Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 2 , Issue 4
Showing 1-21 articles out of 21 articles from the selected issue
  • Horacio A. MOTTOLA
    1986 Volume 2 Issue 4 Pages 317-319
    Published: 1986
    Released: July 27, 2007
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  • Kitao FUJIWARA
    1986 Volume 2 Issue 4 Pages 320
    Published: 1986
    Released: July 27, 2007
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  • Yoshimasa TAKAHASHI, Yuzuru SATOH, Hajime SUZUKI, Hidetsugu ABE, Shin- ...
    1986 Volume 2 Issue 4 Pages 321-323
    Published: August 10, 1986
    Released: June 23, 2006
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    An algorithm for the exhaustive enumeration of all possible unique substructures from a structural formula is described. The algorithm has been implemented in a computer program called GROWSUB. The program allows the chemist to specify his definition of the substructures with a choice of graph theoretical expressions: simple graph, node(atom) weighted, or node(atom) and edge(bond) weighted one. An illustrative example using acesulfame is discussed to describe the program, and applicabilities of the program are mentioned briefly.
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  • Susumu KOHATA, Miaki ASAKAWA, Toshiie MAEDA, Hiroshi SHYO, Akira OHYOS ...
    1986 Volume 2 Issue 4 Pages 325-330
    Published: August 10, 1986
    Released: June 23, 2006
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    By means of thermal analysis, the titled complexes were shown to degradate in two stages up to 500°C. Through the first-stage decomposition of [M(NH3)6][M′(CN)6], 1mol of HCN gas and 4mol of NH3 gas evolved during a pronounced endothermic reaction (except for the complex with Ru-Fe as M-M′). Different combinations of M-M′ can reverse order of the two kinds of gas-evolution in the complexes; the loss of ligand leads to a di- or poly-nuclear complex in which the NH2 and/or the CN group has bridged; the electronic conductivity increased with the progress of bridging; the metal ion in complexes with Co-Fe and Co-Co as M-M′ was reduced. The complex [MCl(NH3)5][Ni(CN)4] also decomposed in two stages with the simultaneous gas-evolution of HCN and NH3.
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  • M. GRATZL, J. FLIGIER, E. PUNGOR
    1986 Volume 2 Issue 4 Pages 331-334
    Published: August 10, 1986
    Released: June 23, 2006
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    Analytical characteristics of air-gap cyanide sensor incorporating metallic silver as indicator electrode have been investigated as function of chemical composition, pH, buffer capacity, concentration and volume of the absorbent electrolyte film covering the indicator electrode. Simple silver nitrate electrolyte provides results equivalent to those obtained with a dicyanoargentate(I) electrolyte, but its preparation is easier. The pH of absorbing solution should be kept at pKHCN=9.3. Convenient buffer capacity can be assured by a medium concentrated (10-1M) appropriate buffer system (e.g. borax-borate). Optimal electrolyte concentration is about 10-4mol/l, while the volume of electrolyte must be of several microlitres for assuring good reproducibility. For interpretation of the results an equation correlating equilibrium activity of the acidified sample solution with that of the absorbing film has been determined, and the relationship between the e.m.f, and the pH of the film has been derived. Thus, the entire 4-phase system (sample solution, air-gap, absorbing film, potentiometric sensor) can be described as a closed equilibrium system.
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  • Nobuo SUZUKI, Yoshihiro IWATA, Hisanori IMURA
    1986 Volume 2 Issue 4 Pages 335-338
    Published: August 10, 1986
    Released: June 23, 2006
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    A new synthetic multi-element reference material (SyRM) with polyacrylate-acrylamide gel matrix was prepared by co-polymerization reactions of homogeneous aqueous solutions of a mixture of acrylic acid and acrylamide containing known amounts of the elements of interest. The matrix elements are analogous to those of biological materials and their composition can simulate the biological samples to be analyzed. The excellent homogeneity and the quantitative retention of minor and trace elements were ascertained by using a radiotracer technique.
