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Kikuo TERADA
1991 Volume 7 Issue 2 Pages
187-198
Published: April 10, 1991
Released on J-STAGE: June 30, 2006
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In the determination of trace elements in complex matrices, enrichment and separation of the analytes is of special importance. A wide variety of methods have been proposed for preconcentration according to the nature of the samples, the types and concentrations of the analytes, and the methods to be used for measurement. Among them, the preconcentration techniques based on sorption seem to be convenient, rapid and capable of attaining a high concentration factor. Various efforts have been made to improve selectivity, rate and capacity of sorption, specially for heavy metals in natural waters. The use of silica gel as a support for loading or chemically immobilizing with complexing agents is a particular example. In this paper, the preparation and characterization of complex-forming adsorbents for the sorption of heavy metals will be critically reviewed, laying stress on the utilization of silica gel as a supporting material.
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Minoru SAKAIRI, Alfred L. YERGEY, K. W. Michael SIU, J. C. Yvec Le BLA ...
1991 Volume 7 Issue 2 Pages
199-202
Published: April 10, 1991
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We demonstrate a high correlation between the natural logarithms of the relative intensities of protonated molecules of amino acids by electrospray and their standard hydration free energies (
r=0.98). This result means that the solvation free energy is an important physical parameter for interpreting the difference in protonated molecule intensities by electrospray.
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Shigeki DAISHIMA, Yoshio IIDA, Fujihiro KANDA
1991 Volume 7 Issue 2 Pages
203-208
Published: April 10, 1991
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The Townsend discharge-nitric oxide chemical ionization mass spectra of 27 alcohols (C
4-C
7) and 24 alkenes (C
6-C
9) were evaluated regarding their isomeric and congeneric distinction. In alcohols, the ion abundance of major ions such as (M-OH)
+, (M-3H)
+, (M-H)
+and (M-2H+NO)
+ appearing in their mass spectra were highly dependent on the class of alcohols. Isomeric distinction and selective detection of alcohol were attained by using these characteristic ions. In alkenes, the determination of double-bond positions and the distinction between cis-trans isomers were possible by comparing the intensity ratios of (M+NO-C
nH
2n)
+/(M-H)
+ (n=0, 2-5).
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Yoshio KOSUGI
1991 Volume 7 Issue 2 Pages
209-211
Published: April 10, 1991
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Sulfur-33 NMR spectra of naphthalenesulfonates have been recorded. Chemical shifts of two kinds of the monosulfonates and two isomers of disulfonates are discussed and compared with
13C chemical shifts and substituent effects in benzenesulfonates. The first example of the compression effect in sulfur NMR spectra was confirmed in naphthalene-1, 5-disulfonate. It has also been shown that the quantitative analyses of these isomers by sulfur-33 NMR were possible with a relative error less than 10% of measurement values.
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Tadahiro NAGATA, Masahito HAYATSU, Nobuo KOSUGE
1991 Volume 7 Issue 2 Pages
213-215
Published: April 10, 1991
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Using a modified method for alleviation of base line hump and short acquisition time, aluminum-27 nuclear magnetic resonance studies were carried out on the accumulated aluminum in intact plant tissue. Hydrangea sepals and leaves of 3 species of the family
Theaceae gave aluminum signals at 10-20ppm. This implies that the forms of aluminum are hexacoordinated complexes. The spin lattice relaxation times were 0.4-1.0ms. The spectra showed that both hydrangea sepals and tea leaves contained more than two forms of aluminum.
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Takeo SATO, Kazui MORI, Toyoaki KATO
1991 Volume 7 Issue 2 Pages
217-221
Published: April 10, 1991
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A simple and effective method has been proposed for self-absorption correction for low energy photons in instrumental photon activation analyses of biological materials. The method involves measurements of mass attenuation coefficients of a given sample by means of a standard source of low-energy photons, and the correction for self-absorption at a relevant energy to evaluate quantitative results. Agreements between theoretical and experimental attenuation coefficients were found to be excellent with respect to the biological materials with known elemental compositions. Validity of the method was verified by analyzing several biological standard reference materials: the Orchard Leaves, Bowen′s Kale, Horse Kidney and Lobster Hepatopancreas. Amounts of several elements in human liver and kidney tissues determined by the proposed method are given.
