BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 41, Issue 11
Displaying 1-17 of 17 articles from this issue
  • Shogo SUZUKI, Shoji HIRAI
    1992 Volume 41 Issue 11 Pages 521-525
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    When γ-rays from short-lived nuclides are counted using a γ-ray spectrometer for an instrumental neutron activation analysis (INAA), a counting loss often occurs due to the high counting rate. A pile-up rejector electric circuit was thus installed in the γ-ray spectrometer (GAMA-III system) in order to correct for this counting loss. To measure the decay of the radioactivities for short-lived nuclides during the counting period, the dead-time rate per second in a multichannel pulse height analyzer of the γ-ray spectrometer was sampled during the counting period. In this system, the counting loss could be exactly corrected up to a 20 kcps counting rate over the total acquired energy region. This system was applied to the determination of vanadium at NIES (National Institute for Environmental Studies of Japan) in No. 6 Mussel and No. 7 Tea Leaves certified reference materials. These reference materials (ca. 47203 mg) and the vanadium standard were irradiated for 1 min at a thermal neutron flux of 1.5 × 1012 n cm-2 s -1 at the reactor of the Musashi Institute of Technology Research. The irradiated samples were cooled for 2 min and counted for 4 min using this system. The vanadium concentration in the Mussel was 0.75 ±0.08 ppm, which was more accurate and precise than the previously reported value (0.45±0.31 ppm). The vanadium concentration in the Tea Leaves was 0.37 ppm.
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  • Motoyuki MATSUO, Takaaki KOBAYASHI
    1992 Volume 41 Issue 11 Pages 527-532
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The chemical states of iron in suspended solids collected from ten sites along the Tamagawa river, which originates in the mountainous area outside Tokyo and flows into Tokyo bay, have been investigated by 57Fe Mossbauer spectroscopy to examine how they reflect the contribution of human activities. The Mossbauer spectra of suspended solids from the upper stream consist of two doublets corresponding to paramagnetic Fe2+ and Fe3+ species, whereas those from the lower stream consist of one doublet ascribable to Fe3+ species. The Fe2+/Fe3+ratios of the samples decrease from upper stream towards downstream. On the other hand, X-ray microanalysis revealed increasing phosphorus and sulfur contents of the suspended solids towards downstream, showing that the lower reaches are polluted by domestic sewage. These facts suggest that the Fe2+/Fe3+ratio decreases with increasing human activity.
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  • Tomoko HARADA, Shigeo TANUMA
    1992 Volume 41 Issue 11 Pages 533-537
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    We have analyzed four kinds of Co-Ni alloys by Auger electron spectroscopy using the low-energy Auger peaks. The used standards specimens were pure cobalt and nickel. We measured the Auger peaks over the range 3090 eV (0.2 eV steps) on every specimen with the beam brightness modulation method in order to take the EN (E) spectrum. Since the Co and Ni peaks of the alloys overlapped each other, we carried out peak separation using the peak-synthesis method with the non-negative least-square curve fitting method developed by Minami et al. Three kinds of filtered spectrum were used. The digital filters used for subtracting the background were the first derivative, the 2nd derivative and the top-hat filter. Every filtered spectrum gave excellent results regarding the peak separation of Co and Ni. No matrix effect corrections were needed for the Co-Ni alloys. The resulting surface Co concentration in the alloys agreed well with the actual bulk concentration of Co.
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  • Syuji OKUYAMA, Toshiyuki MITSUI, Yoshikazu FUJIMURA
    1992 Volume 41 Issue 11 Pages 539-544
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Based on a multivariate analysis of the X-ray diffraction patterns of 112 powder samples of SiO2, Al2O3 and CaO mixtures of known contents, the I/I0 ratios for 9 sets of 2θ values were chosen for further statistic analysis. The data principal component analysis for a data matrix of 6 × 9 gave the approximate contents of SiO2 and Al2O3 in a sample. The accurate SiO2 and Al2O3 contents of 8 samples calculated from the principal component score were identical to the theoretical values within 1.58%.
