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EIJI NIKI
1991 Volume 7 Issue Supple Pages
1-2
Published: 1991
Released on J-STAGE: July 27, 2007
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HIDEO AKAIWA, HIROSHI KAWAMOTO
1991 Volume 7 Issue Supple Pages
3-6
Published: 1991
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An approach to the mutual separation of chemically similar metal ions using chelate extraction is shown on the basis of HSAB rule. The critical separation condition for In
III and Ga
III was obtained by the S
B-σ
B diagram, where S
B and σ
B are the proposed HSAB parameters for a chelating agent. This concept was successfully applied to the design of mutual separation scheme of Cd
II and Zn
II using synergistic extraction.
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HISAO KOKUSEN, YOSHIKI SOHRIN, SORIN KIHARA, MASAKAZU MATSUI
1991 Volume 7 Issue Supple Pages
7-10
Published: 1991
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Extraction behavior of divalent transition and group IIA metals with five polypyrazolylborates, H
4-nB(pz*)
n- (pz: 1-pyrazolyl or 3, 5-dimethyl-l-pyrazolyl; n=2, 3 and 4) has been studied. Bidentate bispyrazolylborate ligands extract divalent transition metals but do not group IIA metals. The selectivity of dihydrobis(1-pyrazolyl)borate for transition metals resembles that of 8-hydroxyquinoline. Methyl substituents in the pyrazole ring increase the stability of chelates through inductive effect and decrease that for small metal ions through steric hindrance. Hydrotris- and tetrakis(1-pyrazolyl)borate, which can act as a tridentate ligand, are highly strong extracting ligands for divalent transition metals. Moreover, these ligands extract Be(II), Mg(II) and Ca(II). Steric characteristics of the ligands contribute to anomalously high stability of the chelates and selectivity for the metal ions.
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CLAUDE MUSIKAS, NICOLE CONDAMINES, CHRISTINE CUILLERDIER
1991 Volume 7 Issue Supple Pages
11-16
Published: 1991
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A review of the actinide and lanthanide extraction chemistry by N, N-dialkylamides and N, N'- tetraalkylamides is given. It includes the extraction equilibria of inorganic acids. The prospects of using. these completely incinerable extractants in the nuclear fuels cycle is discussed.
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YOSHIKI SOHRIN, SORIN KIHARA, MASAKAZU MATSUI
1991 Volume 7 Issue Supple Pages
17-20
Published: 1991
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Methylated and inorganic germanium compounds have been separated by liquid-liquid extraction from aqueous hydrohalogenic acid (HX) solution into carbon tetrachloride. The germanium compounds dissolve in water as their hydroxides ((CH
3)
nGe(OH)
4-n: n=0, 1, 2 or 3), and form their halide complexes ((CH
3)
nGeX
4-n) in HX solution. Large difference in the extraction constants and stability constants of (CH
3)
nGeX
4-nare ascribed to the inductive effect of the methyl groups which reduces the stability of the bond between the germanium atom (hard acid) and a hydroxide ion (hard base).
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TOSHIKI TAYA, TAKASHI OHYABU, KUNIO DOI, HIDEFUMI SAKAMOTO, MAKOTO OTO ...
1991 Volume 7 Issue Supple Pages
21-24
Published: 1991
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Solvent extraxction of nickel(II) complexes with five heterocyclic hydrazones(containing pyridine- or/and quinoline-nitrogen atoms as the coordinating sites) into chloroform or benzene has been studied kinetically at 25°C and μ=01 by means of a spectrophotometric method. The kinetics of extraction of nickel(II) ion is first order in each of the aqueous nickel(II) concentration and the hydrazone concentration in the organic phase. The observed second-order rate constant, k
obs'-pH profiles suggest three rate-determining steps to be considered in the aqueous phase: Ni
2++ H
2L
+→, Ni
2++HL→and Ni(OH)
++HL→ The rate constant for the formation of 1:1 complex with 2-pyridylmethanone 2-pyridylhydrazone (PAPH) was consistent with those for bipyridine and terpyridine. Replacement of pyridyl group by quinolyl group affects the distribution constant(K
d) of the ligand between the two phases rather than the rate constants for rate-determining steps, and consequently the difference in k
obs is chiefly governed by K
d. The influence of the structure of ligands on the rate constants is also discussed.
