BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 41, Issue 3
Displaying 1-11 of 11 articles from this issue
  • Koji MATSUSAKI, Yoshinori HARADA
    1992 Volume 41 Issue 3 Pages 109-114
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A mixture of nickel nitrate, aluminium nitrate and EDTA tetraammonium salt proved to be very suitable as a matrix modifier for the determination of antimony by a graphite furnace AAS. Nickel nitrate (0.01 M) and aluminium nitrate (0.02 M) were added and the amount of EDTA added was varied with the amount of metal ions in the sample solution. Addition of metal nitrates suppressed the sensitivity loss in atomic absorption of the analyte which was caused by EDTA, and permitted the addition of a large amount of EDTA to the sample solution. When the total metal ion content in the sample solution was within the quantity equivalent to the EDTA added, the chloride interference could be removed, because chloride formations of analyte and other metal ions were masked by EDTA. The sulfate interference could also be removed by the addition of this matrix modifier. When the amount of aluminium nitrate added was reduced and magnesium nitrate was further added, the removal effect on the sulfate interference was improved.
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  • Shigeru SUZUKE
    1992 Volume 41 Issue 3 Pages 115-124
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A GC/MS method was developed for the simultaneous determination of airborne pesticides. An activated carbon fiber felt (47 mm in diameter) put between quartz filters in a filter holder was used for the sampling of air borne pesticides. Retention efficiency was determined by spiking a standard solution of 35 pesticides (containing 1 μg of each) on the front quartz filter, and then drawing air (temperature: 35°C, relative humidity : 77% or more) through the filters for 5 or 10 m3 at the rate of 30 l/min. Retention efficiencies of 29 pesticides ranged from 81 to 113% with the R.S.D. of 3 to 15% (n =6) at 5 m3 of air drawn. The minimum detection levels of thses pesticides were generally from 0.1 to 10 ng/m3. A more selective analysis with GC/MS/MS using a tandem mass spectrometer was examined to double-check the trace pesticides. The determinations of pesticides using the chromatograms of daughter ions from GC/MS/MS were effective for several samples showing noisy chromatograms with GC/MS. The working curves by GC/MS/MS were very similar to those by GC/MS, and the minimum detection levels of the former were generally one-tenth those of the latter.
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  • Mikita ISHII, Masako SHIRAI
    1992 Volume 41 Issue 3 Pages 125-133
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A technique to enhance chemiluminescence (CL) with a mixed dye-sensitizer (eosin Y/uranine) was applied to the determination of hydrogen peroxide at ultratrace levels using the luminol CL system. The enhancement technique was based on the energy transfer phenomenon between some dye-sensitizers. The proposed single line FIA system was equipped with two sample injectors (Rheodyne, 7125 type) placed on the flow line at a distance of 30 cm from each other; the large one (100 μl) at a distance of 10 cm from the pump was employed for the CL reagent solution and the small one (20μl) at a distance of 20 cm to the detector for the hydrogen peroxide solution (sample). The analytical characteristics were as follows. The lower detection limit: 1 × 10-11M in a 20 Ml injection volume, the relative standard deviation: 1.7% in 10 repeated runs involving a 20 Ml injection of the 1 × 10-8 M hydrogen peroxide soution, the analytical time: ca. 6 s, and the interference: some metallic ions {cobalt(II), copper(II), iron(III) etc.: 1 × 10-6} gave weak interfering signals to the CL response of the 1× 10 -8 M hydrogen peroxide solution. The recovery of hydrogen peroxide in the tap water was almost quantitative.
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  • Miyuki MORITA, Tamio KAMIDATE, Hiroto WATANABE
    1992 Volume 41 Issue 3 Pages 135-139
    Published: March 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A novel spectrophotometric method was developed for the determination of cysteine. This method was based on the stoichiometric redox reaction between cysteine and a copper(II) complex with 1, 10-phenanthroline in 90% dimethyl sulfoxide solution. An intensely colored copper(I) complex was formed and the molar absorptivity of which was 7000 dm3 mol-1 cm -1 at 444 nm. The calibration curve was linear over the range from the detection limit of 5.0 × 10 -5 to 2.0 × 10-3 mol dm-3 of cysteine. The relative standard deviation of ten successive determinations was 1.0% at 8.0× 10-4mol dm-3 of cysteine. This method was applied to the determination of cysteine in permanent wave solution.
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  • Kazutoku OHTA, Hiroyuki HARADA, Shigeki NAKAJIMA, Kazuhiko TANAKA
    1992 Volume 41 Issue 3 Pages 141-146
    Published: March 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Anion chromatography with conductometric detection combining a silica based low capacity anion-exchange column and an aromatic tricarboxylic acid (trimellitic acid) of high eluting power was applied to the determination of Cl-, NO3 - and SO42- in acid rain waters and their soil waters to elucidate the acidification mechanism of soil. When a 10 cm column and the 1.25 mM trimellitic acid eluent at pH 4.65 were used to separate the 8 common anions (PO43-, Cl-, NO2 -, NO3-, I- SO42-, SCN- and S2 O3 2-), reasonable separation was obtained within 25 min. The calibration curves of the anions were linear up to at least 0.3 mM for monovalent and 0.2 mM for divalent anions. The detection limits (S/N=3) of major anions in rain water were 10 ng/ml for Cl- 25 ng/ml for NO3-and 28 ng/ml for SO42- The method was successfully applied to the determination of anions in soil samples extracted by acid rain waters. The results showed that the amounts of SO42-adsorbed on the soil increased with increasing total anion concentration in the rain water and/or with decreasing pH of the rain water.
