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Hajime KATANO, Mitsugi SENDA
1996 Volume 12 Issue 5 Pages
683-689
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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Facilitated transfer of Pb
2+ ion by macrocyclic polythiaethers across the polarizable nitrobenzene/water and 1, 2-dichloroethane/water interfaces has been studied by means of ion-transfer voltammetry. Well-defined voltammetric waves due to facilitated transfer of Pb
2+ ion by 1, 4, 7, 10, 13, 16-hexathiacyclooctadecane (HTCO) were observed. The voltammetric waves at the nitrobenzene/water interface are shown to be due to the reversible transfer, assisted by the formation of 1:1(metal:ionophore) complex (PbHTCO
2+). The half-wave potential of the facilitated transfer of Pb
2+ ion was shifted to more positive potential with increasing concentration of acetate ion in water phase. This is explained by the formation of complexes of Pb
2+ ion with acetate ion, using the theoretical equations of the half-wave potential of reversible facilitated ion-transfer across the oil/water interface. Also, the negative shift in the half-wave potential observed with increasing concentration of supporting electrolyte in oil phase can be attributed to the ionic association of PbHTCO
2+ with the supporting electrolyte anion. The results suggest a new electrochemical method for the determination of Pb(II).
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Yao Qun LI, Takanori INOUE, Teiichiro OGAWA
1996 Volume 12 Issue 5 Pages
691-693
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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The laser two-photon ionization technique has been applied to an interface region in a two-phase system. Anthracene, which stays preferentially in the hydrocarbon phase, could be determined using laser irradiation through the water phase. The detection limit (
S/N=3) was 1.8×10
-9M.
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Jingli YUAN, Kazuko MATSUMOTO
1996 Volume 12 Issue 5 Pages
695-699
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A new tetradentate β-diketone chelator for europium: 1, 10-bis (4"-chlorosulfo-1′, 1"-Biphenyl-4′-yl)-4, 4, 5, 5, 6, 6, 7, 7-octafluorodecane-1, 3, 8, 10-tetraone (BCDOT), was synthesized. It forms a stable chelate with europium(III) and can be used as a fluorescence label for time-resolved fluorescence spectrometry. BCDOT can be covalently bound to a protein under relatively mild conditions, and forms a strongly fluorescent chelate having a lifetime of 260μs in Tris-HCl buffer and 290μs in carbonate buffer solution containing topo (trioctylphosphine oxide) and SDS (sodium dodecylsulfate), when complexed with europium(III). As a model reaction, bovine serum albumin (BSA) was labeled with BCDOT in carbonate buffer solution. Fluorescence spectrometric determination of the BSA(BCDOT)
n-Eu3+ solution was carried out. Detection limits of 4.5×10-13M (
n=47) in 0.1M Tris-HCl solution of pH 9.1, and 8.3×10-14M (
n=47) in 0.1M carbonate buffer solution of pH 8.4 containing 1.0×10-5M topo and 0.05% SDS, for BSA were obtained by the method. These results show that a tetradentate chelate is superior to hitherto used bidentate ligands, giving ca. two orders of magnitude stronger fluorescence.
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Kiyoharu NAKATANI, Shoji ISHIZAKA, Noboru KITAMURA
1996 Volume 12 Issue 5 Pages
701-705
Published: October 10, 1996
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The fluorescence spectra and relevant dynamics of 1-pyrene sulfonate anion (PSA) at a water/1, 2-dichloroethane (DCE) interface were studied by nanosecond time-resolved total internal reflection fluorometry. Both the fluorescence of PSA at a water/DCE interface and that in the water phase were observed under total internal-reflection conditions; also, the fluorescence characteristics at the interface could be separated from the observed spectrum on the basis of analyses of the fluorescence dynamics. The results are discussed in terms of the adsorption and dimer formation of PSA at the interface.
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Susumu NAKAMURA
1996 Volume 12 Issue 5 Pages
707-712
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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This study presents an equation for the background intensity of argon inductively coupled plasma (Ar ICP), which is very useful in calculating the spatial distribution of the background intensity in all the analytical stages of the Ar ICP. This mathematical equation is based on five assumptions: (1) Background emission is generated by collisions between Ar ions and electrons at the central area of the load coil. (2) Background intensity and r.f. power do not change with time. (3) Ar flows without backmixing in the analytical zones. (4) Background intensity is quenched by Ar atoms in ground state level and by water molecules. (5) The quantity of water introduced into the plasma is proportional to the quantity of water introduced into the nebulizer. Comparisons between the empirical data and the calculated values using the proposed equation indicated that this equation is highly reliable in predicting the spatial distribution of the background intensity. As indicated by the equation, it was empirically demonstrated that the background intensity increased as a square of the increase in r.f. power and decreased exponentially when the height above the load coil was increased. In addition, the background intensity decreased when the quantity of carrier gas in the ICP was increased. However, the effect of adding water to the ICP was not significant. These findings suggest that the background intensity as a spatial parameter in the Ar plasma can be calculated by this parsimonious equation.