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EQUILIBRIUM AND KINETICS
KATSUTOSHI INOUE, YOSHINARI BABA, KAZUHARU YOSHIZUKA
1991 Volume 7 Issue Supple Pages
25-28
Published: 1991
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Solvent extraction of palladium(II) with N, N-dioctylglycine, an amino-acid derivative, from aqueous acidic chloride media was investigated in terms of distribution equilibrium and extraction kinetics. The reagent was found to be dimerized in the organic phase (toluene) and to have high aqueous solubility compared with usual carboxylic acid extractants. Palladium(II) is extracted as a 1:2 metal:reagent chelate of the type PdR
2. From the high aqueous distribution of the reagent and the concentration dependencies of the reactant species on the extraction rate, the extraction kinetics was interpreted on the basis of the heterophase homogeneous reaction model where the rate determining reactions of complexation take place in the aqueous phase.
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Kaoru Fujinaga
1991 Volume 7 Issue Supple Pages
29-30
Published: 1991
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The transition metals such as zinc, cobalt, nickel, and copper were extracted into a carbon disulfide-isoamylalcohol-pyridine ternary mixed solvent. The optimal pH ranges for extraction are 2.6-8.0 for copper, 7.9-8.5 for zinc, 2.0-2.6 for nickel, and 1.6-3.5 for cobalt, respectively.
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YOSHITAKA MASUDA, TETUYA SAWANO, EIICHI SEKIDO
1991 Volume 7 Issue Supple Pages
31-34
Published: 1991
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Hexameric p-t-butylcalix[6]arene(tbca, HmL, m=2 or 1) in the various solvents has shown an ability to extract silver(I), palladium(II) and nickel(II) from the ammonia alkaline solution.The results from liquid liquid extraction study suggested the formation of the 1:1 metal (Ag, Pd and Ni) to tbca complex as the extracted species. A percent extraction (% E) pattern of Pd(II)>Ni(II)>Ag(I) was obtained in 1, 2-dichloroethane, dichloromethane and nitrobenzene solvents. The order of high extractability (pH=11.7 and pH=13.5) corresponds to increase of dielectric constant except nitrobenzene.
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KENSAKU HARAGUCHI, TOSHIO OGATA, KOICHI NAKAGAWA, MANABU OKUYAMA, TOHR ...
1991 Volume 7 Issue Supple Pages
35-38
Published: 1991
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The extraction behavior of scandium (III), yttrium (III) and certain lanthanoid (III) ions, namely praseodymium, europium and ytterbium, from aqueous solutions into carbon tetrachloride solutions containing various N-alkylcarbonyl-N-phenylhydroxylamines(R-PHAs) has been studied at 298K and the ionic strength, 0.1(NaNO
3) The chelating extractants studied were N-octanoyl-N-phenylhydroxylamine (C8-PHA), N-(2-propylpentanoyl)-N-phenylhydroxylamine(PP-PHA) and N-(2-hexyldecanoyl)-N-phenylhydroxylamine(HD-PHA). The metal ions studied were all extracted with all the R-PHAs as self-adducts of the form ML
3(HL)
2, where L and HL represent the ligand anion and neutral ligand, respectively The extraction constants and separation factors for the extraction systems were evaluated. HD-PHA and PP-PHA were excellent extractants for the separation of yttrium from heavy lanthanoids.
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SATSUO KAMATA, NOBUKO WATANABE, HISANORI IMURA, KOUSABURO OHASHI
1991 Volume 7 Issue Supple Pages
39-40
Published: 1991
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The study on the rate and mechanism of the extraction of palladium (II) with o-xylylene bis (pyrrolidinedithiocarbamate) (o-XPDTC) and o-xylylene bis(diethyldithiocarbamate) (o-XEDTC) into chloroform from weakly acidic chloride and bromide media at 25°C has been reported. The extraction rate ca be represented as -d[Pd(II)]/dt=k
1[PdX
3 (H
2O)
-][Q]
O K
DR-1+k
2[PdX
42-][Q]
OK
DR (X=Cl
-, Br
-), where Q denots the extractants and K
DR is the distribution constants between the organic phase and the aqueous phase. The values of k
1 and k
2 are determined and discussed.
