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Hitoshi OGATA
1990 Volume 6 Issue 3 Pages
327-340
Published: June 10, 1990
Released on J-STAGE: June 30, 2006
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Applications of surface-sensitive analytical techniques to research and development of III-V semiconductor materials are illustrated. The studies reviewed are related to the understanding of various aspects of material processing such as epitaxial growth by molcular beam epitaxy, diffusion of group II elements in InP, ion implantation of n- and p-type dopant species, and dry etching in chlorine-containing discharges. In addition, impurity-induced layer disordering of quantum well heterostructures and superlattices will be discussed. Examples are drawn from a number of analytical techniques sensitive to the surface and to the interface. Special emphasis is given to GaAs and InP which are currently under study most extensively.
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Katsumi UCHIYAMA, Keiko OHSAWA, Tetsuya MITA, Yoshihiro YOSHIMURA, Kaz ...
1990 Volume 6 Issue 3 Pages
341-345
Published: June 10, 1990
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Photoacoustic densitometry by using a fast laser beam with sinusoidal scanning was conducted. The signal distortion was improved by using a sinusoidal scanning system combined with a Bessel high-pass filter. However, small distortions were found to remain in the densitograms, compared with those produced by conventional light scanning. Ovalbumin was two-dimensionally electrophoresed, followed by blotting on a nitrocellulose sheet. The signal intensity of ovalbumin on a nitrocellulose sheet was about 5-times greater than that on polyacrylamide gel. The reproducibility (RSD) of measurements for ovalbumin on four different nitrocellulose sheets was in the 8-15% range. However, the value was less than 5% for measurements of ovalbumin on the same plate. The detection limit of ovalbumin was about 150ng. Ovalbumin, 1.67μg of which was spiked in calf serum, was almost recovered by the method.
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Akiko TAKATSU, Sueo NISHI
1990 Volume 6 Issue 3 Pages
347-350
Published: June 10, 1990
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Isotope dilution mass spectrometry with liquid chromatography for the determination of serum creatinine is studied. After adding labeled (
15N
2) creatinine to the serum, creatinine was isolated using high performance liquid chromatography. Measurements were performed by electron impact mass spectrometry with use of a direct insertion device. Analytical results of the NIST (formerly NBS) SRM serum showed satisfactory agreement with the certified value; the relative standard deviation of about 2% was obtained.
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Kazuo UCHIKURA
1990 Volume 6 Issue 3 Pages
351-354
Published: June 10, 1990
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A postcolumn derivatization method using electrochemical oxidation was developed for the determination of vanilmandelic (VMA) and homovanillic (HVA) acids in human urine. Both acids were extracted with ethyl acetate from urine under acidic conditions and separated by ion-exchange chromatography on a Hitachi-gel #3011-N column.They were derivatized to fluorescent products by electrochemical oxidation and their fluorescence intensities were measured (Ex 315nm, Em 420nm). The calibration curves were linear in the range from 5 to 120ng. The detection limits (
S/N=3) for VMA and HVA were 24 and 12ng per ml of urine, respectively. The relative standard deviations (
n=5) for VMA and HVA were 7.5 and 5.5% at mean concentrations of 1.0 and 2.2μg ml
-1, respectively. The method was successfully applied to a simultaneous determination of VMA and HVA in the urine of patients with neuroblastoma and of healthy volunteers.
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Naohiro NISHIMURA, Akimasa SHIBUKAWA, Terumichi NAKAGAWA
1990 Volume 6 Issue 3 Pages
355-359
Published: June 10, 1990
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A high-performance frontal analysis method using a polyvinyl alcohol gel as a stationary phase has been developed for the determination of the free concentration of relatively hydrophilic drugs (salicylate and acetazolamide) in the state of a drug-protein binding equilibrium. When an excess volume of a drug-albumin mixed solution was injected directly to this column, the drug was eluted as a broad peak with a plateau region following the protein peak. When the free drug fraction was higher, a larger injection volume was necessary to obtain the plateau region. The free drug concentration was determined from the plateau height; the results agreed well with those obtained by the ultrafiltration method. The total salicylate concentration could be simultaneously determined from the peak area. The present method was applied to an estimation of the salicylate-albumin binding parameters. The obtained values agreed well with the reported values. The present method enables a simple and rapid determination of free drugs in protein binding equilibrium.
