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2006 Vol. 26, No. 04
Published: 2006-04-26

 
       光谱学与光谱分析
593 Measurement of Time-Dependent Spectra Excited by Pulse Laser Using Multi-Fiber Delayer and Optical Multi-Channel Analyzer
CHENG Juan1, 2,HE Ying-hong1,ZUO Hao-yi1,YANG Jing-guo1*
A new method and technology for measuring time-dependent spectra excited by pulse laser was reported in the present paper, in which a multi-fiber delayer combined with a two dimensional CCD array detector was employed for collecting and processing the spectra. The multi-fiber delayer consists of five fibers with a length difference of 1-2 m (relative delay time 5-10 ns), and the optical multi channel analyzer is PARC OMA-4. The time-dependent spectra, i. e. the spectra of R6G dye laser, the SRS spectra of acetone, and the plasma emission spectra of metal Mo excited by a double frequency YAG pulse laser with a time resolution of 5 ns were obtained.
2006 Vol. 26 (04): 593-596 [Abstract] ( 1751 ) PDF (1040 KB)  ( 443 )
597 Tm3+ Concentration Dependence of Upconversion Intensity of YLiF4:Er3+,Tm3+,Yb3+
ZHAO Su-ling,HOU Yan-bing,XU Zheng,PEI Xiao-jiang
A series of YLiF4:Er3+,Tm3+,Yb3+ samples were synthesized by hydrothermal method. The concentrations of Er3+ and Yb3+ were 1 mol% and 1.5 mol%, respectively. Tm3+ concentration changed from 2 to 8 mol%. The absorption of Er3+,Tm3+ and Yb3+ were observed, and the absorption of Tm3+ increased along with the increase in Tm3+ concentration. The color of upconversion luminescence of YLiF4:Er3+,Tm3+ and Yb3+ excited by 980 nm was white when Tm3+ concentration was low. The blue light resulted from the transition of 1G43H6 of Tm3+,the green light from the transition of 4S3/2 (2H11/2)→4I15/2 of Er3+,and the red light from the transitions 1G43F4 of Tm3+ and 4F9/24I15/2 of Er3+. All the upconversion intensities decreased when Tm3+ concentration increased, but the relative intensity decrease was different due to the interaction between Er3+ and Tm3+.
2006 Vol. 26 (04): 597-600 [Abstract] ( 1135 ) PDF (918 KB)  ( 476 )
601 The Influence of Holes Buffer Layer Doped with Different One-Dimensional Nanomaterials on the Performance of Polymer Light-Emitting Diodes
QIAN Lei, TENG Feng, XU Zheng, QUAN Shan-yu, LIU De-ang, WANG Yuan-min, WANG Yong-sheng, XU Xu-rong*
The effect of holes buffer layer PEDOT doped with one-dimensional nanomaterials on the performance of polymer light-emitting diodes was investigated. The photoluminescence efficiency of double layer sample PEDOT/MEH-PPV was enhanced by doping one-dimensional nanomaterials (TiO2 nanotube and ZnO nanorod) into PEDOT layer. Stronger interaction of one-dimensional nanomaterials and PEDOT suppressed the creation of defect states which can quench radiative recombination of excitons. The electroluminescence efficiency of device was improved by 2 and 2.5 folds by doping TiO2 nanotubes and ZnO nanorods into holes buffer layer PEDOT respectively.
2006 Vol. 26 (04): 601-604 [Abstract] ( 1093 ) PDF (900 KB)  ( 531 )
605 Preparation and Luminescence of Nanocrystalline ZrO2∶Pr3+ and ZrO2∶Pr3+,Sm3+
LIU Jin-xia1,2,Lü Shu-chen1*,LI Xiu-ming1
The nanocrystalline ZrO2∶Pr3+and ZrO2∶Pr3+,Sm3+ powders with room temperature sharp characteristic emissions were prepared by coprecipitation method. Luminescence properties of nanocrystalline ZrO2∶Pr3+ with different sintering temperatures and doping concentrations were studied. The energy transfer between the nanocrystalline ZrO2 host and the dopants was observed. The different Pr3+ concentration dependence of emission intensities of levels 3P0 and 1D2 was discussed. The dependence on Pr3+ concentration in nanocrystalline ZrO2∶Pr3+,Sm3+ of the emission intensity of 4G5/26H7/2 transitions of Sm3+ ions and the energy transfer between Pr3+ and Sm3+ ions were investigated and discussed.
2006 Vol. 26 (04): 605-609 [Abstract] ( 126 ) PDF (933 KB)  ( 448 )
610 Studies on the Properties of Frequency Upconversion of Yb3+/Er3+ Codoped Absolute Oxides
DING Qing-lei,LIU Zheng-wei, XIA Yan-qin, LEI Jun-hui
Samples of Er3+/Yb3+codoped 3CaO-Al2O3-3SiO2 compounds were prepared, and the properties of frequency upconversion of the samples under the excitation of 980 nm diode laser were studied. Green and red emissions centered at 523, 547 and 656 nm, corresponding to the transitions 2H11/24I15/2,4S3/24I15/2, and 4F9/24I15/2,respectively, were observed. The dependence of the upconversion fluorescence intensity on the pumping power, and the phonon energy of each sample were observed, and the mechanism of frequency upconversion based on these two items was discussed.
2006 Vol. 26 (04): 610-613 [Abstract] ( 1138 ) PDF (884 KB)  ( 478 )
614 Identification of Epimedium Koreanum Nakai by Fourier Transfer Infrared Spectroscopy
JIN Xiang-jun1, 2,LI Xiao-ping2,LIU Zhi-qiang3*,ZHAO Bing1*
The herbal plant Epimedium Koreanum Nakai is a native herb growing in the Changbai Mountain region, Jilin province of China, and is used as a tonic, anti-rheumatic and aphrodisiacin traditional Chinese medicine. The analytical method existing for the identification of Epimedium Koreanum Nakai is time-consuming, and can not be used for fast, in situ and nondestructive analysis. Fourier transform infrared spectroscopy was used to identify wilding and planting Epimedium Koreanum Nakai. The spectra of 18 samples were analyzed. They show some differences in the intensity and the shape of absorption peaks in the range of 1 800-1 200 cm-1. The absorption intensity of the spectra changed regularly with the producing area. So FTIR spectra could be used for the identification of Epimedium koreanum Nakai.