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CHIEN. M. WAI, H. S. DU, YOSHIHIRO MEGURO, ZENKO YOSHIDA
1991 Volume 7 Issue Supple Pages
41-44
Published: 1991
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Solvent extraction characteristics of Th, U, Np, Pu, Am and Cm ions of various oxidation states by ionizable crown ethers such as sym-dibenzo-16-crown-5-oxyacetic acid and sym-dibenzo-16-crown-oxyacetylhydroxamic acid were studied. From results of pH-dependence of the distribution ratio of metal ions the ionizable crown ethers are promising for the application in the separation and preconcentration of actinide elements. The extracted species of Th(IV), U(VI) and Am(III) were confirmed to be Th(OH)
2L
2 (L; crown ether), UO
2(OH)L and Am(OH)L
2, respectively.
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HIROSHI ONISHI, HIDEKO DOSHIMA
1991 Volume 7 Issue Supple Pages
45-46
Published: 1991
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This is a little review of the authors' work since 1985 on the extraction of chloro complexes, ReO
4-, and BF
4- with crown ethers and the adsorption of the chloro complexes on a crown ether polymer.
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TATSUO ITOH, MOKARRAM BILLAH, TAKAHARU HONJO, KIKUO TERADA
1991 Volume 7 Issue Supple Pages
47-50
Published: 1991
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A new method for the separation and determination of a trace amount of lithium in ppb-ppm level in water as its thenoyltrifluoroacetone (TTA) complex with 12-crown-4 (12C4) has been established by means of synergic extraction and back extraction combined with flame photometry. The effect of various factors (pH, solvent, reagent concentration, shaking time, preconcentration factor, and foreign ions etc.) on the extraction and back extraction of lithium has been investigated.
Here the lithium TTA chelate in o-dichlorobenzene forms stable adducts with 12C4 (LiTTA•n12C4, n=0-2); the stability constants (β
n) of the adducts determined by means of curve fitting method being β
1=4.46 and β
2=6.45. The amount of lithium in sodium chloride of guaranteed reagent was found to be 9.5 ±0.2ppb by means of the proposed method.
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YOSHIHIRO MEGURO, HIROSHI MUTO, ZENKO YOSHIDA
1991 Volume 7 Issue Supple Pages
51-54
Published: 1991
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Extraction behavior of Am
3+ with six kinds of crown ethers(CE) and 2-thenoyltrifluoroacetone(HTTA) in benzene, cyclohexane and 1, 2-dichloroethane was studied. Synergistic extraction of Am(TTA)
3(CE) was observed using benzene and cyclohexane and adduct formation constants were determined. We found the steric effect of CE is important as well as basicity of CE for the evaluation of the adduct formation constants. Ion-pair extraction of Arrn(TTA)
2(CE)
n+ was observed with 1, 2-dichloroethane.
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JUNJI NORO, TATSUYA SEKINE
1991 Volume 7 Issue Supple Pages
55-56
Published: 1991
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Solvent extraction of La
3+, Eu
3+ and Lu
3+ ions into carbon tetrachloride with thenoyltrifluoroacetone(Htta; HA) in the absence and presence of tetrabutylammonium ions(tba
+) is measured and the effect of various factors on the extraction equilibrium is considered. The data are treated on the basis of association equilibrium of the neutral chelate, MA
3, with the extracted ion-pairs of the reagents, A
-•B
+, in the organic phase. It is concluded that the degree of association is greater in the order of LaA
3>EuA
3>LuA
3 or the stability of the ternary complex in the organic phase is higher in the order of LaA4
-•B
+>EuA4
-•B
+>LuA4
-•B
+
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KENJI CHAYAMA, YUZO TAMARI, HARUO TSUJI, YUZURU KUSAKA, EIICHI SEKIDO
1991 Volume 7 Issue Supple Pages
57-60
Published: 1991
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A new tetrathioether derivative in which two hydroxy-nitrophenyl groups are introduced as the chromogenic groups, 1, 13-bis-(2-hydroxy-5-nitrophenyl)-2, 5, 9, 12-tetrathiatridecane, has been successfully synthesized and its characteristics as an extracting and spectrophotometric reagent of metals have been examined.
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WU-HSIUNG HO
1991 Volume 7 Issue Supple Pages
61-64
Published: 1991
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The extraction constants for ion associates of SDS with several dyes have been determined. Of the dyes examined, methylene blue is the most useful reagent. By use of methylene blue, trace amount of anionic surfactants can be extracted into 1, 2-dichloroethane in a single step extraction and determined spectrophotometrically at 657nm. With a 100mL water sample, the detection limit of this method is 9 parts per billion. The method is simple and rapid.