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Ryoya GOHDA, Kohsuke KIMOTO, Tomofumi SANTA, Takeshi FUKUSHIMA, Hirosh ...
1996 Volume 12 Issue 5 Pages
713-719
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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Using an instrument of automatic fluid injection (batch method), we optimized such reaction conditions as pH, concentration and kinds of buffer for the peroxyoxalate chemiluminscence (PO-CL) detection of fluorescent compounds for high-performance liquid chromatography (HPLC). The results were compared with those obtained by HPLC. Consequently, the usefulness of the batch method for investigating the reaction conditions for PO-CL detection in HPLC was demonstrated. With the optimized condition using a phosphate buffer for the eluent in HPLC, the detection limits for Dns-Val and dipyridamole were 70amol and 20amol on column (
S/N=2), respectively.
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Kazuhiko TSUKAGOSHI, Rika KAWASAKI, Mizuo MAEDA, Makoto TAKAGI
1996 Volume 12 Issue 5 Pages
721-726
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A polymer microsphere having phenylboronic acid sites on its surface was prepared by emulsion polymerization of styrene, butyl acrylate, and m-acrylamidophenylboronic acid. In the process of the preparation, the microsphere was swollen in an alkaline aqueous suspension by adding methylethylketone so that phenylboronic acid sites in the resin would migrate out to the aqueous-organic interface in their ionized forms. The microsphere was confirmed to have dimensions of submicron and assume a neat spherical shape. It was able to be immediately used as saccharide-selective adsorbent without any further treatment, such as grinding and sieving.
D-Glucose was bound onto the microsphere while 1-methyl-α-
D-glucoside was not, due to their different molecular structures. The adsorption of
D-glucose was performed by complex (ester) formation between phenylboronic acid moiety and
cis-diol group of
D-glucose.
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Jun HAGINAKA, Yukiko MIYANO
1996 Volume 12 Issue 5 Pages
727-732
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A chiral stationary phase (CSP) based on a pepsin from porcine stomach mucosa and chicken ovomucoid (OMCHI) from egg whites has been prepared for the separation of basic and uncharged enantiomers. The Pepsin and OMCHI were mixed immobilized onto the same porous aminopropyl-silica materials using an
N, N′-disuccinimidyl carbonate reaction. The retentive and enantioselective properties of the mixed protein phase (MPP), Pepsin-OMCHI CSP, were compared with those of a Pepsin CSP and an OMCHI stationary phase. The Pepsin-OMCHI CSP showed a similar enantioselectivity with the Pepsin CSP. In addition, the Pepsin-OMCHI CSP was more stable than the Pepsin CSP for repetitive injections of samples and the continuous flow of an eluent. The MPP was further stabilized by cross-linking with glutaraldehyde.
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Jung Hag PARK, Yeong Chun WEON
1996 Volume 12 Issue 5 Pages
733-737
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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The interaction properties of some alkylsiloxane-, phenylsiloxane- and cyanopropylsiloxane-bonded silica-based sorbents for solid phase extraction are characterized. The linear solvation energy relationship model is used to estimate the characteristic interaction constants of the sorbents,
s (dipolarity/polarizability),
a (hydrogen bonding basicity),
b (hydrogen bonding acidity),
r (polarizability), and
l (methylene selectivity). For nonpolar alkyl-bonded sorbents, the
l constant is the largest, indicating that the cavity/dispersive interactions term is the dominant term favoring retention on the sorbent. Other interaction terms play minor roles in retention. For the polar cyanopropyl-bonded sorbent the
s and a constants are the largest and are essentially equal, followed by
l,
r and
b constants. For the phenyl-bonded sorbent, the
b coefficient is the largest, followed by
a quite large a coefficient.
