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Volume 52, Issue 10
Displaying 1-18 of 18 articles from this issue
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Research Papers
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Hitoshi NAKAMURA, Keiji TAMURA, Hideshi ISHII, Masanori OWARI, Chuhei ...Article type: Research Papers
2003 Volume 52 Issue 10 Pages 859-863
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSIn order to elucidate the dependence of X-ray photoelectron diffraction (XPED) method on the X-ray source, we investigated XPED patterns from a h-BN/Ni(111) surface by using both Cr-Lα (572.8 eV) and Al-Kα (1486.6 eV). As the first step Ni3p photoelectron diffraction patterns were measured and calculated from a substrate Ni(111) by using both sources. Forward scattering peaks and Kikuchi-like bands were clearly observed in both experimental and theoretical patterns excited by Al-Kα. On the contrary, these features of Cr-Lα excited XPED patterns were more diffuse. This suggests that the usage of a lower energy X-ray source improves XPED structural analysis on ultrathin films composed of light elements.
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Ryuji TSUKAMOTO, Fumiyo KUSUArticle type: Research Papers
2003 Volume 52 Issue 10 Pages 865-871
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSIon-transfer volutammetry at a nitrobenzene/water interface was performed to study the ion-transfer reaction and the adsorption of histamine and anti-histamine drugs, such as dl-chlorpheniramine, clemastine, diphenhydramine, cyproheptadine, meclizine, promethazine, ketotifen, and terfenadine. Ion-transfer volutammograms showed that all anti-histamine drugs gave an anodic wave at a potential less positive than that of histamine. Electrocapillary curves showed that the anti-histamine drugs were adsorbed on the interface with great facility. We assessed the effects of the ionization of these drugs on the ion-transfer reaction and adsorption by ion-transfer volutammograms and electrocapillary curves, respectively. Based on these results, the half-wave potentials for the drugs at pH 4 were plotted against the calculated log KD values obtained by using PALLSA (CompuDrug International). The half-wave potentials had a strong correlation with the calculated log KD values. We conclude that the half-wave potentials determined by the present method would be a more reliable parameter of hydrophobicity for neutral and ionic forms of drugs when dealing with structure-activity relationships of drugs compared to experimental log P values obtained by the conventional methods.
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Masashi ITO, Masayuki ITAGAKI, Kunihiro WATANABEArticle type: Research Papers
2003 Volume 52 Issue 10 Pages 873-879
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThe determination of cadmium in river water was investigated by a flow-injection analysis. In general, it is difficult to determine cadmium in an eluate by uv-vis spectrophotometry, because the eluate includes high concentrations of acid, alkali or complex agents. Therefore, a concentration method was investigated by electrolytic deposition, which does not require an eluant. Dual electrolytic cells were used in this flow system. One of them was for removing copper ion and other ions which interfere with the determination of cadmium. The other cell was used for concentrating cadmium in river water. After cadmium was deposited on platinum electrode for 20 min at −0.8 V vs. SSE, it was eluted for 2 min at 1.5 V from the electrode. The cadmium obtained from the electrode was determined with tetraphenyl-porphinetetrasulfonic acid(TPPS) by spectrophotometry at 434 nm. 2,2'-Bipyridine was added into the sample solution as a catalyst for a Cd-TPPS reaction. The calibration curve was linear at over the range of 0 to 10 ppb. The determination limit of cadmium was 0.45 ppb. The RSD of 10 ppb Cd was 2.1% (n = 5). The proposed method was applied to the determination of river water, including a standard sample.