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SERGUEI DMITRIEV, ALEXANDER KRASNOV, TATIANA SHISHKINA, JUAEN CHIMEG, ...
1991 Volume 7 Issue Supple Pages
65-68
Published: 1991
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The extractive concentrating of Pt and Au from chloride solution and leaching pulp by solid extractants on the basic of quaternary ammonium iodide, TOPO and TBP has been studied as a prior stage of determination of these elements by XRF and NA methods. The optimal conditions for complete isolation of Pt and Au by SE are recommended. The accuracy of the technique was checked using different reference materials. The results agreed within 10%.
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AKINORI JYO, TOMOKO TANOUE, KAZUNORI ETO, HIROAKI EGAWA
1991 Volume 7 Issue Supple Pages
69-70
Published: 1991
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Two approaches are proposed for use of anion carriers. The first approach is development of an adsorbent specific to nitrite based on cobalt(III) complexes of 6-octadecyl-1, 4, 8, 11-tetraazacyclotetradecane-5, 7-dione impregnated in Amberlite XAD-7. The second one is spectrophotometric determination of fluoride followed by selective extraction with molybdenum(V) complex of tetraphenylporphyrin.
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KIKUO TERADA, HIROO KAWAMURA
1991 Volume 7 Issue Supple Pages
71-74
Published: 1991
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Dithiocarbamate-chitin (DTC-chitin) has been synthesized and used for concentration of gold (III), palladium (II) and ruthenium (III) from an acidic solution. The former two metals were quantitatively retained on the polymer from 6M hydrochloric acid even at a high flow rate(15ml min
-1), in contrast to only 80% retention for ruthenium in a narrow pH range, 3.0-4.5. Gold retained on the polymer could be eluted with 1M nitric acid containing 5% thiourea, while palladium with 1.6-fold diluted inverse aqua regia.
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TOSHIO MATSUDA, TOYOSHI NAGAI
1991 Volume 7 Issue Supple Pages
75-78
Published: 1991
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A simple method for reconcentration and separation of trace amounts of bismuth(III) in the presence of large amounts of silver(I) was established by filtration through a membrane filter loaded with hydrous lead dioxide(HLD), which adsorbed 5-10μg of bismuth(III). Bismuth(III) was not affected by the presence of 5-10g of silver(I) at pH 1, because the adsorption of silver(I) on the HLD occurred at a pH above 2. This method is applicable to the determination of bismuth in high purity silver.
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ITSUSEI FUJITA, YUKO NAGANO, MAMORU HARATAKE, KUMIKO HARADA, MORIO NAK ...
1991 Volume 7 Issue Supple Pages
79-82
Published: 1991
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Two series of resins with both polar and nonpolar regions were synthesized by the introduction of α-oxoalkyl and α-hydroxyalkyl groups to a porous low crosslinked styrene-divinylbenzene. These resins showed higher adsorption capacity for nonionic and anionic surfactants than did the starting resin. Resins with shorter alkyl chains were particularly more effective than those with longer chains. The polar groups introduced contributed to the increase in adsorption of the surfactants. These resins were applied to preconcentration of anionic surfactants in environmental specimen.
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AIJUN TONG, YOSHIFUMI AKAMA
1991 Volume 7 Issue Supple Pages
83-86
Published: 1991
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The concentration of metal ions(Cd
2+ Cu
2+ Pb
2+ Mn
2+ Zn
2+ and Fe
3+) on 1-phenyl-3-methyl-4-stearoyl-5-pyrazolone (C18) loaded on silica gel(C18/SG) was investigated by batch and column methods. At pH values higher than 6, these metals were quantitatively retained on C18/SG. The adsorbent did not change its retention efficiency for the metals for at least 6 adsorption/elution cycles. Results of determinations of these metals in environmental samples were satisfactory.
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MASATO AIHARA, HIDEO WATANABE, MITSUO KIBOKU
1991 Volume 7 Issue Supple Pages
87-90
Published: 1991
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Preconcentration/atomic absorption spectrophotometric determination of trace metal ions was investigated with xanthate or dithiocarbamate immobilized silica gels as the chelating functional groups. The preconcentration and determination of trace amounts of palladiu m(III), silver(I), platinum(IV) and gold(III) was performed with good precision.
