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Kiyoharu ISAGAI
1990 Volume 6 Issue 4 Pages
489
Published: 1990
Released on J-STAGE: July 27, 2007
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Andreas MANDELIS
1990 Volume 6 Issue 4 Pages
491-503
Published: August 10, 1990
Released on J-STAGE: June 30, 2006
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Photothermal and photoacoustic detection of semiconductor photoelectrochemical interfaces can be utilized to yield information about the internal quantum and energy efficiencies of the photoelectrode electrochemical process. The theoretical foundations and progress in the experimental state-of-the-art in this field are reviewed. The importance of measurements in the characterization and/or optimization of energy conversion efficiencies of photoelectrochemical cells, as well as their contribution to our understanding of energy transfer physics at the illuminated interface, will be discussed further.
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Kazumi SASAMOTO, Yosuke OHKURA
1990 Volume 6 Issue 4 Pages
505-509
Published: August 10, 1990
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Compounds in which
N-acetyl-D-glucosaminide groups were covalently attached to chromogenic metal chelators at their metal-binding sites were synthesized as substrates for
N-acetyl-β-D-glucosaminidase (NAGase). Upon incubation with NAGase in the presence of Fe(III), Cu(II) or Co(II) at pH 4.5-5.1, these substrates gave an absorbance increase corresponding to respective metal complexes of their aglycons. Although this approach permitted the rate-assay of
NAGase under the conditions of weakly acidic pH (which had not yet been reported), problems using the chelator-conjugated substrates are tend to be hydrolytic instabilities of the substrates and inhibitory effect of the metal ions over the enzyme.
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Kazuaki AKASAKA, Hiroshi OHRUI, Hiroshi MEGURO, Tateo SUZUKI
1990 Volume 6 Issue 4 Pages
511-514
Published: August 10, 1990
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Characterization of electron impact mass spectra of 9-acridinylmethyl esters of fatty acids was reported. The esters gave molecular ions with relatively strong intensity and simple fragmentation patterns. Fragmentation ions appeared with 14 mass unit separations in the spectra of saturated fatty acid esters. In the spectra of unsaturated fatty acid esters, the 26 mass unit separations were observed at the position of double bonds in the molecule. Ions (M-30)
+ and (M-31)
+ suggested the existence of a hydroxymethyl group and the 29 and 30 mass unit separations suggested the positions of hydroxy groups located in the molecule. These fragmentations were useful for the structural analysis of fatty acids.
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Ken-ichi MAWATARI, Fumio IINUMA, Mitsuo WATANABE
1990 Volume 6 Issue 4 Pages
515-518
Published: August 10, 1990
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A high performance liquid chromatographic method involving postcolumn photochemical reaction and fluorometric detection has been developed for the determination of Isonicotinic acid, acetylisoniazid and Isoniazid in human urine. These compounds are separated by reversed phase chromatography using 0.07M phosphate buffer (pH 6.8) containing 100mM hydrogen peroxide as a mobile phase. The compounds in the column effluent are irradiated with ultraviolet
light to give fluorescence. The fluorescence is monitored with excitation at 316nm and emission at 418nm. The calibration curves for Isonicotinic acid, acetylisoniazid and isoniazid are linear over the ranges of 0.1-120, 1.0-180 and 0.5-200ng, respectively. The mean recoveries of isonicotinic acid, acetylisoniazid and isoniazid from urine are more than 92%. This method can be applied for acetylator phenotyping.
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Yoshihiko UMEGAE, Hitoshi NOHTA, Yosuke OHKURA
1990 Volume 6 Issue 4 Pages
519-522
Published: August 10, 1990
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A selective method for the determination of ribonucleotides is described which employs high performance liquid chromatography with on-line postcolumn fluorescence derivatization. Ribonucleotides are separated on a reversed-phased column (TSK gel ODS-80
TM) and automatically converted into fluorescent derivatives by reaction with 1, 2-bis(4-methoxyphenyl)ethylenediamine in an acidic medium after periodate oxidation. The detection limits (
S/N=3) for ribonucleotides are 14-67pmol in a 100μl injection volume. The quantification of ribonucleotides in human erythrocytes is also described.