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  • Isao TOMITA, Yasuhiro KUSANO, Toshihiro NAKAMURA
    1986 Volume 2 Issue 4 Pages 339-342
    Published: August 10, 1986
    Released: June 23, 2006
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    Crystalline α-hafnium phosphate was prepared by the direct precipitation method and NH4+ ion exchange behavior was investigated both in forward and backward directions. The forward ion exchange was a single-step reaction without formation of an intermediate mono-ammonium salt form, whereas the backward ion exchange proceeded in two steps. On the other hand, ammonia gas was contacted with the exchanger, and ammonium salt of α-hafnium phosphate was obtained, which gave the identical X-ray powder patterns to that of the product of the forward exchange experiment. Intercalation of ammonia molecules was suggested for the mechanism of the forward ion exchange.
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  • I. P. SARASWAT, S. K. SRIVASTAVA, G. BHATTACHARJEE, SHARDANAND
    1986 Volume 2 Issue 4 Pages 343-346
    Published: August 10, 1986
    Released: June 23, 2006
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    Titanium(IV) ferricyanide, prepared under the optimum conditions of concentration, acidity etc., has exchange capacity of 0.18meq per g of exchanger material. The sorption of a large number of metal ions have been investigated and the compound shows promising selectivity for Rb+ ions. It is possible to have a large number of clean binary and ternary separations involving Rb+ ions on the columns of this exchanger material.
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  • Kenjiro HAYASHI, Yoshiaki SASAKI, Shoji TAGASHIRA, Yoshiko SOMA, Shinj ...
    1986 Volume 2 Issue 4 Pages 347-350
    Published: August 10, 1986
    Released: June 23, 2006
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    The conditional stability constant and the distribution constant of [M(dtp)3](M3+=As3+ or Sb3+, dtp-=O, O′-diethyl dithiophosphate) were determined by analyzing the relationship between the distribution ratio of arsenic or antimony and the concentration of dtp-. The values for arsenic(III) complex were 1011.2 (mol dm-3)-3(in 2mol dm-3 sulfuric acid solution) and 103.0, respectively. Those for antimony(III) complex were 1010.4(mol dm-3)-3 (in a solution of pH 1.6) and 102.4, respectively. Both arsenic(III) and antimony(III) were quantitatively extracted into hexane with Kdtp of 2mmol dm-3 from 1-2mol dm-3 sulfuric acid solution, only antimony(III) was extracted from a solution of pH 1.3-2.5, and neither of them was extracted at pH 4.2 or above. The separation method of arsenic(III) from antimony(III) and the reverse are proposed.
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  • Motoho MUROI, Akira HAMAGUCHI, Eiichi SEKIDO
    1986 Volume 2 Issue 4 Pages 351-356
    Published: August 10, 1986
    Released: June 23, 2006
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    Two new thiacrown compounds in which benzoazo groups are introduced as the chromogenic group, 4′-(p-hydroxyphenylazo)benzo-1, 4, 8, 11-tetrathiacyclopentadec-13-ene(III) and 4′-(2-hydroxy-5-chlorophenylazo)benzo-1, 4, 8, 11-tetrathiacyclopentadec-13-ene(VI), have been synthesized. Their characteristics as extracting and spectrophotometric reagents have been examined. Silver belonging to the univalent class b metals is extracted with reagent(VI) into 1, 2-dichloroethane. Its absorption maximum shifts to a much longer wavelength than that of the reagent itself. Neither class a and ab metals nor bivalent class b metals such as mercury(II) and palladium(II) were extracted at all. Only copper(II) of class ab metal is appreciably extracted with this reagent. It seems to proceed due to coordination to adjacent azo and phenol groups. In the presence of hydroxylamine sulfate, copper(I) is extracted into 1, 2-dichloroethane-amyl alcohol (4:1).
