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Kichinosuke HIROKAWA
1989 Volume 5 Issue 6 Pages
631
Published: 1989
Released on J-STAGE: July 27, 2007
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Shigeru SHIMOMURA
1989 Volume 5 Issue 6 Pages
633-639
Published: December 10, 1989
Released on J-STAGE: June 30, 2006
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Accurate and rapid measurements of low-concentration mercury and other biologically-related elements in the environment are believed to be very important. A necessary and sufficient elucidation of the physicochemical properties of target elements makes it possible to analyze the elements both more accurately and definitely. In this review the physicochemical properties necessary for analyses are elucidated, taking mercury as an example. The described physicochemical properties of mercury can be divided into three aspects: (1) gas-liquid equilibrium for vaporization and absorption of mercury, (2) permeation phenomenon of mercury vapor through polymer films, and (3) behavior upon irradiation by a mercury lamp.
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Supa POLMAN, Sirirat KOKPOL, Supot HANNONGBUA, Bernd M. RODE
1989 Volume 5 Issue 6 Pages
641-644
Published: December 10, 1989
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Linear models for quantitative electronic structure-activity relationships (QSAR) of mefloquine-type antimalarial drugs have been evaluated on the basis of CNDO/2 molecular orbital calculations. The results indicate that mefloquines could interact via two active sites in a similar mechanism, as proposed for primaquine and chloroquine drugs.
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Osamu YAMAMOTO, Kikuko HAYAMIZU, Masaru YANAGISAWA
1989 Volume 5 Issue 6 Pages
645-650
Published: December 10, 1989
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A computer system for substructure elucidation and chemical shift estimation by the use of nuclear magnetic resonance (NMR) spectra is described. In this system, substructures in a molecule can be elucidated by specifying chemical shift values or ranges, and conversely chemical shift values can be estimated by specifying substructures for both
1H- and
13C-NMR data. The retrieval of data can be performed interactively between
1H- and
13C-NMR data. It is possible to estimate all chemical shift values for a compound by giving its chemical structure. The search file for these purposes is created for signals (or signal groups) from a large number of
1H- and
13C-NMR spectra in our database. The information contained in the search file consists of substructures and the corresponding chemical shift values. A line notation system has been developed to plot chemical structures with spectra assignments of NMR signals and to extract substructures corresponding to particular chemical shift values.
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Kenji KANO, Kazuya MORI, Tomonori KONSE, Bunji UNO, Tanekazu KUBOTA
1989 Volume 5 Issue 6 Pages
651-656
Published: December 10, 1989
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A newly designed three-electrode electrolysis cell for
in-situ electron spin resonance (ESR) spectroscopy and cyclic voltammetry is described. An electrolysis solution near the electrode surface is continuously renewed by an internal-flow method, which makes it possible to record the well-resolved ESR spectra of unstable free radicals. An accurate control of the electrode potential using an ohmic drop corrector has enabled us to obtain a fairy good
voltammogram. This cell can be applicable to both oxidation and reduction experiments in aprotic and protic media at an arbitrary temperature by the use of a temperature-controlled Dewar vessel. Some fundamental experiments are reported.
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Eiko HATAKEYAMA, Norikazu MATSUMOTO, Takeo OCHI, Tateo SUZUKI, Hiroshi ...
1989 Volume 5 Issue 6 Pages
657-661
Published: December 10, 1989
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A sensitive fluorometric method has been developed to determine the thiol and disulfide groups in proteins using
N-(9-acridiny )maleimide as a fuorogenic reagent. Proteins are hydrolyzed with subtilopeptidase (Carlsberg type) in order to eliminate the steric hindrance. Then, thiols are determined by the reaction of
N-(9-acridinyl)maleimide with the hydro ysate. Disulfide can be determined using the same hydro ysate after the derivatization into thins by
electroytical reduction. The fluorescence intensities have shown linear relations between the thin and disulfide contents at nmol/ml levels in the mode proteins. The sensitivity is 1000-times higher than conventional colorimetry with 5, 5′-dithiobis(2-nitrobenzoate).