2006 Vol. 26 (04): 614-616 [Abstract] ( 1059 ) PDF (837 KB)  ( 506 )
617 Application of Near-Infrared Spectra in the Determination of Water Soluble Chloride Ion in Plant Samples
WU Rong-hui, SHAO Xue-guang*
A new method was proposed to extract relevant information from near-infrared(NIR) spectra for multivariate calibration of water soluble chloride ion in complex plant samples. The method is a combination of discrete wavelet transform (DWT) and least squares support vector regression (LSSVR). After data compression and background removal in NIR spectra by DWT, the LSSVR approach was used to build NIR spectra regression models on the retained wavelet coefficients. Compared with partial least square regression (PLSR) and LSSVR, the proposed method is superior both in calculation speed and prediction accuracy.
2006 Vol. 26 (04): 617-619 [Abstract] ( 1712 ) PDF (852 KB)  ( 678 )
620 Multi-Component Analysis of FTIR Spectra of Non-Linear System Using Polynomial Partial Least Squares Method
ZHANG Lin1,ZHANG Li-ming1,LI Yan1*,WANG Xiao-fei1,2,HU Lan-ping1,3,WANG Jun-de1
A non-linear algorithm, polynomial PLS was applied to the simultaneous analysis of OP-FTIR spectra of a five-component system whose FTIR spectra were seriously overlapped. The results were compared with the one obtained from PLS. PPLS yielded good performance, especially for the prediction of benzene and chloroform. RMSEP(root mean squared error of prediction) of benzene and chloroform in PPLS model were 0.043 and 0.087 and the corresponding values in PLS were 0.402 and 0.842, respectively. Meanwhile, variance was accounted by PPLS with fewer latent variables, which indicates the simplicity and robustness of the model. The successful application of PPLS to non-linear system was meaningful for the use of remote sensing FTIR in air monitoring.
2006 Vol. 26 (04): 620-623 [Abstract] ( 1638 ) PDF (894 KB)  ( 489 )
624 Study of FTIR Spectra and Thermal Analysis of Polyurethane
JIANG Zhi1 , YUAN Kai-jun1,LI Shu-fen1*,CHOW W K2
The thermal behavior of polyester-polyurethane and polyether-polyurethane in air atmosphere was investigated by using FTIR analysis in the temperature range from 20 to 400 ℃. The thermal degradation behaviors of polyester-polyurethane and polyether-polyurethane in different atmospheres were investigated by using thermogravimetry analysis(TG) in the temperature range from 20 to 700 ℃. The FTIR results together with the TG investigations showed that polyester-polyurethane has two degradation steps in air, but polyether-polyurethane has only one degradation step. The thermal analysis results also showed that the onset degradation temperature of polyether-polyurethane is lower than that of polyester-polyurethane, suggesting that the thermal stability of polyester-polyurethane is higher than polyether-polyurethane, and the onset degradation temperature of polyurethane in air is lower than that in nitrogen, suggesting that the presence of oxygen affects significantly the break of the polymeric chains.
2006 Vol. 26 (04): 624-628 [Abstract] ( 574 ) PDF (916 KB)  ( 658 )
629 Determination of Geographical Origins of Chinese Medical Herbs by NIR and Pattern Recognition
LIU Shu-hua1,ZHANG Xue-gong1,ZHOU Qun2,SUN Su-qin2*
Geographical origin of medical herbs is an important factor of the quality of many traditional Chinese herbal medicines. The objective of the present study is to investigate whether NIR spectroscopy coupled with pattern recognition techniques could effectively discriminate geographical origins of medical herbs. Nearest neighbor method (NNM) and a SVM-based multiclass classifier were employed to discriminate 269 Angelicae Dahuricae Radix (ADR) samples from 4 provinces and 380 Salviae Miltiorrhizae Radix (SMR) samples from 6 provinces in China. The multiclass classifier achieves leave-one-out cross-validation accuracy of 99% for (ADR) and 95% (SMR). This classification scheme can be a highly accurate approach to the rapid and nondestructive discrimination of medical herbs of different origins.
2006 Vol. 26 (04): 629-632 [Abstract] ( 1110 ) PDF (852 KB)  ( 537 )
633 Simultaneous Determination of Glucose, Fructose and Sucrose in Aqueous Solution by Short-Wavelength Near Infrared Spectroscopy
RAO Zhen-hong1,LI Min-zan2,JI Hai-yan2*
The calibration model for simultaneous determination of glucose, fructose and sucrose in aqueous solution was built by partial least squares and short-wavelength near infrared spectroscopy(800-1 100 nm). Twenty five samples in calibration set and 9 samples in prediction set were designed by orthogonal design. Building models from calibration set and validation for prediction set obtained the better results. For concentrations of glucose, fructose and sucrose in the ranges of 12.23-61.14 mg·mL-1,12.50-62.50 mg·mL-1 and 12.09-60.44 mg·mL-1,the relative standard deviations in the calibration set are 1.43%, 4.51% and 1.59% respectively, and the relative standard deviations in the prediction set are 3.40%, 3.73% and 2.80% respectively. The advantages of the method are simple and effective, with low cost for the simultaneous determination of multi-component system. It may be applied in practice easily.
2006 Vol. 26 (04): 633-635 [Abstract] ( 423 ) PDF (836 KB)  ( 539 )
636 Analysis and Discrimination of Infant Powdered Milk via FTIR Spectroscopy
DENG Yue-e1,2,ZHOU Qun2,SUN Su-qin2*
Six kinds of infant powdered milk were identified by Fourier transform infrared spectra (FTIR) and their corresponding second derivative infrared spectra. The main nutritious components such as lipid (1 747, 2 854 and 2 926 cm-1), protein (1 658 and 1 540 cm-1), and carbohydrate(1 200-900 cm-1) of had distinct fingerprint characteristics of FTIR spectra. Maltodextrin, sucrose and lactose also had obvious spectral characteristics, which changed with different added content. For the samples from the same factory but with different sorts, there was some dissimilarity in the relative intensities of infrared absorption peaks due to the difference in fat, protein and carbohydrate. For the samples of the same sort but from different factories, there are certain similarities in the IR spectra, however, the second derivative infrared spectra present different fingerprint characteristics. This analytical method is fast and direct for evaluating the quality of infant powdered milk.
