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2008 Vol. 28, No. 02
Published: 2008-02-26

 
       光谱学与光谱分析
241 Effects of PBD on the Luminescence Properties of PVK∶Ir(ppy)3
YANG Shao-peng1,YANG Ya-ru1,ZHAO Su-ling2,XU Zheng2,ZHANG Fu-jun2,ZHANG Xue-feng1,LU Su-kui1,QIN Xiang-dong1*
DOI: 10.3964/j.issn.1000-0593.2008.02.001
The effects of PBD on the luminescence properties of PVK∶Ir(ppy)3 codoped with PBD with lower concentration were investigated. Two kinds of devices with the structures of ITO/PVK∶Ir(ppy)3/PBD/Al and ITO/PVK∶Ir(ppy)3∶PBD/Al were fabricated. PVK emission appears in the electroluminescence (EL) spectra of ITO/PVK∶Ir(ppy)3/PBD/Al. The reason is that the Forster energy transfer is not efficient enough in the emission layer, and then the emission layer was doped with PBD. A set of devices were fabricated with the configuration of ITO/PVK∶Ir(ppy)3∶PBD/BCP/Al. The doping weight ratio of PVK∶Ir(ppy)3 was fixed as 100∶1, and the weight ratio of PBD changed from 100∶0 (PVK∶PBD) to 100∶20. The photoluminescence (PL) spectra and electroluminescence (EL) spectra of these devices were measured. Through the analysis of their luminescence, it was found that the brightness of these devices codoped with PBD is improved. The brightness of these devices increases with increasing PBD doping ratio as the ratio does not exceed 100:10(PVK∶PBD). The PBD codoping enhances the injection and transportation of electron, resulting in the enhanced carrier recombination probability. If the doping ratio of PBD exceeds 100∶10(PVK∶PBD), the brightness of the device decreases. There are two reasons. One is that the superfluous PBD causes the carriers to be imbalanced and induces a larger leakage current. The other is that the superfluous PBD may block the hoping of holes or electrons between the PVK chains. The brightness is the strongest when the weight ratio of PVK to PBD is 100∶10.
2008 Vol. 28 (02): 241-245 [Abstract] ( 1298 ) PDF (1936 KB)  ( 479 )
246 Effect of Hydrogen Passivation on Photoluminescence Intensity of Si Nanocrystals
CHEN En-guang1,YI Li-xin1*,WANG Shen-wei1,LIU Rao-ping1,SU Meng-chan1,TANG Ying2,WANG Yong-sheng1
DOI: 10.3964/j.issn.1000-0593.2008.02.002
SiO/SiO2 superlattices samples were prepared on Si substrates by reactive evaporation of SiO powder in vacuum or an oxygen atmosphere. The samples were annealed in nitrogen atmosphere at high temperature subsequently. And then, H+ with a dose of 3.0×1014·cm-2 and 3.0×1015·cm-2 respectively was implanted into these samples with formed Si nanocrystals at 20 keV. The PL spectra showed that the PL intensities of samples with H+ implanting dropped sharply compared with the samples without H+ implanting. The PL intensity increased gradually with increasing re-annealing temperature; and it even could exceed that of samples without H+ implanting if the dose of H+ was enough. Our further investigations showed that the varieties of the PL intensities were mainly dependent on the area density of the defects formed in the samples, and also the area density of the defects was influenced by the dose of H+ and the further re-annealing temperatures.