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Hee-Kyoung JEON, Hitoshi NOHTA, Kenji OHTSUBO, Yosuke OHKURA
1989 Volume 5 Issue 6 Pages
663-666
Published: December 10, 1989
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A highly sensitive method for the determination of
L-threo-3, 4-dihydroxyphenylserine (
L-DOPS) and
L-α-methyldopa in rat serum is described. The method uses high performance liquid chromatography with fluorescence detection. L-DOPS and L-α-methy dopy (analyte and internal standard, respectively, andvice versa) in serum, after cleanup with a cation exchanger cartridge (Toyopak IC-SP S), are converted into the corresponding fluorescent compounds by reaction withmeso-1, 2-diphenylethylenediamine. The derivatives are separated by reversed phase chromatography on a TSK gel ODS-120T column. The detection limits (
S/N=3) for L-DOPS and L-α-methyldopa are 6 and 9fmol for an injection volume of 100μl.
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Tadao KONISHI, Masafumi KAMADA, Hiroshi NAKAMURA
1989 Volume 5 Issue 6 Pages
667-670
Published: December 10, 1989
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The separation of amino acids and peptides on a strong cation-exchange polymer column (Polyspher PE A) has been investigated. Retentions of hydrophobic amino acids and peptides were affected by hydrophobic interaction with the polymer matrix, which was useful for separation of peptides with close pl values. Simultaneous separation of acidic, neutral and basic peptides was successfully performed by linear gradient elution.
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Tetsuharu IWATA, Hiroshi HANAZONO, Masatoshi YAMAGUCHI, Masaru NAKAMUR ...
1989 Volume 5 Issue 6 Pages
671-673
Published: December 10, 1989
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A simple, highly sensitive, high performance liquid chromatographic method with fluorescence detection for the determination of 7-dehydrocholesterol in human skin surface is described. 7-Dehydrocholesterol, extracted with hexane-ethanol (1:1, v/v) from skin surface using a handy extraction device, is converted into a fluorescent derivative by reaction with 3, 4-dihydro-6, 7-dimethoxy-4-methyl-3-oxo-quinoxaline-2-carbonyl azide. The derivative is separated from biogenic interfering substances on a reversed-phase column (TSK gel ODS-120T) with aqueous 90% (v/v) acetonitrile and detected fluorometrically. The detection limit (
S/N=3) is 1.6pmo (0.61ng) cm
-2 of human skin surface [corresponding to 18fmol (6.8pg) in a 10μl injection volume]. The correlation between age and the concentration of 7-dehydrocholesterol in skin surface is also described.
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Yoshihiko UMEGAE, Hitoshi NOHTA, Yosuke OHKURA
1989 Volume 5 Issue 6 Pages
675-680
Published: December 10, 1989
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A sensitive method for the determination of reducing sugars is described which employs high performance liquid chromatography with on-line postcolumn fluorescence derivatization. Reducing sugars are separated by borate complex anion-exchange chromatography on a trimethylammonium-bonded resin column (TSK gel Sugar AXG) and automatically converted into fluorescent derivatives by reaction with 1, 2-bis(4-methoxypheny)ethylenediamine in an alkaline medium. The detection limits (
S/N=3) for reducing sugars are 30-160pmol in a 100-μl injection volume. The quantification of reducing sugars in human urine and serum is also described.
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Yong-Moon LEE, Hiroshi NAKAMURA, Terumi NAKAJIMA
1989 Volume 5 Issue 6 Pages
681-685
Published: December 10, 1989
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Free fatty acids were determined by high performance liquid chromatography after derivatization with monodansyl Cadaverine (MDC) at room temperature for 15min in the presence of diethyl phosphorocyanidate as a coupling reagent. The fluorescence properties (λ
ex340nm, λ
em 518nm) of MDC-arachidic acid (C
20:0) were identical to those of dansyl alanine. The MDC derivatives of saturated and unsaturated fatty acids were completely separated within 50min by gradient elution on a TSK-gel 80
TM ODS column. When fluorometrically detected, the detection limits (
S/N=3) of fatty acid were below 100fmol. The calibration curves passed through the origin and gave good linearity in the range from 5 to 200pmol. The method was successfully applied to the determination of fatty acids in the rabbit plasma. This method would be quite useful for the analysis of various biological samples for thermolabile carboxylic acids, since it requires no heating procedure.