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Tetsuharu IWATA, Masatoshi YAMAGUCHI, Hiroshi HANAZONO, Yuki IMAZATO, ...
1990 Volume 6 Issue 3 Pages
361-366
Published: June 10, 1990
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A column-switching high performance liquid chromatographic method with fluorescence detection for the determination of vitamin D
3 and 25-hydroxyvitamin D
3 in human and rat sera is described. The vitamins in a lipid extract from serum, obtained by solid-phase extraction technique using a Bond-Slut C
18 cartridge, are converted with 3, 4-dihydro-6, 7-dimethoxy-4-methyl-3-oxoquinoxaline-2-carbonyl azide into the corresponding fluorescent derivatives. The derivatives are separated from endogenous interfering substances by column-switching chromatography. The chromatographic system consisted of a precolumn chromatography for clean-up of the derivatives and an analytical column chromatography for the complete separation of the derivatives. The derivatives are detected fluorometrically at excitation and emission wavelengths of 360 and 440nm, respectively. The detection limits (
S/N=3) for vitamin D
3 and 25-hydroxyvitamin D
3 are 15 and 8fmol, respectively, in a 10μl injection volume. The sensitivity permits simultaneous determination of the vitamins in 1ml of normal human and rat sera.
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Kozo HIKIDA, Yoshimasa INOUE, Norio KOJIMA, Yosuke OHKURA
1990 Volume 6 Issue 3 Pages
367-370
Published: June 10, 1990
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An automated column-switching high performance liquid chromatographic method with ultraviolet detection is described for rapid and sensitive determination of clocapramine, a psychotropic drug, and its two metabolites, clospipramine and dehydroclospipramine, in dog and human plasmas. The drug and the metabolites were extracted together with trifluperidol as an internal standard with a heptane-chloroform mixture from plasma. The extract was subjected to column-switching high performance liquid chromatography using a bovine serum albumin-coated cyanopropyl silica gel column, a newly developed sample clean-up column, and a reversed phase column (TSK gel ODS-80TM) for analytical separation.The detection limits (
S/N=3) of clocapramine, clospipramine and dehydroclospipramine were 0.5-1.0ng ml
-1.
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Kenji SUEOKA, Yoshimi NAGAI, Masatoshi NAGATA, Sadao SEGAWA
1990 Volume 6 Issue 3 Pages
371-374
Published: June 10, 1990
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Compositional analyses of liquid crystalline aromatic polyesters prepared from p-hydroxybenzoic acid (PHB), terephthalic acid (TA) and biphenol (BP) were examined using NMR, IR, pyrolysis-GC and hydrolysis-HPLC. The best method was hydrolysis-HPLC. Hydrolysis of the polymers was carried out under the condition of strong alkalinity and high temperature; the obtained monomers were determined by HPLC. Small amounts of other comonomers and impurities could be determined at the same time. This method is also applicable to the compositional analysis of other systems of liquid crystalline polyesters.
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Vlastimil REZL, Alena BURESOVÁ
1990 Volume 6 Issue 3 Pages
375-378
Published: June 10, 1990
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A general method for the simultaneous determination of the carbon, hydrogen and oxygen content in terms of the oxygen balance during combustion suitable for elemental microanalysis by instrumental methods is described. The substance to be analyzed is burnt in either a mixture of helium and oxygen, or in a known amount of oxygen. The oxygen content is determined in terms of the total combustion by balancing the combustion by carbon and hydrogen and from the oxygen contribution from the sample. This method was verified on a CHN analyzer based on a separation of the reaction products by a frontal gas chromatographic technique. An example of determining solid samples by the usual method and liquid samples without weighing is presented. The principles and conditions ensuring good results and also possibilities to use the method for other elements are discussed.
