BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 43, Issue 5
Displaying 1-12 of 12 articles from this issue
  • Yoshinori INOUE, Yukiko DATE
    1994 Volume 43 Issue 5 Pages 365-370
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    1-(Salicylideneamino)-8-hydroxynaphthalene-3, 6-disulfonic acid (Azomethine H) was used for the determination of boron as a reagent in a postcolumn drivatization method.Boron was separated by ion-exclusion chromatography (IEC). The eluate was subsequently mixed with Azomethine H solution to form a complex. The complex was detected at 420nm. The reaction parameters were optimized for boron as follows : reaction coil for reaction with azomethine H, 5m×0.5mm i.d. ; concentration of Azomethine H, 0.5% in 1.5mol dm-3 CH3COONH4; flow rate of the reagent, 0.8 cm3min-1; reaction temperature, 40°C. The chromatographic conditions were as follows : column, IEC column (150mm×7.8mm i.d.) packed with hydrogen form sulfonated polystyrene gel (ion exchange capacity : 3.5meq g-1·dry) ; mobile phase, 1×10-3mol dm-3 sulfuric acid ;flow rate, 1.0 cm3min-1; detection wavelength, 420nm. The detection limit (S/N=3)for boron was 7.9×10-3mg dm-3. The linear range was over 3 orders of magnitude, from 0.01 to 10 mg dm-3. The relative standard deviation (RSD) was 5.5% (n=10) for 0.02 mg dm-3boron solution. The relationship between the postcolumn-IEC method and ICP-MS showed good correlation (r2=0.921, n=50).
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  • Hirotomo OCHI, Tadahiro SHIOTA, Makoto NISHINO
    1994 Volume 43 Issue 5 Pages 371-376
    Published: May 05, 1994
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    Film thicknesses of several kinds of polymers such as polyester and polypropylene were determined by theoretical calculation of the Rh KαCompton scattering from each polymer. The intensities of Rayleigh and Compton scattered continuous and characteristic X-rays which comprise the Rh KαCompton scattering were calculated. As the reference standard, a polytetrafluoroethylene plate (thickness: 10mm) was used. All of the determined thicknesses are in good agreement with the reference values or those measured with a universal horizontal metroscope. The differences between these values were 01μm for the thickness range of 4260μm. This method of determining polymer film thickness has the following features. (1) Bulk reference standards can be used. (2)Different kinds of polymer films can also be determined using same analytical conditions. This thickness determination for polymer films may be used for magnetic tapes, optical magnetic disks, wrapping films, painted steels, etc.
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  • Akitoshi OKINO, Hiroaki ISHIZUKA, Yuji NOMURA, Ryuichi SHIMADA
    1994 Volume 43 Issue 5 Pages 377-382
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Aiming at generating a helium plasma source for the analysis of aqueous samples, a new torch for a helium inductively coupled plasma (He-ICP) was developed. By utilizing flow visualization along with a spark-tracing method, it was found that with a conventional torch for Ar-ICP an adequate helium gas vortex flow to sustain a stable plasma doesn't form in the plasma-generating region. To enhance the vortex flow, compared with that using the Ar-ICP torch, the new He-ICP torch has the following two characteristics : (a) a smaller diameter gas inlet and (b) a shorter distance from the gas inlet to the plasma-generating region. As a result of this change, a stable doughnut-type helium plasma can be produced when using 40.68 MHz RF input power that is >500 W, a plasma gas flow rate >161 min-1, and a carrier gas flow rate >1.01 min-1. A spatial measurement of the helium emission intensity was performed, and the generation of a doughnut-type plasma was confirmed.
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  • Syuji OKUYAMA, Toshiyuki MITSUI, Yoshikazu FUJIMURA
    1994 Volume 43 Issue 5 Pages 383-387
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    The chloride ion and sulfate ion in waste acid were determined by an X-ray diffraction method. Chloride ion was transformed to silver chloride by silver nitrate and sulfate ion was transformed to barium sulfate by barium chloride. Obtained samples were analysed by an X-ray diffraction method. Cluster analysis and principal component analysis were carried out using the intensities of the relevant peaks in order to estimate the content of chloride ion and sulfate ion. In the analysis, silver iodide and iron(III) oxide were used as an internal standard for chloride ion and sulfate ion, respectively. Furthermore, the blend composition ratio was calculated more accurately by principal component score. Consequently, we could obtain accurate experimental values.