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Hiroki SAITOH, Keiji GAMOHArticle type: Research Papers
2003 Volume 52 Issue 10 Pages 923-929
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSIn chromatographic analysis, a suitable derivatization of the functional groups has sometimes been used to enhance the sensitivity and selectivity for detection. Transforming low molecular organic acids to the corresponding 2-nitrophenylhydrazide derivatives has been more extensively used as a suitable derivatization method for liquid chromatographic UV-VIS detection. In the present study, liquid chromatography/mass spectrometric (LC-MS) detection with electro spray ionization was successfully applied to the analysis of low-molecular organic acids, glycolic, acetic, lactic, 2-hydroxy-n-butyric, propionic and n-butyric acid as their 2-nitrophenylhydrazide derivatives. Of a range of analytical conditions that were tested, the optimum results were obtained by using reversed-phase liquid chromatography and a mixture of methanol/water or methanol/ammonium formate. The positive- and negative-ion spectra of 2-nitrophenylhydrazides of the organic acids showed molecular-related ions, [M + H]+ and [M−H]−, whose ions were the most abundant, respectively. The effects of the chromatographic and ionization parameters, mobile phase, concentration of ammonium formate, pH and cone voltage on the sensitivity and linearity were examined. Linear plots of the peak area versus the concentration were obtained for MS detection over the range of 0.05∼10 μM for propionic acid and 0.1∼10 μM for lactic acid. Full-scan mass spectra were readily obtained from 34 nM of n-butyric acid derivative, while a limit of detection of 1.4 nM (signal-to-noise ratio 3) was attained in the selected-ion monitoring mode. These results showed that 2-nitrophenylhydrazide of low molecular organic acids contributes to the enhancement of the LC-MS detection compared with their UV-VIS detection.
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Technical Papers
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Kunikazu IDE, Yoshisuke NAKAMURA, Shin-ichi HASEGAWA, Hitoshi YAMAGUCH ...Article type: Technical Papers
2003 Volume 52 Issue 10 Pages 931-937
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThe determination of trace amounts of refractory metal elements (Ti, V, Zr, Nb, Mo and Ta) in high-purity iron by inductively coupled plasma mass spectrometry (ICP-MS) was examined. We examined a separating technique involving trace amounts of refractory metal elements from a high-purity iron matrix using the cupferron coprecipitation separation method and the measurement conditions of ICP-MS. Using the established analysis method, after 150 cm3 of hydrochloric acid (1 + 4) was added to 1 g of high-purity iron sample, they were decomposed on a 453 K hot plate. After the sample solutions were cooled at room temperature, an ascorbic acid solution and cupferron solutions were added to 10 cm3 portions, and then filtered. The paper filter and sediment were then added to 10 cm3 of nitric acid and 10 cm3 of perchloric acid, and dried through evaporation. After 150 cm3 of hydrochloric acid (1 + 4) was added to salt, it was dissolved; this operation was then repeated again. After 2 cm3 of nitric acid was added to this salt and it was dissolved, it was dried through evaporation. After the process of evaporation to dryness was performed 3 times, nitric acid (1 + 100) was added to the salt and dissolved. The sample solution was measured by ICP-MS. The concentration of the iron matrix in sample solution was decreased to about 200 μg cm−3, and it didn’t change. The background signal at mass 90 was decreased by nitric acid-treatment process, which enabled this difficult experiment to be carried out. The recovery rates of 6 added elements were 99% for Ti, 95% for V, 98% for Zr, 98% for Nb, 96% for Mo and 96% for Ta, respectively. The detection limits were 0.08 ng cm−3 for Ti, 0.009 ng cm−3 for V, 0.01 ng cm−3 for Zr, 0.008 ng cm−3 for Nb, 0.01 ng cm−3 for Mo and 0.004 ng cm−3 for Ta, respectively.
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Notes
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Satoshi HORIKIRI, Norio TESHIMA, Yurie SARUKI, Harumitsu NISHIKAWA, Ta ...Article type: Notes
2003 Volume 52 Issue 10 Pages 881-885
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThree photocatalysts were newly synthesized. The materials consisted of Al2O3 or SiC and anatase-type TiO2. The characteristics of the materials were analyzed by X-ray spectroscopy and TEM. Also, the photocatalytic activity upon the decomposition of methylene blue was investigated by measuring the decomposition rate of methylene blue with the UV(λ 369 nm) irradiation time. In addition, the derivatives of methylene blue produced after 2 and 4 hours of irradiation were analyzed by HPLC and MS. As a result, azur A and azur B were observed.
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Takuji KIYOHARA, Katsuro ANAZAWA, Hayao SAKAMOTO, Takashi TOMIYASUArticle type: Notes
2003 Volume 52 Issue 10 Pages 887-890
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThe adsorption of mercury(II) from aqueous solutions on green tea leaves, coffee beans and activated carbons has been studied comparatively. The adsorption capacity of those adsorbents was little affected by pH and EDTA. The coffee beans and the activated carbons adsorption capacity were highly affected by chloride ion, whilst the green tea leaves were less affected. The adsorption data obtained from equilibrium experiments were well-fitted to Freundlich isotherms.
