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Katsumi GOTO, Shigeru TAGUCHI
1993 Volume 9 Issue 1 Pages
1-7
Published: February 10, 1993
Released on J-STAGE: July 04, 2006
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Trace elements can be enriched by collecting them on a solvent-soluble filter, followed by dissolution of the filter in a small volume of suitable solvent. The filter serves not only as a sieve but also as a sorbent. For the element to be sorbed, it must be converted into an electrically neutral, hydrophobic species. Ionic species are poorly retained by the filter, but made collectable by adding counter ions with hydrophobic groups. In effect, this enrichment method resembles solvent extraction, but has many advantages. A number of papers have been published on its application since our proposal in 1984. This article summarizes applications of this method and presents a brief description of the mechanism of retention by the filter and some points which may help those who attempt to apply this method to their own field.
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Guo-Qing ZHANG, Masaaki KAI, Hitoshi NOPHTA, Yoshihiko UMEGAE, Yosuke ...
1993 Volume 9 Issue 1 Pages
9-14
Published: February 10, 1993
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High-performance liquid chromatography with postcolumn fluorescence derivatization for the simultaneous determination of glycated albumin and D-glucose in human serum is described. Glycated albumin and D-glucose were separated along with other glycated proteins on a size exclusion column (TSKgel G2000SW
XL) and converted into fluorescence derivatives by reaction with 4-methoxybenzamidine or
meso-1, 2-bis(4-methoxyphenyl)ethylenediamine in
an alkaline medium. The method required only 1μl of serum. The detection limits for glycated albumin and D-glucose (pmol on column) were 100 and 3 with the former reagent, and 150 and 5 with the latter, respectively.
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Masami EDANI, Hideo IMAI
1993 Volume 9 Issue 1 Pages
15-17
Published: February 10, 1993
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An automated enzyme analysis was designed for trypsin and Chymotrypsin. The technique consisted of a hydrophobic chromatography of the enzyme and coupled postcolumn substrate reaction. In a desalted aqueous medium, trypsin and chymotrypsin were adsorbed on a phenyl modified adsorbent gel by hydrophobic interaction, and eluted by the concentration gradient of an electrolyte. After the substrate for the enzyme was reacted in a postcolumn reaction coil, the product was spectrophotometrically detected at 410nm. The separatory determination of trypsin and chymotrypsin was carried out by using the suitable substrate solution. Each calibration plot was a good straight line at 5-100μg of enzyme. The relative standard deviation of 50μg trypsin and the same quantity of chymotrypsin was 2% and 3.5% (
n=5, within-run) respectively. The method was applied to the determination of trypsin and chymotrypsin activity of rat pancreatic juice.
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Kikuo TAKATERA, Tadashi WATANABE
1993 Volume 9 Issue 1 Pages
19-23
Published: February 10, 1993
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The effects of Cu
2+, Zn
2+and Cd
2+ ions on the induction of metallothionein (MT) in a cyanobacterium
Anacystis nidulans R-2 have been studied by high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometric (ICP/MS) detection. After growing the cells in media of systematically varied metal concentrations, the contents of each metal in induced MT were determined by HPLC-ICP/MS. By separate dosing of a metal ion, MT induction was clearly observed with Zn
2+and Cd
2+, but not with Cu
2+ However, Cu
2+induced MT in the presence of a high level (0.77μM) of Zn
2+ A high level of Zn
2+ also significantly promoted MT induction by Cd
2+. These synergistic effects have revealed the predominant role of Zn
2+in heavy-metal detoxification by the organism. The partition of Cu, Zn and Cd between the cytoplasm and the cell wall was studied for cells grown in a medium fairly enriched in the three heavy-metal ions.
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Eijiro KOJIMA, Masaaki KAI, Yosuke OHKURA
1993 Volume 9 Issue 1 Pages
25-27
Published: February 10, 1993
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A simple fluorometric method is described for the determination of the total (free+albumin-bound) and free tryptophan in human serum. After eproteinization of the serum (perchloric acid precipitation for total tryptophan; ultrafiltration for free tryptophan), the samples are treated with phenylglyoxal in dilute perchloric acid to develop fluorescence. The method is sensitive and fairly selective for tryptophan in serum; the limit of detection is 0.84nmol ml
-1 in serum, thus giving a fluorescence intensity that is twice that of the blank.