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Osamu KUJIRAI, Muneyuki KOHRI, Kei YAMADA, Haruno OKOCHI
1990 Volume 6 Issue 3 Pages
379-383
Published: June 10, 1990
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Traces of hydride-forming elements in Mo have been simultaneously determined by continuous hydride generation and inductively coupled plasma-atomic emission spectrometry. The hydride-forming elements in higher oxidation states are coprecipitated with lanthanum hydroxide to separate them from the Mo matrix. Arsenic(V), Bi(III), Sb(V), Se(IV) and Te(IV) are measured by hydride generation. Effects of pH, amount of La and diverse elements on the recoveries and interferences are discussed. A standard addition method is necessary to compensate for the interferences from impurities in Mo. Detection limits of As, Bi, Sb, Se and Te in Mo are 0.2, 0.7, 2, 0.5 and 2μg g
-1, respectively.
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Hirofumi ISOYAMA, Tetsuo UCHIDA, Kyoko OGUCHI, Chuzo IIDA, Genkichi NA ...
1990 Volume 6 Issue 3 Pages
385-388
Published: June 10, 1990
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Trace metals in some biological samples were measured by the discrete nebulization technique in inductively coupled plasma atomic emission spectrometry. The small spray chamber and the time-sharing background correction system were used for the rapid measurements. Small amounts of the samples were decomposed quickly in a sealed PTFE vessel in a microwave oven. The analytical results for Al, Cu, Fe, Mn and Zn agreed well with the certified values and also with those obtained by continuous nebulization.
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Noboru IMAI
1990 Volume 6 Issue 3 Pages
389-395
Published: June 10, 1990
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A multielement analysis in rocks, based on inductively coupled plasma mass spectrometry, is described. Major interferences observed were the background signals for P, K, Mn, Fe and the doubly charged and oxide ions for Ni, Cu, Zn, Ga, Eu, Tb, Yb, Lu. Both geological certified reference material JB-1 as standard and indium internal standard were used to correct the matrix effect; 49 major and minor elements in rocks were determined successfully by using this method.
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Tasuku AKAGI, Takafumi HIRATA, Akimasa MASUDA
1990 Volume 6 Issue 3 Pages
397-400
Published: June 10, 1990
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A combination of bismuth hydride generation with a merging introduction technique, where analytes are merged with spray mist from a nebulizer on the way to ICP, has been developed for sensitive determination of bismuth. A sample solution of 20μl was led to a reaction cell inside a merging chamber and was mixed with reductant solution. The generated bismuth tetrahydride was transported to and measured by ICP-MS. With the adoption of flow system, a cyclic procedure of introductions of solutions, reactions and evacuations could be performed sequently with keeping ICP power on. The effects of acidity and volumes of sample solution and reductant on the signal were investigated in detail. The signal intensity was proportional to the amount of bismuth in solution loaded on a reaction cell in the merging chamber. The absolute detection limit of bismuth using reductant of analytical grade was 72fg, which corresponds to 1.8 ppb in 40μl solution. The present method was applied to the solutions of digested standard rocks. Results with good precision and accuracy were obtained.
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Yasuaki OKAMOTO, Teruo TAKAHASHI, Ken ISOBE, Takahiro KUMAMARU
1990 Volume 6 Issue 3 Pages
401-405
Published: June 10, 1990
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A high-enrichment method by liquid-liquid extraction using liquid surfactant membranes was developed for the determination of cobalt at pg cm
-3 levels by graphite furnace atomic absorption spectrometry (GF-AAS). Two cubic centimeters of w/o [water in oil, in this case dilute hydrochloric acid in kerosene (1:1) containing 2-ethylhexyl hydrogen 2-ethylhexylphosphonate (PC-88A)] emulsion droplets coated with sorbitan monooleate are dispersed in a resulting volume of 1000cm
3 of an aqueous sample solution (pH 4.7-5.8) containing less than 1mg of cobalt(II). The analyte is extracted into the organic phase to form a complex with PC-88A and successively back-extracted into the inner acidic aqueous phase. After the w/o emulsion phase is separated from the outer aqueous phase, the emulsions are demulsified into the organic and inner aqueous phases. The cobalt content is then determined by GF-AAS with an injection volume of 10mm
3 of the inner aqueous phase. By this procedure, a concentration factor of 550 was achieved for cobalt(II). As a result, the detection limit of cobalt was 10pg cm
-3, and the calibration graph was linear up to 1mg cm
-3 of cobalt(II). The relative standard deviation for ten replicate measurements of 50pg cm
-3 cobalt(II) was 7.1%. The results of an analysis of simulated nuclear reactor coolant water are given.
