Analytical Sciences
Online ISSN : 1348-2246
Print ISSN : 0910-6340
ISSN-L : 0910-6340
Volume 23 , Issue 12
Showing 1-19 articles out of 19 articles from the selected issue
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Original Papers
  • Eiji FUJIMORI, Tatsuya KOBAYASHI, Masanori AOKI, Masahiro SAKAGUCHI, T ...
    2007 Volume 23 Issue 12 Pages 1359-1366
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    PM10 samples were collected at an urban site of Nagoya City during September, 2003, to August, 2004, and annual variations of the concentrations of the elements in PM10 samples were examined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The annual concentration variations of ca. 30 elements in ambient air were in the range from sub-ng m-3 to several µg m-3. From an evaluation by the enrichment factors of the elements, elements such as Al, Ca, Fe, Mg, Ti, Mn, Ba, Sr, Ce, La, Nd, Co, Cs, and Pr, in PM10 samples were found to have originated mostly from natural sources, while the elements such as S, Zn, Pb, Cu, Ni, Sb, Sn, Cd, Bi, W, Tl, and In originated from anthropogenic emission sources. Furthermore, in seasonal variations of the elemental concentrations of PM10 samples in ambient air, the elements originated mostly from natural sources provided significantly high concentrations in spring during the “Kosa” period (the dust season from March to May). On the other hand, the elements mainly from anthropogenic emission sources provided relatively higher concentrations in autumn and winter, which may be explained by the fact that the urban atmospheric structure is stabilized by the temperature-inversion layer formed over the city in those seasons. In addition, all of the elements provided significantly low concentrations in the summer, due to the dilution effect of the oceanic winds as well as due to the convection of air mass up to the high levels.
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  • Michihiro AIMOTO, Hiroyuki KONDO, Akihiro ONO
    2007 Volume 23 Issue 12 Pages 1367-1371
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    A flow-injection procedure combining electrolytic sample decomposition and inductively coupled plasma atomic emission spectrometry (ICP-AES) is proposed in order to rapidly determine the content of silicon in high-silicon electrical steel. This system is characterized by sample decomposition through electrolysis directly coupled to ICP-AES. A steel sample is dissolved by electrolysis using a 6 mol L-1 HCl solution as an electrolyte with a flow rate of 5 mL min-1; the electrolyte containing a dissolved sample is subsequently introduced into ICP-AES via a nebulizer. The effects of the electrolysis current and the temperature on the decomposition of the sample were studied. Samples were electrolyzed under the condition of a 1.5 A constant current, at room temperature (25°C) to avoid the hydrolysis of silicon to precipitate. Comparing the analytical results of steel samples obtained by this analytical system with those obtained by the gravimetric method, determined values agreed well quantitatively. The RSD of silicon at approximately 3% was 0.3% (n = 6).
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  • Xiaoli WANG, Bo SHEN, Huichun ZHAO, Linpei JIN
    2007 Volume 23 Issue 12 Pages 1373-1376
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    This paper reports the determination of ulifloxacin (UFX) by terbium-sensitized fluorescence using a second-order scattering method. UFX and Tb(III) ion form a fluorescence complex in aqueous solution, and its maximum excitation and emission wavelengths are located at 273 and 545 nm, respectively. In optimum conditions, the relative intensity at 545 nm has a linear relationship to the concentration of UFX in the range of 2.0 × 10-8 - 1.0 × 10-5 mol L-1 and the detection limit is 3.9 × 10-9 mol L-1. The proposed method was applied to the determination of UFX in spiked human serum and urine satisfactorily. The luminescence property of UFX is also discussed by comparing with norfloxacin (NFLX) and ofloxacin (OFLX).
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  • Jin-Fang NIE, Hai-Long WU, A-Lin XIA, Shao-Hua ZHU, Ying-Chao BIAN, Sh ...