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Mitsuhiro MASUDA, Shinichi KOIKE, Mitsuichi HANDA, Kazuhiko SAGARA, Ta ...
1993 Volume 9 Issue 1 Pages
29-32
Published: February 10, 1993
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The determination of retinol palmitate and tocopherol acetate in a hydrophobic ointment by a coupled supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) system is described. The ointment, triturated with diatomaceous earth powder, was subjected to SFE with carbon dioxide, and the extract containing fat-soluble vitamins was trapped on a trimethylsilyl silica-gel column by reducing the fluid pressure. The trapped components were analyzed on an octadecylsilyl silica-gel column by SFC using carbon dioxide containing ethanol as a mobile phase and UV absorption monitoring at 284nm. In this method, retinol palmitate and tocopherol acetate in preparations could be determined within ten minutes without any manual products after placing the sample into the system.
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Yasuhiko NISHIKAWA
1993 Volume 9 Issue 1 Pages
33-37
Published: February 10, 1993
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The separation of enantiomers of synthetic pyrethroids by subcritical and supercritical fluid chromatography was investigated using the Pirkle-type Chiral stationary phases developed for high-performance liquid chromatography. The enantioselectivities of these stationary phases were found to be sufficient in tests with reference chemicals. Using these stationary phases, enantiomers of compounds with one or two chiral centers in acid and alcohol moieties were resolved; attempts were made to improve their resolution. Significant improvement resulted with the use of lower temperature, and thermodynamic considerations suggested the effectiveness of subcritical fluid chromatography for chiral separation of pyrethroids. The elution order of enantiomers was the same as in high-performance liquid chromatography in the two cases studied. This technique is very promising, as it requires a shorter analysis time.
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Yasuhiko NISHIKAWA
1993 Volume 9 Issue 1 Pages
39-42
Published: February 10, 1993
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The parameters affecting the retention of synthetic pyrethroids on stationary phases of five polarities in capillary supercritical fluid chromatography were examined. Correlations between the logarithms of the capacity factor of the pyrethroids and the molecular weight, molar volume or polarizability were investigated. Although molar volume and polarizability were expected to exert the greatest effects because of steric parameters, the molecular weight had the highest correlation. For a series of compounds having a common framework, the molecular weight is one of the main factors affecting retention in addition to polarizability and other parameters. In general, better correlation coefficients were observed for nonpolar stationary phases than for polar stationary phases in studies of specific parameters.
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Toshihiko HANAI, Hiroyuki HATANO, Noriyuki NIMURA, Toshio KINOSHITA
1993 Volume 9 Issue 1 Pages
43-46
Published: February 10, 1993
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The van der Waals volume and enthalpy of alkanes and alkylalcohols were calculated using the CAChe-MOPAC-BlogP program. These values were correlated with van der Waals volumes calculated by Bondi′s method and enthalpies measured using a capillary column gas chromatograph. Further, the boiling points were analyzed by using their capacity ratios and physicochemical properties. The proposed boiling point of the alkanes and alkylalcohols are presented.
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Kazunaka ENDO, Kyonosuke YAMAMOTO, Ryoichi KADO
1993 Volume 9 Issue 1 Pages
47-51
Published: February 10, 1993
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Fluorine-19 nuclear spin relaxation rates for fluorocarbon solutions involving oxygen have been measured over a wide frequency range (10 to 235MHz) at 25°C. The
19F relaxation of the solvents involving paramagnetic oxygen can be explained by Bipolar electron spin-nuclear spin interaction modulated by both translational diffusion (τ
d of 2.0×10
-11 and 2.5×10
-11s for C
6F
6and C
6H
4(CF
3)
2, respectively) and the lifetime of the short-lived complex (τ
h of 7.6×10
-13 and 1.3×10
-12s for C
6F
6 and C
6H
4 (CF
3)
2, respectively), although the translational contribution is dominant. The translational motions account for 81 and 70% of the relaxation process and are characterized in the present analysis by closest distances of 3.6 and 3.8A for C
6F
6 and C
6H
4(CF
3)
2, respectively.