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N. MISHRA, A. GHOSH, R.K. MISHRA, K.S. PATEL
1990 Volume 6 Issue 3 Pages
407-410
Published: June 10, 1990
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A procedure for extraction-spectrophotometric determination of Mo(VI), W(VI) and Re(VII) with thiocyanate and thioacetanilide (RSH) at trace level in the complex materials e.g. ores, steel, cement dust, coal ash and waste water is described. These metals in reduced state e.g. Mo(V), W(V) and Re(IV) react with thiocyanate and RSH to give benzene- extractable colored complexes with molar absorptivity in the range of (1.90-3.06)×10
4 l mol
-1 cm
-1 at λ
max 410-470nm. The Mo and W determinations are free from interferences of the metals which are generally associated with them. The effect of various analytical variables on extraction of the metals, and the composition and the conditional extraction
constants of the complexes are discussed.
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Liliana FERNANDEZ, Roberto OLSINA
1990 Volume 6 Issue 3 Pages
411-414
Published: June 10, 1990
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The reagent 2-(3, 5-dichloro-2-pyridylazo)-5-dimethylaminophenol (3, 5-diClDMPAP) has been synthesized and its Analytical properties investigated. This reagent can be used for the spectrophotometric determination of La(III) in concentrations ranging from 0.045 to 0.72ppm. The reaction takes place at a pH between 9 and 10.8. In the presence of Triton X-100 this complex is soluble in water (ε=1.45×10
5l mol
-1 cm
-1). The maximun tolerances for cations as well as for any anions were determined. In order to overcome difficulties caused by the presence of other lanthanides, an ion exchange chromatographic technique was used.
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Joanna SZPUNAR-LOBINSKA, Marek TROJANOWICZ
1990 Volume 6 Issue 3 Pages
415-419
Published: June 10, 1990
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Several salts of
N, N-substituted derivatives of dithiocarbamic acid were studied as potential reagents for flow-injection extraction-spectrophotometric determination of copper. A specific and sensitive method for the determination of copper was developed. Copper is extracted with a chloroform solution of lead diethyldithiocarbamate (DDTC) and the absorbance of the Cu-DDTC complex is measured at 436 nm. Effects of total flow rate, sample volume, mixing and extraction coils length are studied. The detection limit is 0.04ppm of Cu and calibration graph is linear up to 2ppm Cu. The method developed was applied to the determination of copper in samples of water and plant materials showing good precision and accuracy.
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Hideko KOSHIMA, Hiroshi ONISHI
1990 Volume 6 Issue 3 Pages
421-424
Published: June 10, 1990
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A flow-injection method has been developed for the separation and determination of thallium and gold. It is based on the chromatographic separation of chloro complexes of thallium(III) and gold(III) on a Sephadex G-25 column, followed by an extraction-photometric determination with Rhodamine B. The peaks of thallium and gold are completely separated with 0.5M hydrochloric acid and 1M lithium chloride as the eluent; the retention times are 5.5 and 11.0min, respectively. The two metals can be separated and determined within the range 0-5mg l
-1 for each metal. All foreign substances examined are eluted before thallium. Thallium and gold were determined in coal fly ash and ore samples by the proposed method.