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Koichi YAMAMOTO, Mariko ENDO
1996 Volume 12 Issue 5 Pages
739-746
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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The distribution behavior of the ion-association complexes of tetrahalogenothallate(III) ions (TlX
4-(X
-=chloride, bromide and iodide ions)) with quaternary ammonium cations (Q
+) between three organic phases (chloroform (CF), chlorobenzene (Cl-B) and benzene (B)) and an aqueous phase was examined, and the extraction constants (log
Kex) were determined. The extractability of TlX
4- was TlCl
4-<TlBr
4-<TlI
4-; the differences in log
Kex between two successive ions were 2.1±0.8 and 2.2±1.5. Among the ion associates examined, the extractability of the extracting solvents was generally in the order B<Cl-B_??_CF; the differences in log
Kex between two successive solvents in this order were 0.4±0.8 and 0.0±1.4. A linear relationship was found between log
Kex and the total number of carbon atoms in Q
+; from the slope of the line, the contribution of a methylene group in Q
+ to log
Kex was calculated to be 0.5±0.2. From the obtained extraction constants, a highly sensitive extraction-spectrophotometric method of thallium was developed.
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Tatsuya SEKINE, Akiko HOKURA, Ichiro TANAKA
1996 Volume 12 Issue 5 Pages
747-753
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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The rate and equilibrium of the liquid-liquid distribution of 2-thenoyltrifluoroacetone (Htta) was studied in carbon tetrachloride-aqueous 0.1mol dm
-3 sodium perchlorate solution systems at 298K. The distribution equilibrium of Htta reached after two-phase agitation for 90min and the distribution constant of the total Htta was 2.2×10; however, that of the enol form of Htta was higher than 2×10
2 and that of the keto form of Htta was 5.8×10
-1. By a spectrophotometric method and by a liquid-liquid partition method, the rate constant of the enolization and ketonization in the organic phase was measured. The former was 10
2 times higher than that of the latter; both were several orders lower than those in the aqueous phase. From these results, it was assumed that when Htta was initially added to the organic phase the main route of the two-phase distribution reaction was a transference of the enol form from the organic to the aqueous phase and its change to the keto form. In contrast to the change in the distribution ratio of Htta during two-phase agitation, the solvent extraction of metal ions from the aqueous phase with Htta did not change very much after a transient equilibrium was reached within a short time. This was examined with the extraction of indium(III).
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Akinori ISOZAKI, Yukitoki MORITA, Tadao OKUTANI, Toshiro MATSUMURA
1996 Volume 12 Issue 5 Pages
755-759
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A simple and rapid method for the determination of trace lead in suspended particulate matter in air has been investigated. The sample is collected on a cellulose nitrate filter (diameter: 44mm, pore size: 0.65μm) with a low-volume air sampler (flow rate: 15l/min). For direct determination, a small disc (diameter: 2.0mm) is cut from the filter with a paper punch, and it is introduced into a tungsten furnace. Then, 1.0μg of palladium (palladium chloride solution) as a matrix modifier which accomplishes available atomization of lead is added to the disc. The optimal thermal programs are as follows: drying at 300°Cfor 30s, ashing at 1000°C for 30s, and atomization at 2000°Cfor 2s in a mixed gas atmosphere (flow rate: hydrogen 1.0l/min, argon 4.0l/min). The 283.3nm line was used for lead on the peak-area method under deuterium lamp-background correction. The relative standard deviation was 14.3% for 7 times determination on 0.035μg/m
3 lead in a suspended particulate matter.
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Yoshio SHIJO, Hideaki YOSHIDA, Teruo KITAMURA, Eiji YOSHIMOTO, Nobuo U ...
1996 Volume 12 Issue 5 Pages
761-766
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A method for the simultaneous determination of Bi, Cd, Cu, In, Ni and Pb by high-performance liquid chromatography is presented. These metals are preconcentrated on poly(chlorotrifluoroethylene) resin particles as their hexamethylenedithiocarbamate (HMDC) complexes, and eluted with dimethyl sulfoxide, followed by HPLC separation and determination using an ODS column. The conditions for the adsorption of metal-HMDC complexes, such as the pH, HMDC concentration, amount of the resin particles and elution times with dimethyl sulfoxide, are discussed. The resulting solution is suitable for injection into reversed-phase HPLC. The detection limits for the metals were found to be at sub μg l
-1 levels. The application of this principle to the trace analysis of Bi, Cd, Cu, In, Ni and Pb in high-purity aluminum is demonstrated.