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Hisako MURAKAMI, Hironori KURATA, Mikio KUZUYAArticle type: Notes
2003 Volume 52 Issue 10 Pages 891-897
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSA laser pyrolysis gas chromatograph (LPGC) system has been developed, which allowed for the direct analysis of solid samples. The LPGC system consists of a Q-switched Nd:YAG laser (pulse energy, 0∼230 mJ; repetition rate, 1∼15 Hz) as a fragmentation source, a gas chromatograph, a sample chamber, and a data-acquisition/processing system. A commercial tube-furnace type pyrolyzer was used as the sample chamber, and the sample was placed in a quartz tube. The LPGC system was applied to the analysis of a polystyrene sample, and its analytical performance were investigated. The chromatographs obtained from polystyrene showed the characteristic component peaks of ethylene, benzene, toluene, and styrene monomer. The relative standard deviations of the peak intensity, the FWHM, and the retention time were in the ranges of 5.3∼22%, 3.1∼16%, and 0.06∼1.1%, depending on the components, respectively. The effects of the laser energy and laser focusing on the chromatograms were investigated. The results showed that moderate energy and defocusing of the laser radiation brought about an increase in the signal intensity.
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Maiko NAKATA, Yoshiyuki MURATA, Mikiro TADA, Yasuaki SHIMOISHIArticle type: Notes
2003 Volume 52 Issue 10 Pages 899-902
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSA simple spectrophotometric method for the determination of polyoxyethylene nonionic surfactants, such as TritonX-100 with 1-(p-phenylphenacyl)-4-(4-aminonaphthylazo)-pyridinium bromide(PPAP), was developed. PPAP was synthesized by quarternizing 4-(4-aminonaphthylazo)-pyridine with p-phenylphenacyl bromide. Because PPAP was easily associated with nonionic surfactants to produce a blue ion associate in aqueous solution, the concentration of nonionic surfactants were determined by measuring the absorbance of ion associates at 612 nm. The apparent molar absorptivity of the TritonX-100 ion associate was 1.0×103 dm3 mol−1 cm−1 at 612 nm. The calibration graph for TritonX-100 was linear over the range from 6.0×10−5 to 8.0×10−4 M, and the relative standard deviation for 5.6×10−4 M of TritonX-100 was 2.0%. The proposed method was applied to the determination of nonionic surfactants in commercial domestic detergents.
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Chikako SAKAMOTO, Yuji OKADA, Hideko KANAZAWA, Akihiko KIKUCHI, Teruo ...Article type: Notes
2003 Volume 52 Issue 10 Pages 903-906
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSWe have developed a new method of chromatography, temperature-responsive chromatography, using packing materials modified with poly(N-isopropylacrylamide) (PNIPAAm). The temperature-responsive polymer, PNIPAAm, shows a reversible and sharp phase transition in an aqueous solution. The PNIPAAm-modified stationary phase alters the properties of the surface from hydrophilic to hydrophobic in response to temperature changes at the phase-transition temperature. In this study, we examined the separation of five catechins (epigallocatechin, epicatechin, catechin, epigallocatechin gallate and epicatechin gallate) using a PNIPAAm-modified column without changing the composition of the mobile phase. In this method, interactions between catechins and the stationary phases were controlled by the temperature. The retention times of all catechins were retarded, because the interaction increased at elevated temperature. We achieved the separation of catechins using only an aqueous solution as a mobile phase by temperature-responsive chromatography.
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Jun IWATA, Yuji SONETA, Kazuo MIYAMURAArticle type: Notes
2003 Volume 52 Issue 10 Pages 907-910
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSSignificant solvatochromism has been observed in the UV-Vis spectra of an alkylquinolinium salt of [Ni(dmit)2]. In particular, a large blue shift was observed when chloroform was used as the solvent. From a UV-Vis spectral analysis, it was concluded that the [Ni(dmit)2] anion forms adducts with cations, and that the change in the electronic state induced by the formation of adducts was responsible for the solvatochromism. In the course of our study, it was found that the oxidation of the complex by oxygen in air was strongly accelerated by the presence of methanol. An investigation of the reaction kinetics of this reaction revealed that the reaction rate is proportional to the methanol concentration.
