BUNSEKI KAGAKU
Print ISSN : 0525-1931
Volume 44, Issue 11
Displaying 1-13 of 13 articles from this issue
  • Yoshinobu BABA
    1995 Volume 44 Issue 11 Pages 883-893
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    Capillary electrophoresis equipped with a multi-color detectable laser-induced fluorescent DNA detector (CE-LIF) was developed. We examined the efficiency and the performance of the CE-LIF system for high-speed DNA sequencing and gene diagnosis. The effect of the gel composition, electric field strength, and capillary length on the separation of DNA sequencing reaction product was investigated in order to achieve highspeed DNA sequencing for large-scale sequencing in the Human Genome Project. The CE-LIF system is successfully applied to ultrafast cDNA sequencing for human and yeast genomes. Under optimum separation conditions, only 10 min is required to sequence 300 base DNA. A polymer solution of cellulose derivative was utilized as a sieving medium for the CE-LIF system and gave excellent resolution of polymerase chain reaction (PCR) amplified human apolipoprotein B and E genes. The CE-LIF system is successfully applied to gene diagnosis for heart disease through VNTR (variable number of tandem repeat) analysis of human apolipoprotein B gene and Alzheimer's disease through RFLP (restriction fragment length polymorphism) analysis of human apolipoprotein E gene with high-speed and high resolution.
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  • Jun YOSHINAGA
    1995 Volume 44 Issue 11 Pages 895-903
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    Application of plasma ion source mass spectrometry (ICP-MS, ICP-high resolution MS, and N2-MIP-MS) to trace element analysis of clinical samples was described. Multi-element analysis of human organs by ICP-MS provided fairly abundant information on the levels of various trace elements. However, enormous Ca and P matrices of human bone hampered sensitive determination of trace elements in this matrix. Analysis of metals in human serum by ICP-quadrupole MS was thought to be difficult because of the low levels involved and matrix-related problems, i.e., spectral interference and matrix effect, although this did not hold true for the analysis of I in human body fluids. Use of ICP-high resolution MS was found to be promising for sensitive determination of Al, V, Cr and Mn in human serum at their normal levels. Isotope dilution analysis by plasma ion source mass spectrometry was an accurate and precise analytical method and it has been used for the certification of Hg and Se concentrations in a candidate reference material (human hair). Micro sampling followed by flow injection ICP-MS revealed that the distribution profile of T1 along single strands of hair allows reconstruction of the recent past history of exposure in a poisoned patient.
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  • Osamu SHIRAI, Sorin KIHARA, Yumi YOSHIDA
    1995 Volume 44 Issue 11 Pages 905-920
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    Voltammograms for ion transfer from one aqueous (W1) to another (W2) through a liquid membrane (LM), VITTM, were recorded by scanning the potential applied between W1 and W2 and measuring the current between W1 and W2. A method to analyze the VITTM by comparing VITTM with voltammograms at the W1/LM and LM/W2 interfaces was proposed. The membrane transport was demonstrated to be controlled mainly by the complementary ion transfers at the W1/LM and LM/W2 interfaces when W1, W2 and LM contained sufficient electrolytes. The influence of coexisting ions in LM or W2 on the membrane transport of an objective ion from W1 to W2 and the change of ion transfers at the W1/LM and LM/W2 interfaces during the electrolysis under an applied membrane potential were discussed. Based on the comparison of the VITTM recorded using a bilayer lipid membrane, BLM, with that recorded using an LM, the ion transport through a BLM was found to be analogous to that through anLM when the BLM contained sufficient ions. When very hydrophobic ion was added to one of the two aqueous phases in the presence of high concentration (e.g., 0.1 M) of hydrophilic salt, large symmetrical current peaks were observed in the VITTM even though the concentration of the added ion was extremely low. These peaks were attributed to transfers of the hydrophilic ion, which had been concentrated spontaneously into BLM by the distribution as the counter ion of the hydrophobic ion, from BLM to W1 and W2. Employing various ions as the additive, 4 types of VITTMs which were determined by hydrophobicities (and hence abilities to distribute into BLM) were observed. Ion transfer reactions determining each type of VITTM were elucidated. The relation between the shapes of VITTMs and properties of added ions, coexisting ions and BLMs was also discussed.
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  • Kusdiana HILMAN, Takashi GOTO
    1995 Volume 44 Issue 11 Pages 921-926
    Published: November 05, 1995
    Released on J-STAGE: January 18, 2010
    JOURNAL FREE ACCESS
    The use of trioctylmethylammonium chloride (capriquat) loaded silica gel adsorbent has been studied for the separation and determination of chromium(VI) and chromium(III). The proposed adsorbent is prepared as follows: ten grams of silica gel is shaken into 25 ml of 10% capriquat-xylene solution for 2 h. After drying in an infrared drying oven, capriquat loaded silica gel was used as an adsorbent. In this study, the adsorption of chromium(VI) and chromium(III) onto capriquat loaded silica gel was pH dependant. The optimal pH for the adsorption of chromium(VI) and chromium(III) was about 5.0 and 9.0, respectively. It was found that heated perchloric acid solution is suitable for elution of chromium(VI) and chromium(III). The eluate was determined by graphite furnace atomic absorption spectrometry. This method was applied to the determination of chromium(VI) and chromium(III) in river water samples.