2008 Vol. 28 (02): 246-248 [Abstract] ( 1875 ) PDF (1120 KB)  ( 885 )
249 Investigation on Electroluminescence of MEH-PPV/ZnSe Nanocomposite Device
XIONG Sha,HUANG Shi-hua*,TANG Ai-wei,TENG Feng,LIANG Chun-jun,XU Zheng
DOI: 10.3964/j.issn.1000-0593.2008.02.003
ZnSe nanocrystals were synthesized in aqueous solution by using mercapto-acetate acid as stabilizer. Products were characterized by X-ray diffraction patterns (XRD) and X-ray photoelectron spectra (XPS). A surfactant was used to transfer the nanocrystals from the aqueous solution to organic solvent, so that ZnSe and MEH-PPV could be mixed sufficiently and were used as an emitting layer in a multilayered electroluminescence device: Glass/ITO/MEH-PPV∶ZnSe /BCP/Alq3/LiF/Al. A comparison between absorption spectra and photoluminescence spectra of ZnSe nanocrystals and MEH-PPV thin film exhibits an effective energy transfer from ZnSe nanocrystals to MEH-PPV, which is one reason for the existing difference between photoluminescence spectrum and electroluminescence spectrum of MEH-PPV∶ZnSe nanocomposite film. The recombination mechanism of the nanocomposite film under photoexcitation and electric injection was discussed respectively. The authors investigated the photo- and electroluminescence properties of the device, and found that the EL intensity of ZnSe nanocrystals increased with the applied voltages. The I-V characteristic of this device is similar to that of a classic diode.
2008 Vol. 28 (02): 249-252 [Abstract] ( 1223 ) PDF (1601 KB)  ( 556 )
253 Structural and Optical Characterization of ZnO Thin Films Grown by Plasma-Assisted Molecular Beam Epitaxy
LAN Zhen-li1,ZHANG Xi-qing1,YANG Guang-wu2,SUN Jian1,LIU Feng-juan1,HUANG Hai-qin1 ,ZHANG Rui3, YIN Peng-gang3,GUO Lin3,SONG Yu-chen4
DOI: 10.3964/j.issn.1000-0593.2008.02.005
High-quality ZnO thin films were grown by plasma-assisted molecular beam epitaxy (P-MBE) on Al2O3(0001) substrate with a low temperature ZnO buffer layer. Structural and optical characterization were studied for ZnO thin films. Only a peak at (0002) were observed in the X-ray reflectivity(XRD) spectra with the full-width at half maximum (FWHM) value 0.18°, and two peaks 1LO(579cm-1) and 2LO(1 152 cm-1) were detected in the resonance Raman scattering spectra at room temperature. These results indicated that ZnO thin films had single orientation of c axis and high-quality of crystal wurtzite structure. The absorption of free-exciton and exciton-LO phonon appeared in the absorption spectra, which confirmed that the exciton state in the ZnO thin films were stable even at room temperature. And the energy spacing between these two peaks is 71.2 meV, corresponds to the longitudinal optical phonon energy of 71 meV of ZnO. Besides, from the photoluminescence spectra, no defect-related deep emission were observed, but just a remarkable free-exciton emission located at 376nm were obtained at room temperature, it proved that the ZnO thin films had high-quality but low density of defect.
2008 Vol. 28 (02): 253-255 [Abstract] ( 1583 ) PDF (1213 KB)  ( 574 )
256 Optical Properties of One-Dimensional Metallodielectric Photonic Crystals
LUO Ya-heng,WANG Yong-sheng*,WANG Dong-dong,DENG Li-er,SUN Jian
DOI: 10.3964/j.issn.1000-0593.2008.02.004
The optical characteristics of one-dimensional metallodielectric photonic crystals (MDPC),constructed by inserting metal aluminum layers of certain thickness into the Si/SiO2 system, were studied theoretically with the transfer matrix method. The results show that the reflection efficiency can be enhanced considerably after the introduction of metallic layers, e.g. the rejection level of each period increased from 7.2 dB([Si(46 nm)/SiO2(120 nm)]5) to 20 dB([Si(46 nm)/SiO2(60 nm)/Al(10 nm)/SiO2(60 nm)]5). In addition, high omnidirectional reflection band with broader width can be obtained, e.g. bandwidth of 550 nm can be offered with [Si(46 nm)/SiO2(60 nm)/Al(30 nm)/SiO2(60 nm)]5. Rules of how the absorption, thickness and position of the metal layers affect the optical characteristics of the MDPC are also discussed. These MDPC structures may be used as compact-size, low-loss and broad-band optical reflectors.