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  • Yuji SUZUKI, Yoshikatsu SAKAGISHI
    1992 Volume 41 Issue 3 Pages 147-152
    Published: March 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    We present an assay for serum bilirubin using a new diazonium salt of 4-nitro-o-anisidine which reacts readily with intermediate formed in the diazo coupling reaction of bilirubin. The values of the present method correlated well with the values obtained by Michaëlsson method and enzymatic method. However, in the determination of total and direct bilirubin in serum, the values by the present method were significantly higher than those of the Michaëlsson method and the enzymatic method. Thus obtained laboratory data were 0.30.6 mg/dl for the direct bilirubin and 0.51.6 mg/dl for the total bilirubin.
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  • Kunio NAGASHIMA, Jin GUO, Toshiyuki HOBO
    1992 Volume 41 Issue 3 Pages 153-155
    Published: March 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Cupric ion selective membrane was prepared by using Cu(5-octyl oxymethyl-8-quinolinol), as the ion-sensing material, dioctyl phenyl phosphonate (DOPP) as the solvent mediator and PVC as the membrane matrix. A linear log ace-potential curve was obtained within the cupric ion activity range from 8× 10-6 to 10-1 mol dm-3: the slope was 35 mV decade-1 when the ISE membrane was composed of 5 mg of cupric ion-sensing matrial, 250 mg of DOPP and 50 mg of PVC. The ISE exhibited a constant potential within the pH range from 2.8 to 5.2. The selectivity coefficients of the ISE for Zn2+, Mg2+ and Ni2+ were one several thousandths compared with those of the ISE which was made of Cu(8-quinolinol)2 as the cupric sensitive matrial. These effects should be ascribed to the steric effect of 5-octyl oxymethyl of the ion-sensing matrial.
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  • Morimasa FUKUI, Hiroaki KONISHI, Kazutoku OHTA, Kazuhiko TANAKA
    1992 Volume 41 Issue 3 Pages T27-T31
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Ion-exclusion chromatography of alkanolamines was investigated on a PS/DVB based strongly basic anion-exchange resin column (9 × 300 mm) in the OH-form using UV detection at 200 nm. When using water as an eluent, although monoethanolamine (MEA), diethanolamine (DEA) and triethanolamine (TEA) were separated depending on their pkb, and the peak shape of these amines showed tailing, depending on to their hydrophobicities. The calibration curves were also non-linear. When using a 2% glycerine eluent, the tailing was decreased by the effect of OH-group in glycerine, and the high resolution chromatogram for these amines was obtained. Accordingly, linear calibration graphs were obtained for all alkanolamines. The present method was applied successfully to the determination of TEA in cream and shampoo.
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  • Osamu HAMAMOTO, Yukio NAKAMURA, Shunichi UCHIYAMA, Shuichi SUZUKI, Tos ...
    1992 Volume 41 Issue 3 Pages T33-T37
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A portable coulometric analyzer equipped with a electrolytic cell using a porous carbon felt electrode has been manufactured. In this analyzer (17.5×9.5×4.5cm, 0.43 kg), the electrolytic current is converted to voltage and the frequency counted to integrate this current. It was found that the precision (<2%) and sensitivity (0.01 ppm) of the coulometric results for residual chlorine in tap water and L-ascorbic acid in juices obtained by this apparatus were similar to those obtained by commercially available equipment (potentiostat and coulometer). In order to broaden the range of determinable species, indirect coulometric determinations of electroinactive species (chloride ion, sulfate ion, phosphate ion, tartaric acid and citric acid) were carried out by using precipitation reactions. The excess precipitant ions (Ag+, Pb2+ or Bi3+) were electrolyzed within one minute and the absolute determinations of these electroinactive species were carried out by using the precipitation reactions which had taken place prior to the electrolysis. The precisions of these measurements were below 4.1% and the sensitivities were about 1×10-6 M.
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  • Noriko FUDAGAWA, Akiharu HIOKI, Masaaki KUBOTA, Akira KAWASE
    1992 Volume 41 Issue 3 Pages T39-T44
    Published: March 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Calcium, iron, magnesium, sodium and zinc in highly purified water samples were determined by AAS using a tungsten furnace. Three kinds of preconcentration methods were applied to the samples before AAS measurements. The methods include (1) on-boat concentration with a microfeeder, (2) on-boat concentration with a micropipet, and (3) heating with a Teflon beaker in a clean bench. Samples were corrected for contamination during the preconcentration and measurement procedures by subtracting blank values from measured values. The blank values obtained by performing the same procedures without a sample were negligibly smaller.
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  • Masanobu SAHARA, Hirotoshi YOSHIMURA, Fumio SAGARA, Keihei UFAO, Isao ...
    1992 Volume 41 Issue 3 Pages T45-T47
    Published: March 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Acidic ferric chloride solution is widely used as an etching solution for processing the copper coated printed circuits. Determination of free acid (HG!) in ferric chloride solu tion according to the JIS K 1447 method often results in a large negative errors. Principle of the JIS method involves the preliminary separation of ferric ion as K3FeF3 by adding a neutralized potassium fluoride solution, followed by the alkalimetry on an aliquot of the filtrate. However, it was found that hydrofluoric acid which results in the mixture after the addition of potassium fluoride, reacts with glass-ware with the consumption of proton, thus giving negative errors. Accordingly, all glass-wares which come in contact with acidic potassium fluoride solution, have been replaced with polypropyrene laboratory wares. The analytical results obtained under this condition was in good agreement with the calculated values.
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