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  • Toshio YAO, Ikuko HARADA, Taketoshi NAKAHARA
    1995 Volume 44 Issue 11 Pages 927-932
    Published: November 05, 1995
    Released on J-STAGE: January 18, 2010
    JOURNAL FREE ACCESS
    A sol-gel silicate-based biosensor for glucose was made up by dip coating the end surface of a platinum-disk electrode in a sol solution comprising 50μl of tetramethyl orthosilicate (TMOS) and 100 μl of 10 mM phosphate buffer (pH 5.5) containing 1.5 mg glucose oxidase (GOD), followed by drying for two days under ambient conditions. Although the prepared sensor responded rapidly (ca. 15 s) at 0.6 V (vs. Ag/AgCl), the presence of an electroactive species, such as ascorbate, interfered with the measurement of glucose. Subsequently, another sol-gel biosensor was constructed from a gel solution comprising TMOS, GOD, and peroxidase by a similar sol-gel procedure, to improve the selectivity of the sensor. This sensor responded rapidly (ca. 2030 s) to glucose at 0 V in the presence of a mediator, such as hexacyanoferrate(II) or ferrocenecarbonate, without any interference from ascorbate below 0.2 mM. A plot of the current response vs. the glucose concentration gave a straight line over the 1×10-52×10-3 M range. In addition, this sensor was well suited as a detector of a flow-injection system. Reliable results were obtained in the assays of glucose in controlled human sera.
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  • Kunihiro WATANABE, Kazuhiro ROKUGAWA, Masayuki ITAGAKI
    1995 Volume 44 Issue 11 Pages 933-938
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    The determination of manganese(II), which catalyzed a reaction between 2, 3-dihydroxynaphthalene (DHN) and ethylenediamine (en), has been investigated in the presence of hydrogen peroxide. A change in the reactants was detected by absorption and fluorometric methods. Two kinds of the intermediates, obtained from a mixture of DHN, en and H2O2, were confirmed by changes in the fluorometric spectra. One of them was used for the determination of manganese(II). The fluorescence intensity of the intermediate was measured at 500 nm with an excitation wavelength of 400 nm. The mechanism of the reaction between DHN and en is discussed based on the change in the fluorescence spectra with the reaction time. The formation of 2, 3-naphthoquinone was estimated by the reactivity of DHN and its related compounds. The 2, 3-naphthoquinone reacted with en to form a quinoxaline derivative. The role of manganese(II), which forms the DHN-Mn complex in the presence of H2O2, was only to accelerate the formation reaction of 2, 3-naphthoquinone. The reactivity of DHN to amine is discussed based on the distribution of the DHN electron density calculated by ZINDO. The limit of detection of Mn(II) by the proposed method was 3 ppt. The determination range of Mn(II) was from 10 to 140 ppt. The conditions for the determination of Mn(II) were as follows : DHN concentration, 3.6×10-4 M; H2O2, 1.2%; pH, 10; en concentration, 1.2 M; reaction time, 5 min; measurement wavelength, 400 nm/500 nm ; temperature, 30°C.
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  • Kazuo WATANABE, Yukio TOIDA
    1995 Volume 44 Issue 11 Pages 939-942
    Published: November 05, 1995
    Released on J-STAGE: January 18, 2010
    JOURNAL FREE ACCESS
    The wet oxidation decomposition of graphite materials has been studied for the accurate determination of boron using a curcumin photometric method. A graphite sample of 0.5 g was completely decomposed with a mixture of 5 ml of sulfuric acid, 3 ml of perchloric acid, 0.5 ml of nitric acid and 5 ml of phosphoric acid in a silica 100 ml Erlenmeyer flask fitted with an air condenser at 200°C. Any excess of perchloric and nitric acids in the solution was removed by heating on a hot plate at 150°C. Boron was distilled with methanol, and then recovered in 10 ml of 0.2 M sodium hydroxide. The solution was evaporated to dryness. To the residue were added curcumin-acetic acid and sulfuric-acetic acid. The mixture was diluted with ethanol, and the absorbance at 555 nm was measured. The addition of 5 ml of phosphoric acid proved to be effective to prevent any volatilization loss of boron during decomposition of the graphite sample and evaporation of the resulting solution. The relative standard deviation was 48% for samples with 2 μg g-1 levels of boron. The results on CRMs JAERI-G5 and G6 were in good agreement with the certified values.
