Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 1 , Issue 4
Showing 1-23 articles out of 23 articles from the selected issue
  • Hideo AKAIWA
    1985 Volume 1 Issue 4 Pages 305
    Published: 1985
    Released: July 27, 2007
    JOURNALS FREE ACCESS
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  • Shizuo FUJIWARA
    1985 Volume 1 Issue 4 Pages 306
    Published: 1985
    Released: July 27, 2007
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  • Toyoaki KATO, Kenzo NAGASE, Hiroko YOKOBAYASHI
    1985 Volume 1 Issue 4 Pages 307-311
    Published: 1985
    Released: June 13, 2006
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    An instrumental photon activation analysis has been developed for the determination of trace elements in boron samples. A simultaneous irradiation of the sample and multielement standards with 30MeV bremsstrahlung produced by a linear electron accelerator for 2-3 hours was applied to measure levels for up to 28 elements nondestructively with practical limits of detection ranging from 0.02 to 10μg. Degrees of inter-element interferences were evaluated. Analytical results for boron samples are presented.
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  • Akio MASUI, Makoto NOSHIRO, Motoharu KURATA
    1985 Volume 1 Issue 4 Pages 313-319
    Published: 1985
    Released: June 13, 2006
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    Laser Raman spectroscopy has been applied to the identification of solid and gaseous inclusions in glass. Both macro- and micro-Raman techniques are employed in this study. The measurements are non-destructive and solid inclusions are identified without any special sample preparation. As for bubble analysis, N2, O2, CO2, SO2, H2 and HCl were found as gas phase inclusions from a variety of sources. Frequently the gases inside bubbles consisted of two or more components. The minimum detectable size of SO2 bubble was 0.28mm in diameter. Sample analyses of fine deposits on the wall of bubbles are also reported.
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  • Kunio SHIRAISHI, Hisao KAWAMURA, Gi-ichiro TANAKA
    1985 Volume 1 Issue 4 Pages 321-325
    Published: 1985
    Released: June 13, 2006
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    The purpose of the present study is to investigate the application of inductively coupled plasma atomic emission spectrometry (ICP-AES) to the direct, multielement analysis of total diet samples for major, minor and trace elements. Sodium, potassium, phosphorus, magnesium and calcium were first determined as major matrix elements in the ashed total diet sample using a polychromator with relatively high dispersion. These elements were determined within a relative error of 3 per cent. After performing the matrix matching between the sample and standard solutions with respect to acidity and the amount of major elements, thirteen minor and trace elements, i.e., iron, zinc, manganese, aluminium, strontium, copper, barium, chromium, nickel, molybdenum, cadmium, cobalt and yttrium, were measured. Of these, iron, zinc, manganese, aluminium, strontium, copper and barium were determined with a relative error of ca. 5 per cents, and chromium, nickel, molybdenum, cadmium and cobalt within 20 per cents. Recovery of the added standard was 100±5% for all the elements except cobalt and molybdenum.
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  • Koichi SHIOMI
    1985 Volume 1 Issue 4 Pages 327-334
    Published: 1985
    Released: June 13, 2006
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    A precutting Multi-Dimensional Capillary Gas Chromatograph (MDCGC) was made of a commercially available capillary GC only by making simple modification of its flow control units. The MDCGC system was applied to the selective determination of aromatic hydrocarbons in gasoline and kerosene. Gasoline was introduced into a polar precutting capillary column, on which aromatic hydrocarbons were more retained than the other hydrocarbons and removed by precutting operation. Paraffins, naphthenes and olefins which were introduced into nonpolar main capillary column were chromatographed without being interfered by aromatic hydrocarbons (except benzene and toluene). Kerosene injected to a nonpolar precutting capillary column was eluted out of it in the order of boiling points regardless of the chemical structure. The peaks of n-paraffins were used as the scale of classification. The aromatic hydrocarbons eluted between two n-paraffin peaks were isolated as a group and then separated on a polar capillary column. Aromatic hydrocarbons were separated and eluted after saturated hydrocarbons.