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Yuji SUZUKIArticle type: Notes
2003 Volume 52 Issue 10 Pages 939-944
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThe reaction between four pH indicators with a large pKa value and human serum albumin and its application to the determination of the serum albumin concentration were studied. In the reaction of Bromothymol Blue (BTB), Phenol Red, Cresol Red and Thymol Blue with serum albumin, although a change in the color shade did not occur, the absorbance of the reaction mixture decreased. Since this absorbance decrease was largest in the reaction of BTB(the molar absorbance decrease at pH 7.4 was 7.59×104 l mol−1 cm−1), which was sufficiently sensitive to measure the serum albumin concentration, the BTB color reagent at pH 7.4 was applied to its determination. The measurement values by the BTB method correlated with those by the dye-binding method using the Bromocresol Green method(r = 0.965, y = 1.21x−4.25, n = 90) and with those by a method using Bromocresol Purple(r = 0.953, y = 1.04x + 3.56, n = 90). The mean value of the BTB method (41.8 g/l) was higher than those of the Bromocresol Green method (38.1 g/l) and the Bromocresol Purple method(36.6 g/l). Since the reaction of BTB was carried out at pH 7.4, where serum protein does not precipitate, the addition of a detergent for preventing the precipitation of serum protein is not required. Therefore, the use of this color reagent contributes to decreasing water pollution by the detergent and acid used in the conventional methods.
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Technical Letters
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Shin-ichiro NAGASHIMA, Yoshiko YANO, Toshihiko TAKURAArticle type: Technical Letters
2003 Volume 52 Issue 10 Pages 911-915
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSThis research aimed to verify the restoration of a water vein in Hachioji-Minamino City. The developer of the new town had made an attempt to link some separated water veins with artificial strata of gravel. An aqueous solution of Sr2+ was injected into a probable upstream point (B12-3) of a vein, and every 2 weeks after that the Sr2+ levels in water samples from four probable downstream points were analyzed. About 40 days after at one (S-16) of the four points, an extraordinary increase in the Sr2 concentration was observed. At the same time, the concentration levels of Ca2+, Mg2+ and Na+ and the electric conductivity suddenly increased. These show that the two points, B12-3 and S-16, are linked to each other and that Sr2+ is a suitable stable indicator for analyzing underground water veins. The concentration levels of the above-mentioned cations were also observed every month for underground water samples from several sampling points where the water vein was supposed to be independent of the present tracer investigation. The quartile deviations for the observed values were shown mostly within 5% for a very long time, a max. of 34 months.
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Kohki KOBAYASHI, Isoshi NUKATSUKA, Fumihide MIYASHITA, Kunio OHZEKIArticle type: Technical Letters
2003 Volume 52 Issue 10 Pages 917-921
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSA Teflon tube of 1.5 m in length and 0.5 mm in inner diameter was used to extract Cu(II) after complexation with oxine-5-sulfonate in in-tube solid-phase microextraction/electrothermal atomic absorption spectrometry. Prior to extraction, Zephiramine was loaded onto the inner wall of the Teflon tube, the sample solution was adjusted to pH 5.6, and then placed in a ca. 1 or 2-ml sample vessel. Subsequently, extraction was carried out in such a way that the sample solution was sucked into the Teflon tube and discharged to the original vessel with a syringe pump included in the auto-sampler. The suction and discharge actions were repeated several times to attain equilibrium and to improve the amounts of copper extracted. The percent extraction after equilibrium was 79% for a 200-μl sample solution. The effect of the sample volume was examined in the range of 0.5∼2.0 ml. The suction and discharge actions were repeated 7 times with 295 μl of the sample solution, which was the inner volume of the Teflon tube. The results showed that the amounts of copper extracted increased with increasing volume of the sample solution up to 1.0 ml, although the percent extraction decreased with the sample volume. When copper extracted from 1.0 ml of a 0.3 ng ml−1 sample solution was eluted by 30 μl of methyl acetate (10% methanol), a reasonable repeatability with a relative standard deviation of 2.8% (n = 3) was obtained. A linaer calibration graph was also obtained in the range of 0∼0.5 ng ml−1 Cu(II). The detection limit(3σ) was 0.01 ng ml−1. The slope of the calibration graph was 14.2-times greater than that obtained by injecting 20 μl of standard solutions into the atomization furnace.