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Sunao YAMADA
1991 Volume 7 Issue 2 Pages
223-227
Published: April 10, 1991
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Characteristics of a two-color multiphoton ionization method with ultraviolet and visible pulsed laser excitation have been investigated for polycyclic aromatic molecules in nonpolar solvents. The photocurrent signal generated by the irradiation at 355nm was enhanced by the additional action of the 532-nm light much more effectively than that at 1064nm in terms of photon flux, except for a few molecules. The extent of the photocurrent enhancement depended on the solvent as well as on the laser pulse energy. The SN ratio was also affected by the laser pulse energy. Detection limits have been determined for selected molecules. The additional action of the 532-nm light certainly improved the detection sensitivity; the lowest detection limit (
S/
N=3) for the two-color method was 9.4×10
-12M (1.7pg ml
-1) for anthracene.
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Norinobu YONEHARA, Shuji KOZONO, Hayao SAKAMOTO
1991 Volume 7 Issue 2 Pages
229-234
Published: April 10, 1991
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A flow injection analysis method is proposed for the spectrophotometric determination of trace amounts of iodide based on its catalytic effect on the oxidation of 4, 4′-bis(dimethylamino)diphenylmethane (tetrabase) by Chloramine T in a weakly acidic solution. Iodide in water samples can be determined at a sampling rate of 85 h
-1 with 300μl sample injections. The detection limit is 0.1μg l
-1 and the calibration graph for iodide is linear up to 2μg l
-1, showing a slightly negative deviation in the higher concentration range. The relative standard deviations are 2.8 and 0.8% for 0.40 and 4.0μg l
-1 iodide, respectively. Although free iodine shows a somewhat lower catalytic effect and iodate no catalytic effect up to at least 50μg l
-1 as iodine, these species show the same effect as iodide upon being reduced with thioacetamide in an acidic solution. The procedure has been applied to the determination of iodide in natural water samples as well as iodine impurity in both distilled and redistilled water samples. It has also been used to examine iodine contamination in ambient air.
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Toshinobu HONDO, Miki KUWAJIMA, Yuzuru SATO, Kazuyo OKAMURA, Yuichiro ...
1991 Volume 7 Issue 2 Pages
235-239
Published: April 10, 1991
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A new computer-assisted analytical strategy has been proposed for both quantitative and qualitative analyses of complex mixture samples. This method is based on simultaneous peak detection at 6 different wavelengths using a photodiode-array multiwavelength detector. It was applied to the analysis of polycyclic aromatic hydrocarbons in petroleum pitch with reference to the NBS standard reference material (SRM-1647). Our new strategy has allowed a tentative identification of 14 compounds among 16 Priority Pollutants contained in pitch through a retention comparison. However, the identification of 4 components was cancelled due to a comparison with the UV spectrum. The method proposed here allows even an inexperienced operator to do analysis work on complex mixture samples with the aid of a computer.
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Takashi NISHIKAWA, Satomi SUZUKI, Hideki OHTANI, Masatoshi SHIRAI, Sus ...
1991 Volume 7 Issue 2 Pages
241-246
Published: April 10, 1991
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ATP and its metabolites, such as ADP, AMP, adenosine, inosine and hypoxanthine, were separated by reversed-phase high performance liquid chromatography with isocratic elution on uncapped and capped silica-based columns, and detected by measuring the absorbance at 254nm. An investigation of the effects of an organic solvent as well as the ionic strength, ion-pairing reagents and pH of the mobile phase allowed us to establish chromatographic conditions which are suitable for the determination of these compounds in biological specimens.
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Kiwao KADOKAMI, Misuzu MORIMOTO, Kimiko HARAGUCHI, Minoru KOGA, Ryota ...
1991 Volume 7 Issue 2 Pages
247-252
Published: April 10, 1991
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The authors have developed an analytical method for determining trace amounts of 39 kinds of pesticides in water with high precision and accuracy by gas chromatography/mass spectrometry with a selected ion monitor (GC/MS-SIM). One liter of water was extracted with dichloromethane; the extract was concentrated to 1ml with a Kuderna-Danish concentrator. After the internal standards, perdeuterated n-alkanes (C
16, C
20 and C
24), were added to the concentrate, quantitative analyses by GC/MS-SIM were performed to measure the recovery efficiencies of the 39 compounds spiked into water samples at concentrations of below μg/l. The recovery efficiencies of the tested compounds, except monocrotophos and bentazone, yielded more than 95% and their relative standard deviations were less than 6%. The developed method was applied to the determination of pesticides in river and tap water. Sixteen pesticides ranging from ng/l to μg/l were detected. This method is useful to elucidate the fates and the concentration levels of pesticides in the aquatic environment.