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  • O. A. SHPIGUN, I. N. VOLOSHIK, Yu. A. ZOLOTOV
    1985 Volume 1 Issue 4 Pages 335-339
    Published: 1985
    Released: June 13, 2006
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    The possibility of utilization of monoaminocarboxylic acids as eluents in ion chromatography with suppression has been studied. Ion chromatographic behavior of valine, leucine, lisine, glicine, α-alanine, β-alanine and n-aminobenzoic acid has been investigated. Salts of acids are weak eluents, whereas salts of aminobenzoic acid are eluents of middle strength. The application of these eluents wakes it possible to increase the sensitivity of determination, in comparison with the use of mixture Na2CO3/NaHCO3, and to obtain accurate separation of mixtures of F-, Cl-, NO3-, SO42- and HPO42-.
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  • Kosuke IZUTSU, Masatoshi ITO, Eiji SARAI
    1985 Volume 1 Issue 4 Pages 341-344
    Published: 1985
    Released: June 13, 2006
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    A silver-silver Cryptate(2, 2) ion electrode (Ag/0.005M AgCryp(2, 2)ClO4, 0.005M Cryp(2, 2), 0.05M Et4NClO4- (S)//0.05M Et4NClO4(S)//) was studied with respect to its applicability as the reference electrode in acetonitrile (AN), propylene carbonate (PC), methanol (MeOH), dimethyl sulfoxide (DMSO) and N, N-dimethylformamide (DMF). The apparent formation constant of AgCryp(2, 2)+ and the potential of the AgCryp(2, 2)+/Ag electrode vs. ferrocene/ferricinium reference system, respectively, were 7.8 and -422mV in AN, 15.5 and -400mV in PC, 9.8 and -253mV in MeOH, 7.3 and -463mV in DMSO, and 9.9 and -466mV in DMF. The exchange current densities of the AgCryp(2, 2)+/Ag electrode were in the range of (3-5)×10-6A cm-2 in all the solvents. The electrode potential was not influenced by the total concentration of (AgCryp(2, 2)++Cryp(2, 2)), provided that the ratio of both species was kept 1:1. The effect of water on the potential was also relatively small. The disadvantages of the silver-silver ion reference electrode especially encountered in PC and DMF were removed with this electrode, and the potential was reproducible and stable enough in all the solvents.
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  • Keiichi FUKUSHI, Kazuo HIIRO
    1985 Volume 1 Issue 4 Pages 345-347
    Published: 1985
    Released: June 13, 2006
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    To establish the optimum conditions for the simultaneous determination of EDTA, Mg(II)-EDTA and Ca(II)-EDTA complexes by capillary type isotachophoresis, effects of the length of the precolumn and the main column, kinds of viscous agents, counter ions and terminating electrolytes, pH of leading electrolyte and the amount of sample injected into the analyzer were studied. The isotachophoretic separation was performed with analyzer equipped with a potential gradient detector. The migration current was i zitially set at 200μA and then changed to 100μA. The best result was obtained with a main column (40cm in length and 0.5mm in inner diameter) connected to a precolumn (4cm in length and 1.0mm in inner diameter) using a leading electrolyte containing 0.01M hydrochloric acid and 0.5% methyl cellulose buffered at pH 8.5 with tris(hydroxymethyl)aminomethane, and a terminating electrolyte containing 0.01M hexanoic acid. Under these conditions, Cu(II)-EDTA and Mn(II)-EDTA were also determined successfully. The error in the determination of the mixtures of these EDTA complexes was less than ±14%.
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  • Shunsuke IDE, Akira OHKI, Makoto TAKAGI
    1985 Volume 1 Issue 4 Pages 349-354
    Published: 1985
    Released: June 13, 2006
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    The extraction of anionic metal complexes was investigated by use of diphosphonium-type liquid anion-exchange extractants, which bear two cationic centers at various distances within a molecule (R3P+-(CH2)n-P+R3: R=octyl, n=2-10; abbreviated as CnBP). When MIIX42- type anionic complexes of divalent metal ions (zinc(II), cadmium(II), and palladium(II)) were extracted, the metal extractability decreased in the order: C10-≈C6-C4-C3- C2BP monocationic extractants (R3R′P+, abbreviated as MP). However, in the extraction of MIIIX4- type complexes of trivalent metal ions (iron(III) and indium(III)), the extractability order was different: MP≈C10-≈C6-C4- C3-C2BP. The unique metal extraction selectivity of the dicationic extractants is discussed in terms of charge interactions within the extracted ion-pair complexes.