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  • Akira SANO, Shoji TAKITANI
    1986 Volume 2 Issue 4 Pages 357-360
    Published: August 10, 1986
    Released: June 23, 2006
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    A simple and sensitive fluorometric method for determination of sulfide ion was developed. Sulfide ion gave a blue fluorescence (λex 338nm and λem 450nm) after alkylation reaction with methyl p-toluenesulfonate in dilute alkaline medium and the successive condensation reaction with taurine and o-phthalaldehyde at pH 8.0. Sulfide ion can be determined in the range 0.03-5nmol/100μl with relative standard deviations (n=10) of 1.6% at 0.2nmol and 2.7% at 3nmol. A 100-fold molar amount of each of common anions did not interfere the analysis, except cyanide, thiosulfate, sulfite and carbonate, the tolerance ratios of which were 5, 10, 30 and 50, respectively. Interferences caused by metal ions such as calcium(II ), magnesium(II) and zinc(II) can be removed by addition of EDTA, but copper(II) and manganese(II) must be absent.
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  • Toshiyuki HOBO, Katsurou YAMADA, Shigetaka SUZUKI
    1986 Volume 2 Issue 4 Pages 361-364
    Published: August 10, 1986
    Released: June 23, 2006
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    An ion flotation-atomic absorption spectrometric method is described for the determination of six heavy metal ions: Fe(III), Ni(II), Co(II), Cu(II), Cd(II) and Zn(II), in water. Heavy metal ions in 1000ml samples were chelated with 1, 10-phenanthroline at pH 4.0 and were floated with the aid of sodium lauryl sulfate and nitrogen bubbles. Each metal ion concentration was determined by a conventional flame atomic absorption spectrometry after diluting to 10ml. The linear calibration curve of each ion was obtained in the concentration range of 4×10-8M-8×10-7M. The proposed method was successfully applied to the determination of these ions in hot spring waters.
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  • Noritaka OYAMADA, Mutsuo ISHIZAKI
    1986 Volume 2 Issue 4 Pages 365-369
    Published: August 10, 1986
    Released: June 23, 2006
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    Fractional determination of trimethylselenonium ion(TMSe), Se(IV) and Se(VI) in water samples was studied by graphite furnace atomic absorption spectrometry. After coexisting cations formed a complex with thiosulfate to prevent being adsorbed on cation-exchange resin, separation and concentration of TMSe were carried out by column chromatography on Dowex 50 W-X8 resin. For concentration of inorganic selenium (Se(IV), Se(VI)) in water samples, column chromatography was carried out with an anion-exchange column using Dowex 1-X4 resin and the selenium were eluted simultaneously with 1M hydrochloric acid. Se(IV) in the eluent was extracted with dithizone solution under the condition of 4M hydrochloric acid. Se(VI) could be extracted with dithizone solution after the reduction to Se(IV) with hydroxylamine hydrochloride. In this procedure, the recovery of selenium was in the ragne of 86-102.8%, and the variation coefficient was 4.2-11.3%. The detection limit of TMSe was 10ng/21 and that of Se(IV) and Se(VI) was 5ng/l.
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  • Hisatake NARASAKI
    1986 Volume 2 Issue 4 Pages 371-374
    Published: August 10, 1986
    Released: June 23, 2006
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    Trace antimony in river water was determined by hydride-generation atomic absorption spectrometry. The water was concentrated after the addition of mineral acids. Siliceous residues deposited during the concentration were solubilized with hydrofluoric acid and expelled by evaporation in the presence of sulfuric acid. After chelating resin separation, the effluent was acidified with sulfuric acid to ionize the hydrolyzed antimony. The accuracy checked with a biological standard reference material was satisfactory when the insoluble residues in the material were treated with hydrofluoric acid after acid digestion. Antimony contents in the water ranged between 0.1 and 0.9ng ml-1.