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Hideaki KITAMI, Tetsuo WATANABE, Takio KITAHARA, Yoshimi ISHIHARA, Jir ...Article type: Technical Letters
2003 Volume 52 Issue 10 Pages 945-949
Published: 2003
Released on J-STAGE: January 30, 2004
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Tsutomu MIURA, Kazushige NAKAYAMA, Hiroshi KIRITAArticle type: Technical Letters
2003 Volume 52 Issue 10 Pages 951-954
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESS210Pb, 210Po, 232Th, 230Th, 228Th, 238U, 235U and 234U in Geological Survey of Japan manganese nodule standard rock sample JMn-1 were determined by radioactive isotope dilution/alpha ray spectrometry. Extraction chromatography, anion exchange chromatography and solvent extraction were applied to the analysis. The analytical results of Th and U in JMn-1 were in agreement with the literature values determined by ICP-MS (inductively coupled plasma mass spectrometry) or INAA (instrumental neutron activation analysis). It was found that the concentration of 210Pb in JMn-1 was higher than that in other certified reference materials for environmental radioactivity. JMn-1 proved to be useful for quality control sample in the analysis of environmental radioactivity.
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Yûetsu DANZAKI, Kazuaki WAGATSUMAArticle type: Technical Letters
2003 Volume 52 Issue 10 Pages 955-958
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSProper dissolution methods for various V alloys were examined for elemental determination in inductively coupled plasma-optical emission spectrometry (ICP-OES). Several kinds of V alloys were developed for various purposes. Among them, alloys co-containing Ti, Nb, and Ta are being employed as structural materials. Hydrolytic reactions of these elements occur in aqueous solution easily; therefore, an agent should be added to prevent their hydrolysis. Hydrogen peroxide is an effective agent against hydrolysis. However, when H2O2 is added to solutions containing V, it accelerates the decomposition of H2O2 and then O2 gas generates, which leads to poor precision of the analytical results in ICP-OES. Therefore, a proper dissolution method for each V alloy should be developed without usage of H2O2. V-Cr, V-Fe and V-Mo alloys were dissolved in a HNO3-HCl solution. V-Zr, Ti-Al-V and Ni-Ti-V alloys were finished as a H2SO4 solution after dissolving in HNO3-HF and fuming with H2SO4. A V-Nb alloy was added to a H2SO4-tartaric acid solution after dissolving in HNO3-HF and fuming with H2SO4. A Nb-Al-V alloy was dissolved in NO3-HF at room temperature. Nb-Cr-V alloys were finished as a H2SO4-HF solution after dissolving in HNO3-HCl-HF, followed by fuming with H2SO4 and adding HF.
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Short Communications
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Tamiyuki IGARI, Tatsuro NAKAGAMA, Katsumi UCHIYAMA, Toshiyuki HOBOArticle type: Rapid Communications
2003 Volume 52 Issue 10 Pages 959-962
Published: 2003
Released on J-STAGE: January 30, 2004
JOURNAL FREE ACCESSIn micro liquid chromatography, a method for the reversible control of the elution order of enantiomers by light irradiation was developed. Two photo-responsive chiral stationary phases (CSP(1) and CSP(2)) with an azobenzene moiety were prepared using D- and L-valine, respectively. The prepared stationary phases were continuously packed into a UV-permeable polymer-coated fused-silica capillary tubing (100 μm, i.d.) with 20 cm of length, respectively, and used as a micro column. When 3,5-dinitrobenzoyl-D,L-leucine isopropyl ester and 3,5-dinitrobenzoyl-D,L- alanine methyl ester were used as test samples, the samples were eluted in the order D-form and L-form, after UV light was irradiated to only the part of CSP(1) in the column. Continuously, when UV light was irradiated to the part of CSP(2) after visible light was irradiated to the CSP(1), the elution order became L-form and D-form. It could be seen that a reversible change in the retention order was caused by the reduction of the enantio-selectivity of the stationary phase by UV light irradiation.
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