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  • Natsuo FUKUMOTO, Yoshinori KOBAYASHI, Masayasu KURAHASHI
    1992 Volume 41 Issue 11 Pages 545-550
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    An X-ray fluorescent element mapping spectrometer (XEMS) with spatial resolution better than 20μm has been developed. X-Rays from a fine focus X-ray tube (Cu target) were finely focused by a glass capillary (internal diameter ca. 20 μm) and the fluorescent X-rays detected with high efficiency by two large sensitive area (80 mm2 each) Si(Li) detectors placed in close proximity to the sample position. Changes of elemental distributions in leaves of a leguminous plant damaged by artificial acid rain and highdose X-ray irradiation were studied. In the case of the sample exposed to artificial acid rain, quick reduction of K, Mn and Ca concentrations in the damaged area was followed by accumulation of the former two elements. On the other hand, high dose X-ray irradiation caused intense accumulation of Ca around the damaged part. A sliced tissuefrom an autopsied patient with brain calcification was also investigated. A formalinfixed brain slice embedded in methyl methacrylate was cut about 200 μm in thickness with a diamond cutter and examined by the XEMS. Concentrations of elements such as Ca, Fe and P were found to be high in what was probably the internal surface of a capillary vessel. This finding supports the hypothesis that calcification may begin with segregation of hydroxyapatite in vessels.
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  • Jun ITO, Norio TERAMAE, Masahide NOJI, Hiroki HARAGUCHI
    1992 Volume 41 Issue 11 Pages 551-554
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    FT-Raman spectra of several platinum phosphine complexes were measured for the frequency region from 150 cm -1 to 3400 cm -1. A Nd : YAG laser (1064 nm) was used as the excitation source for Raman measurements. Powdered samples were placed in a rotatable quartz capillary cell, and Raman scattering from a sample was collected with a back-scattering optical arrangement. Raman shifts of platinum-ligand stretching frequency were assigned for each complex. Based on the assignments, the following relationship was found. That is, as the Pt-N stretching frequency is increased, the Pt-P stretching frequency decreases. This relationship was discussed in terms of the trans effect. This means that FT-Raman spectroscopy can help predict the activity of a complex.
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  • Ji-Ye JIN, Wataru FUJITA, Jun ITO, Norio TERAMAE, Hiroki HARAGUCHI
    1992 Volume 41 Issue 11 Pages 555-559
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The adsorption of aniline on the surface of a silver electrode in a neutral electrolyte aqueous solution was studied by FT-surface enhanced Raman scattering (SERS). A strongly enhanced Raman spectrum of aniline adsorbed on a silver surface was observed after roughening the silver electrode with an oxidation reduction cycle treatment. The SERS spectra revealed that aniline adsorbed on the electrode could be polymerized, even at a much less positive potential (+0.15 V vs. SCE) under laser-beam irradiation. The product on the electrode surface was also characterized by FT-IR microspectroscopy. As a result, it was indicated that polyaniline was formed only at the laser-irradiated site.
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  • Nobuaki ISHIDA, Hiromi KANO, Hidejiro OGAWA
    1992 Volume 41 Issue 11 Pages 561-566
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A method for measuring the spectra of the 1H-NMR of localized region on an image of a food material was devised using a spectrometer (JEOL GSX-270 WB) and its microimaging system. The spin-echo two-dimensional FT method was used for the measurements. The slice thickness of a sample was regulated by a copper cover with a 1.5 mm slit in the sample holder. The area on the X-axis was restricted by selective excitation under an X-axis gradient magnetic field. The position on the Y-axis was selected after FT of the spectral data incorporated with phase encoding. The spectra in areas of 0.3 mm × 0.05 mm on the 1H-NMR image were obtainable by this method. The localized spectra of sausages made of three different materials and processes were measured in order to discuss their tissue structures.
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  • Nobuaki ISHIDA, Hiromi KANO, Hidejiro OGAWA, Hisahiko WATANABE
    1992 Volume 41 Issue 11 Pages 567-572
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Since many biological events are carried out in the water phase or in organelles surrounded by water in plant tissues, the mobility of cell-associated water is affected by and controls cell activities. Hence, in this investigation, the self-diffusion coefficient of water (mobility) and its fluctuation map in Welsh onion (Allium fistulosum L. var. caespitosum Makino) tissues were measured using an NMR microscope equipped with a generator providing a pulse gradient magnetic field. Gradient magnetic fields up to 278 mT/m for the diffusion measurement were applied between 90° and 180° pulses, and between the 180° pulse and acquisition time of an imaging pulse sequence. The self-dififfusion coefficient of H2O estimated by the Stejskal and Tanner's equation at room temperature was (2.11 ± 0.08) × 10 -5 cm2/s, agreeing well with the reported value (2.14 ×10 -5 cm2/s). The diffusion emphasized image of Welsh onion leaves was similar to theT1 emphasized image. The self-diffusion coefficient of cell-associated water of Welsh onion leaves varied from 0.4 to 1.7 × 10 -5 cm2/s among and within tissues. Water in the leaf epidermis and vascular bundles showed higher values than that inside leaves.