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Toshihiko TOIDA, Hidenao TOYODA, Toshio IMANARI
1993 Volume 9 Issue 1 Pages
53-58
Published: February 10, 1993
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The proton nuclear magnetic resonance (
1H-NMR) spectra of chondroitin sulfates (chondroitin, chondroitin 4-sulfate, chondroitin 6-sulfate and dermatan sulfate) have been obtained at 500MHz and 333K in deuterium oxide. The
J connectivities of sugar ring protons of chondroitin sulfates are revealed by the uses of homonuclear two-dimensional (2D) multiple-relayed-chemical-shift-correlated spectroscopy (multiple-relayed COSY), homonuclear Hartman-Hahn spectroscopy (2D HOHAHA), and multiple-quantum-filtered COSY. Formation of sulfate ester on
N-acetylgalactosamine hydroxy group causes predictable 0.4-0.6ppm deshielding of the proton directly attached to the sulfation site. Furthermore, the partial structure of low-sulfated chondroitin sulfate chain isolated from human urinary trypsin inhibitor was determined from the obtained
1H-NMR data.
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Tetsuo OKADA
1993 Volume 9 Issue 1 Pages
59-64
Published: February 10, 1993
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Micellar mobile phases allow the separation of ionic and nonionic compounds with a single mobile phase/column combination. Nonionic compounds such as phenols are separated together with metal ions using mobile phases containing anionic micelles and a suitable ligand. Also, the use of cationic micellar mobile phases permits the simultaneous separation of inorganic anions as well as nonionic compounds. In both cases, nonionic compounds are partitioned to the micelle and the stationary phase according to either the hydrophobicity or the lipophilicity, whereas inorganic ions electostatically interact. The separation of phenols is therefore described using an usual partition model; that of inorganic ions obeys a model involving ion-exchange equilibria. These models facilitate the prediction of the retention as well as the optimization of the separation.
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Satoshi TSUKAHARA, Koichi SAITOH, Nobuo SUZUKI
1993 Volume 9 Issue 1 Pages
65-70
Published: February 10, 1993
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Physical characteristics are presented of the liquid-liquid partition coefficients (P) measured for tris(β-diketonato)chromium (III) and bis(β-diketonato)palladium(II) in the system using dodecane and acetonitrile (AN)-water mixtures as the nonpolar and polar liquid phases, respectively. The P values of all the complexes (fifteen complexes) studied decrease with increases in mole fraction of AN in the polar liquid, phase. In series of the Cr(III) complexes and of the Pd(II) complexes, the P values tend to increase with increasing molecular size of complex. The P value of Cr(III) complex is smaller than that of the Pd(II) complex having comparable molecular size. The difference in the P values between two geometrical isomers of the complex depends on the functional group of the β-diketone. Scaled particle theory is applied to the discussion of the factors governing the P value.
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Satoshi TSUKAHARA, Koichi SAITOH, Nobuo SUZUKI
1993 Volume 9 Issue 1 Pages
71-76
Published: February 10, 1993
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Liquid chromatographic capacity factors (
k′) were measured for thirty two compounds including alkanes, aromatic hydrocarbons, esters, ketones and alcohols in an octadecyl bonded silica gel (ODS)/(methanol-water) system. The
k′ of each compound was compared with the partition coefficient (
P) in the liquid-liquid system consisting of dodecane and the methanol-water of a composition identical to that used in the chromatography (the molar fraction of methanol in the mixture, 0.4-1.0). A ratio,
k′/
P, increased with decrease in
P. The
k′/
P ratio of a relatively polar compound was noticeably affected by the composition of methanol-water. The energy difference in the solute-solvent interactions occurring in the methanol-water phase and in the dodecane phase was estimated using the scaled particle theory. It was found that the more strongly a solute interacted with a polar solvent, such as methanol and/or water, than a nonpolar solvent such as dodecane, the more easily the solute transfer tended to occur from the polar phase to the ODS phase rather than to the dodecane phase.
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Minoru ARAI
1993 Volume 9 Issue 1 Pages
77-82
Published: February 10, 1993
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Fourier-transform infrared spectroscopy (FT-IR) was applied to a continuous measurement of unregulated emissions from a diesel engine. Improvements in measuring the diesel exhaust gas were achieved by heating the gas sampling line, adapting the filter to remove particles in the exhaust gas, and modifying the window material of the sampling cell. An increase in the sample flow rate as well as a volume reduction of the sampling cell could improve the response of FT-IR, though it was insufficient under transient conditions. It was confirmed that FT-IR could continuously and simultaneously detect unregulated emissions, such as HCHO and NH
3, as well as regulated emissions. The measured concentration level of unregulated emissions was very low. It was suggested that FT-IR might be useful in estimating any change in the combustion process by measuring the intermediate products, including HCN and HONO, which are related to NO production during combustion. It was also demonstrated that gaseous unregulated emissions from vehicles can be measured in real-time by FT-IR.