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Mamoru HARATAKE, Naotake OGAWA, Atsushi SUGII
1989 Volume 5 Issue 6 Pages
687-690
Published: December 10, 1989
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In order to evaluate anion-exchange resins possessing a spacer arm (ω-oxoalkyl(-CO(CH
2)
n-) or ω-hydroxyalkyl
(-CH(OH)-(CH
2)
n-)) between the quaternary ammonium group and the polymer backbone, sorption behavior for bile acids was investigated for three series of resins prepared from polystyrene beads having different cross linkages. In the highly crosslinked resins, the resins having the spacer arms gave higher exchange capacities for bile acids than conventional-type resins did. The sorption was also affected by the length and chemical structure of the spacer arm. Thus, a spacer arm allows for more favorable sorption of sterically hindered anions.
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Kazuichi HAYAKAWA, Seiji NAKAMURA, Kotoe INAKI, Motoichi MIYAZAKI
1989 Volume 5 Issue 6 Pages
691-695
Published: December 10, 1989
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Carboxylesters, carboxylic and inorganic anions were determined separately by photometric ion chromatography with an enzyme immobilized column. In the system, a carboxylesterase immobilized column (4.6mm i.d.×10mm), which converted carboxylesters to carboxylic anions completely, was set between a sample injector and an analytical column. The other chromatographic conditions were as follows: an anion exchanger-type separation column (4.6mm i.d.×250mm); phthalate-
N-2-hydroxyethylpiperazine-
N′-2-ethanesulfonic acid e uent (pH 6.5); an oven of temperature 40°C; a flow rate of 1.0ml/min; 280-nm UV detection; and an injection volume of 20μl. Calibration curves for ethyl esters of acetate, propionate, butyrate and isova erate were linear with the range 5×10
-10mol to 1×10
-7mol according to the peak-height method; their detection limits were 10
-10 mol levels. The present method was applied for the determination of carboxylesters in practical samples.
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Kenji KATO, Yoshinori SUGITANI
1989 Volume 5 Issue 6 Pages
697-699
Published: December 10, 1989
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An attempt was made to determine the iron in an aluminum hydroxide gel powder by an X-ray photoacoustic measurement. It was conducted using a monochromated X-ray beam (1.504Å) of synchrotron radiation as an excitation source. The iron in the sample was also determined by a spectrophotometric method, while the water content in the sample was determined from the weight loss by a thermal analytical method. Photoacoustic signal intensities roughly agreed with those calculated from the elemental compositions of the samples. The rough agreement is due to the fact that the background signal from the aluminum hydroxide gel was not negligibly small. However, the background signal decreased in measurements at high chopping frequency, and the calibration curves of iron showed good linearities. The photoacoustic signal intensity of samples containing iron varied as
f-1, where
f is the chopping frequency. This was different from that for a sample without iron.
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Masaaki KUBOTA, Noriko FUDAGAWA, Akira KAWASE
1989 Volume 5 Issue 6 Pages
701-706
Published: December 10, 1989
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The ion signals of oxide-forming elements (M
+) and their monoxides (MO
+) have been investigated as functions of inductively coupled plasma operating parameters. An appropriate selection of the radio frequency power, carrier-gas flow rate and sampling depth was essential in order to minimize the signal ratio,
SMO(+)/
SM(+). Signals
SMO(+) and
SM(+) decreased drastically with increasing radial distance from the plasma center. The signal ratios
SMO(+)/
SM(+) for various analytes, in consideration of partition functions and mass numbers, showed a linear relation with the oxide dissociation energies. Equivalent concentration data are also given for typical oxide interferences.