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  • Shin-ichi WAKIDA, Takashi TANAKA, Akinori KAWAHARA, Kazuo HIIRO
    1985 Volume 1 Issue 4 Pages 355-358
    Published: 1985
    Released: June 13, 2006
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    An automated chromatographic system for the determination of nitrate in lake water has been prepared in conjunction with a personal computer. The calibration curve in the concentration range of 0-200ppb nitrate-nitrogen was linear. The percent of standard deviation was 0.45% for 20 measurements of 40ppb nitrate-nitrogen solutions. The correlation coefficient between the results obtained by the proposed method and the Autoanalyzer method for 16 samples was 0.990. Nitrate at parts per billion level could be determined within 10min. Moreover, a quantitative range of nitrate measurement can be selected by changing the enrichment period of the sample solution. The results of continuous measurement of nitrate at Lake Biwa are reported in this paper.
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  • Tohru NAGAHIRO, Katsuya UESUGI, Masatada SATAKE
    1985 Volume 1 Issue 4 Pages 359-362
    Published: 1985
    Released: June 13, 2006
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    A spectrophotometric method has been developed for the determination of iron(II) via extraction of its ion- associated complex with 3-(2-pyridyl)-5, 6-diphenyl-1, 2, 4-triazine and tetraphenylborate anion into molten naphthalene. The optimum pH range for extraction of the complex is 1.9-5.9. The solid naphthalene containing the ion-associated complex is separated by filtration and dissolved in acetonitrile. Beer′s law is obeyed in the concentration range 2.0-23.8μg of iron in 10cm3 of acetonitrile solution. The molar absorptivity and Sandell′s sensitivity are 2.54×104l mol-1 cm-1 and 0.0022μg cm-2 at 553nm, respectively. Ten replicate analyses of a sample containing 11.9μg of iron give a mean absorbance of 0.542 with the relative standard deviation of 0.54%. The interference of various ions has been studied. The present method has been successfully applied to the determination of iron in standard alloy samples and metallic aluminum powder.
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  • Eiichi SEKIDO, Keiitsu SAITO, Yoshiaki NAGANUMA, Hiroko KUMAZAKI
    1985 Volume 1 Issue 4 Pages 363-368
    Published: 1985
    Released: June 13, 2006
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    Liquid-liquid extraction of some class b metals, silver(I), mercury(II), palladium(II) and cadmium(II) using thiacrown compound, 1, 4, 8, 11-tetrathiacyclotetradecane(TTCT) and picrate(Pic-) was stoichiometrically examined. Silver(I) and mercury(II) are extracted into 1, 2-dichloroethane as ion-pair compounds, [Ag(ttct)2]+Pic- and [Hg-(ttct)]2+Pic2- respectively. Palladium(II) is extracted into nitrobenzene as [Pd(ttct)]2+Pic2- or [Pd(ttct)2] 2+Pic2- depending on the concentration ratio of TTCT to palladium(II). The extraction constants for silver(I) and mercury(II) and also the distribution coefficient of TTCT in various solvents were determined. The extraction behaviors of these class b metals including copper(I) were compared and discussed in connection with the composition and the conceivable conformation of their extracts.
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  • Keiko YOKOFUJITA, Kazuyoshi TAKIYAMA
    1985 Volume 1 Issue 4 Pages 369-371
    Published: 1985
    Released: June 13, 2006
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    The coprecipitation of calcium and barium carbonates was investigated as a problem in analytical chemistry. Carbon dioxide gas was introduced into solutions of calcium and barium at 80°C. The particles produced were composed of rod-shaped, spindle-shaped and cubic-shaped crystals. The composition of calcium and barium in the reaction mixture changed with bubbling period of carbon dioxide gas. The shape of particles was dependent on the composition of residual calcium and barium in the reaction mixture. The particles were solid solutions of calcium and barium carbonates, whose crystal structures were a little different from each other.