2008 Vol. 28 (02): 256-259 [Abstract] ( 1650 ) PDF (1668 KB)  ( 494 )
260 Preparation and Luminescence Properties of Tb3+ Ion and Na2WO4 Co-Doped SiO2 Materials
WANG Xi-gui1,LI Xia1,2
DOI: 10.3964/j.issn.1000-0593.2008.02.006
Tb3+ and Na2WO4 co-doped SiO2 materials were prepared by sol-gel method and the structure of materials were measured by DTA-TG, IR and XRD techniques. The results indicate that the materials were in amorphous phase and the Si—O—Si bond was still observed in samples annealed at 800 ℃. The influence of Na2WO4 on luminescence properties of terbium glasses was investigated by three-dimension fluorescence spectra, excitation and emission spectra. It is approve that when sample excited by 230 nm showed the characteristic emission peaks of terbium corresponding to 5D47Fj(j=4, 5, 6) and 5D37Fj(j=4, 5, 6) transitions. Doping Na2WO4 has less influence with the emission position of SiO2 materials with terbium, but has a great effect with the emission intensity. It is find that the blue transition of 5D47F6 was activated and the green transition of 5D47F5 was quenched and the materials radiate green blue fluorescence light under ultraviolet light. The mechanism of sample was analyzed by the energy levels of Tb3+ and Na2WO4 co-doped glasses.
2008 Vol. 28 (02): 260-264 [Abstract] ( 660 ) PDF (2125 KB)  ( 525 )
265 Multiplayer White Organic Light-Emitting Diodes with Different Order and Thickness of Emission Layers
XU Wei, LU Fu-han,CAO Jin,ZHU Wen-qing,JIANG Xue-yin*,ZHANG Zhi-lin,XU Shao-hong
DOI: 10.3964/j.issn.1000-0593.2008.02.007
In multilayer OLED devices, the order and thickness of the emission layers have great effect on their spectrum. Based on the three basic colours of red, blue and green, a series of white organic light-emitting diodes(WOLEDS)with the structure of ITO/CuPc(12 nm)/NPB(50 nm)/EML/LiF(1 nm)/Al(100 nm) and a variety of emission layer’s orders and thicknesses were fabricated. The blue emission material:2-t-butyl-9,10-di-(2-naphthyl)anthracene(TBADN) doped with p-bis(p-N, N-diphenyl-amono-styryl)benzene(DSA-Ph), the green emission material:tris-[8-hydroxyquinoline]aluminum(Alq3) doped with C545, and the red emission material:tris-[8-hydroxyquinoline]aluminum(Alq3) doped with 4-(dicyanomethylene)-2-t-butyl-6-(1,1,7,7-tetramethyljulolidyl-9-enyl)-4H-pyran (DCJTB) were used. By adjusting the order and thickness of each emission layer in the RBG structure, we got a white OLED with current efficiency of 5.60 cd·A-1 and Commission Internationale De L’Eclairage (CIE) coordinates of (0.34, 0.34) at 200 mA·cm-2. Its maximum luminance reached 20 700 cd·m-2 at current density of 400 mA·cm-2. The results were analyzed on the basis of the theory of excitons’ generation and diffusion. According to the theory, an equation was set up which relates EL spectra to the luminance efficiency, the thickness of each layer and the exciton diffusion length. In addition, in RBG structure with different thickness of red layer, the ratio of the spectral intensity of red to that of blue was calculated. It was found that the experimental results are in agreement with the theoretical values.