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Wakako TSUZUKI, Susumu SHIMURA, Kazuaki AKASAKA, Tateo SUZUKI
1991 Volume 7 Issue 2 Pages
253-256
Published: April 10, 1991
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A simple and highly sensitive method for the measurement of lipase activity has been developed using a fluorescent labeling reagent, 9-bromomethylacridine (9-BMA). With an organic solvent-soluble lipase prepared with synthetic detergent, triglycerides were hydrolyzed in a homogeneous solvent system (such as aqueous tetrahydrofuran). The enzyme reaction was terminated by the addition of DMSO containing 9-BMA; then the liberated fatty acid was labeled in the following derivatization reaction at room temperature for 40min. The 9-acridinylmethyl derivative of the fatty acid was separated and determined by high performance liquid chromatography (HPLC). The sensitivity of the method was so high that several nmol level of fatty acid in 200μl of the reaction mixture could be determined. The effects of the pH and of the concentration of buffer on the fluorescent labeling reaction were examined. This method was found to be useful for studying the kinetic properties of lipase.
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Hee-Kyoung JEON, Hitoshi NOHTA, Hiroaki NAGAOKA, Yosuke OHKURA
1991 Volume 7 Issue 2 Pages
257-262
Published: April 10, 1991
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A simple separation method involving isocratic elution and a selective postcolumn derivatization method involving chemical oxidation followed by a fluorescence reaction are described regarding a simultaneous high performance liquid chromatographic determination of catecholamines (three species) and their precursor (one species) and metabolites (nine species, all in the free form). These compounds, isoproterenol and 3, 4-dihydroxyphenylpropanoic acid, are separated by ion-pair reversed-phase chromatography using a mixture of citrate buffer (pH 2.5) containing sodium octanesulfonate and methanol; they are then oxidized with periodate to the corresponding o-quinones, which are converted into fluorescent derivatives by reactions with meso 1, 2-diphenylethylenediamine. The detection limits (
S/
N=3, on column) vary from 15 to 570fmol, depending on the compounds.
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Yuuko ISHII
1991 Volume 7 Issue 2 Pages
263-266
Published: April 10, 1991
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Determinations of calcium oxalate in vegetables were carried out by extraction and ion chromatography of free and total oxalic acids. The free oxalic acid was extracted from the vegetables by immersion for 20min in boiling water. The total oxalic acid was extracted by immersion for one night in 0.1M HCl. The concentration of oxalic acid in the extracts was determined by ion chromatography. The amount of combined oxalic acid was calculated from the difference between the amount of the total oxalic acid and that of the free one; the content of calcium oxalate was also calculated. The contents of the free oxalic acid and calcium oxalate in several vegetables determined by the present method are presented.
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Shinobu KUDOH, Hiroshi NAKAMURA
1991 Volume 7 Issue 2 Pages
267-272
Published: April 10, 1991
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A high performance liquid chromatography method for the simultaneous determination of various types of
β-lactamase with detection specific to enzyme activity has been developed. Separation was achieved on a hydroxyapatite column utilizing a two-step gradient elution of potassium phosphate buffers, with no loss of enzyme activity. A postcolumn reaction based on an enzyme-substrate reaction with Nitrocefin, a well known chromogenic substrate for
β-lactamases, was also optimized to give a highly selective determination using a photometric monitor at 495nm. Using the established method, several
β-lactamases, either commercial or clinically isolated, were successfully separated and detected in a single run. The method was applicable for the measurement of various
β-lactamases.
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Yozo KABASAWA, Kazufusa SHINOMIYA, Hiroyuki NAKAZAWA, Takenori TANIMUR ...
1991 Volume 7 Issue 2 Pages
273-276
Published: April 10, 1991
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The purification of Food Blue No. 1 was examined using rotation locular countercurrent chromatography, which uses the different partition between two immiscible liquids for the chromatographic purification of various substances. Commercially available reagent-grade Food Blue No. 1 allowed the presence of ca. 92% of the main dye and many kinds of subsidiary colors by high performance liquid chromatography. The phase system used for purification comprised 1-butanol-water (1:1 by volume). Purified Blue No. 1 (ca. 220mg) was obtained in a proportion 99.7% higher from ca. 2g of the commercial dye.