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  • Masashi OKAMOTO, Masako MAEDA, Akio TSUJI
    1994 Volume 43 Issue 5 Pages 389-394
    Published: May 05, 1994
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    We have developed a chemiluminescent assay for glucose-6-phosphate dehydrogenase (G6PDH) and alkaline phosphatase (ALP) using NADH oxidase (NOD) purified from S. mutans, and an ALP assay system applied to enzyme immunoassay. Regarding the assay for G6PDH, we could measure a range covering 1.0μU/ml to 0.5mU/ml. The detection limit was 1.0×10-18mol/assay by the 2SD method. On the other hand, when we used an enzyme-cycling system with alcohol dehydrogenase (ADH) and NOD, we could measure from 20 fM to 10 pM of ALP, and the detection limit was 4.0×10-19mol/assay by the 2SD method. We applied this ALP assay system to an enzyme immunoassay for hCG; its measuring range was 0.2100 mIU/ml in serum. The hCG assay gave good results for both inter and intra assays, a dilution test and a recovery test. It also gave a good correlation with a Delfia hCG kit in a TR-FIA assay; we could measure 9 samples below 1.0 mlU/ml, which was the detection limit of the Delfia hCG kit. We had confirmed NOD is a useful enzyme on EIA, and so on.
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  • Kunihiro WATANABE, Yoneichi HIRATA
    1994 Volume 43 Issue 5 Pages 395-401
    Published: May 05, 1994
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    A new method, which is similar to a liquid membrane method, was investigated for simultaneous extraction and back-extraction using two vessels with Teflon phase separators. The absorbance of metal complexes extracted was measured by a spectrophotometer with a flow cell. PAN [1-(2-pyridylazo)-2-naphthol] was used as a ionophore because of its high sensitivity. The conditions for the separation and the determination of iron(III), cobalt(II) and nickel(II) were examined under high speed stirring (2500rpm). After extraction of iron and cobalt complexes to the chloroform phase, iron complex was back-extracted with 6 M HNO3 solution immediately. The cobalt complex remained in the organic phase. Nickel-PAN complex was partially extracted at pH 4 after 40 min by a conventional extraction-procedure, which used a separatory funnel, in spite of the slow complex formation reaction. By the present method, the excess reagent (PAN) with iron complex was back-extracted into 6 M HNO3 solution. The extraction rate for the nickel-PAN complex decreased with the extraction time. Consequently, the nickel-complex was not extracted at pH 4 into the chloroform by the present method. The nickel, iron and cobalt were separated in three phases. The cobalt complex in the chloroform was determined directly in the range of 125μg by measurement of the absorbance at 570nm. The nickel remaining in the extraction vessel and the iron in the back-extraction vessel were determined with PAN after pH adjustment.
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  • Masashi GOTO, Kazuo MORIKAGE, Yukihiro ESAKA, Bunji UNO, Kenji KANO
    1994 Volume 43 Issue 5 Pages 403-408
    Published: May 05, 1994
    Released on J-STAGE: January 15, 2010
    JOURNAL FREE ACCESS
    Two kinds of simple, micro-enzyme electrodes were devised for a more highly sensitive detection of acetylcholine and choline. The first electrode was made by directly cross-linking acetylcholinesterase (AChE) and choline oxidase (ChO) using glutaraldehyde vapor on a micro platinum disk (diameter 200μm). The second electrode was made by cross-linking with glutaraldehyde vapor after adsorbing AChE and ChO into platinum black particles. By micro flow injection analysis the amperometric performance of the first electrode was found to be better than that of the second one. The detection limit was 20fmol for acetylcholine and 10fmol for choline in the first electrode. The first electrode was successfully utilized as the amperometric detector for micro high performance liquid chromatography.
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  • Hiroshi IMAIZUMI, Kazuhiko FUNAYAMA
    1994 Volume 43 Issue 5 Pages 409-413
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    The hydrogen-isotope exchange reaction between ethanol (unlabeled) and one of three cation-exchange resins labeled with tritium has been observed at 4080°C. The acidity (acidity based on kinetic logic) at each temperature has been obtained from a A "-McKay plot based on the respective data obtained. The following results have been obtained on the basis of both the acidities obtained in this work and the acidities (of several materials) obtained previously. (1) The order of the reactivity is (Amberlite IRC-76) >(Dowex A-1) >(PVA2000) > (Amberlite IRC-50) at 60°C. (2) The higher the temperature, the larger is the reactivity of each material. (3) The temperature dependence of the reactivity of Dowex A-1 is the largest in the four. (4) The reactivity of the functional group (i.e., COOH group or OH group) bonded to the polymer chain can be clarified using the A"-McKay plot method. (5) It seems that method can be applied to analyze other reactions, e.g., other isotope-exchange reactions, surface reactions, catalytic reactions, etc.