2008 Vol. 28 (02): 265-268 [Abstract] ( 2713 ) PDF (1395 KB)  ( 605 )
269 Flow-Injection Chemiluminescence Determination of Procaterol Hydrochloride
RAO Zhi-ming1,ZOU Ping1,CHEN Mei1,XIU Fu-rong1,CHEN Yu-lin2,HONG Ke-jun2
DOI: 10.3964/j.issn.1000-0593.2008.02.009
A new flow injection chemiluminescences method for the determination of procaterol hydrochloride has been developed. It is based on the chemiluminescence reaction of procaterol hydrochloride with Ce(Ⅳ)-rhodamine B in sulphuric-chlorhydric acid medium and the experimental fact of the enhancement of chemiluminescence by surfactant CTMAB. The concentration of the analyte shows a good linear relationship with the produced luminescence intensity in the range of 2.0×10-8g·mL-1 to 1.0×10-6g·mL-1. The detection limit of the proposed method is 6×10-9g·mL-1 and the RSD is 1.6%(n=11) at 2×10-7g·mL-1. This result is satisfactory compared with the method mentioned in the pharmacopoeia of People’s Republic of China.
2008 Vol. 28 (02): 269-272 [Abstract] ( 1854 ) PDF (1261 KB)  ( 619 )
273 Predicting Nitrogen Concentrations from Hyperspectral Reflectance at Leaf and Canopy for Rape
WANG Yuan1,2,HUANG Jing-feng1,3*,WANG Fu-min1,2,LIU Zhan-yu1,2
DOI: 10.3964/j.issn.1000-0593.2008.02.011
An experiment was designed to determine whether nitrogen concentrations could be predicted from reflectance (R) spectra of rape leaves in laboratory, and, if so, whether the predictive spectral features could be correlated with nitrogen concentration of simple canopies of rape. The best predictors for nitrogen in leaves appeared with first-difference transformations of R, and the bands selected were similar to those found in other studies. Shortwave infrared bands were best predictors for nitrogen. In the shortwave infrared region, however, the absolute differences in reflectance at critical bands were extremely small, and the bands of high correlation were narrow. High spectral and radiance resolution are required to resolve these differences accurately. Variability in canopy reflectance in shortwave infrared region was at least an order of magnitude beyond that necessary to detect signals from chemicals. The variability in first-difference R and log 1/R on canopy scales were related to the arrangement of trees with respect to direct solar radiation, instrument noise, leaf fluttering, and small change in atmospheric moisture. The first-difference of reflectance R based regressions prediction of nitrogen concentration at canopy level gets a good fitness.
2008 Vol. 28 (02): 273-277 [Abstract] ( 635 ) PDF (1646 KB)  ( 625 )
278 Radiation Properties of Plasma Produced by Ultraviolet Laser Ablation of Metal Cu
HUANG Qing-ju
DOI: 10.3964/j.issn.1000-0593.2008.02.010
Time-resolved measurement of plasma plume emission spectra from XeCl excimer laser ablation of copper in nitrogen is reported. The experimental results indicate that the plasma emission spectra are mainly composed of atomic spectrum, univalent ion spectrum and continuous radiation, and these spectral lines have different number, intensity and duration. The main detailed mechanism of species excitation was discussed. The electrons obtain high-kinetic energy through reverse bremsstrahlung, the continuous radiation comes from the bremsstrahlung emission of energetic electrons ejected from the target, the excitation mechanism of atomic and univalent ion is inelastic collision between the elemental species and high kinetic-energy electron, and recombination of electron and ion in the plasma, and the model can be used to explain the experimental results qualitatively.