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  • Hiromu SATAKE, Miho WAKATSUKI, Shoji KANESHINA, Atsuko YOKONO, Satoshi ...
    1992 Volume 41 Issue 11 Pages 573-580
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    A coated-wire electrode sensitive to a local anesthetic bupivacaine cation was prepared by coating copper wire (0.6 mm or 0.2 mm diameter) with a poly(vinyl chloride)(PVC) membrane of 0.30.6 mm thickness. The PVC membrane included a plasticizer and an ion-exchanger forming an ion-pair with bupivacaine. Five ion-exchangers and three plasticizers were used for the electrode membrane. The response time and the slope of the electromotive force vs. bupivacaine concentration curve were examined for electrodes with various membrane compositions. The best results were obtained from an electrode with a PVC membrane composition as follows: (1) ion-exchanger: {sodium tetrakis[3, 5 bis(trifluoromethyl)phenyl] borate (15 mg) or dodecatungstophosphoric acid (25 mg)} or ion-pair: bupivacaine-dodecatungstophosphate (2 mg) ; (2) one of the plasticizers: dioctyladipate (100 mg), dioctylsebacate (100 mg), dioctylphthalate (150 mg) ; (3) PVC (100 mg) ; and (4) solvent: tetrahydrofuran (1.5 ml). The electrodes showed linear responses with Nernstian slopes (5863 mV/decade) over a concentration range of 3 × 10-5 10-2 M. In measurements with the electrode incorporating dodecatungstophosphoric acid or its ion-pair with bupivacaine used as the sensing material, the change in the pH within a range of 28 did not affect the electrode potential at 10-4 M bupivacaine. None of the inorganic and organic cations which occur in important biological samples was found to interfere, as judged by the very small values of the selectivity coefficients. The selectivity coefficients of the bupivacaine electrode toward other local anesthetics decreased in the order dibucaine>tetracaine>mepivacaine = lidocaine = procaine. A bupivacaine electrode with the PVC membrane, in which bupivacainedodecatungstophosphate ion-pair and dioctylphthalate were incorporated, was applied to monitoring the bupivacaine concentration in the artery of a rabbit. This electrode is available for measurements of the bupivacaine concentration in vivo.
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  • Chushiro YONEZAWA, Hideki IMAI, Tetsuro HONGO, Michio HOSHI, Enzo TACH ...
    1992 Volume 41 Issue 11 Pages 581-587
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    An instrumental neutron activation analysis (INAA) method for simultaneously determining the Se and Zn concentrations in serum specimen was developed in order to study and clarify the associations between prediagnostic serum Se and Zn, and the subsequent risk of lung and stomach cancer in which the amount of available sera was quite limited. Cerium was used as an internal standard in order to maintain the accuracy and precision, even with less than 0.2 ml of a sample and short measuring time. Samples, (0.10.2 ml), and Se-Zn standard solutions were mixed with exact amounts of the Ce standard solution, respectively. After lyophilization, the samples were sealed in a high-purity quartz tube. The Se-Zn standard solutions were also sealed in a quartz tube without lyophilization. The samples and standards were irradiated in the JRR-2 with a thermal neutron flux of more than 2.2 × 1013 n cm-2 s-1 for 265.5 hours. After cooling for one month, about 5 μm surface layers of the quartz ampule for the samples and standards were etched with hydrofluoric acid; γ-ray spectra were then measured with a Ge(Li) detector. The contents of Sc and Zn were obtained from the peak area of γ-rays of 145, 265 and 1115 keV for 141Ce, 75Se and 65Zn, respectively. The relative standard deviations of the analytical results among the 14 independent samples were 3.0 and 5.0% for Se and Zn, respectively. The accuracy of the present method was confirmed by the satisfactory agreement between the results obtained by the present method and those obtained by other methods, including the certified values of NIST Standard Reference Materials of Bovine Liver (SRM1577, SRM1577a).