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  • Kunishige NAITO, Shuichi SUMIYA, Kunito IMAMURA, Shinsuke TAKEI
    1986 Volume 2 Issue 4 Pages 375-378
    Published: August 10, 1986
    Released: June 23, 2006
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    New chemically bonded column packings were prepared by treatment of alumina with some titanate coupling reagents. Isopropoxytitanium(IV) tristearate(TTS) was found to be the most effective modifier among the titanate coupling reagents used. Using the column packed with ITS-bonded alumina, hydrocarbons and dialkyl ethers were eluted as symmetric and slightly skewed peaks, respectively, but alcohols were not significantly eluted. t-Butyl alcohol and t-butyl methyl ether were, however, eluted as sharp peaks in a very short time. The specific surface area of the TTS-bonded alumina and the retention volume of a solute were analyzed as a function of the amount of surface-bonded TTS.
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  • Mitsuo IKEDA, Masatoshi HATTORI, Ushiho MATSUMOTO
    1986 Volume 2 Issue 4 Pages 379-383
    Published: August 10, 1986
    Released: June 23, 2006
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    In high performance liquid chromatography on a silica gel column, elution of phospholipids (PLs) can be accelerated in the presence of magnesium chloride or calcium chloride in water-containing eluents composed of n-hexane-isopropanol-water. In particular, the addition of these metal chlorides results in markedly reduced retention of the chloline-containing PLs such as phosphatidylcholine, sphingomyelin and lysophosphatidylcholine. The effect on the retention increases with increases in concentration of the metal chlorides and in water content in the eluent systems. Two types of Aquasil SS columns packed with Hypersil-5 of 60 or 120Å pore size showed the same retention time for the PLs. These columns retain PLs more weakly than LiChrosorb Si-60. Seven kinds of phosphoglycerides and sphingolipids (sphingomyelin) can be separated within 40-60 minutes by the use of Aquasil SS column and the isocratic eluent composed of n-hexane-isopropanol-0.2mol dm-3 magnesium chloride (36:48:5, v/v). Five classes of PLs were identified from PL fraction of human platelets by the proposed method.
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  • Hiroshi TANAKA, Masamichi KOIKE, Terumi NAKAJIMA
    1986 Volume 2 Issue 4 Pages 385-388
    Published: August 10, 1986
    Released: June 23, 2006
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    The effective isolation of small peptides has been achieved by HPLC with alumina supports and hydrophilic eluents combined with a reversed phase HPLC. Of the four kinds of alumina supports tested, only Spherisorb A5Y showed the high column efficiency and a good reproducibility. Its elution mode appeared to be the same as the open column system, judging from the chromatograms of synthetic phyllolitorin and bradykinin. A mixture of the tryptic fragments of egg white lysozyme was separated by the combination of alumina and ODS columns, with a linear gradient elution of acetonitrile. The peaks which could not be isolated by one column were effectively separated by a second column; this was confirmed by determining their amino acid compositions. Spherisorb A5Y was found by the fluorescent X-ray analysis to be a complexed material of aluminum oxide and titanium oxide.
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  • Akinori UEJIMA, Masanobu HABIRO, Fumio ITOGA, Yoshinori SUGITANI, Kenj ...
    1986 Volume 2 Issue 4 Pages 389-390
    Published: 1986
    Released: July 27, 2007
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  • Toshishige M. SUZUKI, Osamu ITABASHI, Tomio GOTO, Toshiro YOKOYAMA, Te ...
    1986 Volume 2 Issue 4 Pages 391-392
    Published: 1986
    Released: July 27, 2007
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  • Kazuhiro IMAI, Toshio ARAMAKI
    1986 Volume 2 Issue 4 Pages 393-394
    Published: 1986
    Released: July 27, 2007
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  • Hiromasa KATO, Akihiro SHIMURA, Hidenaga OUCHI, Kazuo KUMAMOTO
    1986 Volume 2 Issue 4 Pages 395-396
    Published: August 10, 1986
    Released: June 23, 2006
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