2008 Vol. 28 (02): 278-281 [Abstract] ( 1193 ) PDF (1269 KB)  ( 727 )
282 Studies on IR Spectroscopy and Quantum Chemical Calculation of Chloroaluminate Ionic Liquids Acidity
WU Qin1,2,HAN Ming-han2*,XIN Hong-liang2,DONG Bin-qi2,JIN Yong2
DOI: 10.3964/j.issn.1000-0593.2008.02.012
The acidity of chloroaluminate ionic liquids and the interaction mechanism of Lewis acid site Al2Cl-7 of chloroaluminate ionic liquid and pyridine were experimentally investigated by IR characterization by using pyridine as molecular probe and increasing pyridine adsorption, and theoretically confirmed by quantum chemical calculations at density functional theory (DFT) and ab initio levels. It was found that the anions,Al2Cl-7 and AlCl-4,which could withdraw lone pair electrons of pyridine, were characteristic of Lewis acid. Therefore, they displayed pyridine coordinated to Lewis acidic site using pyridine as probe. The acidity of Al2Cl-7 was found stronger than that of AlCl-4 by analyzing IR absorption frequency, bond length and charge distribution. The mechanism of forming and evolvement of the Lewis acid site Al2Cl-7 of chloroaluminate ionic liquid was proposed. When the amount of pyridine is small, only the adsorption state of Py-Al2Cl-7 exists. The highly Lewis acidic adsorption state of Py-Al2Cl-7 complex was converted into Py-AlCl-4 complex and Py-AlCl3 complex with increasing pyridine contents, leading to the changes in IR absorption spectra.
2008 Vol. 28 (02): 282-284 [Abstract] ( 734 ) PDF (1328 KB)  ( 639 )
285 Review of Progress in Application Visible/Near-Infrared Spectroscopy in Liquid Food Detection
LIN Tao,YU Hai-yan,YING Yi-bin*
DOI: 10.3964/j.issn.1000-0593.2008.02.008
As a rapid, non-destructive new testing technology, Vis/near-infrared spectroscopy is increasingly widely used in agriculture products and food quality evaluation research. The United States, Japan and many European countries have made a great deal of progress in the Vis/near-infrared spectroscopy for agriculture products and food quality evaluation. Although our country has got some fruits in this area, in comparison with foreign countries, there is still a lot of work to strengthen. In the present paper, from aspects of alcohol, dairy products, fruit juices and edible oil, the authors reviewed the latest research progress in Vis/near-infrared spectroscopy in the quality evaluation of liquid food with the emphasis on the recent 5 years, analyzed the advantages of this technique’s application to the quality evaluation of liquid foods. Finally, problems existing in the applications were analyzed and solutions to them were proposed. Based on a study of the issue, this article outlined the further study and made a number of recommendations.
2008 Vol. 28 (02): 285-290 [Abstract] ( 137 ) PDF (1107 KB)  ( 949 )
291 Measurement and Analysis of Nanometer Particles of Silica and Carbon Black by Diffuse Reflection FTIR Spectra
YANG Xiao-zhan1,TANG Chong-min1,LIU Zi-li2,YAO Yong-yi1,LI Rui-xia1,WU Da-cheng1*
DOI: 10.3964/j.issn.1000-0593.2008.02.014
By using FTIR-FTS3000 spectrometer and infrared diffuse reflection accessory, the spectra of the nanometer particles of silica, carbon black and their blends with different weight ratio were collected and characterized. It was found from the measured results that blue-shift and broadening phenomenon occurred in the nanometer particle materials in comparison with the mass ones. These phenomena could be explained by the little size effect and quantum size effect. No perfect spectrum could be collected because of the strong absorbance of the nanometer particle materials. For the blends of silica and carbon black there was a maximum absorption corresponding to the critical concentration, where the weight ratio of silica to carbon black was 100∶20, and below this ratio the relationship between the function F(R) and the concentration obeyed Lambert-Beer’s law. Above this ratio, the absorbance will not increase with increasing the proportion of the carbon black in the system.