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Kazuaki WAGATSUMA, Kichinosuke HIROKAWA
1993 Volume 9 Issue 1 Pages
83-88
Published: February 10, 1993
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In an Ar-He mixed gas inductively coupled plasma (ICP) the role of helium in the excitation of the zinc species was investigated through spectroscopic analyses on both the argon and zinc emission lines. Whereas the spectral widths of the argon lines were only slightly affected by helium addition, the emission intensities of the zinc lines apparently increased. Helium contributes to the increase in zinc excitation, though it causes a slight alternation of the electron density of the plasma. This results from an increment in the plasma temperatures in only the central channel where the zinc species is dominantly excited. These observations could suggest that helium acts as an energy carrier from the induction zone to the central channel of the ICP, due to the fairly high heat conductivity.
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James E. deVRIES, Walter O. SIEGL, Ray A. DICKIE
1993 Volume 9 Issue 1 Pages
89-94
Published: February 10, 1993
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X-Ray photoelectron spectoscopy has been used to study the structure and bonding of Binuclear oxygen-bridged copper(II) complexes. The aromatic onstituency of the complexes gives rise to π*←π shakeup satellites in the spectra of the ring carbons and the adjacent oxygen atoms. The O ls π*←π shakeup satellite peak positions were determined relative to the main core level lines in samples with known structure, allowing alkoxy and phenoxy bridging to be differentiated. The methodology was applied to a Binuclear copper(II)
o-hydroxybenzylamine complex of previously undefined molecular structure.
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Masaaki IWATSUKI, Tsutomu FUKASAWA
1993 Volume 9 Issue 1 Pages
95-98
Published: February 10, 1993
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This paper describes a nondestructive and complete analysis of magnetite(FeO•Fe
2O
3)-maghemite(γ-Fe
2O
3) solid solutions including minor constituents: the proposed method consists of measurements of the lattice constant and X-ray
fluorescent determination of the minor constituents. The diffraction angles of the solid solution were corrected using a silicon internal standard for calculation of the lattice constant, a
0. Intensity ratios of Mn K
α/Fe K
α and Zn K
α/Fe K
α were measured for the determination of manganese and zinc and for the correction of the lattice constant due to the minor elements. The final analysis was done using the linear relation between a
0 and the sum total of converted mole percentages of divalent metal oxides. Differences between the analytical results obtained by the present method and those obtained by the wet methods were within 3.4 wt% for Fe
2O
3, within 1.5 wt% for FeO, and within 0.08 wt% for MnO and ZnO. Time required for a complete analysis is about 30min.
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Yoshifumi HARADA, Natsuko KURATA, Giichi FURUNO
1993 Volume 9 Issue 1 Pages
99-103
Published: February 10, 1993
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A simple, precise and sensitive method is described for the simultaneous determination of major constituents (Al
2O
3 and SiO
2) and impurities (Ca, Cr, Fe, K, Li, Mg, Mn, Na, Sr, Ti, V, Y, Zn and Zr) in high-purity mullite (3Al
2O
3•2SiO
2). A 0.5g amount of the powder sample was decomposed with 5ml of H
2SO
4 (1+2) at 230°C for 16h in a polytetrafluoroethylene pressure vessel. The decomposed mixture was separated to a solution and a precipitate by filtration. After the solution was diluted to a constant volume with water, inductively coupled plasma atomic emission spectrometric analysis for the impurity elements and conventional volumetric analysis for Al
2O
3 were carried out. The precipitate was ashed in a platinum crucible and gravimetric analysis for SiO
2 was carried out. The proposed method was successfully applied to the simultaneous determination of Al
2O
3, SiO
2 and the impurities in commercial mullite samples. The analytical results were in good agreement with those obtained by other methods. This method has advantages in simplicity, good precision and high sensitivity for the comprehensive analysis of high-purity mullite.
