selenium(VI) was obtained by subtracting that of elenium(IV) from the total for selenium. The established method is apid and convenient (taking about 2h for 10 sample treatments) ecause the precipitate is easily separable without aging. The method is able to detect nanogram amounts of selenium, for use with high urity zirconium reagents (containing 0.003ng Se in 1mg of Zr) and with two sub-closed glass vessels to avoid any contamination.
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  • Sadayuki KOIZUMI, Toshihiko IMATO, Nobuhiko ISHIBASHI
    1987 Volume 3 Issue 4 Pages 319-325
    Published: August 10, 1987
    Released: June 27, 2006
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    A system is described for the separate determination of anions using HPLC with a potentiometric detector based on an ion selective electrode (ISE). The ISE consists of an oleophilic anion-exchange resin membrane impregnated with an organic solvent. A sodium sulfate solution containing a trace level of a primary ion for the electrode was used as an eluent. Sensitivity and selectivity of the ISE detector varies with a solvent species imbibed in the detector membrane and an ionic form of the membrane. Chromatograms for oxyacid anions (lO3-, BrO3-, ClO3- and NO3-) are shown, and relationships between chromatographic sensitivity and selectivity coefficients of the ISE detector are discussed.
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  • Yuko YAMASHOJI, Takayuki MATSUSHITA, Toshiyuki SHONO
    1987 Volume 3 Issue 4 Pages 327-331
    Published: August 10, 1987
    Released: June 27, 2006
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    A series of bis(dioctylphosphinyl)alkanes (DOPO)2R, where R can bep-xylydyl and (CH2)n(n=2, 3, 4, 5, 8 and 10), has been applied as extractants for gallium(III) ions from aqueous solutions of hydrochloric acid. These bis-type ligands have been found to be superior to the monodentate ligands such as trioctylphosphine oxide (TOPO) and benzyl dioctylphosphine oxide (Bz)DOPO. The extractability of the bis-type ligands, (DOPO)2(CH2)n, depends on the methylene length (n) and decreases in the order of 5_??_10>3_??_4_??_8>2. The complexation of the gallium(III) ion with phosphoryl groups of the ligand has been confirmed by UV, IR and NMR spectroscopy.
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  • Kenjiro HAYASHI, Yoshiaki SASAKI, Shoji TAGASHIRA, Yoshiko MURAKAMI, Y ...
    1987 Volume 3 Issue 4 Pages 333-336
    Published: August 10, 1987
    Released: June 27, 2006
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    The spectra of antimony(III)-Pyrocatechol Violet(PV) complexes were given rise to bathochromic shifts about 100 nm by the addition of tetraphenylphosphonium cation in aqueous solution. An absorbance at 630nm was little affected by that of reagent blanks and gave a good sensitivity for the spectrophotometric determination of antimony(III). The molar absorptivity was 16500dm3 mol-1 cm-1 in the presence of 0.024mol dm-3 TPPC and 2.0×10-4mol dm-3 PV concentrations at the pH ranges from 2.5 to 4.5, and this solution was stable up to 20h in the presence of 0.1% gum arabic.
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  • Yeong-Dae HONG, Kazuhisa YAMAYA, Minoru YOSHIDA
    1987 Volume 3 Issue 4 Pages 337-341
    Published: August 10, 1987
    Released: June 27, 2006
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    A spectrofluorimetric method for the microdetermination of sulfide was established. This will eventually be applied to silicate rock analysis. An excess amount of Cu2+ is added to precipitate copper(II) sulfide with sulfide ion. The remaining Cu2+ forms a chelate with 2-(o-hydroxyphenyl)benzoxazole (HPB) and quenches the fluorescence of HPB. The amount of sulfide is determined by measuring the fluorescence of the remaining HPB. The optimum reaction conditions, in which all the concerned reactions proceed stoichiometrically, were examined. By the proposed method, 5-640ng sulfide can be determined with a relative standard deviation of 1.14% at 250ng S2- level.
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  • Hiroshi KAWAMOTO, Tsunemi AIBAT, Hideo AKAIWA
    1987 Volume 3 Issue 4 Pages 343-346
    Published: August 10, 1987
    Released: June 27, 2006
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    A simple and accurate HPLC method was developed for the determination of pheophytinatoiron(III) chloride (PheoFeCl) prepared by the replacement of magnesium(II) in chlorophyll [pheophytinatomagnesium(II)] with iron( III). The good separation of PheoFeCl was obtained by using a stationary phase of C18 chemically bonded to silica gel and a mobile phase of acetone-acetonitrile (50:50, v/v). A tailing of the PheoFeCl peak due to the dissociation of ion pairs was improved by addition of tetramethylammonium chloride to the mobile phase. The spectrophotometric method was also used for a comparison to the HPLC method. For the synthetic samples prepared by mixing (pheophytinato a)iron(III) chloride [(Pheo-a)FeCl] and (pheophytinato b)iron(III) chloride [(Pheo-b)FeCl], analytical values by the spectrophotometric method were extremely high compared to those by the HPLC method because of interferences from the absorption of coexistent pigments. In the proposed HPLC method, (Pheo-a)FeCl and (Pheo-b)FeCl could be determined in the concentration range of 0.025-30μg cm-3and 0.06- 30μg cm-3with relative standard deviations (n=10) of 6.2% and 18%, respectively.