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Masahiko KAN, Toshiko NASU, Mitsuhiko TAGA
1989 Volume 5 Issue 6 Pages
707-712
Published: December 10, 1989
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A spectrophotometric method is described regarding the determination of germanium. A colored complex of germanium with phenylfluorone was collected on an organic solvent-soluble membrane filter made of cellulose nitrate. The complex, together with the filter, was dissolved into N, N-dimethylformamide (3cm
3), and the absorbance of the solution was measured. The obtained calibration curve was linear from 0.05 to 1.0μg of germanium and the molar absorption coefficient was 1.9×10
5dm
3 mol
-1 cm
-1. The relative standard deviation of the absorbance obtained at 1.0μg of germanium was 0.4% (
n=11). The interference of molybdenum(VI) could be eliminated by hydrogen peroxide. The time required for one run was about ten minutes and germanium at 1μg dm
-3 levels could be easily determined. This method has been applied to the determination of germanium in samples of hot-spring water.
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Hajime ISHII, Yasuhiro SATOH, Katsuhiko SATOH
1989 Volume 5 Issue 6 Pages
713-717
Published: December 10, 1989
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Three cationic porphyries, 5, 10, 15, 20-tetrakis(1-methyl-2-pyridinio)porphine [T(2-MP
y)P], 5, 10, 15, 20-tetrakis(1-methyl-3-pyridinio)porphine [T(3-MP
y)P] and 5 10, 15, 20-tetrakis(1-methyl-4-pyridinio)porphine [T(4-MP
y)P], react rapidly and quantitatively with silver(I) to form yellow complexes in alkaline solutions of pH 9.6-12.0, which are oxidized to the corresponding red silver(II) complexes by dissolved oxygen at room temperature. The silver(II) complexes formed were stable and remained unchanged for at east 2h. The composition of the silver(II) complex was determined to be 1:1 (metal:ligand) by both the continuous variation method and the molar ratio method. Highly sensitive spectrophotometric methods for the determination of the trace amounts of silver have been developed. The apparent molar absorptivities of the silver(II) complexes of T(2-MP
y)P, T(3- MP
y)P and T(4-MP
y)P were 3.00×10
5, 3.36×10
5 and 2.30×10
5lmol
-1 cm
-1, respectively. Cadmium(II), coba t(II), copper(II), mercury(II), manganese(II), zinc(II), halogenides, thiocyanide and cyanide interfered with the silver determination.
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Masaaki TABATA, Naoko KAJIHARA
1989 Volume 5 Issue 6 Pages
719-724
Published: December 10, 1989
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The formation constant of lead(II) complex of 5, 10, 15, 20-tetrakis(4-sulfonatophenyl)porphine (H
2TPPS
4) (log K) defined as Pb
2++H
2TPPS
4_??_Pb(II)(TPPS
4)+2H
+ was found to be -9.97±0.02, which is approximately 10
9 times as small as that of Zn(II)(TPPS
4). In addition, Pb(II)(TPPS
4) was rapidly replaced with EDTA at a half-life time of 200ms. On the other hand, Zn(II)(TPPS
4) is stable and not replaced with EDTA even after 2h. The large difference in the equilibrium and kinetic behavior between Zn(II)- and Pb(II)(TPPS
4) allows the determination of zinc(II) at as low as 10
-7mol dm
-3 concentration level in the presence of 10
-2mol dm
-3 lead(II). The molar absorptivity of Zn(II)(TPPS
4) is 4.66×10
5mol
-1 dm
3cm
-1. The method was applied to the determination of zinc(II) in lead chemicals (lead(II) nitrate, lead(II) acetate and lead metal) and in tap and waste waters by measurement of the absorbance at 421nm. The optimum conditions of the ligand-buffer solution containing aminopolycarboxylates and lead(II) are described to remove the interference of copper(II), cobalt(II) and manganese(II).