2008 Vol. 28 (02): 291-294 [Abstract] ( 817 ) PDF (2134 KB)  ( 855 )
295 Real-Time Analysis of Soil N and P with Near Infrared Diffuse Reflectance Spectroscopy
CHEN Peng-fei1,2,LIU Liang-yun1,WANG Ji-hua1*,SHEN Tao1,LU An-xiang1,ZHAO Chun-jiang1
DOI: 10.3964/j.issn.1000-0593.2008.02.015
Improving the efficiency of fertilization is an effective method of enhancing income for farmers, but it depends on measuring the soil nutrients accurately and rapidly. Near infrared reflectance spectroscopy (NIRS) is a fast method to detect the soil nutrients. In order to evaluate the feasibility of using NIRS to determine the soil N and P contents, the soil samples were collected from different LULC (land use and land cover) types in Daxing district, Beijing, and their biochemical parameters were determined by traditional chemical method. Then, the near infrared reflectance spectra of the samples were acquired, and NIRS models were built using partial least square regression (PLS) and Fourier transform technology for the total N and total P. The determination coefficients of cross validation for the total N and total P were 0.862 6 and 0.668 5 respectively. Ten samples were used to test the performance of the models. The coefficients of correlation between the chemically determined value and the NIRS predicted one were 0.969 8(N) and 0.830 7(P) respectively. The root mean standard error of prediction for N and P were 0.009 5(%) and 0.008 6(%), respectively. The ratios of RMSEP to SD(RPD) were 3.78(N) and 1.69(P). The results showed that the NIRS could be used to evaluate the soil N accurately and the soil P roughly.
2008 Vol. 28 (02): 295-298 [Abstract] ( 517 ) PDF (1165 KB)  ( 1045 )
299 Method of Infrared Spectrum Analysis of Hydrocarbon Mixed Gas Based on Multilevel and SVM-Subset
BAI Peng1,2,XIE Wen-jun3,LIU Jun-hua2
DOI: 10.3964/j.issn.1000-0593.2008.02.016
The hydrocarbon mixed gas was characterized by multi-component and varied density. In order to deal with the difficulties that can not be actually solved with mass mixture gas spectrum data samples, 15 kinds of subset patterns were determined on the basis of investigations and studies, which needed 5 500 spectrum data samples for training and testing. On the basis of this, a method of hydrocarbon mixed gas infrared spectrum analysis based on 2-levels and 15 SVM-subsets was proposed in the light of the idea of working pattern recognition→mixture gas analysis→the final result output. In order to solve the problem of new subset working pattern, the SVM online categorization algorithm based on spectrum data relational rule was used. The experimental results show that the component concentration maximal deviation is 0.41% and the maximal average deviation is 0.04%. The method can be used in other mixture gas infrared spectrum analyses, and has the theoretic and application value.
2008 Vol. 28 (02): 299-302 [Abstract] ( 259 ) PDF (1330 KB)  ( 581 )
303 Application of Near-Infrared Reflectance Spectroscopy in Grass Breeding with Space Flight Mutagenesis
REN Wei-bo1,3,HAN Jian-guo1,ZHANG Yun-wei1*,GUO Hui-qin2
DOI: 10.3964/j.issn.1000-0593.2008.02.017
Near infrared reflectance spectroscopy is a new fast and efficient analysis method. It has been wildly used in many areas such as evaluation of feedstuff, assessment of soil fertilizer and so on. In the present paper, the principle, technique method and merits of NIRS were introduced. The potential application of NIRS in grass breeding with space flight mutagenesis was discussed in areas such as analysis of grass nutrition, estimate of secondary metabolism compounds, forecast of disease and insects resistance, and evaluation of abiotic stress. The conclusion is that application of NIRS in grass breeding with space mutagenesis is significant in both academic and technical areas because it not only improves the efficiency of mutation selection but helps uncover the mechanism of space mutation breeding.