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  • Hajime ISHII, Tsugikatsu ODASHIMA, Takashi HASHIMOTO
    1987 Volume 3 Issue 4 Pages 347-352
    Published: August 10, 1987
    Released: June 27, 2006
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    Three new hydrazones, in which the hydrogen at the 5-position of the pyridine ring in the hydrazine moiety of 2- pyridinecarbaldehyde 2-pyridylhydrazone was substituted by a methyl, chloro or nitro group, have been synthesized and their chromogenic properties, reactivities with metal ions and extractabilities of the metal complexes studied. The acid dissociation constants (ka) of the synthesized hydrazones were determined spectrophotometrically. These values obeyed Hammett′s law, the inductive effect of the substituents being found to reflect the pka values. Of the synthesized hydrazones, 2-pyridinecarbaldehyde 2-(5-nitro)pyridylhydrazone (PANPH), in which a electron-withdrawing nitro group was introduced, was most sensitive for metal ions. Its copper and nickel complexes showed molar absorptivities of the order of 105. A highly sensitive and selective extraction-spectrophotometric method for the determination of nickel with PANPH is proposed and has been successfully applied to the determination of nickel in steel samples. The method has been further sensitized by employing analogue derivative spectrophotometry.
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  • Kenji FURUYA, Hidenari INOUE, Tsuneo SHIRAI
    1987 Volume 3 Issue 4 Pages 353-357
    Published: August 10, 1987
    Released: June 27, 2006
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  • Akira SANO, Makoto OGAWA, Shoji TAKITANI
    1987 Volume 3 Issue 4 Pages 359-362
    Published: August 10, 1987
    Released: June 27, 2006
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    1, 4-Dimethyl-3-carbamoylpyridinium chloride (DCP•Cl) has been synthesized as a new fluorogenic reagent for aromatic aldehydes. Aldehydes gave a green fluorescence (λex420-439nm and λem504-519nm) after reaction with DCP•Cl at 37°C for 50min in the presence of alkali and sodium sulfite. The method is simple and sensitive for aromatic aldehydes except for those having hydroxy or dimethylamino group. Aliphatic and arylaliphatic aldehydes and substances other than aldehydes showed no or weak fluorescence. By the proposed method, benzaldehyde, furfural and 4-methoxybenzaldehyde could be determined in the ranges 0.06-3nmol/ml, 0.08- 3nmol/ml and 0.3-6nmol/ml, respectively, with relative standard deviations of 0.5-2.5%.
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  • Yoshie KOBAYASHI, Hiroaki KUBO, Toshio KINOSHITA
    1987 Volume 3 Issue 4 Pages 363-367
    Published: August 10, 1987
    Released: June 27, 2006
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    A water-soluble 9, 10-phenanthrenequinone-3-sulfonate was synthesized as a fluorogenic reagent which reacted with guanidino group in an alkaline solution. The reagent was used for the determination of guanidino compounds by high performance liquid chromatography where the mobile phase contained the fluorogenic reagent. Several guanidino compounds were separated within 20min on a Nucleosil C8 column (3μm, 75mm×4.6mm i.d.) by an isocratic, reversed phase and ion-pair chromatography and detected as fluorophores derived from condensation with the reagent in an alkaline solution. The chromatographic system, in which the mobile phase contained the reagent, was simple because only two pumps were required to deliver the mobile phase and the alkaline solution. The relative standard deviation (within-run, n=10) and the limit of detection for the assay of the compounds were 3.00% and 0.1nmol, respectively. This method was applied to the determination of guanidino compounds in serum obtained from patients on haemodialysis therapy.
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  • Masatoki KATAYAMA, Yoshio MUKAI, Hirokazu TANIGUCHI
    1987 Volume 3 Issue 4 Pages 369-372
    Published: August 10, 1987
    Released: June 27, 2006
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    A simple and sensitive fluorometric method for the determination of vanillin is described. Vanillin gave an intense blue fluorescence (excitation maximum at 337nm and emission maximum at 400nm) in an alkaline medium after reaction with 4, 5-dimethyl-o-phenylenediamine in an acidic medium. Vanillin was determined in the range of 1-2000ng ml-1, and the relative standard deviation at 10ng ml-1 vanillin was 1.80% (n=10). The fluorescent product from the vanillin was identified as 2-(4-hydroxy-3-methoxyphenyl)-5, 6-dimethylbenzimidazole by comparison with the authentic sample separately synthesized. The application of this fluorometric method to other aldehydes was examined.
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  • Noritaka OYAMADA, Masakazu KIKUCHI, Mutsuo ISHIZAKI
    1987 Volume 3 Issue 4 Pages 373-376
    Published: August 10, 1987
    Released: June 27, 2006
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    Determination of dimethyl selenide(DMSe) in the breath air of mice was studied by GC. Collection of DMSe was carried out using a charcoal column(0.9×10cm) packed with 2g of activated charcoal granules. The charcoal was transferred into a 25ml glass-stoppered tube, and the tube was placed in chilled water. After 10ml of CS2 was added to the tube, the tube was immediately stoppered and the mixture was shaken for 30min. The extracts were filtered through glass wool and adjusted to 10ml. The extraction was repeated twice. A 5μl-aliquot of the extract was injected into the GC apparatus using a VZ-7 column and the peak height of the associated component was measured (Rt=2.5min). The recovery was 70-76%, and the observed relative standard deviation was 4.2-9.6%. The amounts of DMSe in the breath air of 10 mice after the oral administration of selenite (50 μmol-Se/kg/d) for 5 consecutive days were in a range of 32-78μg.
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  • Chihiro UEDA, Kaoru TANIUCHI, Hidenobu OHMORI, Masaichiro MASUI
    1987 Volume 3 Issue 4 Pages 377-378
    Published: 1987
    Released: July 27, 2007
    JOURNALS FREE ACCESS
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  • Koichi SHIOMI, Seiji TAKAHASHI
    1987 Volume 3 Issue 4 Pages 379-382
    Published: August 10, 1987
    Released: June 27, 2006
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