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Kazumasa UEDA, Hideaki MATSUDA, Osamu YOSHIMURA
1989 Volume 5 Issue 6 Pages
725-728
Published: December 10, 1989
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4-(2-Thiazolylazo)-6-bromoresorcinol (TAR-Br) was synthesized and its usefulness for spectrophotometric determination of 14 lanthanoid(III) ions was examined. The acid dissociation constants of the reagent and the stability constants of the complexes (1:1) were determined, and the complexing behavior was studied. The optimum pH for complexation lies between 6.8-8.7. Beer′s law holds up to about 2.5ppm of each lanthanoid, with a molar absorptivity of 6×10
4l mol
-1 cm
-1 eve near 553nm. The addition of ethanol produced some sensitization effect, due to solvation with the complexes. Both the molar absorptivities and the stability constants were larger in light Lanthanoids with the atomic number, but the latter were slightly lower in heavy Lanthanoids. TAR-Br was classified as a second ligand group member according to the Moeller′s type classification.
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Noboru OYAMA, Takeo OHSAKA, Shin IKEDA, Katsumi OKUAKI
1989 Volume 5 Issue 6 Pages
729-734
Published: December 10, 1989
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A solid-state reference electrode has been fabricated. Its design is based on a field effect transistor, the gate of which is coated with two kinds of polymeric films in a Bilayer state: the inner layer is an electroactive electropolymerized poly(
p, p′ biphenol) film and the outer one is a polyimide film. The electrode characteristics have been examined. The bilayer film-coated reference field effect transistors (RFET
s) thus fabricated were
insensitive to electrolyte ions (including H
+ and OH
-) under the condition of a constant concentration (
e.g., 0.1M) of an electrolyte; thus they could function as a reference electrode. These RFET
s showed insensitivity to O
2 and less sensitivity to CO
2 (compared with the RFET coated with the polyimide film alone), long-term stability and little drift. The results demonstrate that the bilayer film-coated FET
s are promising as a solid-state reference electrode coupled with conventional ion-sensitive field effect transistors in a biological system.
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Kensaku HARAGUCHI, Mamoru NISHIDA, Akimi AYAME, Masayo MUROZUMI, Tohru ...
1989 Volume 5 Issue 6 Pages
735-738
Published: December 10, 1989
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N-Phenylhydroxylamines (HL) with an alkylcarbonyl group containing 3 to 10 carbon atoms were synthesized and used for the extraction of several divalent metal ions from an aqueous solution to carbon tetrachloride. The distribution constants,
KD, of these chelating reagents increased with an increase in the carbon number in the alkylcarbonyl group. The increment of the logarithmic distribution constant, log
KD, was about 0.5 per carbon atom in the alkylcarbonyl group. Extracted species CuL
2, CoL
2, PbL
2, NiL
2HL and ZnL
2HL were found for extraction with
N-hexanoyl- and
N-octanoyl-
N-phenylhydroxylamines. The extraction constants for these chelates were evaluated.
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Shigeto NAKAMURA, Yosyong SURAKITBANHARN, Kenichi AKIBA
1989 Volume 5 Issue 6 Pages
739-743
Published: December 10, 1989
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The extraction behavior of Lanthanoid elements has been investigated using such β-diketone derivatives (HA) as dodecylbenzoyltrifluoroacetone (LIX 51), benzoylisooctanoylmethane (LIX 54) and dibenzoy methane (DBM) in kerosene. Trivalent Lanthanoid ions (M
3+) were extracted as tris-β-diketonate (MA
3); the extraction tendency followed the sequence L1×51_??_L1×54>DBM. The extraction constants (
Kex) for lanthanoid elements increased with an increase in their atomic number, and a "tetrad effect" was approximately observed for each extraction system. The mean separation factor between adjacent elements was evaluated to be 1.71 for LIX51, 1.95 for LIX54 and 2.23 for DBM.
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Koichi YAMAMOTO, Shoji MOTOMIZU
1989 Volume 5 Issue 6 Pages
745-749
Published: December 10, 1989
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Malachite Green (MG), Crystal Violet (CV) and Ethyl Violet (EV). Chlorobenzene was used for the extraction of the chloro complex with MG and CV; benzene for the bromo complex with MG and CV; and toluene for the iodo complex with MG and CV, and the chloro complex with EV. Out of the extraction systems examined, the benzene-extraction of dibromocuprate(I) ion with Crystal Violet was best for the spectrophotometric determination of copper; low reagent blank, high sensitivity, stable coloration and only little interference from the coexisting ions. This method could be applied to the determination of trace amounts of copper.