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Masaharu NAKAJIMA, Hiroyuki WAKABAYASHI, Susumu YAMATO, Kenji SHIMADA
1990 Volume 6 Issue 4 Pages
523-527
Published: August 10, 1990
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A high performance liquid chromatographic method for polyamines using 1-phenylsulfonyl-3, 3, 3-trifluoropropene as a precolumn derivatization reagent for UV detection has been developed. Polyamines were derivatized with 1-phenylsulfonyl-3, 3, 3-trifluoropropene by addition reaction in the presence of sodium carbonate under mild conditions to convert the corresponding UV-absorbing compounds quantitatively. The derivatized polyamines were separated on a reversed-phase column, Shim-pack CLC-ODS, with aqueous methanol-acetonitrile used as an eluent. Secondary amines like diethylamine and diisopropylamine did not react with this reagent. The detection limits for spermidine, putrescine, cadaverine and spermine at a signal-to-noise ratio of 3, were 0.3, 0.4, 0.4 and 0.6pmol on column, respectively. The derivatization procedure was successfully applied to the determination of the polyamines in rat tissues.
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Masanosuke TAKAGI, Yoshiyuki DAIDO, Masao KURIYAMA, Naofumi MORITA
1990 Volume 6 Issue 4 Pages
529-534
Published: August 10, 1990
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Quinoxaline derivatives derived from glycogen and amylopectin-like glucans by treatment with acid or β-amylase, were used for evaluation of the degree of branching by an alkalineo-phenylenediamine (OPD) method. Ion-exchange resin column chromatography of quinoxalines derived from an amylopectin-β-limit dextrin showed that the glucan had an average chain length (CL) of 9.9 on the C-chain and 1.55 units of branched chains. A glycogen-β-limit dextrin had the CL of 7.8 on the C-chain, with 2.38 units of branch. The degree of branching obtained from this alkaline OPD method agreed with those estimated by other conventional methods.
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Takashi SAITO
1990 Volume 6 Issue 4 Pages
535-539
Published: August 10, 1990
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A badge-type passive sampler has been developed for the determination of formaldehyde (HCHO) in the atmosphere. The filter used in the sampler to collect HCHO comprises Toyo No. 1 filter paper impregnated with a NaHSO3 solution. A passive sampler was attached around either the neck or chest of the examiner; after a definite time smpler was recovered. The concentration of HCHO exposed on the filter of the sampler was then determined using a chromotropic acid-spectrophotometric method, and the HCHO concentration in the atmosphere was estimated. The permissible limit of HCHO concentrations to be measured with the sampler used in the study was 0.200-630ppm-h as a time-weighted average concentration when monitored for 8h. The reproducibility of the determined value of HCHO was excellent, with 4.3% (
n=5) at the relative standard deviation. The recovery of HCHO exposed on the filter was 94.7%. The samplers exposed to HCHO showed no notable change in the HCHO concentration on filters either stored at room temperature or refrigerated for 2 weeks.
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Hiroki OHURA, Toshihiko IMATO, Yasukazu ASANO, Sumio YAMASAKI, Nobuhik ...
1990 Volume 6 Issue 4 Pages
541-545
Published: August 10, 1990
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The selective determination of ethanol in alcoholic beverages is performed by a flow-injection analysis method using gas-diffusion separation. The determination is based on the oxidation of alcohol permeating across a porous membrane with dichromate and the reduction of excess dichromate with ferrous ion in a flow system. The concentration of ferric ion formed is potentiometrically measured with an oxidation-reduction potential electrode and is indirectly related to the alcohol content of the sample. Analytical results using the proposed method are in agreement with those obtained by a specific-gravity method (current official method in Japan) as well as by a gaschromatographic determination.