2006 Vol. 26 (04): 636-639 [Abstract] ( 1195 ) PDF (958 KB)  ( 548 )
640 The Determination of Beef Tenderness Using Near-Infrared Spectroscopy
ZHAO Jie-wen1,ZHAI Jian-mei1*,LIU Mu-hua2,CAI Jian-rong1
The prediction of beef tenderness was studied using near-infrared spectroscopy. The absorption spectra of beef samples were collected between 4 000 and 10 000 cm-1,the maximum shear force of these samples was obtained using the Warner-Bratzler attachment, and subjective judgment for the tenderness grade of beef was studied. Beef samples with the maximum shear force less than 6 kg were regarded as tender, and their tenderness grade was defined as the value of 1. Those with the maximum shear force greater than 9 kg were regarded as tough, and their tenderness grade was defined as the value of 3. And those with the maximum shear force between 6 and 9 kg were regarded as medium, and their tenderness grade was defined as the value of 2. The study shows that the absorption value of tougher beef is generally higher than that of tender beef. Multiple linear regression was used to build the model between the absorption value and tenderness grade. The results give the correlation coefficient r is 0.806. The accuracy of the model for predicting tenderness grade of beef was 84.21% for a validation set including 19 samples. This result indicates that NIR spectroscopy is capable of predicting tenderness grade of beef.
2006 Vol. 26 (04): 640-642 [Abstract] ( 1677 ) PDF (836 KB)  ( 721 )
643 Determination of Polyether Silicon Oil by IR
WANG Wen-bo, SHEN Shu-chang, AN Hong
In the present paper, with polyoxyethylene(10) octylphenol ether and hydrogenous silicon oil used as raw materials, and stannous octoate used as catalyst, polyoxyethylene(10) octylphenolether-hydrogenous silicon oil polymer was synthesized in toluene solvent. Residual hydrogenous silicon oil in the polymer was determined by IR. There is a characteristic peak at 2 167 cm-1 for Si—H bond in hydrogenous silicon oil. Using span-60 as internal standard, depending Lambert-Beer law and some calculation process, the linear relation between the absorbance ratio(y) and the mass ratio(x) of sample was obtained. The linear regression equation is y=2.07 2x+0.296 3 with a correlation coefficient(r2) of 0.998 9. The experimental results of the precisions and recoveries are satisfactory. An IR method to determine the content of hydrogenous silicon oil in polyether was established. The method is very necessary for confirming the reaction extent and controlling product quality and adjusting polyether silicon oil characters. The best process parameter was chosen in experiments. The polyether has good charactesistic for extracting alcohols and benzene homologues with bright future of application.
2006 Vol. 26 (04): 643-645 [Abstract] ( 1710 ) PDF (881 KB)  ( 474 )
646 Study of Poly (3,4-Ethylene Dioxythiophene):Poly (Styrene Sulfonate) by In-Situ Resonance Raman Spectroscopy
LIN Hai-bo, XU Xiao-xuan*,WANG Bin, WU Bin-lin, XU Jia-lin, YU Gang, ZHANG Cun-zhou
Poly (3,4-ethylene dioxythiophene)(PEDOT): Poly (styrene sulfonate)(PSS) has attracted a lot of interest for application in organic electronics due to good stability and high electronic conductivity in its doped state. Indeed, thin layers of PEDOT: PSS was regularly used in light emitting diodes (PLEDs) as hole injection and transportation layer. Here, Doping and dedoping states of PEDOT:PSS were studied by absorbance spectra and Raman spectra. A new absorption band centered at 620 nm was observed on dedoped PEDOT:PSS. Consistently, Raman signals of dedoped PEDOT:PSS are resonantly intensified since the Raman excitation wavelength (633 nm) is set in the enhanced absorption band. So it gives a sensitive way to study the doping and dedoping states of PEDOT:PSS. Furthermore, for the encapsulated polymer light-emitting diodes, Raman spectroscopy is a powerful way to study the polymer layers inside the devices.
2006 Vol. 26 (04): 646-648 [Abstract] ( 1408 ) PDF (907 KB)  ( 472 )
649 Surface Enhanced Raman Scattering Spectra of Carbozole and Azobenzene Disperse Red Polymer
WANG Xiu-ru1,SUN Run-guang1*,WANG Chang-shun2, 3,MO Yu-jun3
Surface enhanced resonance Raman scattering(SERRS) was employed to study the molecule alignment of carbozole and azobenzene disperse red polymer on the surface of rough silver thin film. According to the selection rule of optical transitions and experiment results, it was found that the surface geometry of carbozole and azobenzene disperse red polymer was: this was physical adsorption between the carbazole group, which is from the monomer of carbazole and nitro-group which is from the monomer of azobenzene on the surface of rough silver film, and there is almost no interaction between the principal chain and the substrate because of the distance. This geometrical configuration of CAP on the surface of the substrate was proposed to damage the stabilities and efficiency of azobenzene derivatives based optical storage devices.
2006 Vol. 26 (04): 649-652 [Abstract] ( 631 ) PDF (936 KB)  ( 439 )
653 Comparison of Influences of Different Intervals of Ultraviolet Irradiation on Calf Thymus Studied by Raman Spectroscopy
TANG Yu-long, GUO Zhou-yi*
Raman spectroscopy was used to investigate the effect of different intervals of ultraviolet (UV) to calf thymus DNA in aqueous solution. At the same time, the different influences of these three UV parts were compared, and a complete damaging mechanism of UV to DNA was obtained. The results showed that UVC damages DNA in a complete way, while UVA and UVB damage DNA in a selective way, and the speed effect of UVB on DNA was faster than that of UVA. UVC seemed to be less valid in reducing the B conformation of DNA than UVA and UVB. Among all the groups of DNA, the pyrimidine bases and the deoxyribose experienced the most severe damages. Moreover, with UVA or UVB irradiation for 3 h, the photoreactivation of DNA occured. The experimental results partly supported the formation of several types of dimeric lesions between adjacent pyrimidine bases, most notably cyclobutane pyrimidine dimers (CPD), 6-4 photoproducts (6-4PP) and the Dewar valence isomers.