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SHIGERU TAGUCHI, KOSHIRO TOMIZAWA, SHIN-ICHIRO HIYOSHI, NORIKO HATA, I ...
1991 Volume 7 Issue Supple Pages
91-94
Published: 1991
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A simple and rapid preconcentration technique is proposed for the ETA-AAS determination of traces of aluminum in water. Aluminum at μg/l levels in 100ml of water sample is converted into an anionic complex with Chromazurol B. The anion is collected on a polytetrafluoroethylene (PTFE) membrane filter as an ion-associate with benzyldimethyltetradecylammonium ion (Zeph
+) by filtration under suction. The ion-associate on the membrane is eluted in 5ml of a mixture of ethanol and N, N-dimethylformamide. The aluminum in the concentrate is determined by ETA-AAS. Once the complex is formed, it takes only 5minutes for the collection and elution of the ion-associate. This technique was applied to the analyses of tap waters.
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KAZUYUKI KASUGA, KAZUHISA HIRATANI
1991 Volume 7 Issue Supple Pages
95-98
Published: 1991
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Several new triamide compounds having two 8-quinolyl groups have been synthesized from L-glutamic acid and their Cu(II) transport abilities as carriers through liquid membranes were investigated. It has been found that the Cu(II) transport ability of the carrier is significantly affected by the N-substituent of the 2-amido group. Among of these compounds, 2-acetylamino and 2-n-butyrylamino derivatives show excellent Cu(II) transport ability
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OSAMU KUJIRAI, KEI YAMADA, MUNEYUKI KOHRI, HARUNO OKOCHI
1991 Volume 7 Issue Supple Pages
99-102
Published: 1991
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Ten elements (Co, Cr, Cu, Fe, Mn, Ni, Ti, V, Zn and Zr) in molybdenum disilicide are quantitatively coprecipitated with lanthanum hydroxide. Sample treatment and effects of acids, pH and La are studied. Traces of impurities are determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES) using matrix-matched calibration solutions.
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BEATA WALCZAK
1991 Volume 7 Issue Supple Pages
103-107
Published: 1991
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The selectivity of E-s-cis and Z-s-cis X, Y substituted chalcones in 36 HPLC systems has been compared. The main factors influencing the selectivity of these isomers in the both RP-HPLC and NP-HPLC systems with different stationary and mobile phases were analyzed by means of Principal Component Analysis (PCA). Separation of the isomeric chalcones was found to be well related to the substitution pattern on the chalcone core.
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TADAO OKUTANI, AKIO SAKURAGAWA, MICHIO MURAKAMI
1991 Volume 7 Issue Supple Pages
109-112
Published: 1991
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Iron, cobalt and nickel-4-(2-pyridylazo) resorcinol complexes are extracted into chloroform with counter-cations. The complexes are separated on a column of Waters μ-BONDAPAK
TMC
18 with the eluent of methanol-chloroform-water containing phosphate buffer(pH 5.0) (53:2:45, v/v) and are detected at 510nm. The determination limit is 0.50ppb of cobalt, and 1.50ppb of iron and nickel when the ion-pair extraction is applied.
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KENJI KARUBE, YOSHIHIRO IWASAKI, RIEKO MATSUSHITA, SOEI KOIZUMI, WATAR ...
1991 Volume 7 Issue Supple Pages
113-116
Published: 1991
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In determination of nonionic surfactants in cold rolling oil of emulsion type, new pretreatment which is not filtration of iron fines but dissolution of iron fines by combination of citric acid and a microwave irradiation(2.45GHz) was investigated. In addition, by combination of silica gel packed column chromatography and HPLC, the nonionic surfactants were determined in the yields from 82% to 98%.
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SHIN-ICHI SUZUKI, YASUHIRO SUZUKI, YOSHIYASU HIGASHIKAWA, TOHRU KISHI, ...
1991 Volume 7 Issue Supple Pages
117-120
Published: 1991
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Three classes of dyes and synthetic fibers (including dyed fibers), such as disperse dyes (polyester or diacetate), cationic dyes (acryl) and acid dyes (nylon) were examined for the extraction from a single fiber and successive analysis by high performance liquid chromatography (HPLC) with multi-wavelength detection.