2008 Vol. 28 (02): 303-307 [Abstract] ( 2294 ) PDF (960 KB)  ( 813 )
308 Study on the Malignant and Normal Rectum Tissues Using 1H NMR Spectroscopy
ZHAO Mei-xian1,2,GAO Xiu-xiang2,QI Jian2,YAO Hong-wei3,LI Hui-zhen2,XU Yi-zhuang2*,TANG Guang-shi1,WANG Jing4,WU Jin-guang2
DOI: 10.3964/j.issn.1000-0593.2008.02.018
Cancer is one of the most serious diseases, a threat to human body’s health and a causes of death. The early diagnosis of cancer and timely therapy is significant for improving the survival. Owing to the complexity and limit of conventional medical diagnosis, misdiagnosis of ten occurs in many cases. NMR spectroscopy is an effective technique for characterizing molecular structure and component changes. The component and structural information of nucleic acid, protein, lipid and glucide in the biologic tissues can also be distinguished from NMR data. In the present paper, a new method was developed for the diagnosis of tumor using the advanced physical chemistry (NMR) and biomedicine technique. Nine rectum tissue samples and their corresponding normal tissues of rectum were measured using NMR spectroscopy. Each tissue sample obtained from the operation was quickly separated into two parts averagely: one was dipped into 10% formalin solution and prepared for conventional pathological examination; the other was preserved in liquid nitrogen for further NMR detection. Before NMR detection, the corresponding sample was thawed at room temperature and was dipped into 0.5 mL D2O. Dioxane was used as external reference. The obtained NMR spectra were analyzed and compared by OMNIC5.0TM and SPSS 11.0TM Software. The differences of metabolite in the tissues samples were studied and a method for the diagnosis of cancer using NMR data was initially explored. The result indicates that the 1H NMR spectra of rectum cancer tissues are significantly different from those of their corresponding normal rectum tissues. This is shown by the differences in the integral area ratio at characteristic peak region. A0.9/A3.0, A1.3/A3.0, A2.0/A3.0, A1.3/A0.9 and A4.1/A3.0 of the normal rectum tissues are higher than those of their corresponding cancer tissues, but A3.2/A3.0 is lower than that of the rectum cancer tissues. From the above result it is concluded that the concentration of fatty acid, inositol and lactate is lower in the rectum cancer tissues than in the normal tissues, while that of choline bases compounds is higher. The NMR judgments were also consistent with the pathological examination results. So the NMR spectra may be developed into a method of early diagnosing rectum cancer through these differences.
2008 Vol. 28 (02): 308-312 [Abstract] ( 2371 ) PDF (1511 KB)  ( 561 )
313 Investigation on the Quality Indicators of Beers Using NIR
LIU Hong-xin1,2,ZHANG Jun3*,HUANG Fu-rong3,HUANG Yong3,HE Li-jun4,ZENG Yu-ping4, CHEN Xing-dan1, 3,LU E1
DOI: 10.3964/j.issn.1000-0593.2008.02.019
Near infrared spectroscopy (NIR) has been used to determine important indicators of the quality of undeaired beers by a partial least squares (PLS) regression and stepwise multiple linear regression (SMLR). The indicators are original, real extract and alcohol contents. Absorbance spectra in transmission mode of 83 samples were obtained with 1 mm and 5 mm pathlength quartz cell. The selected resolving powers are 8, 16 and 32 cm-1. Air and water were used as background respectively. It was concluded that the calibration and prediction results are similar with different background, pathlength and resolving power. The SMLR method seems to be better than PLS method. The results of this paper provide a foundation for the application and further development of NIR on-line beer analyzer.
2008 Vol. 28 (02): 313-316 [Abstract] ( 2431 ) PDF (1087 KB)  ( 963 )
317 Prediction of Leaf Concentration in Alfalfa Using Near Infrared Reflectance Spectroscopy
NIE Zhi-dong1,HAN Jian-guo1*,YU Zhu1,ZHANG Lu-da2
DOI: 10.3964/j.issn.1000-0593.2008.02.020
Leaf concentration in alfalfa is an important factor affecting the nutritive value, forage intake and digestibility. Estimates of leaf concentrations commonly used currently involve a labor intensive process of hand separating leaf and stem fractions. In the present study, a total of 41 artificial alfalfa samples were mixed with different leaf concentrations ranging from 15% to 55%. The object was to develop 3 calibrations for predicting alfalfa leaf concentrations using 15,25 and 35 calibrated samples by near infrared reflectance spectroscopy. The root mean square error of prediction(RMSEP)was 1.02, 1.97 and 0.51, respectively. External validation had a coefficient of determination (r2) ranging from 0.979 8 to 0.998 9. The ratio of performance to standard deviation (RPD) varied from 2.85 to 25.93.The results showed that 15 samples could develop accurate NIRS model of alfalfa leaf concentrations;the calibration equations got better accuracy with the increase in calibrated samples numbers from 15 to 35.