2006 Vol. 26 (04): 653-657 [Abstract] ( 1500 ) PDF (966 KB)  ( 450 )
658 Study on the Vibrational Spectra of Two Nitrobenzoyl Substituted Guanidines
WU Wen-jing1,LU Run-hua1, 2,SHI Yan-ping1*
p-nitrobenzoyl tetramethylguanidine and m-nitrobenzoyl tetramethylguanidine were synthesized by simple methods. Their main IR and Raman spectra were measured, quantum-calculated, and assigned by the program Gaussian 98. The results showed that the theoretical spectra were in good agreement with the experimental ones, and can be used as a guidance in the interpretation of experimental spectra.
2006 Vol. 26 (04): 658-662 [Abstract] ( 1690 ) PDF (880 KB)  ( 481 )
663 Synthesis, Characterization and Fluorescent Property of Ternary Complexes of Rare-Earth, Cinnamic Acid and 2,2’-Bipyridine
YANG Yong-li, DENG Yu-heng*,NIE Feng-mei,WANG Shao-ting, ZONG Rui-fa
The ternary rare-earth complexes were synthesized using cinnamic acid (L), 2,2’-bipyridine (bipy) and rare-earth (RE= Tb, Eu, Gd, Nd) in ethanol solution. Their compositions were confirmed to be REL3·bipy by the element analysis, infrared and ultraviolet absorption spectra, and DTA-TGA, respectively. The spectral properties of complexes and the fluorescent property of EuL3·bipy were discussed. The fluorescence intensity of EuL3 is 4.5 times stronger than that of EuL3·bipy·H2O.
2006 Vol. 26 (04): 663-665 [Abstract] ( 1184 ) PDF (836 KB)  ( 559 )
666 Synthesis and Characterization of Chitosan-Imine-Palladacycle
LIU Pu, LI San-hua, WANG Xiang-yu, LI Li-min
Chitosan was grafted with salicylaldehyde to obtain Schiff base. The Schiff base reacted with Li2PdCl4 in methanol to synthesize chitosan-imine-palladacycle. The structure of chitosan, schiffbase and chitosan-imine-palladacycle was characterized by IR, XRD, DTA-TG, fluorescence and XPS. According to the results of analysis, the structure of Schiff base and chitosan-imine-palladacycle can be inferred.
2006 Vol. 26 (04): 666-669 [Abstract] ( 1617 ) PDF (871 KB)  ( 462 )
670 Synthesis,Characterization and Relaxivity of Dimeric DTPA-Gadonium(Ⅲ) Complexes with Long Chain Alkyl Esters of L-Lysine
YU Kai-chao1,2,LI Liu-yi1,WAN Fu-xian1,ZHOU Jin-lan1*, DING Shang-wu2,YE Chao-hui3
To look for new MRI (magnetic resonance imaging) contrast agents with higher relaxivity as well as liver-selecsivity, four novel ester-amino ligands were synthesized by bis-acylation of octadecanyl, hexadecanyl, tetradecanyl and dedecanyl L-lysine with diethylenetriaminepentaacetic acid mono-anhydride (DTPA-MA), respectively. The corresponding dimeric Gd(Ⅲ) complexes were gained by the reaction of these ligands with GdCl3·6H2O. All ligands and complexes were characterized by FTIR, 1H NMR and elemental analysis. The longitudinal relaxation time (T1) was measured, and relevant longitudinal relaxivity (R1) of these neatral binuclear Gd(Ⅲ) complexes is: 6.48, 6.02, 5.76 and 5.68 L·mmol-1·s-1,respectively, and all are higher than that of Gd-DTPA (4.98 L·mmol-1·s-1)(300 MHz).
2006 Vol. 26 (04): 670-673 [Abstract] ( 1863 ) PDF (868 KB)  ( 447 )
674 Fluorescence Spectroscopy Study of Humen Serum Albumin Quenched by Rifampicin Capsules
CHEN Xiao-bo, KANG Dong-guo, LI Song, ZHAO Cheng-yi, CHEN Xiao-shan, DING Huan-ping
It is obvious that the albumin is a kind of important large biophysical molecular. The albumin is the main component of plasma within cell. It is also the matter basis of life phenomenon. The fluorescence spectroscopy of humen serum albumin(HSA) and the interaction of HSA and the rifampicin capsules (lfp) were studied. When the rifampicin capsules(lfp) was added into HSA solution gradually, an interesting new phenomenon emerged in emission spectrum. The combination constant of rifampicin capsules(lfp) is about K=5.149×104 L·mol-1,and the dissociation constant is about Kd=19.42×10-6 mol·L-1. The quenching process of rifampicin capsules(lfp)-HSA is not dynamic quenching, which resulted from the molecular diffusion and collision. That is the static quenching process resulting from the chemical component between molecules. The energy transfer efficiency between rifampicin capsules(lfp) and HSA is E=0.42. According to these calculation results, the combination position between the binding site of rifampicin capsules(lfp) and the tryptophane of HSA is about R=2.567 nm. The critical distance, when transfer efficiency equals 50%, is about R0=2.433 nm.
2006 Vol. 26 (04): 674-677 [Abstract] ( 128 ) PDF (870 KB)  ( 597 )
678 Studies on Luminescence Properties of Seven Ternary Complexes of Terbium with 1,10-Phenanthroline and Benzoic Acid and Its Derivatives
GAO Zhi-hua, WANG Shu-ping, LIU Cui-ge, MA Rui-xia, WANG Rui-fen*
Seven ternary complexes of Tb(Ⅲ) were synthesized with benzoic acid(BA), o-, m-, p-methylbenzoic acid (o-MBA, m-MBA, p-MBA), and o-, m-, p-methoxybenzoic acid(o-MOBA, m-MOBA, p-MOBA) as the first ligand, and 1,10-phenanthroline(phen) as the second ligand. The content of C, H and N were measured by using a Flash-EA model 1112 elemental analyzer. Excitation and luminescence spectra of the title solid complexes were recorded by using a Hitachi F-4500 fluorescence spectrophotometer at room temperature. The effects of different varieties and different positions of replacing benzoic acid as the first ligand on fluorescence properties of the ternary complexes of terbium were discussed. The results indicated that the intensity of 5D47F6(489 nm) and 5D47F5(545 nm) of substituting benzoic acid complexes was stronger than benzoic acid. Three ternary complexes of Tb(Ⅲ) with o-, m-, p-methylbenzoic acid showed emission intensity in the consecution: Tb(o-MBA)3phen<Tb(m-MBA)3phen·H2O<Tb(p-MBA)3phen. However,for the complexes with o-, m-, p-methoxybenzoic acid as the first ligand: Tb(o-MOBA)3phen·H2O>Tb(m-MOBA)3phen·H2O>Tb(p-MOBA)3phen.