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S. BEKTAS, S. AKMAN
1990 Volume 6 Issue 4 Pages
547-554
Published: August 10, 1990
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Potassium chloride, calcium chloride, sodium chloride and magnesium chloride cause many different types of interference in the determination of lead and chromium by graphite furnace atomic absorption spectrometry. Simultaneous volatilization of the analyte and the interferent from different, but close, points in the tube are very helpful in the explanation of interference mechanisms. The kind of interference that affects the sensitivity of the determination depends on the thermal behavior of the matrix before and during atomization of the elements. If chloride vapor is formed by decomposition of the matrix before or during atomization of the analyte elements, the formation of a metal chloride in the gas phase may be responsible for decreasing in the sensitivity. If, on the other hand, the matrix is present as a solid or liquid while the elements atomize, the occlusion of the analyte in the bulk of the matrix and the loss by a carrier-type mechanism or a slower transfer of heat to the analyte delaying the atomization cause some changes in the sensitivity. Expulsion of analyte vapors by expanding matrix gases was not effective due to the low heating-rate of the system used
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Hirofumi ISOYAMA, Syuji OKUYAMA, Tetsuo UCHIDA, Masaaki TAKEUCHI, Chuz ...
1990 Volume 6 Issue 4 Pages
555-560
Published: August 10, 1990
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Electrothermal vaporization-inductively coupled plasma atomic emission spectrometry was applied to the determination of trace metals in some biological samples on in-furnace standard addition method. Powdered samples were decomposed using a sealed PTFE vessel and a microwave oven; the sample solution served for measurements without any additional treatment. The sample solution was injected into a graphite furnace and a standard solution containing ammonium dihydrogenphosphate, as a matrix modifier, was added; the two solutions were mixed in the furnace. The present method was applied to the determination of trace metals in some reference materials; the analytical results agreed well with the certified values.
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Byung Mok YOON, Sang Chul SHIM, Hyung Chik PYUN, Dong Soo LEE
1990 Volume 6 Issue 4 Pages
561-566
Published: August 10, 1990
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An ultrasensitive method is described for the measurement of picogram amounts of tellurium species in environmental samples. The method involves selective Te(IV) reduction by sodium borohydride to hydrogen telluride, trapping
in situ in a modified graphite furnace, and subsequent atomic absorption detection. The total amount of Te is determined after Te(VI) reduction to Te(IV) by boiling in hydrochloric acid. The difference between the amounts of Te(IV) and total-Te is taken as the amount of Te(VI). The absolute detection limit ranges from 2 to 4pg of tellurium. The precision of the method is 5.1% for 20pg and 2.5% for 200pg of tellurium. Analytical results are presented for natural waters, aerosol particles, geological and biological materials.
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Sinkichi YAMADA, Noriyuki TAKI, Takeshi KATOH, Akira MURATA
1990 Volume 6 Issue 4 Pages
567-572
Published: August 10, 1990
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Kinetics and thermodynamics of the ligand substitution reactions of niobium and tantalum complexes involving oxalic, tartaric or citric acid as an auxiliary complexing agent with 4-(2-pyridylazo)resorcinol have been studied spectrophotometrically. The equilibrium constant and the rate equation for the respective color reactions were determined at 25°C and
I=0.1 (NaClO
4). A kinetic consideration of the values of the second-order rate constants for the niobium complexes shows that the order of labilizing power of the auxiliary complexing agents is: tartaric acid_??_citric acid>oxalic acid. For a given auxiliary complexing agent, the niobium complex reacts faster with this metallochromic reagent than does the corresponding tantalum complex, irrespective of this order. The thermodynamic effect of the auxiliary complexing agents on this color reaction is discussed.