    2007 Volume 23 Issue 12 Pages 1377-1382
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    This paper proposes a new and effective approach for the quantitative analysis of sulpiride, a significant antipsychotic drug, in human urine samples by the incorporation of excitation-emission matrix (EEM) fluorescence and second-order calibration methodologies based on the alternating fitting residue (AFR) and self-weighted alternating trilinear decomposition (SWATLD) algorithms. With the application of a second-order advantage, the proposed strategy could be utilized for a direct concentration determination of sulpiride with a simple pretreatment step, even in the presence of serious natural fluorescent interferences. The average recoveries of sulpiride in complex urine samples by using AFR and SWATLD with an estimated component number of three were 101.2 ± 2.1 and 94.4 ± 0.7%, respectively. Moreover, the accuracy of the two algorithms was also evaluated through elliptical joint confidence region (EJCR) tests as well as the figures of merit, such as sensitivity (SEN), selectivity (SEL) and limit of detection (LOD). The experimental results demonstrated that both algorithms, as promising quantitative alternatives, have been satisfactorily applied to the determination of sulpiride in human urine, but the performance of AFR was slightly better than that of SWATLD.
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  • Patrícia Los WEINERT, João Roberto FERNANDES, Leonardo P ...
    2007 Volume 23 Issue 12 Pages 1383-1389
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    A sensitive flow-injection (FI) procedure with spectrophotometric detection in a micellar medium is proposed for the determination of novalgin. The method is based on the instantaneous formation of a red-orange product (λmax = 510 nm) after the reaction between novalgin and p-dimethylaminocinnamaldehyde (p-DAC) in a dilute acid medium. The sensitivity of this reaction was increased by a factor of 5.6 in the presence of sodium dodecyl sulfate (SDS). Experimental design methodologies were used to optimize the chemical and FI variables. The calibration curve was linear in the range of 1.45 × 10-6 to 2.90 × 10-5 mol L-1 with an excellent correlation coefficient (r = 0.9999). The detection limit was 1.31 × 10-7 mol L-1 (n = 20, RSD = 2.0%). No interferences were observed from the common excipients. The results obtained by the proposed method were favorably compared with those given by the iodometric reference method at 95% confidence level.
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  • Pawel K. ZARZYCKI, Hatsuichi OHTA, Filip B. HARASIMIUK, Kiyokatsu JINN ...
    2007 Volume 23 Issue 12 Pages 1391-1396
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Thermostated micro planar chromatography was applied for systematic separation studies of C60 and C70 fullerenes using n-alkanes as mobile phases on TLC and HPTLC plates coated with polyamide, silica gel, aluminum oxide as well as two types of octadecylsilica (C18) sorbents. Retention data were collected at constant temperature at 20°C (±0.05°C) using an unsaturated chamber mode with an eluent, such as n-pentane, n-hexane and n-heptane. The separation results under both saturated and unsaturated chamber modes for selected mobile/stationary phases were also examined, and several parameters, including separation factor (α) and resolution (RS), were compared with data obtained with high-performance liquid chromatography conditions. Interestingly, C60/C70 fullerenes separation performed on HPTLC plates with a developing distance of 45 mm was better for those observed on a 25 cm length analytical HPLC column under similar conditions to that on carbon coverage of the stationary phase, n-hexane as the mobile phase and separation temperature (RS = 1.84 and 1.68 for HPTLC, and HPLC, respectively). Moreover the advantage of the planar chromatographic separation of fullerenes studied is a short elution time of less than 6 min. Furthermore, the reported separation protocol shows a capability for the evaluation of fullerenes quantity in commercial samples.
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  • Yoko KAWATA, Yuko ADACHI, Saori HAGA, Junko FUKUTOMI, Hirohiko IMAI, A ...
    2007 Volume 23 Issue 12 Pages 1397-1402
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Temperature and pressure dependences of the 129Xe NMR chemical shift and the signal intensity have been investigated using ZSM-5 as an adsorbent under routine conditions without using any high-pressure or especially high-temperature facilities. The use of a rigorously shielded system and a calibration sample for the signal intensity was found to be valuable to obtain reliable data about the chemical shift and the signal intensity. The 129Xe NMR data obtained between 0.05 and 1.5 atm and from 24 to 80°C were analyzed based on the Dubinin-Radushkevich equation as well as the Langmuir type equation. In both analyses, chemical shift data succeeded only partially in providing the profile of adsorption, such as energetic aspects, surface area, saturated amount of Xe adsorption and specific parameters of 129Xe chemical shift. It was shown that the reliable total analysis was achieved when the chemical shift data were used together with the intensity data. Such an analysis of the chemical shift data, aided by the intensity data, will be useful in performing nano-material analysis on 129Xe NMR without invoking the traditional methodology of gravimetric or volumetric adsorption experiments.