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SAIJUN LI, HIDENARI INOUE
1991 Volume 7 Issue Supple Pages
121-124
Published: 1991
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Manganese(III) chlorophyll-a [Mn(III)-chl-a] has been synthesized in almost pure form from pheophytin-a and manganese(II) acetate. A good separation of Mn(III)-chl-a has been achieved by reversed-phase high performance liquid chromatography. The chromatographic behavior, absorption spectra and elemental analyses have demonstrated that manganese(II) chlorophyll-a [Mn(II)-chl-a] and Mn(III)-chl-a are formulated as [Mn(II) (chlorophyll-a) ] and [Mn(III) (chlorophyll-a) (CH
3COO)
- (H
2O)] respectivery. A comparison of visible absorption spectra has revealed that Mn(II)-chl-a has Soret and Q bands characteristic of metallochlorophylls of divalent transition metal ions. On the other hand, the absorption spectrum of Mn(III)-chl-a makes a great difference in shape and intensity. This consequence is interpreted on the basis of a strong metal-ligand mixing in Mn(III)-chl-a
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YOSHIHIDE YASUI, MORIMASA HAYASHI
1991 Volume 7 Issue Supple Pages
125-128
Published: 1991
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It has been found that ascorbic acid (AA) and dehydroascorbic acid (DHAA) can be derivatized to the compounds having a maximum absorption wavelength of 300nm under alkaline conditions, and that derivatization of DHAA is accelerated in the presence of a reducing agent such as sodium borohydride. This reaction has been applied to post-column derivatization in high performance liquid chromatography (HPLC) for the simultaneous determination of AA and DHAA. In this system, AA in the range of 1ng 2μg and DHAA in the range of 2ng 2μg have been determined simultaneously with good reproducibility, C.V 1.5% (n=10).
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SHENGXIANG JIANG, LIREN CHEN
1991 Volume 7 Issue Supple Pages
129-131
Published: 1991
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A multi - dimensional high performance liquid chromatography for the determination of trace petroleum sulfonates in crude oil is presented in this paper. Two columns are used; a reversed-phase column and an anion-exchange one. Good separation of crude oil, petroleum mono-selfonate and petroleum disulfonate can be obtained within 8 minutes, with recoveries between 96-106%. The minimum detection limits are; 50ppm for mono-sulfonate and 10ppm for disulfonate.
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Hiroshi Suzaki, Manabu Igawa
1991 Volume 7 Issue Supple Pages
133-134
Published: 1991
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An analytical procedure that couples HPLC with the postcolumn reaction detector of flow injection method was developed to analyze aldehydes in fogwater samples. The aldehydes were derivatized with 3-methyl-2-benzothiazolinone hydrazone (MBTH) in the reactor and detected at 640nm. The optimal condition was established and formaldehyde, glyoxal, and glycolaldehyde concentrations were determined. The data obtained by this method were consistent with those obtained by 2, 4-dinitrophenylhydrazine (DNPH) method.
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Wenzhi Hu, Toyohide Takeuchi, Hiroki Haraguchi
1991 Volume 7 Issue Supple Pages
135-138
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A selective, method for the determination of the determination of monophosphate-type nucleotides based on the molybdenum blue method has been developed. The monophosphates were decomposed to produce the orthophosphate-molybdenum blue complex by heating at 140°C without any oxidizing agent, while di- or triphosphates hardly produced the complex under the same condition. The separation of monophosphates was carried out in the ion-exchange mode, and the detection limits were 25ppb as P for the monophosphates examined.
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ION-INTERACTION CHROMATOGRAPHY
ROKURO KURODA, KATSUAKI SATO, KOICHI OGUMA
1991 Volume 7 Issue Supple Pages
139-142
Published: 1991
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Preconcentration and ion-interaction chromatography of scandium have been worked out for the determination of scandium in geological materials. Scandium can be enriched by cation-exchange in thiocyanate-hydrochloric acid medium after wet decomposition of rock sample with hydrofluoric-perchloric acids. Subsequent ion-interaction chromatography in lactate medium allows scandium to be determined selectively and sensitively with post-column reaction detection with Arsenazo III. About 5 to 50μg Sc/g of silicate rocks has been determined with good precision.
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TOSHIAKI SATO, KAZUYUKI OHUCHI, ICHIROU KOHNO, SATOSHI FUJINUMA, KAZUH ...