2006 Vol. 26 (04): 678-681 [Abstract] ( 315 ) PDF (981 KB)  ( 533 )
682 Aggregation Number Determination of Gemini Anionic Surfactant Micelle by Intrinsic Fluorescence Quenching
LIU Jin-yan, ZHAO Jian-xi*,YANG Lian-zhi
The p-phendioxyl base in the spacer of gemini surfactant C11pPHCNa emits fluorescence under exciting. When the gemini concentration is over 0.45 mmol·L-1,the topological structure of the excitation spectra yields various changes resulting in them being significantly different from the corresponding absorption spectra. As the aromatic base in the spacer of C11pPHCNa obviously quenches the fluorescence of pyrene that is as additional probe, it is hardly to determine the average micelle aggregation number by the usual method of quenching pyrene. In the present paper, using the property of methylviologen (MV2+) effectively quenching the fluorescence of C11pPHCNa, the authors established the method to determine the average aggregation number N of C11pPHCNa micelle. For individual C11pPHCNa micelle, N was determined to be 20.6 at c=2 mmol·L-1,while the average aggregation number of C11pPHCNa/C12-2-E1-C12·2Br mixed micelle in the aqueous solution with a total concentration of 2 mmol·L-1 and C11pPHCNa of mole fraction 0.3 in the bulk was obtained to be 11.8.
2006 Vol. 26 (04): 682-685 [Abstract] ( 448 ) PDF (895 KB)  ( 449 )
686 Study on the Spectra of Cal-Red-Cu(Ⅱ) Complex with Bovine Serum Albumin and Its Analytical Application
CHEN Dan-dan1,ZHANG Tao1,REN Li-ping1*,SHI Deng-rong2,YU Jin-lian2
The Resonance light scattering (RLS) spectra, fluorescence spectra, and absorption spectra of Cal-Red-Cu(Ⅱ) metal complex with bovine serum albumin(BSA) were studied. As the Cal-Red-Cu(Ⅱ)-BSA complex formed, the RLS spectra and fluorescence spectra enhanced, but the absorption spectra weakened and the absorption peak at 594 nm disappeared. At pH 5.65-5.75,the enhanced RLS of Cal-Red-Cu(Ⅱ) metal complex with BSA system was characterized by the maximum scattering at 317 nm, and the RLS intensity is proportional to the concentration of BSA. Under optimal conditions, the linear range of calibration was 0.75-10 μg·mL-1,the linear regression equation was I=150.88+201.48c(BSA,μg·mL-1)with r=0.997 3, and the limit of detection was 5.62×10-2 μg·mL-1. The method was applied to the determination of BSA in synthetic samples satisfactorily. A mechanism of electrostatic force was suggested for the interaction between BSA and Cal-Red-Cu(Ⅱ).
2006 Vol. 26 (04): 686-689 [Abstract] ( 1772 ) PDF (923 KB)  ( 443 )
690 Study on the Preparation and Spectral Characteristics of Nano-NiO
WANG Yan-ping, ZHU Jun-wu, ZHANG Li-li, YANG Xu-jie, LU Lu-de*,WANG Xin
The NiO nanoparticles with the size of 9-30 nm were prepared by solid state method using nickel acetate and sodium hydroxide as the raw materials, and Tween 80 as the dispersant. The structure, morphology, size, and infrared and UV-Vis spectra were characterized by XRD, TEM, FTIR and UV-Vis, respectively. The XRD and TEM revealed that the products are spherical with cubic structure. The infrared absorption band of the NiO nanoparticles (437 cm-1) red-shifts 47 cm-1 compared with that of bulk NiO(484 cm-1). The UV-Vis optical absorption is related with the size of the particles. The bulk NiO has no absorption in the UV-Vis region, while the 10 nm NiO nanoparticles have stronger absorption observed at the wavelength about 309 nm, and the direct band gap energy is estimated to be about 4.2 eV which is obviously blue-shifted 0.55 eV compared to that of bulk NiO (3.65 eV). The surface effect and quantum size effect of the NiO nanoparticles indicated that the products will have potential application in the optical and electrical areas.
2006 Vol. 26 (04): 690-693 [Abstract] ( 1578 ) PDF (933 KB)  ( 486 )
694 Study on Structure and Spectral Properties of Carbon Nanotubes Doped Silica Gel Glass Composites
ZHENG Chan, ZHAN Hong-bing*,CHEN Wen-zhe
Carbon nanotubes(CNTs) were successfully introduced into silica gel glass matrix by physically doped sol-gel technique. The characterization of structure and spectra of the CNTs doped composites were carried out by X-ray diffraction, transmission electronic microscope, UV-Vis spectra,IR spectra and Raman spectra. The results show that CNTs are homogeneously dispersed in the silica gel glass matrix and the sol-gel processing does not appear to affect the intrinsic structure of CNTs. The introduction of CNTs doesn’t make any noteworthy changes in the UV-Vis and IR spectra of silica gel glass matrix.
2006 Vol. 26 (04): 694-697 [Abstract] ( 1151 ) PDF (1082 KB)  ( 419 )
698 Study on Spectroscopic Properties of Rare Earth Complexes with Poly(N-Vinylacetamide)
SUN Yong1,CHEN Ming-qing1,LU Tian-hong2, 3,Mitsuru Akashi4, HUANG Xiao-hua1, 2*
Terbium-lanthanum(or gadolinium)-poly(N-vinylacetamide) complexes were synthesized and characterized by UV-Vis absorption spectroscopy, FTIR, XPS and fluorescence spectroscopy. The results of UV-Vis, FTIR and XPS suggested that terbium and lanthanum(or gadolinium) ions were bonded to amide group of PNVA polymer. Fluorescence experiment indicated that the characteristic emission intensity of terbium ion was greatly increased and possibly sensitized by lanthanum ion(or gadolinium). Moreover, the wavelengths of terbium characteristic emissions were changed slightly.Also the characteristic emission intensity of terbium ion doped with lanthanum ion was better than that with gadolinium ion.