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  • Toshihisa MARUTA, Shigeru YOKOYAMA, Hideki KOBAYASHI, Takeshi YAMANE
    1992 Volume 41 Issue 11 Pages 589-592
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A simple, rapid method for the simultaneous determination of the major and minor elements in high-purity mullite by XRF analysis is presented. The preparation of glassbead samples with a lower dilution factor was studied in detail in order to improve thes tability of XRF measurements and analytical sensitivity. A 1.5 g sample was fused with a 4.5 g flux (mixture of LiBO2 and Li2B4O7 in a 1 : 1 ratio) in a platinum crucible containing 5% Au at 1100°C for 6 min. Lithium bromide (75 μl of 50% solution) was added into a flux as a removing additive. The proposed method was applied to the simultaneous determination of Al2O2, SiO2, ZrO2, MgO, TiO2, Na2O, CaO, Y2O3, Fe2O3, K2O, HFO2 in high-purity mullite; the results agreed well with those obtained by an ICP-AES analysis.
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  • Shigeaki YONEMORI, Eiji ICHIKURA, Masuo SUGIZAKI
    1992 Volume 41 Issue 11 Pages 593-595
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    A quantitative analysis of an oxygen-containing co-monomer in organic copolymers by an XRF oxygen analysis was investigated. An X-ray fluorescence spectrometer was equipped with a diffraction device having synthetic multilayers (2d=8.06 nm) and a gasflow proportional counter as a detector for the O Kα line with a 0.6 μm polyester film window. The X-ray tube was used with a large current under low potential (40 kV-70 mA); the intensities of the O Kα peak (2θ=34.325°) and those of the background (2θ=33.00, 36.03°) were measured three times for 100 s and 3 times for 50 s, respectively. A calibration curve was constructed based on the oxygen contents of tetrafluoroethylene/perfluoro(propylvinyl ether) copolymer, determined by the IR method. It showed good linearity over an oxygen content range of 0.12% (110 mol % as co-monomer); the relative standard deviation was 2.7% for seven measurements of a 1.12 % oxygen-containing polymer. A rapid, nondestructive determination method of an oxygen-containing co-monomer by XRF was thus established.
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  • Nobuaki KUCHITSU, Yoshimitsu HIRAO
    1992 Volume 41 Issue 11 Pages 597-599
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Mineral mapping of the surface of deteriorated cultural property was attempted with a micro X-ray diffractometer. The profile of the surface rust on a bronze object has been analyzed as an example. Atacamite (Cu2Cl(OH)3) has mainly been observed in the outer green rust area, whereas cuprite (Cu2O) has been observed in the inner red area. This result positively shows the stratified structure of bronze rust. This mineral mapping method may be effective for nondestructive analysis of not only cultural property but also any other materials which have a microstructure or heterogeneity.
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  • Hidehiko KANETA, Machiko TEZUKA, Shigeyuki TANAKA
    1992 Volume 41 Issue 11 Pages 601-603
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    The carbonate and clay mineral contents in oil-reservoir rock samples were determined from their diffuse reflectance IR spectra. Both rapidity and simplicity are required for this method, since many samples must be treated. Rock samples were ground into fine particles and measured without dilution. We used the peak-hight ratios of 2500 cm-1 (carbonate) and 3600 cm -1 (clay) to 1880 cm-1. The peak at 1880 cm -1 is characteristic of quartz. We confirmed the high reproducibility of this method by carrying out examinations with mixtures of standard mineral samples (RSDs were within 10%). The actual results for 39 rock samples showed a good correlation with those by XRD.
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  • Yasuyuki HOSHIKA
    1992 Volume 41 Issue 11 Pages 605-608
    Published: November 05, 1992
    Released on J-STAGE: February 16, 2010
    JOURNAL FREE ACCESS
    Two critical-point dry pellet samples of a human foot articulation hypodermic tumoral carcinosis by direct paracentesis and mass extirpation were investigated by particle-induced X-ray emission spectrometry (PIXE) and X-ray powder diffractometry. The data show that the Cu-high concentration due to rheumatoid arthritis, uric acid(-Na) monohydrate, CaHPO4·2H2O, (NH4)2FeP2O7·2H2O are represented as major uric acid (-Na) and minor pyrophosphate in the samples
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  • Minoru KAWASAKI
    1992 Volume 41 Issue 11 Pages T135-T140
    Published: November 05, 1992
    Released on J-STAGE: June 30, 2009
    JOURNAL FREE ACCESS
    Nondestructive analysis methods represent an indispensable condition for stamper quality evaluations. The nondestructive analysis methods used for stamper quality evaluations take advantage of ultrasonic microscopes, fluorescent microscopes, magnetic stress measurements, scanning electron microscopes, scanning tunnel microscopes and laser measurements. These nondestructive analysis methods all have their merits and demerits ; the establishment of stamper quality evaluation technology is aimed at while making good use of their characteristics to expand the application range.
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