1991 Volume 7 Issue Supple Pages
143-146
Published: 1991
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The chromatographical behaviors of proteins on FAP column are described. Firstly the elution patterns from PAP column were aproximately same as those from HAP column. The recovery estimated with cytochrome c and others were aproximately 100% but the less recovery was estimated for denatured proteins. The pH dependancy of protein adsorption on FAP was determined. All of proteins including very acidic proteins were adsorbed at pH 5 and were eluted at pH 8.
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A UNIQUE REVERSAL OF ELUTION ORDER ON CHANGING THE NATURE OF THE MOBILE PHASE MODIFIER
MASAHIKO OKAMOTO, HIROSHI NAKAZAWA
1991 Volume 7 Issue Supple Pages
147-150
Published: 1991
Released on J-STAGE: July 27, 2007
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The enantiomeric separation of pyriproxyfen(Sumilarv
®), a new insect growth regulator- was investigated on several commercially available chiral stationary phases consisting of cellulose esters coated on silica. The resolution has been only achieved by using a cellulose Iris (4-methylbenzoate)-coated silica gel. The enantiomeric elution order changed according to the steric bulk of the alcohols. The possible mechanisms of the reversal of elution order are discussed.
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NAOBUMI OI, HAJIMU KITAHARA, REIKO KIRA, FUMIKO AOKI
1991 Volume 7 Issue Supple Pages
151-152
Published: 1991
Released on J-STAGE: July 27, 2007
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HPLC separation of enantiomers on the reversed phase silica gel coated with a chiral Schiff base copper complex (the binuclear copper(II) complex of N-salicyliden-(R)-2-amino-l, 1-bis(2-butoxy-5-tert-butylphenyl)-3-phenylpropanol-1) was examined. Various enantiomers of aminoalcohol, amino acid and amine were well resolved with Cu(IE) ion solution as eluent at room temperature. This copper complex is promising as the stationary phase for the enantiomer separation by HPLC.
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YO KOMATSU, YOSHINORI FUJIKI, TAKAYOSHI SASAKI
1991 Volume 7 Issue Supple Pages
153-156
Published: 1991
Released on J-STAGE: July 27, 2007
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An ion exchanger, composed of dihydrogen tetratitanate hydrate fibers, H
2Ti
4O
9•nh
2O, was prepared by synthesizing K
2Ti
4O
9 and converting it to a H
+ farm. Ion-exchange equilibria of alkaline earth metal ions on the crystalline fibers were measured at 298K. The ion-exchange reaction is explained in terms of two hydrogen-ions from the fibers being Ion exchanged with one alkaline earth metal ion in the aqueous solution. The separation factors were determined for the combinations of barium(II) and other alkaline earth metal ions. The effluent curves for such combinations suggest a successful separation of these metal ions in the aqueous solution.
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QUN SUN, SHIFEN MOU, JIHONG LIN, DEPEI LU
1991 Volume 7 Issue Supple Pages
157-160
Published: 1991
Released on J-STAGE: July 27, 2007
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Anion-Exchange Chromatography followed by pulsed amperometric detection (AE-PAD) was applied to the analysis of the monosaccharides in lipopolysaccharides (LPS). Under alkaline condition, nine underivatized monosaccharides (fucose, rhamnose, galactosamine, arabinose, glucosamine, galactose, glucose, xylose and mannose) were separated within 25 minutes at an eluent flowrate of 1.0ml/min. Based on this method, the LPS samples, which were extracted from Salmonella abortus equi, were analyzed. The results revealed the monosaccharide constituents in LPS samples.
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Y. S. FUNG, K. L. DAO
1991 Volume 7 Issue Supple Pages
161-164
Published: 1991
Released on J-STAGE: July 27, 2007
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A method for indirect UV detection of carbonate in solution using potassium phthalate as eluent has been developed. The detection limit for carbonate is 0.5mg/l in solution. The application of the analytical method developed to the analysis of trace organic carbon in deionised water and total carbon in air particulate was investigated and the results indicate satisfactory recovery, good accuracy and precision of the method.
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HIROKI KUMAGAI, YOSHINORI INOUE
1991 Volume 7 Issue Supple Pages
165-166
Published: 1991
Released on J-STAGE: July 27, 2007
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3 types of anion exchange resins using hydrophilic polymers as base material (polyhydroxymethacrylate [PMA] and polyvinylalcohol [PVA] gels were used) have been synthesized to investigate the influence of base material's nature. It has become apparent that in ion chromatography the elution characteristics of anions has been influenced by base material's nature, e.g., hydrophobicity, π-π interaction, and base material's nature can be used to improving characteristics of anion exchange resins.