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Masaki MIFUNE, Junichi ODO, Noriko MOTOHASHI, Yutaka SAITO, Akimasa IW ...
1991 Volume 7 Issue 2 Pages
277-281
Published: April 10, 1991
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The serum components, glucose, cholesterol and triglyceride, form hydrogen peroxide by corresponding oxidases. The hydrogen peroxide produced was determined by the chromogenic reaction of
N, N-diethylaniline and 4-aminoantipyrine catalyzed by an anion-exchange resin modified with Mn(III)-tetrakis(sulfophenyl)porphine (MnTPPS
r) in place of peroxidase (POD). The calibration curves obtained by the use of MnTPPS
r were linear. The apparent molar absorption coefficients and the relative standard deviations were comparable with those in the POD method. The foreign substances examined did not give any significant interference. MnTPPS
r was a good artificial mimesis of peroxidase or immobilized-peroxidase for the determination of some serum components such as glucose.
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Yukio OKAMOTO
1991 Volume 7 Issue 2 Pages
283-288
Published: April 10, 1991
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A high-power high-efficiency microwave-induced nitrogen and air plasma (N
2 and air MIP) for trace element analysis is presented using a new simple surface wave excitor. The plasma is annular-shaped at atmospheric pressure. The excitor consists of two parts: one part is a flat rectangular waveguide with a reduced height, and the other part is a mode transfer consisting of an inner conductor and an outer cylindrical conductor terminated by a front plate. The surface wave is excited in the gap between the front edge of the inner conductor and the front plate. The microwave power (2.45GHz, 1kW) is coupled to new concentric quartz tubes placed inside the gap. The preliminary analytical performance of the N
2 MIP was examined by measuring the line intensities of Ca II (393.4nm), Zr II (343.8nm) and N
2+ (391.4nm). The plasma is a sensitive ionization source.
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Kazuaki WAGATSUMA, Kichinosuke HIROKAWA
1991 Volume 7 Issue 2 Pages
289-293
Published: April 10, 1991
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A dual-cathode glow discharge lamp was successfully applied to the determination of vanadium in commercial tool steels. A unique feature of our lamp is its capability to eliminate undesired argon emission signals. In the case of the vanadium determination, an analytical line, VI 437.92nm overlaps with the Ar II 437.97nm line. However, an interference-free detection of this line can be performed using the lamp, leading to accurate analyses of 0.1-2.5% vanadium in steel samples.
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Kenji KATO, Yoshinori SUGITANI
1991 Volume 7 Issue 2 Pages
295-298
Published: April 10, 1991
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Surface and subsurface layers of structured materials were observed as the amplitude and phase images of X-ray photoacoustic signals. An X-ray beam from synchrotron radiation was narrowed with the use of a lead slit and allowed to irradiate the sample in the photoacoustic cell. A laminated sheet of aluminum and lead foils and a flexible print circuit board were used as samples. For the laminated sample, the empty space in the subsurface lead layer was clearly visualized in the images of both amplitude and phase delay. The results were compared with those of the photoacoustic measurement in the visible region. For the flexible print-circuit board, the printed copper strips were observed in both the amplitude and the phase images. The circuit pattern below the surface polymer layer was observed as signals with large phase delays.
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Hiromasa KATOH, Yuka FUJIMOTO, Shin-ichi KUWATA
1991 Volume 7 Issue 2 Pages
299-302
Published: April 10, 1991
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The cathode reaction in Karl Fischer coulometric titration is discussed. The cathodic reduction products varied depending on the electrolyte used. In the case of a catholyte which contained carbon tetrachloride, it was easily reduced to chloroform with the reduction products not interfering with water measurements. In case of any catholyte, some of the reduction products showed a potential for possible interference.