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Kazuhiko OZUTSUMI, Yoshihiko UCHIMA, Takuji KAWASHIMA
1990 Volume 6 Issue 4 Pages
573-577
Published: August 10, 1990
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The structure of iron(III) complexes with 1, 2-dihydroxybenzene-3, 5-disulfonate (tiron
4-) ion in aqueous solution has been studied by means of extended X-ray absorption fine structure (EXAFS) spectroscopy. EXAFS analyses of solutions containing [Fe(tiron)]
-, [Fe(tiron)
2]
5- and [Fe(tiron)
3]
9- complexes as the main species, respectively, revealed that the complexes have an octahedral structure. The Fe-O bond lengths within the [Fe(H
2O)
6]
3+, [Fe(tiron)(H
2O)
4]
-, [Fe(tiron)
2(H
2O)
2]
5- and [Fe(tiron)
3]
9- complexes are 202(1), 205(1), 202(1) and 204(1) pm, respectively, and are practically the same as that within the [Fe(H
2O)
6]
3+ ion (200pm) determined by the X-ray diffraction method. The Fe-O distances are thus practically the same for all the complexes, within experimental uncertainties. The similar distances may reflect the pure electrostatic interaction between iron(III) ion and oxygen atom in ligands.
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M. Tarek M. ZAKI, S. M. ATTIYA
1990 Volume 6 Issue 4 Pages
579-583
Published: August 10, 1990
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The complexation reactions of copper(II) and lead(II) with phenylfluorone in aqueous micellar solutions of different surfactants were investigated. Maximum sensitization of the color reactions was obtained in the presence of benzyldimethyltetradecylammonium chloride (Zephiramine). The sensitized 1:2 copper- and lead-phenylfluorone chelates were formed within the pH ranges 8.8-9.8 and 8.8-9.5, with molar absorptivities of 9.3×10
4 and 6.2×10
4M
-1 cm
-1, respectively. Beer′s law was obeyed up to 0.42ppm of copper and 1.96ppm of lead at 562nm. The sensitivity indexes were 0.0007μg cm-2 (Cu) and 0.0033μg cm
-2 (Pb). The developed methods were successfully applied to determine copper and lead in some double-base propellants. Moreover, a two-step procedure was proposed to determine copper and lead mixtures, through the reaction of two increments of a mixture with phenylfluorone and Zephiramine at pH 9.0±0.1, in both the absence and presence of thiourea as a selective masking agent for copper.
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Akira OHKI, Masanobu YAMURA, Makoto TAKAGI, Shigeru MAEDA
1990 Volume 6 Issue 4 Pages
585-588
Published: August 10, 1990
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An ion selective electrode was prepared which exhibited selectivity for terephthalate over various interfering anions including phthalate under alkaline conditions; a dionium cation, decamethylenebis(trioctylphosphonium) (abbreviated as C
10BP), was used as the sensing material. Ion selective electrodes based on conventional monoonium cations such as "Capriquat" did not exhibit such selectivity. The butyl analogs of C
nBPs were examined as ion-pair reagents in ion-pair chromatography for phthalates. Under alkaline elution conditions, the base-line separation of three phthalate isomers (phthalate, isophthalate and terephthalate) was achieved. When monoonium reagents such as tetrabutyl-ammonium were used, the retentions of these isomers considerably decreased, compared to the case of dionium reagents, and the separation could not be attained. The superiority of the dionium cations in both the sensing and separation systems was discussed.
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Keiko OHSAWA, Katsumi UCHIYAMA, Yoshihiro YOSHIMURA, Asayo TAKASUKA, K ...
1990 Volume 6 Issue 4 Pages
589-592
Published: August 10, 1990
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Photoacoustic spectroscopy by the rear-surface detection method was proposed for an aluminum-foil thin-layer chromatography (TLC) plate. The aluminum-foil TLC plate was attached to a photoacoustic cell (15mm id.; chamber volume,
ca. 0.7ml). The surface of the TLC plate was illuminated by a chopped laser-beam (30Hz; beam size 0.75 mmφ). The photoacoustic signal of the aluminum-foil TLC plate was detected by an electret condenser microphone located at the other end of the cell. The photoacoustic signal of the sample on the TLC plate was seen as a signal superposed on a background signal of the aluminum foil. Background signals caused by light absorption at the surface of aluminum foils were measured for foils 17, 40, 110μm thick. A 40μm-thick aluminum foil showed the largest signal intensity. The amount of cobalt-PAN (1-(2-pyridylazo)-2-naphthol) chelate on a TLC plate was determined by the proposed method. A linear relationship between the amount of cobalt-PAN and the signal intensity was obtained within the range 20-300ng. The detection limit of cobalt-PAN was about 5ng. The reproducibility of measurements for 150ng cobalt-PAN on seven different TLC plates was 0.246 (RSD).