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  • Yukio SAKAI
    1985 Volume 1 Issue 4 Pages 373-376
    Published: 1985
    Released: June 13, 2006
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    A highly sensitive and selective method for the photometric determination of copper with 2-(5-bromo-2-pyridylazo)- 5-diethylaminophenol (5BrPADAP) is described. Copper in the sample solution is sorbed as its N-(dithiocarboxy)-sarcosine (DTCS) chelate onto Amberlite XAD-2 resin and stripped with a pH 9 borate buffer (0.2M) in 60% methanol. The copper-DTCS chelate in the eluate is decomposed with hydrogen peroxide, and copper is determined with 5BrPADAP. Almost all other metal ions do not interfere with the determination because they are masked with nitrilotriacetic acid, sodium pyrophosphate and EDTA, the resulting complexes not being sorbed on the resin. the method is successfully applied to the determination of copper in river water.
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  • Keiko KOBAYASHI, Nobuko NARITA, Satoshi KAWAI, Shohichi KOUCHI
    1985 Volume 1 Issue 4 Pages 377-379
    Published: 1985
    Released: June 13, 2006
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    A new method for the gas chromatographic determination of uric acid in serum using uricase-catalase system is described. This method is based on the combination of the enzymatic conversion of methanol into formaldehyde through the action of hydrogen peroxide formed from uric acid with uricase and derivatization of the resulting formaldehyde with pentafluorobenzyloxylamine. Suitable conditions for the use of uricase and influence of presence of co-existing compounds were investigated. The method is superior to the colorimetric method with respect to specificity and sensitivity. Linear calibration graphs passing through the origin were obtained in the range 8-200μg ml-1 uric acid in serum for FID and 1-12μg ml-1 for ECD using 0.1ml of serum.
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  • Minoru KOGA, Ryota SHINOHARA, Takashi AKIYAMA
    1985 Volume 1 Issue 4 Pages 381-384
    Published: 1985
    Released: June 13, 2006
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    A highly sensitive gas chromatographic (GC) method for the determination of hexamethylenetetramine (HMT) in water was developed. HMT was quantitively extracted into CH2Cl2 forming a charge-transfer complex with iodine. The complex was decomposed by adding a methanolic KOH and liberated HMT was detected by GC equipped with a flame thermionic detector. The linear calibration curve of HMT was observed within the concentration range of 0.5-500μg/l in 100ml of the sample. The recovery efficiencies of HMT added to water at μg/l level were found to be 66-86% with relative standard deviation of 1.2-6.0%.
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  • Kazuko KONDO, Mikio NAKAMURA, Ryota NISHIOKA, Satoshi KAWAI
    1985 Volume 1 Issue 4 Pages 385-387
    Published: 1985
    Released: June 13, 2006
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    A simple and rapid method for routine measurement of valproic acid in serum has been established by high performance liquid chromatography. To 0.2ml of serum sample is added 0.2ml of acetonitrile solution containing thymol as an internal standard (2μg ml-1). After centrifugation, a 20μl aliquot of the supernatant is injected directly into a liquid chromatograph. The chromatographic procedure utilizes a reversed phase ODS column with a mobile phase consisting of 0.05M phosphate buffer(pH 3.0)-acetonitrile-isopropanol (60:25:15) at a flow rate of 0.7ml min-1. Valproic acid was detected by UV absorption at 220nm. The calibration curve was linear from 20 to 120μg ml-1 valproic acid in serum. This method has been applied successfully to monitoring routine serum levels of valproic acid. The results agreed fairly well with those obtained by gas chromatography.
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  • Hideko KOSHIMA, Hiroshi ONISHI
    1985 Volume 1 Issue 4 Pages 389-390
    Published: 1985
    Released: June 13, 2006
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  • Tadahiro TETSUMI, Masao SUMI, Minoru TANAKA, Toshiyuki SHONO
    1985 Volume 1 Issue 4 Pages 391-392
    Published: 1985
    Released: June 13, 2006
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  • Yoshiki KATAYAMA, Hiroshi NAKAMURA, Makoto TAKAGI
    1985 Volume 1 Issue 4 Pages 393-394
    Published: 1985
    Released: June 13, 2006
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  • Tsunemi TOKIEDA, Toshio TOKUDA, Masanori ISHIDA
    1985 Volume 1 Issue 4 Pages 395-396
    Published: 1985
    Released: June 13, 2006
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  • Shizuo FUJIWARA, Rokuro KURODA, Eiichi FURUYAMA, Nobuaki KONDO, Hideto ...
    1985 Volume 1 Issue 4 Pages 397-398
    Published: 1985
    Released: June 13, 2006
    JOURNALS FREE ACCESS
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