2006 Vol. 26 (04): 698-702 [Abstract] ( 1717 ) PDF (910 KB)  ( 434 )
703 Spectral Study of Two Compounds of Molybdate Salt with β-[Mo8O26] Anion
CHEN Yi-ping1,ZHANG Han-hui1, 2*,HUANG Chang-cang1,SUN Rui-qing1,YANG Qi-yu1
Two compounds of organic molybdate-alkali salt: [H(4,4’-bipy)]2[K2Mo8O26](Ⅰ) and H3[Na Mo8O26](4,4’-bipy)5(H2O)4(Ⅱ), with β-[Mo8O26]4- anion, were synthesized. The relationship between their properties and structures was studied by using FTIR, Raman, NIR-Vis and fluorescence etc. They possess isolating β-[Mo8O26]4- anion, whose terminal O atoms combine with alkali. The FTIR and Raman spectra showed that the vibrational frequencies of the group are related to the structure of the materials. In UV-Vis spectra of compound (Ⅰ) and (Ⅱ), there is a characteristic wide peak at 280-300 nm. The fluorescence spectra of compound (Ⅰ) and (Ⅱ) were studied, which showed that the wide emission peak is from 450 to 650 nm and excited by 350 nm for compound (Ⅰ), and the emission peak is from 400 to 550 nm and excited by 325 nm for compound (Ⅱ). For compound (Ⅰ), the intensity of emission becomes stronger with decreasing of temperature, and so does the fluorescence lifetime.
2006 Vol. 26 (04): 703-706 [Abstract] ( 2010 ) PDF (905 KB)  ( 439 )
707 Study on Interaction of Adriamycin and DNA with a Resonance Light Scattering Technique and Its DNA Analytical Application
FENG Shuo1,2,LI Zheng-ping1*,ZHANG Shu-hong2,FANG Zheng2
The interaction of adriamycin (ADM) and DNA results in strongly enhanced resonance light scattering (RLS) spectra characterized by two peaks at 322 and 564 nm, respectively. The interaction of ADM and DNA was investigated by using absorption spectra, fluorescence spectra, and RLS spectra. The results indicate that RLS spectra have the highest sensitivity. It was found that the enhanced RLS intensity at 322 nm was proportional to the concentration of DNA in the range of 0-8.0 μg·mL-1. An RLS method for the determination of DNA was accordingly described. The limit of determination was 36.8 and 40.1 ng·mL-1 for calf thymus DNA and fish sperm DNA, respectively. The proposed method has a high sensitivity and good selectivity due to the specificity of the interaction of ADM and DNA.
2006 Vol. 26 (04): 707-710 [Abstract] ( 1925 ) PDF (890 KB)  ( 471 )
711 Study on the Interaction Mechanism of Targeting Molecules Carboxymethyl Polysaccharide with DNA
ZHANG Hai-rong1, 2,GUO Si-yuan2,LI Lin2,CAI Miao-yan2
The interaction of chitosan(CTS),carboxymethyl chitosans(CMCTS), and carboxymethyl cellulose(CMCL) with DNA was investigated through ethidium bromide(EB) as a sensitive fluorescence probe, and ultraviolet absorption spectra. The constant D can directly denote the degree of interaction of polysaccharide with DNA.The results indicated that the interraction sequence of biological polysaccharides with DNA is as follows: CTS>CMCTS>CMCL. The polysaccharides were mainly bound to DNA by intercalated binding, which resulted in fluorescence quenching effect of EB-DNA.
2006 Vol. 26 (04): 711-714 [Abstract] ( 1141 ) PDF (909 KB)  ( 401 )
715 Research on the Interaction of Aristolochic Acid and Bovine Serum Albumin
LIU Jia-qin1, 2,TIAN Jian-niao3,BIAN Qing-quan1,HU Zhi-de2
The interaction between aristolochic acid and bovine serum albumin(BSA) under physiological conditions was investigated by fluorescence quenching methods. The results indicate that there is a strong interaction between aristolochic acid and BSA, and the distances between the binding location and tryptophan residue is 2.8 nm. The binding location of aristolochic acid in BSA is in subdomain ⅢA. In addition, the effects of aristolochic acid on the protein second structure were studied using CD and FTIR techniques. The results of CD proved that the α-helix contents of BSA decreased from 43.5% to 36.7% after binding with aristolochic acid.
2006 Vol. 26 (04): 715-719 [Abstract] ( 1090 ) PDF (952 KB)  ( 405 )
720 Determination of Trace Elements in Cerebrospinal Fluid(CSF) of Patients Suffering Cerebrovascular Disease by Atomic Absorption Spectrometry
SUN Rui-xia1,SU Yong-xiang2,SUN Jian-hui1*
The contents of some trace elements such as zinc, copper, iron and cadmium in cerebrospinal fluid(CSF) of normal persons and the patients who suffered cerebral hemorrhage or infarction were determined directly by atomic absorption spectrometry. The method is simple and convenient with a recovery ratio by standard addition being 97.6% to 104.8%, and a relative standard deviation(RSD) is lower than 5%. The test showed that except for the content copper lower than normal, the patients suffering cerebrovascular disease have much higher contents of zinc, iron and cadmium. The result provides useful data for studying the relation between the contents of these trace elements and cerebrovascular disease, as well as diagnosing, treating and preventing this disease.
2006 Vol. 26 (04): 720-722 [Abstract] ( 1543 ) PDF (869 KB)  ( 522 )
723 Study on Measurement of Liquid Refractive Index by Analyzing SPR Spectrum Character
ZENG Jie, LIANG Da-kai, ZENG Zhen-wu, DU Yan
The principle of optic fiber surface plasmon resonance sensor is discussed in detail based on the electromagnetic theory and radial theory in the present paper. The relationship between SPR spectrum resonance wavelength and liquid refractive index is also analyzed. Through relative spectrum measurement technology, SPR spectrum curves, whose resonance wavelength increases with increasing liquid refractive index, were obtained for eight different kinds of chemical liquids. The measurement of concentration of mixed solution including ethanol and glycol was performed by analyzing the spectrum attribute. The experimental results show that the sensing system features simple structure and all light transmitted by fiber. It not only realizes rapid, accurate and real time measurement for target medium, but also can be used in some special situations and easily realize long distance measurement.