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  • Takenao FUJII, Matashige OYABU
    1995 Volume 44 Issue 11 Pages 943-951
    Published: November 05, 1995
    Released on J-STAGE: January 18, 2010
    JOURNAL FREE ACCESS
    Recently, X-ray photoelectron spectrometers equipped with a magnetic immersion lens have been widely used. Low-energy electrons ejected from a filament are guided to the sample surface by a magnetic field and bias voltage for neutralization. This charge neutralization method was investigated using a smooth surface of polyethylene and polypropylene as a sample, and using beads of polypropylene with X-rays of Mg Kα source and monochromatized Al Kα source. The charge shift with a monochromatized source was extremely large compared to that of Mg Kα source. The optimum bias voltage was found to be -4.0V to -4.5V. Although the "differential charging" phenomenon was observed in the analysis of polypropylene beads, it was compensated by a bias of -4.0V. Thus, the dependences of the optimum bias voltage on the magnitude of the charging and form of the sample are small in the neutralization method. This neutralization method was applied to an analysis of polyethylene and polypropylene, photo-resist film and polymer alloy. Polyethylene and polypropylene were distinguished from each other by mapping using valence-band spectra. The high-resolution spectrum of C1s was obtained from a photo-resist film of 150μm square on a silicon substrate. Mapping of the small particles of polypropylene which were dispersed in rubber was successfully achieved.
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  • Hiroyuki NAGASAWA, Yasaburo KATO, Masahisa ENOMOTO
    1995 Volume 44 Issue 11 Pages 953-956
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    We report a novel method for analyzing trace metallic impurities on a Si wafer. The technique using an indicator-rod was developed for collecting metallic impurities, and their concentrations were measured by graphite furnace AAS. Since the operation of the impurity-collecting apparatus was simple and easy, no additional contamination was found on the sample wafer during the collecting operation. The use of a small amount of hydrofluoric acid solution was sufficient to collect metallic impurities completely. For a 6-inch Si wafer, the present method was applicable to the determination of 108109 atoms cm-2 for most metallic impurities.
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  • Syuji OKUYAMA, Toshiyuki MITSUI, Yoshikazu FUJIMURA
    1995 Volume 44 Issue 11 Pages 957-959
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    The phosphate ion in beverage was determined by multivariate analysis with standard addition method. Sodium phosphate and sodium chloride was added to the drink as a standard solution and internal standard, respectively. Phosphate ion was transformed to silver phosphate and chloride ion was transformed to silver chloride by silver nitrate. Obtained samples were analyzed by an X-ray diffraction method. Principal component analyses were carried out using the intensities of the relevant peaks and the principal component score was obtained. The content of phosphate ion in beverage was calculated from the obtained score.
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  • Minato ANDO, Masahiro OKUBO, Takashi KATO, Koji OKADA, Junichi TOKUMOT ...
    1995 Volume 44 Issue 11 Pages 961-964
    Published: November 05, 1995
    Released on J-STAGE: January 18, 2010
    JOURNAL FREE ACCESS
    The application of tubular liquid membrane to an ethanol sensing device was tried using FIA. The membrane was formed by impregnating methyl hydrogene polysiloxan (MHPS) in the porous wall of a ceramic tube. When the tube containing water was immersed in an aqueous ethanol solution, the ethanol dissolved in MHPS and diffused into the water, forming a radial gradient of ethanol concentration. A laser beam transmitted through the tube was expanded by concave-lens effect. The drop in power density of the transmitted beam was roughly correlated with the ethanol concentration. However, reproducibility of data was unsatisfactory, possibly due to disturbance of the boundary between the ethanol solution and carrier water.
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  • Shigeru TERASHIMA, Noboru IMAI, Masumi UJIIE
    1995 Volume 44 Issue 11 Pages 965-969
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    In order to know the level of analytical errors caused by an uneven element distribution in the analyses of small amount of geological materials, twelve selected rock reference samples from the Geological Survey of Japan were analyzed by AAS and ICP-MS after dissolving each sample with HClO4 and HF. The relative standard deviation in the analyses of six major elements for four 5 mg portions of each sample were smaller than 8%, and those of twenty-nine minor elements for three 10 mg portions were within 15 %, except for Cu, Zr, Mo, Th, and U in a few reference samples. The analytical errors of plutonic rocks were generally larger than those of volcanic rocks, reflecting the particle size of rock-forming minerals. The analytical errors originating from the heterogeneous distribution of each elements in the small amounts of rock reference samples were found to be less than or similar to the variation range of analytical data reported recently from collaborating laboratories.
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  • Miho SUZUKI, Takeshi MISUMI, Tadashi MOCHIZUKI, Yoichi ISHIBASHI
    1995 Volume 44 Issue 11 Pages 971-975
    Published: November 05, 1995
    Released on J-STAGE: June 19, 2009
    JOURNAL FREE ACCESS
    Rapid method has been developed for the spectrophotometric determination of silicon in high silicon steel samples. The steel samples were placed in a polypropylene volumetric flask and decomposed with a mixture of 20 ml of (1+3) HNO3 and 4 ml of 20% NH4FHF at 50°C. The clear contents obtained were diluted with distilled water after the addition of H3BO4. The sample solutions were analyzed with a flow-injection system involving a measurement of the absorbance of yellow Si-Mo complexes at 450 nm. The analytical results agreed with the results obtained by the gravimetric method. The proposed method permitted the analyses of 30 samples per 4 h.
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