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Kitao FUJIWARA, Atsumi KURAMOCHI, Hiroyuki TSUBOTA
1990 Volume 6 Issue 3 Pages
425-430
Published: June 10, 1990
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An ozone-gas phase chemiluminescence determination of arsenic was performed for samples such as rain water, atmospheric moisture and sea water in which the arsenic concentration was less than 1ng/ml. This method is based on a combination of arsine generation from arsenite and/or arsenate, and the measurement of the chemiluminescence which occurs upon mixing ozone and arsine. The analytical results were intercalibrated with those obtained by flow injection analysis-atomic absorption spectrometry. Both results coincide with each other within 15%. It has been found by the present method that arsenic is continuously contained in rain water during rainfall. Arsenic was also measured in condensed atmospheric moisture, which was derived from aerosol particles of >0.8μm diameter. The distributions of the total and inorganic arsenic in seawater are also given. The present method is simple and can be established in observation fields, such as on a research vessel.
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M. C. MEHRA, C. PELLETIER
1990 Volume 6 Issue 3 Pages
431-434
Published: June 10, 1990
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The anions H
2PO
2-, H
2PO
3- and H
2PO
4- along with Cl
-, NO
3- and SO
42- have been simultaneously determined by single-column ion chromatography in an indirect ultraviolet detection mode. The analytical approach employs 4- amino-2-hydroxybenzoic acid as an eluent at 4mM in the pH range 5.5-6.5 and at a 2ml/min flow rate. Clean separations occur on a polymeric analytical column within 10min, and the anions can be quantified in the sub-ppm range.
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Shigenori NAKANO, Shinji KINOSHITA, Masaki IKUTA, Takuji KAWASHIMA
1990 Volume 6 Issue 3 Pages
435-438
Published: June 10, 1990
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A simple and sensitive method has been developed for the fractional determination of nanogram amounts of vanadium(IV) and vanadium(V) in natural waters. It is based on the solvent extraction of these ions with
N- cinnamoyl-
N-(2, 3-xylyl)hydroxylamine into toluene at different pH values, followed by back-extraction into a sodium hydroxide solution and on the determination of vanadium by a catalytic method using the oxidative coupling reaction of 4-aminoantipyrine with N, N-dimethylaniline. Vanadium(IV) and vanadium(V) at the 0.1-1.0ng ml
-1 level can be determined. The proposed method suffers few interferences and can be successfully applied to the fractional determination of vanadium in natural water.
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Hiroko KANEKO, Masahiro YAMADA, Koichi AOKI
1990 Volume 6 Issue 3 Pages
439-442
Published: June 10, 1990
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Cyclic and differential pulse (DP) voltammograms of dopamine (DA) in Ringer′s solution were measured at a graphite-reinforcement carbon (GRC) electrode. GRC is available as the lead of mechanical pencils. Cyclic voltammograms of DA exhibited two anodic peaks, at
ca. -0.0V and
ca. 0.4V
vs. SCE, and a cathodic peak at 0.05V vs. SCE in the solution of pH 6.8. Ascorbic acid (AA) presented an irreversible anodic wave at 0.2V at pH 6.8. Voltammograms in the mixed solution of AA and DA were not a simple sum of each voltammogram, and hence were associated with chemical complications between AA and DA. DP voltammograms of the mixed solution had an anodic and a cathodic peak at
ca. 0.05V, which were stable during 4 days′ soaking of the electrode in the solution. The anodic peak height was proportional to the concentration of DA in the range from 5.0×10
-6 to 1.2×10
-4mol dm
-3. DA could be determined quantitatively from a calibration curve in the presence of AA from 5 to 20 times larger than DA concentrations.
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Zhu-ping BAI, Toshio NAKAMURA, Kosuke IZUTSU
1990 Volume 6 Issue 3 Pages
443-447
Published: June 10, 1990
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The stripping voltammetric behavior of various anions at a chitin-containing carbon paste electrode was studied and compared with that at a chitin-free carbon paste electrode. In the pH range of solutions at which the acetylamide group of chitin was protonated, the chitin worked as an anion exchanger. Such anions as chromate, nitrite, permanganate, hexacyanoferrate(III) and vanadate were effectively accumulated onto the chitin-containing electrode, giving highly sensitive reduction or oxidation peaks. The analytical applicability of the chitin-containing electrode was investigated for chromate, nitrite and permanganate ions. The linear range of the calibration curve and the detection limit were 5×10
-8-1×10
-5 M and 3×10
-8 M for both chromate and nitrite ions, and 1×10
-7-1×10
-5 M and 6×10
-8 M for permanganate ions. The relative standard deviations were between 4 and 5% in all cases for 8×10
-7 M. The influence of diverse anions was rather significant in some cases.