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  • Takeshi YAMADA, Takeshi SAKAI, Akio KIN, Masanori SATO
    1994 Volume 43 Issue 5 Pages 415-418
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    A chemical bimetal comprises a combination of two kinds of polymer plates having different characteristics regarding certain physical quantities of a dipping solution. One plate does not shrink or expand in the solution. The other plate contains a substance that is sensitive to the dipping solution, and either shrinks or expands. The chemical bimetal thus curves according to the reactive substance concentration in the solution. A copper ion-responsive chemical bimetal comprised a reaction film, which was made from 25% 7-(dodecenyl)-8-quinolinol (LIX26), 25% dioctyl phthalate (DOP) and 50% polyvinyl chloride (PVC), and polyester film. The thickness of the reaction layer was 0.6 mm and that of the polyester film was 0.1 mm. This chemical bimetal responded to the copper ion and showed an almost linear response from 0.01 to 0.15 mM. The amount of change in the position (ACP) of the chemical bimetal was 7.9 mm in a 0.1 M acetate buffer solution containing 0.15 mM copper ion (pH 4.5). The interferences of Fe3+, Ni2+, Zn2+, Al3+, and Cd2+ on the response of copper ion by the chemical bimetal were investigated at various reaction times and pH.
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  • Hirofumi KURAYASU, Yasuo INOKUMA, Masanari KIMOTO
    1994 Volume 43 Issue 5 Pages 419-423
    Published: May 05, 1994
    Released on J-STAGE: May 25, 2010
    JOURNAL FREE ACCESS
    A method for determining 480 mg m-2of Tl, Pb, Cd, Sn, In, Cu and Sb in zinc electroplated films on steel sheets has been developed. Although (1+9)H2SO4 containing 100 μg cm-3 of N, N-dimethylthiourea (Acid A) was capable of dissolving the films without dissolution of the steel sheets, Sb was reduced in the presence of nascent hydrogen to escape as volatile SbH3 and Cu was incompletely dissolved to remain on the steel sheets. Dissolution with conc. HNO3 under cooling resulted in the complete recovery of Sb and Cu, although the steel sheets were dissolved a little. Therefore, dissolution with Acid A was adopted for the determination of Tl, Pb, Cd, Sn and In, and conc. HNO3 for Cu and Sb. Nitric acid was removed by fuming with H2SO4 after dissolution of the films. Thallium, Pb, Cd, Sn, In, Cu and Sb were determined by differential pulse anodic stripping voltammetry according to the procedure described in a previous paper. A relative standard deviation (n=5) of about 3% was obtained. In addition, the quantities of these elements in the films were correlated with the concentrations of the elements in the electroplating baths.
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  • Yuji NISHIKAWA, Kunihiro FUJIWARA, Kiyoko TAKAMURA
    1994 Volume 43 Issue 5 Pages 425-429
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
    Surface-enhanced infrared spectroscopy was applied to the trace analysis of residual additives on several agricultural product surfaces. The surface species were transferred onto silver-coated barium fluoride substrates by pressing the substrates. To clarify the optimum sampling conditions, the effects of the pressure and pressure time were examined with the use of model samples (polyethyleneterephthalate films coated with several amounts of silicone resin). The best obtained conditions were 200g/cm2 and 1 min.The correlation between the amounts of surface silicone and the SEIRA intensity was also studied. A good correlation was obtained between the sample amounts of 50200ng/cm2. The method was actually applied to four different cultivated fruits (lemon, grapefruit, cherry and mandarin orange). Small amounts of silicone additive were identified from the lemon, grapefruit and cherry surfaces. These fruits were produced in foreign countries.
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  • Hisashi MORIKAWA, Jun NISHIMOTO
    1994 Volume 43 Issue 5 Pages 431-434
    Published: May 05, 1994
    Released on J-STAGE: May 29, 2009
    JOURNAL FREE ACCESS
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