2006 Vol. 26 (04): 723-727 [Abstract] ( 1817 ) PDF (1021 KB)  ( 863 )
728 Fluorescence Analysis of Crude Oil Samples with Different Spectral Approaches
WANG Chun-yan, WANG Xin-shun, WANG Yan-hua, GAO Ju-wei, ZHENG Rong-er*
Fluorescence techniques based on emission spectrum, synchronous fluorescence spectrum(SFS), or three-dimensional (3D) fluorescence spectrum, have been widely used in medical, biological and chemical analyses. In the present paper, 25 crude oil samples from 15 different borefields in the concentration range from 10-4 g·L-1 to 10 g·L-1 have been investigated with different spectral approaches. It was shown that, compared with conventional emission spectrum based technique used in oil logging, the 3D fluorescence technique can provide much more information in the analysis of crude oil samples but at the price of time consuming. While the SFS spectrum of a crude oil sample, taken under the emission and excitation wavelength synchronous scan with Δλ=40 nm, can represent the main characteristic of the 3D spectrum provided, with even better spectral qualities. All the results suggest that SFS technique is a more suitable approach in crude oil sample analysis than the other two, and has a great potential to be developed as a new quantitative analysis method in petroleum logging.
2006 Vol. 26 (04): 728-732 [Abstract] ( 1201 ) PDF (1132 KB)  ( 469 )
733 The Spectral Properties of an Intense Lightning Return Stroke
YUAN Ping1, 2,QIE Xiu-shu2,Lü Shi-hua2,CHEN Guan-ying1,ZHANG Guang-shu2
The spectrum in the range of 400-600 nm from the first return stroke of an intense cloud-to-ground lightning flash was obtained by a slit-free spectrograph. Applying the atomic structure theory to the research work on lightning spectra, the wavelengths, oscillator strengths and excitation energies of upper levels were calculated for the transitions of related lightning spectrum. Multi-configuration Dirac-Fock method was employed in the calculation. From the results, re-identifications were carried out for the lines of 419.0 and 425.3 nm. It was found by spectral analysis combined with corresponding electrical information finds that the spectrum characteristic is closely related to the intensity of lightning discharge, as during an intense lightning return stroke the lines of OⅡ with high excitation energies are enhanced.
2006 Vol. 26 (04): 733-737 [Abstract] ( 1727 ) PDF (915 KB)  ( 433 )
738 MOA Spectral Analysis of Additive Element Contents in Lube Oil
WEI Hai-jun,YU Hong-liang,GUAN De-lin,SUN Pei-ting,WANG Hong-zhi
The determination of the additive contents of marine lubrication oil by using atomic emission spectrometry is described. A new measuring method is suggested in accordance with the working principle of MOA atomic emission spectral instrument. The additive element contents, if not within the precision limits of MOA atomic emission spectra, are to be measured by being diluted with a standard oil. Error analysis is conducted and the calibration curve method is used. The testing result indicates that the RSD of Ca, P and Zn is 1.6%, 4.8% and 4.6% respectively, and the error result of oil sample before and after diluting is 4.21%, 6.99% and 5.09% respectively.
2006 Vol. 26 (04): 738-740 [Abstract] ( 525 ) PDF (828 KB)  ( 594 )
741 Simultaneous Determination of Trace Platinum, Palladium and Rhodium in Environmental Dust Samples by ICP-MS after Open-Digestion
SHI Yan-zhi1,HE Run-juan2,WANG Juan2,ZHU Ruo-hua2*
A sensitive method for simultaneous determination of Pt, Pd and Rh in dust samples by ICP-MS after open-digestion was developed. The digestion method for the samples and conditions for measurement for ICP-MS were studied in detail. Aqua-regia was proved to be a better solvent for the digestion of dust samples. Under the optimum conditions, the limits of detection of Pt, Pd and Rh were 0.48, 4.22 and 0.42 ng·g-1,respectively. The proposed method was applied to the real sample analysis, and good recoveries were obtained. The recoveries of Pt, Pd and Rh were found to be between 87.6%-88%, 85.2%-87.8%, and 93%-95%, respectively.
2006 Vol. 26 (04): 741-746 [Abstract] ( 403 ) PDF (910 KB)  ( 526 )
747 A Study of the Reactions of H3O+,NO+ and O2 Ions with Nine Alkoxy Alcohols
Tianshu WANG
Following a selected ion flow tube mass spectrometry(SIFT-MS), analysis of the headspace of a commercial available nail polish remover pad in which γ-butyrolactone (GBL) and 2-butoxy-1-ethanol were found to be the major volatiles, a study of the reactions of H3O+,NO+ and O2 ions with nine alkoxy alcohols (R1—O—R2OH) was carried out using selected ion flow tube(SIFT) at a carrier gas (helium) pressure of 9.3×101 Pa. Experiments were also performed at various carrier gas pressures (4×101-1.1×102 Pa) for some reactions and under moist air condition. The number and distribution of the hydrates for the product ions were used to identify their structures and to investigate reaction mechanisms. The H3O+ reactions proceed via nascent ion-molecule complex (H3O+.M)*,then produce R1—O—R2OH.H+,(R1—O—R2)+,HOR2OH.H+ and R2O.H+ ions through various channels. Similarly, via a nascent complex (NO+.M)*, NO+.M,(M—H)+ and (M—ROH)+ ions were produced in the NO+ reactions. The collisions between the nascent complexes (H3O+.M)* and (NO+.M)* with a third body (He, N2 and O2 etc) have influence on the product ion distributions. The O2 reactions produce mainly dissociative product ions and it is uncertain whether they proceed via the nascent ion-molecule complex (O2.M)*. This study provides rate coefficients and product ions in the SIFT-MS database for the analysis of these compounds in normal and humid air samples. It will be further utilised into addiction and drug abuse, respiratory medicine and other research areas using SIFT-MS.
2006 Vol. 26 (04): 747-752 [Abstract] ( 246 ) PDF (900 KB)  ( 390 )
753 Surface and Interface Analysis of PTCDA/ITO Using X-Ray Photoelectron Spectroscopy (XPS)
OU Gu-ping1, 2,SONG Zhen3,GUI Wen-ming1,ZHANG Fu-jia1*
X-ray photoelectron spectroscopy (XPS) of surface and interface of PTCDA/ITO in PTCDA/p-Si organic-on-inorganic photoelectric detector was investigated. From C1s fine spectrum we found that the binding energy of C atoms in perylene rings was 284.6 eV; and the binding energy of C atoms in acid radical was 288.7 eV; moreover, some C atoms were oxidized by O atoms from ITO. The binding energy of O atoms in CO bonds and C—O—C bonds was 531.5 and 533.4 eV, respectively. At the interface, the peak of high binding energy in C1s spectrum disappeared, and the main peak shifted toward lower binding energy.