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Yasuaki OKAMOTO, Hiromi KAKIGI, Takahiro KUMAMARU
1993 Volume 9 Issue 1 Pages
105-109
Published: February 10, 1993
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For electrothermal sample introduction, a commercially available tungsten boat atomizer for atomic absorption spectrometry was transformed to a vaporizer for inductively coupled plasma atomic emission spectrometry. By placing diammonium hydrogenphosphate in the boat as a matrix modifier prior to analysis, the loss of cadmium and lead which would occur during the ashing stage was suppressed. With this method, an enhancement in cadmium sensitivity and no severe interference from foreign ions was observed. The detection limits (3σ) for cadmium and lead were 0.28 and 2.8ng ml
-1, respectively. The relative standard deviations for 7 replicate determinations were 7.9% for 2ng ml
-1 of cadmium and 3.4% for 20ng ml
-1 of lead. The calibration graphs were linear in the tested range of up to 10μg ml
-1 for both elements. Analytical results of some biological and environmental samples are given.
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Ushio HASE, Kazuhisa YOSHIMURA
1993 Volume 9 Issue 1 Pages
111-115
Published: February 10, 1993
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Gel-phase absorptiometry has been improved for determining silicic acid in highly purified water, in which the absorbance of Molybdenum Blue adsorbed on Sephadex G-25 is measured directly. The gel amount used was reduced to one-sixth of that required in the previously reported method by employing a smaller volume cell and a gel-aliquotting device. Less than 0.05g of the gel could be measured rapidly with good reproducibility and the detection limit of silicon was 0.04μg dm
-3.
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Luis Fermín CAPITAN-VALLVEY, Enrique Jesús ALONSO, Ramir ...
1993 Volume 9 Issue 1 Pages
117-120
Published: February 10, 1993
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A rapid method for the determination of anthracene ultratraces in water by solid-phase fluorometry is described.Anthracene is fixed on C-18 silica to give fluorescence at λ
ex=357nm and λ
ex=405nm wavelengths. An anthracene-silica-gel system packed in a 1mm quartz cell was measured directly using a solid-surface attachment. The applicable concentration range was 50-1000ng dm
-3 with a relative standard deviation of 0.7% and a detection limit of 21ng dm
-3. The method was applied to the determination of anthracene in natural, tap and seawater samples. The recoveries were 100, 105 and 110%, respectively. The method is very simple and more sensitive than other methods described in the literature.
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Kazuo UCHIKURA, Makoto KIRISAWA, Atsusi SUGII
1993 Volume 9 Issue 1 Pages
121-123
Published: 1993
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Kenji HAMASE, Hiroshi NAKAMURA, Terumi NAKAJIMA
1993 Volume 9 Issue 1 Pages
125-127
Published: 1993
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Yasuyuki SHIBATA, Jun YOSHINAGA, Masatoshi MORITA
1993 Volume 9 Issue 1 Pages
129-131
Published: 1993
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Koji NAKANO, Hiroaki TAIRA, Mizuo MAEDA, Makoto TAKAGI
1993 Volume 9 Issue 1 Pages
133-136
Published: 1993
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Yong-Nam PAK, Tomokazu TANAKA, Hiroshi KAWAGUCHI
1993 Volume 9 Issue 1 Pages
137-139
Published: February 10, 1993
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Hideko KOSHIMA, Hiroshi ONISHI
1993 Volume 9 Issue 1 Pages
141-142
Published: February 10, 1993
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Hideko KOSHIMA, Hiroshi ONISHI
1993 Volume 9 Issue 1 Pages
143-144
Published: February 10, 1993
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Hiroshi KAWAMOTO, Tohru NISHIMURA, Kin-ichi TSUNODA, Hideo AKAIWA
1993 Volume 9 Issue 1 Pages
145-147
Published: February 10, 1993
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Hiroshi IWASE
1993 Volume 9 Issue 1 Pages
149-151
Published: February 10, 1993
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Matashige OYABU, Yasushi OHNO, Eisaku TERASHITA
1993 Volume 9 Issue 1 Pages
153-155
Published: February 10, 1993
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Raul A. REIMER, Akira MIYAZAKI
1993 Volume 9 Issue 1 Pages
157-159
Published: February 10, 1993
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Yoshiharu NAWATA, Yoshito YUTANI, Mikio SAWADN
1993 Volume 9 Issue 1 Pages
161-162
Published: February 10, 1993
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