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Nagao KOBAYASHI, Kayo ADACHI, Tetsuo OSA
1990 Volume 6 Issue 3 Pages
449-453
Published: June 10, 1990
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Tetrapyrazinoporphyrazine and its iron and cobalt derivatives have been studied by UV-visible absorption and magnetic circualr dichroism spectroscopy, electrochemistry and spectroelectrochemistry. Iron and cobalt complexes adsorbed onto a carbon electrode catalyze electroreduction of oxygen by two electrons to hydrogen peroxide over a wide range of pH values. Different from phthalocyanines, these compounds are conjectured to be protonated at nitrogens in pyrazino rings in concentrated sulfuric acid. Other results are stated in comparison with those reported for phthalocyanines.
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Mitsuhiko TAGA, Shunitz TANAKA, Masami FUKUSHIMA
1990 Volume 6 Issue 3 Pages
455-458
Published: June 10, 1990
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A method to evaluate the complexing ability of copper(II) with L-glutamic acid was studied using a weak-base anion exchanger, diethylaminoethyl Sephadex A-25 (A-25). The species of copper(II) complex with L-glutamic acid were Cu(Glu)
0(1:1 complex) and Cu(Glu)
22-(1:2 complex). The 1:2 complex was retained on A-25 since this complex was anionic. The amount of copper retained on A-25 as a 1:2 complex and that which flowed out as free copper(II) ion and a 1:1 complex were determined by flame atomic absorption spectrometry. From the concentration of the 1:2 complex measured, the equations to calculate the stability constants (β
1 and β
2) were derived in terms of the equilibria of the solution; the stability constants obtained were in good agreement with values in the literature. The distribution curves of copper species at various pH were also in good agreement with curves simulated from the estimated stability constants.
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Hideho MIKI, Tamio KAMIDATE, Hiroto WATANABE, Mamoru TAMURA, Isao YAMA ...
1990 Volume 6 Issue 3 Pages
459-460
Published: 1990
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Kazutake SHIMADA, Tomoyuki OE
1990 Volume 6 Issue 3 Pages
461-463
Published: 1990
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Hiroyuki FUJINO, Shujiro GOYA
1990 Volume 6 Issue 3 Pages
465-466
Published: 1990
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Shunitz TANAKA, Takashi KANETA, Hitoshi YOSHIDA
1990 Volume 6 Issue 3 Pages
467-468
Published: 1990
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Nohuo UEHARA, Mitsunori KASAHARA, Yoshio SHIJO
1990 Volume 6 Issue 3 Pages
469-470
Published: June 10, 1990
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Masaaki YANAGISAWA, Kazuo KATOH, Kuniyuki KITAGAWA
1990 Volume 6 Issue 3 Pages
471-472
Published: June 10, 1990
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Shinobu NAGA, Hisashi KOIKE
1990 Volume 6 Issue 3 Pages
473-474
Published: June 10, 1990
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Shunitz TANAKA, Kazuharu SUGAWARA, Mitsuhiko TAGA
1990 Volume 6 Issue 3 Pages
475-478
Published: June 10, 1990
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Masataka HIRAIDE, Hiroshi HOMMI, Hiroshi KAWAGUCHI
1990 Volume 6 Issue 3 Pages
479-480
Published: June 10, 1990
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Kenji KATO, Takaya TAKEI, Yoshinori SUGITANI
1990 Volume 6 Issue 3 Pages
481-483
Published: June 10, 1990
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Chieko OKUMURA, Yasuko T. OSANO, Tetsuo MURAYAMA, Takao MATSUZAKI
1990 Volume 6 Issue 3 Pages
485-486
Published: June 10, 1990
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