2006 Vol. 26 (04): 753-756 [Abstract] ( 1987 ) PDF (909 KB)  ( 771 )
757 XPS Investigation on the Modified Nano-Al2O3 by Surface Grafting
CHE Jian-fei, GONG Jie, YANG Xu-jie, LU Lu-de, WANG Xin
Steric hindrance layer can be established when the surfaces of nano-Al2O3 were grafted with polyacetal, which increased the dispersibility of the nano-particles as well as the compatibility between the particles and the resin matrix. Examination of X-ray photoelectron spectroscopy (XPS) demonstrated that the peak of Al(2p) on polyacetal grafted Al2O3 surfaces almost disappeared, while that of O(1s) increased. On the contrary, peak of C(1s) increased obviously. Results of fine scanning and deconvolution into multiple sub-peaks of C(1s) indicated that 61.92% of carbon on the surfaces of nano-Al2O3 was attributed to the grafting polyacetal. This shows that an effective modification layer formed on Al2O3 surfaces, and the grafting polyacetal was chemically bound with nano-Al2O3. Based on XPS and TG analysis, it is conjectured that the grafting polyacetal is mainly distributed on nano-Al2O3 surfaces.
2006 Vol. 26 (04): 757-760 [Abstract] ( 1582 ) PDF (1016 KB)  ( 574 )
761 Application and Research Progress of Composition Analysis of Urinary Calculi
DENG Sui-ping, CHEN De-zhi, OUYANG Jian-ming*
The analyses of compositions of urinary stones can provide significant reference to the treatment and prevention of recurrence of urolithiasis. In the present paper, the application and research progress of composition analyses of various urinary stones such as calcium oxalates, phosphates, uric acid, urates, cystine etc. by means of modern instruments are summarized. These techniques include Raman spectroscopy, thermogravimetry analysis/differential thermal analysis (TGA/DTA), nuclear magnetic resonance (NMR), high-performance liquid chromatography (HPLC), Fourier infrared (FTIR) spectroscopy, etc.
2006 Vol. 26 (04): 761-767 [Abstract] ( 1054 ) PDF (974 KB)  ( 563 )
768 The Oxidation Degradation of Great Green SF by Fenton Reagent
ZHENG Huai-li1,2,ZHANG Zhan-mei1,TANG Ming-fang3,YI Qian1,CHEN Chun-yan1,PENG Zhi-cong1
Photo-Fenton method, the combination of Fenton reagent with light, is an efficient method for waste water treatment. In the present paper, the degradation of great green SF using this method was studied. Great green SF is a kind of permanent and nondegradable dye. Through numerous experiments, the influences of various parameters including the UV absorption curve of great green dye SF, the concentration-absorbency curve of great green dye SF, dosage of Fe2+,dosage of H2O2,initial pH, different light sources, and cation-exchange resin on the degradation were researched intensively. The optimum condition for dye SF degradation was given. Under the experiment condition, the sun light can promote this reaction apparently. The reaction time can greatly be shortened too. After the cation-exchange resin was introduced into the Fenton system, the activation of H2O2 can be enhanced to a great extent. The dosage of H2O2 will be decreased. The degradation effect of the great green SF is better. Under optimal conditions, the overall color removal is more than 96.7% within 40 min; COD can be removed effectively at the same time.
2006 Vol. 26 (04): 768-771 [Abstract] ( 1144 ) PDF (856 KB)  ( 518 )
772 Application of Fractal Theory to Spectral Signal Recognition
XIONG Yu-hong, WEN Zhi-yu, ZHANG Liu-qiang, WEN Zhong-quan, LIANG Yu-qian
The fractal theory is a discipline that studies a kind of irregular and chaotic object with similarity of its part and whole. The fractal dimension is a basic index mark of irregularity and self-similarity in the fractal theory. The present paper takes the spectral signal according with Lambert-beer’ law as the object, introduces the basic theory of fractal geometry in brief, puts forward the method of fractal dimension as the feature of spectral signal recognition, makes use of reconstructing phase space to gain the fractal dimension of spectral signal, compares different values of the fractal dimension to recognize different spectral signal, and gives an example for explanation.
2006 Vol. 26 (04): 772-774 [Abstract] ( 1660 ) PDF (844 KB)  ( 560 )
775 A High Sensitivity Optical Multichannel Analyzer
SONG Yu, ZHOU Wen-yuan*,YE Qing, ZANG Wei-ping, TIAN Jian-guo
Noise sources of the CCD as the photoelectric detection device in an optical multichannel analyzer (OMA) were analyzed, and noise suppression methods were discussed. A high sensitivity OMA was developed successfully on the basis of the noise suppression techniques, and the 7th spectral lines of Balmer series of hydrogen and deuterium were resolved clearly by the OMA. Its sensitivity was enhanced by one order of magnitude, compared with those reported in the literatures. This OMA also showed high resolution, high precision and good reliability in the authors’ experiments.
2006 Vol. 26 (04): 775-778 [Abstract] ( 1073 ) PDF (882 KB)  ( 511 )
779 Design of a Portable UV-Vis Spectrophotometer
WAN Feng1,SUN Hong-wei2,FAN Shi-fu1
In the present paper, a method for how to design a portable UV-Vis spectrophotometer is introduced. The Hamamatsu multichannel detector S3904-1024Q and a flat field concave grating are employed to design a miniaturized dispersion system. In order to solve the contradiction between the spectral width and energy-utilizing ratio of the light source, a multi-band optical fiber is employed, one side of which is arranged to be rectangle as the entrance slit. The touch screen is employed as the input and output system of the spectrophotometer, and the miniaturized fiber-optic UV-Vis light source is employed as the light source. The research results and testing results of the prototype show that the new spectrophotometer based on the authors’ new method is of miniaturization in volume(190 mm×170 mm×100 mm), can realize multi-wavelength-detection on-line, and is easily handled (touch screen control), and its performance accords with the Chinese national standard.
2006 Vol. 26 (04): 779-783 [Abstract] ( 463 ) PDF (953 KB)  ( 517 )