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Hidekazu DOE, H. FREISER
1991 Volume 7 Issue 2 Pages
303-311
Published: April 10, 1991
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The mechanism of transfer of Mn
2+ ion from an aqueous to a dichloroethane (DCE) solution of a phenanthroline derivative (Phen); 1, 10-phenanthroline (phen), 4, 7-dimethyl-1, 10-phenanthroline (4, 7-DMP), 4, 7-diphenyl-1, 10-phenanthroline (4, 7-DPP) and 2, 9-dimethyl-1, 10-phenanthroline (2, 9-DMP), was investigated by current scan polarography with the ascending water electrode. The transfer process involves (a) diffusion of Phen to the aqueous/DCE interface, (b) formation of 1:1 Mn
2+-Phen complex, whose kinetics are sufficiently slow to influence but not entirely control the polarographic process, (c) transfer of the 1:1 complex from the aqueous into the DCE phase and (d) further reaction of this complex with two additional Phen molecules at the interfacial area in DCE phase. The apparent reaction rates of step (b) were determined in the dimension of the ordinary electrode reaction rate; 8.2×10
-2, 5.5×10
-2 and 9.3×10
-3dm M
-1 s
-1 for phen, 4, 7-DMP and 4, 7-DPP, respectively. The rate for Mn
2+-2, 9-DMP complex was too slow to be determined.
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Hidekazu DOE, H. FREISER
1991 Volume 7 Issue 2 Pages
313-319
Published: April 10, 1991
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The transfer mechanism of Ni
2+, Co
2+, Zn
2+ and Cd
2+ ions from an aqueous to a dichloroethane (DCE) solution of phenanthroline derivatives (Phen) was studied. Included were 1, 10-phenanthroline (phen), 4, 7-dimethyl-1, 10-phenanthroline (4, 7-DMP), 4, 7-diphenyl-1, 10-phenanthroline (4, 7-DPP) and 2, 9-dimethyl-1, 10-phenanthroline (2, 9-DMP). The investigation was carried out by current-scan polarography at the ascending water electrode (AWE). Some polarographic waves were observed that can be attributed to the slow formation of 1:1 M
2+-Phen complexes. In some cases, as with the Ni
2+-Phen systems and the Co
2+-4, 7-DPP system, no wave was observed, because the complexation rates are too slow. All of the Cd
2+-Phen and all of the Zn
2+-Phen systems, except for the Zn
2+-4, 7-DPP system which exhibits a kinetic wave, yielded diffusion-controlled waves. Furthermore, a number of these systems appear to be affected by significant interfacial adsorption of the M
2+-Phen complexes.
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O. N. OBREZKOV, V. I. SHLYAMIN, O. A. SHPIGUN, Yu. A. ZOLOTOV
1991 Volume 7 Issue 2 Pages
321-325
Published: April 10, 1991
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Different modes of kinetic detection in ion chromatography have been proposed. Equipment schemes have included an ion chromatograph with a conductometric detector and multichannel flow mounting with a spectrophotometric detector. Complex formation of Cr(III) with EDTA accelerated by carbonate has been used as a model indicator reaction. This system has proved to be both selective and universal. A simultaneous determination of carbonate, Cr(III) and various inorganic anions has been possible. A number of objects have been analyzed.
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Yoshikazu FUJITA, Itsuo MORI, Minako TOYODA
1991 Volume 7 Issue 2 Pages
327-328
Published: 1991
Released on J-STAGE: July 27, 2007
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Yuzuru HAYASHI, Rieko MATSUDA
1991 Volume 7 Issue 2 Pages
329-331
Published: April 10, 1991
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Kazumi SASAMOTO, Yoshifumi WATAZU, Yosuke OHKURA
1991 Volume 7 Issue 2 Pages
333-335
Published: April 10, 1991
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Takeo KATAMI, Masamichi FURUKAWA, Tadao SAKAI
1991 Volume 7 Issue 2 Pages
337-339
Published: April 10, 1991
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Oscar HERNANDEZ, Virginia CASTRO, Juan J. ARIAS
1991 Volume 7 Issue 2 Pages
341-344
Published: April 10, 1991
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Tatsuhiko TANAKA, Takayoshi YOSHIMORI
1991 Volume 7 Issue 2 Pages
345-346
Published: April 10, 1991
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Masaya AOYAGI, Yoshiaki YASUMASA, Akemi NISHIDA
1991 Volume 7 Issue 2 Pages
347-348
Published: April 10, 1991
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Yoshihiro NISHIDA, Hiroshi OHRUI, Hiroshi MEGURO, Chizuko KABUTO
1991 Volume 7 Issue 2 Pages
349-350
Published: April 10, 1991
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Atomi YOSHIDA, Reimei MOROI
1991 Volume 7 Issue 2 Pages
351-352
Published: April 10, 1991
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Atomi YOSHIDA, Reimei MOROI
1991 Volume 7 Issue 2 Pages
353-354
Published: April 10, 1991
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