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  • Mohammad M. HASSANIEN, Ibrahim M. KENAWY, Adel M. EL-MENSHAWY, Ahmed A ...
    2007 Volume 23 Issue 12 Pages 1403-1408
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Ga(III), In(III) and Tl(III) ions in the presence of different sulfate salts have been successfully separated using 1-(3,4-dihydroxybenzaldehyde)-2-acetylpyridiniumchloride hydrazone (DAPCH) loaded on Duolite C20 in batch and column modes. The obtained modified resin as well as the metal complexes was characterized by elemental analysis and infrared spectra. The extraction isotherms were determined at different pH values. Ga(III) and In(III) are sorbed from aqueous solution at pH 2.5 - 3.0 while Tl(III) is sorbed at 2.0. The stripping of the adsorbed ions can be carried out using different concentrations of HCl as eluent. The saturation sorption capacities of Ga(III), In(III) and Tl(III) were 0.82, 0.96 and 0.44 mmol g-1, where the preconcentration factors are 150, 150 and 100, respectively. The metal(III):Duolite C20-DAPCH ratio was 1:2 for Tl(III) and 1:1 for In(III) and Ga(III). The loaded resin can be regenerated for at least 50 cycles. The utility of the modified resin was tested in aqueous samples and the results show an RSD value of < 5% reflecting their accuracy and reproducibility.
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  • Jianding QIU, Pengfei HU, Ruping LIANG
    2007 Volume 23 Issue 12 Pages 1409-1414
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Poly(dimethylsiloxane) microfluidic channels alternately modified by poly(diallyldimethylammonium chloride) and poly(sodium 4-styrenesulfonate) were successfully used to separate uric acid and ascorbic acid. Results show that uric acid and ascorbic acid can be well separated and detected simultaneously in modified microchips coupled with in-channel electrochemical detection. Under the optimal conditions, the linear ranges of uric acid and ascorbic acid were both from 25 to 600 µM, with the correlation coefficients of 0.997 and 0.996, respectively. The detection limits were 8 µM for uric acid and 5 µM for ascorbic acid. Factors influencing separation and detection, including buffer solution, detection potential and separation voltage, were investigated and optimized. In addition, the dependences of the current response on sensitivity and reproducibility were studied, and the stability of the device was also evaluated in detail. This method was successfully used to determine uric acid and ascorbic acid in human urine.
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  • Masanori KANAZAWA, Shinobu SATO, Keiichi OHTSUKA, Shigeori TAKENAKA
    2007 Volume 23 Issue 12 Pages 1415-1419
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Messenger RNA (mRNA) poly(A)+RNA (from mouse kidney) was immobilized on a N-hydroxysuccinimide(NHS)-activated carboxylic acid modified electrode prepared by the treatment of a gold electrode with 3,3′-dithiodipropionic acid, followed by NHS and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC). An electrochemical measurement using this mRNA electrode was carried out in an electrolyte containing ferrocenylnaphthalene diimide (1), and showed an electrochemical signal based on 1 concentrated on immobilized mRNA. After treating this electrode with water containing varied amounts of ribonuclease A (RNase A), the current peak based on 1 decreased with increasing in the amount of RNase A with a linear correlation in the range of 0.2 - 10 pg of RNase A.
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  • Yanping CUI, Changzhu YANG, Wei ZENG, Munetaka OYAMA, Wenhong PU, Jing ...
    2007 Volume 23 Issue 12 Pages 1421-1425
    Published: 2007
    Released: December 11, 2007
    JOURNALS FREE ACCESS
    Seed-mediated growth of gold nanoparticles on glassy carbon (GC) surfaces was developed. The field emission scanning electron microscopy (FE-SEM) and electrochemical characterization confirmed the effective attachment of gold nanoparticles on GC surface with such a wet-chemical method. The as-prepared gold nanoparticles attached glassy carbon electrode (Au/GCE) presented excellent catalytic ability toward the oxidation of nitrite. Compared with bare GCE and planar gold electrode, the Au/GCE obviously decreased the overpotential of nitrite oxidation and improved the peak current. The catalytic current was found to be linearly proportional to the nitrite concentration in the range of 1 × 10-5 - 5 × 10-3 M, with a detection limit of 2.4 × 10-6 M. The Au/GCE was successfully applied to the electrochemical determination of nitrite in a real wastewater sample, showing excellent stability and anti-interference ability.
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