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Hisanori IMURA, Qi Lu, Nobuo SUZUKI
1989 Volume 5 Issue 6 Pages
751-754
Published: December 10, 1989
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The synergistic extraction of holmium(III) with 2-thenoyltrifluoroacetone (Htta) in the presence of neutral bidentate heterocyclic amines such as 2, 2′-bipyridine (bpy), 4, 4′-dimethyl-2, 2′-bipyridine (dmbpy), and 4, 4′-diphenyl-2, 2′-bipyridine (dpbpy), and a neutral terdentate amine of 2, 2′:6′, 2"-terpyridine (tpy) in benzene has been investigated. The synergism was found to be due to the formation of an adduct complex of Ho(tta)
3S (S denotes a heterocyclic amine) in all of the systems studied. The extraction constant and the adduct formation constant (β
s, 1) for Ho(tta)
3S are given. The values of
βs, 1 increased in the order tpy<dpbpy<bpy<dmbpy. The order for the bidentate amines was in agreement with that of the acid-dissociation constant (
KHS+) for their conjugate acids, while the value or β
s, 1 for tpy was fairly lower than that expected from its
KHS+ value.
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Hiroshi KAWAMOTO, Tsunemi AIBA, Hideo AKAIWA
1989 Volume 5 Issue 6 Pages
755-757
Published: December 10, 1989
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The synergistic extraction of copper(II), zinc(II) and cadmium(II) with monothiothenoyltrifluoroacetone (STTA=HR) and 1, 10-phenanthroline (phen=S) was examined. The main synergistic adducts extracted into the organic phase were found to be MR
2S (M=Cu, Zn, Cd) and MR
2S
2(M=Zn). The rather small stability constant for CuR
2S is attributable to the Jahn-Teller effect. The results were applied to establish a method of separation of cadmium(II) from zinc(II).
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Hiroshi MIYANO, Ei-ichiro SUZUKI, Satoko AKASHI, Mami FURUYA, Takashi ...
1989 Volume 5 Issue 6 Pages
759-761
Published: 1989
Released on J-STAGE: July 27, 2007
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Masahiro KAWAHARA, Hiroshi NAKAMURA, Terumi NAKAJIMA
1989 Volume 5 Issue 6 Pages
763-764
Published: 1989
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Masaaki YANAGISAWA, Keiichi IDA, Kuniyuki KITAGAWA
1989 Volume 5 Issue 6 Pages
765-766
Published: 1989
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Shoji MOTOMIZU, Mitsuko OSHIMA, Tomoko IKEGAMI
1989 Volume 5 Issue 6 Pages
767-769
Published: 1989
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Toshiyuki OSAKAI, Sadayuki HIMENO, Atsuyoshi SAITO
1989 Volume 5 Issue 6 Pages
771-773
Published: 1989
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Hiromiti SAWAMOTO, Keiji GAMOH
1989 Volume 5 Issue 6 Pages
775-776
Published: 1989
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Toshihiko IMATO, Akiko KATAFUCHI, Taeko HAMAZOE, Jun-ichi YACI, KOZO T ...
1989 Volume 5 Issue 6 Pages
777-779
Published: 1989
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Teiji KAKIZAKI, Satoshi HIKIMA, Kiyoshi HASEBE
1989 Volume 5 Issue 6 Pages
781-782
Published: December 10, 1989
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Takeshi YAMANE, Eiichi GOTO
1989 Volume 5 Issue 6 Pages
783-784
Published: December 10, 1989
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Atomi YOSHIDA, Reimei MOROI, Masahiro ARIMOTO, Minoru FURUKAWA
1989 Volume 5 Issue 6 Pages
785-786
Published: December 10, 1989
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