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Susumu KAWAKUBO, Hideaki SUZUKI, Masaaki IWATSUKI
1996 Volume 12 Issue 5 Pages
767-771
Published: October 10, 1996
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A highly sensitive fluorometric method was developed for the determination of molybdenum using the molybdenum-catalyzed oxidation of L-ascorbic acid with hydrogen peroxide and the successive condensation of dehydroascorbic acid with o-phenylenediamine to produce fluorescent quinoxaline derivatives. The fluorescence intensity (λ
ex=350nm; λ
em=425nm) was proportional to the square of the reaction time (
t) in the initial reaction at pH 3.2 and 25°C. Using the slope of the fluorescence intensity
versus t2 graph, a calibration graph for molybdenum was constructed with a linear range of 0-3μg l
-1. The detection limit was 0.04μg l
-1 (0.2ng). The addition of
trans-1, 2-cyclohexanediamine-
N, N, N′, N′-tetraacetic acid eliminated the interferences from Cu(II), V(IV), V(V) and W(VI) of up to 50-100μg l
-1 and from Fe(II), Fe(III) and humic acid of up to 500-2000μg l
-1. The proposed method was successfully applied to analyses of river, lake and rain water samples.
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Takashi HASEBE, Takuji KAWASHIMA
1996 Volume 12 Issue 5 Pages
773-777
Published: October 10, 1996
Released on J-STAGE: July 04, 2006
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A flow-injection method is proposed for the determination of trace amounts of ascorbic acid. This method is based on the lucigenin chemiluminescence emitted by ascorbic acid in a basic medium. In this reaction the presence of iron(III) together with a nonionic surfactant Brij 35 (polyoxyethylene-23-lauryl ether), enhanced the intensity of the chemiluminescence signal to as high as 100-times compared to that in their absence. The present method allows the determination of ascorbic acid over the range 2.0×10
-7-6.0×10
-5mol dm
-3. The relative standard deviation was 1.9% for five determinations of 5.0×10
-6mol dm
-3 ascorbic acid; the detection limit (signal-to-noise ratio=3) was 2.0×10
-9 mol dm
-3 with a sampling rate of 30 samples h
-1.
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Toshimasa TOYO'OKA, Toshiaki SUZUKI, Tomomi WATANABE, Yi-Ming LIU
1996 Volume 12 Issue 5 Pages
779-782
Published: 1996
Released on J-STAGE: July 27, 2007
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L. C. ROBLES, A. J. ALLER
1996 Volume 12 Issue 5 Pages
783-787
Published: October 10, 1996
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Yasuhiro TAKAGI, Miyuki OHKURA, Ryuji NAKATA
1996 Volume 12 Issue 5 Pages
789-792
Published: October 10, 1996
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Naoyoshi EGASHIRA, Yasushi NABEYAMA, Yoshiaki KURAUCHI, Kazuya OHGA
1996 Volume 12 Issue 5 Pages
793-795
Published: October 10, 1996
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Koji MATSUSAKI, Tomoki YAMAGUCHI, Toshikatsu SATA
1996 Volume 12 Issue 5 Pages
797-800
Published: October 10, 1996
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Kazutoshi HANADA, Makoto SHIMURA
1996 Volume 12 Issue 5 Pages
801-802
Published: October 10, 1996
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Yasuaki OKAMOTO, Kenji FUJIWARA, Takahiro KUMAMARU
1996 Volume 12 Issue 5 Pages
803-805
Published: October 10, 1996
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Mitsuhiro WADA, Naotaka KURODA, Toshihiko IKENAGA, Shuzo AKIYAMA, Keni ...
1996 Volume 12 Issue 5 Pages
807-810
Published: October 10, 1996
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Kazuhiko TSUKAGOSHI, Ayumi KENMOCHI, Riichiro NAKAJIMA, Tadashi HARA
1996 Volume 12 Issue 5 Pages
811-814
Published: October 10, 1996
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Shuko FUJIEDA, Yoshihiro MOGAMI, Wei ZHANG, Tsunehisa ARAISO
1996 Volume 12 Issue 5 Pages
815-818
Published: October 10, 1996
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Masaaki IWATA, Kimiko KOBAYASHI, Sei TSUBOYAMA
1996 Volume 12 Issue 5 Pages
819-820
Published: October 10, 1996
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Kimiko KOBAYASHI, Sei TSUBOYAMA, Kaoru TSUBOYAMA, Takeshi ITO
1996 Volume 12 Issue 5 Pages
821-822
Published: October 10, 1996
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Kaliyamoorthy PANNEERSELVAM, Manuel SORIANO-GARCIA, Alicia REYES-ARELL ...
1996 Volume 12 Issue 5 Pages
823-824
Published: October 10, 1996
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Hisashi MORIKAWA, Katsuya KATO, Hiroshi KIMOTO, Ping GE, Kenneth L. KI ...
1996 Volume 12 Issue 5 Pages
825-826
Published: October 10, 1996
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