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YASUYUKI MIURA, TOMOZO KOH
1991 Volume 7 Issue Supple Pages
167-170
Published: 1991
Released on J-STAGE: July 27, 2007
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A sensitive and simple method has been developed for the determination of thiocyanate in human urine samples by suppressed ion chromatography with conductivity detector in which a carbonate solution mixed with trace amount of 1, 3, 5-benzenetricarboxylate (BTC) was used as an eluent. This eluent made thiocyanate elution earlier than a single eluent of carbonate, and also caused the peak of chromatogram for thiocyanate to be sharper When a 3mM carbonate -2μM BTC solution was used for a 50-μl aliquot of sample solution, the calibration graph obtained for thiocyanate plotted as peak height vs. concentration was linear up to 0.05mM, and the detection limit as S/N 3 was 0.2μM of thiocyanate. The proposed method was successfully applied to the determination of thiocyanate in various human urine samples.
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APPLICATION TO THE DETERMINATION OF 7-DEHYDROCHOLESTEROL IN HUMAN SKIN SURFACE
TOMOYUKI OE, TATSUHITO MIZUGUCHI, KAZUTAKE SHIMADA
1991 Volume 7 Issue Supple Pages
171-172
Published: 1991
Released on J-STAGE: July 27, 2007
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One of the Cookson-type reagents, 4-(1-anthryl)-1, 2, 4-triazoline-3, 5-dione, has been applied to the determination of 7-dehydrocholesterol in human skin surface. The extract from human skin surface was derivatized with the reagent and the obtained adduct was selectively detected using a UV detector.
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M. Nakajima, H. Wakabayashi, S. Yamato, K. Shimada
1991 Volume 7 Issue Supple Pages
173-176
Published: 1991
Released on J-STAGE: July 27, 2007
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New labeling agent, 2-[2-(azidocarbonyl)ethyl]-3-methyl-1, 4-naphthoquinone (AMQ), has been synthesized and developed for the analysis of alcohols in HPLC with fluorescence or electrochemical detection after post column reduction with platinum catalyst. Optimal reaction conditions of AMQ were examined with 1-eicosanol selected as a model compound of alcohols. Alcohols were reacted with the reagent in acetone at 100°C for 15min to form the corresponding carbamic acid esters, which were separated on an Inertsii C8 reversed-phase column with aqueous methanol containing 0.05M sodium perchlorate. The detection limit for 1-eicosanol with electrochemical detection was 16fmol/10μl injection volume.
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Riichiro NAKAJIMA, Eiji NAKAMOTO, Hiroki KAMIUCHI, Youko UEDA, Susumu ...
1991 Volume 7 Issue Supple Pages
177-180
Published: 1991
Released on J-STAGE: July 27, 2007
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To emphasize the capability of a fluorescent thienylpyridine skeleton, the derivatization of carboxylic acid, aldehyde, ketone, and glycine were examined and applied to the following determinations: glycine with 5-(4-pyridyl)-2-thiophene-carbaldehyde using CE, carboxylic acids with 5-(4-pyridyl)-2-thiophenemethanol or 4-(5-diazomethyl-2-thienyl) pyridine using HPLC, carboxylic acids with 1-(2-ammonioethyl) -4-(2-thienyl) pyridinium dibromide using CE, and aldehydes and ketones with 4-(2-thienyl) pyridinium acetohydrazide chloride.
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HIROSHI NAGASARA, YONEZO MATSUMOTO, NAOBUMI OI, SHIGERU YOKOYAMA, TETS ...
1991 Volume 7 Issue Supple Pages
181-182
Published: 1991
Released on J-STAGE: July 27, 2007
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As porous glass under severe contorolled condition has the very narrow range of pore size distribution and similar pore shape irrespective of its size, the effects of pore size can be examined clearly. Effects of pore size on the retention time for several kinds of standard materials were examined by reversed-phase chromatography using five kinds of octadecyl silanized (ODS-) porous glasses with different pore diameters. The result shows that the retention time is greatly influenced by the pore diameter, i.e., the larger the pore diameter, the shorter the time required for elution. Thus the retention time can be adjusted by controlling the pore diameter.
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