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Tadashi IWACHIDO, Takahiko IKEDA, Michio ZENKI
1990 Volume 6 Issue 4 Pages
593-597
Published: August 10, 1990
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The separation of NH
4+ from Na
+, K
+, Mg
2+ and Ca
2+ on silica gel columns was investigated using natural water samples and lithium oxalate as a retention modifier. The pore size of silica gels was found to be the most important factor affecting the retention of the cations. When a 0.0025mol dm
-3 lithium oxalate solution of pH 7 was used as the mobile phase these cations could be completely separated on a short silica-gel column (Develosil 30-3, 35mm×4.0 mm i.d.) within about 20min. NH
4+ contents in river (0.01-0.27ppm) and rain (1-1.8ppm) water samples were determined successfully.
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Shunske IDE, Makoto TAKAGI
1990 Volume 6 Issue 4 Pages
599-603
Published: August 10, 1990
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N-Phenyl-
N′-(2-butylthiophenyl)thiourea (PBT, HL) was synthesized by the reaction of 2-butylthioaniline with phenylisothiocyanate and was studied for extracting Cu(II), Zn(II), Co(II), Cd(II), Ni(II), Hg(II) and Pd(II) from aqueous solution. Pd(II), Hg(II) and Cu(II) were readily extracted into chlorobenzene at low pH. Though the extraction of Co(II) and Zn(II) from an acidic solution was not complete, extraction from an alkaline aqueous solution
containing potassium oxalate was quantitative. The composition of the complexes, Cu(II)-PBT and Cd(II)-PBT, formed in the organic phase, was found to be ML
2 by studying the pH dependence and the metal-PBT mole ratio dependence of metal extraction. The synergistic effect of 4-benzylpyridine and trioctylphosphine oxide in the metal extraction was small. PBT is suited for separating Cu(II) from a mixture of conventional metal ions other than Pd(II)
and Hg(II).
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Takashi MASADOME, Toshihiko IMATO, Nobuhiko ISHIBASHI
1990 Volume 6 Issue 4 Pages
605-606
Published: 1990
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Yoshikazu FUJITA, Itsuo MORI, Minako TOYODA
1990 Volume 6 Issue 4 Pages
607-608
Published: 1990
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Masataka HIRAIDE, Koichiro NAMBA, Hiroshi KAWAGUCHI
1990 Volume 6 Issue 4 Pages
609-610
Published: 1990
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Mitsuhiko TAGA, Shunitz TANAKA, Masami FUKUSHIMA
1990 Volume 6 Issue 4 Pages
611-612
Published: 1990
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Satomi ISHIMARU, Rokuro KURODA
1990 Volume 6 Issue 4 Pages
613-615
Published: August 10, 1990
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O. N. OBREZKOV, V. I. SLYAMIN, O. A. SHPIGUN
1990 Volume 6 Issue 4 Pages
617-618
Published: August 10, 1990
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Hideo SAISHO, Yasuhiko FUJIMURA
1990 Volume 6 Issue 4 Pages
619-621
Published: August 10, 1990
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Takunori KATO, Seiji NAKAMURA, Masatoshi MORITA
1990 Volume 6 Issue 4 Pages
623-626
Published: August 10, 1990
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Mitsuko OSHIMA, Shoji MOTOMIZU, Zou JUN
1990 Volume 6 Issue 4 Pages
627-628
Published: August 10, 1990
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Akinori JYO, Takashi KOHNO, Yuichi TERAZONO, Shigeaki KAWANO
1990 Volume 6 Issue 4 Pages
629-630
Published: August 10, 1990
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