2008 Vol. 28 (02): 317-320 [Abstract] ( 1391 ) PDF (1116 KB)  ( 610 )
321 Fourier Transform Infrared Spectroscopic Study of Coprinus Comatus
ZHOU Ji-guo1,LIU Gang1*,LIU Jian-hong2,SONG Ding-shan3,SHI Yong-ming1
DOI: 10.3964/j.issn.1000-0593.2008.02.013
In the paper, Fourier transform infrared (FTIR) spectroscopy was used to study the fruiting body of wild growing and cultivated Coprinus comatus and the cap of the mushroom before and after deliquescing into inky liquid. The results show that the infrared spectra of Coprinus comatus are mainly composed of the absorption bands of protein and polysaccharide. Remarkable differences are observed in the absorption bands of polysaccharide between the spectra of the wild growing and cultivated mushrooms, by which the wild growing and cultivated Coprinus comatus can be discriminated. It was also found that the absorption bands of polysaccharide become weaker obviously in the black-inky samples of deliquescing cap compared with the un-deliquescing cap, indicating that the polysaccharides in the cap of Coprinus comatus are transformed during the process of cap deliquescing into a black, inky liquid. The spectral results can offer useful information for a further study of Coprinus comatus.
2008 Vol. 28 (02): 321-323 [Abstract] ( 1226 ) PDF (1227 KB)  ( 661 )
324 Determination of Isorhamnetin in Hippophae Rhamnoides Linn from West Sichuan Plateau Using Near Infrared Diffuse Reflectance Spectroscopy
YE Li-ming1,ZHOU Min1,ZHANG Hao1,CHEN Chu1,LI Zhang-wan1*,CHEN Cong1,WANG Yan-ping2
DOI: 10.3964/j.issn.1000-0593.2008.02.022
The objective of this study was to develop a method for the determination of isorhamnetin in Hippophae rhamnoides Linn from West Sichuan plateau using near infrared diffuse reflectance spectroscopy. Applying the method of mixing with SiO2,the near infrared spectra (NIS) with the range of 12 000-4 000 cm-1 were recorded for the Hippophae rhamnoides Linn containing isorhamnetin with the content of 0.1%-0.8%. Calibration models were established using the PLS (partial least squares). Different spectra pretreatments methods were compared. The study showed that spectral information can be extracted thoroughly by constant offset elimination (COE) pretreatments method with the correlation coefficient(r2) of 0.739 8, SEC of 0.107 (standard deviation of the calibration sets) and SEP of 0.073 (standard deviation of the prediction sets). The results indicate that near infrared diffuse reflectance spectroscopy is more rapid and convenient than conventional methods.
2008 Vol. 28 (02): 324-326 [Abstract] ( 1215 ) PDF (1354 KB)  ( 813 )
327 FTIR and Classification Study on the Chinese Compound Recipe
WANG Jing-juan1,ZHANG Gui-jun1*,ZHOU Qun2,SUN Su-qin2*
DOI: 10.3964/j.issn.1000-0593.2008.02.023
On the basis of building a model of main components and with the fingerprint infrared spectrum as the object- Xiaoerchoufeng powders were rapidly classified and closely studied by using the method of clustering analysis. Because of the tiny difference between the spectra of different compound recipes, including the compound recipe without scolopendra, the compound recipe without scorpio, the compound recipe without bombyx batryticatus, the compound recipe without eupolyphaga seu steleophaga and the compound recipe without periostracum cryptotympanae, the outcome of the clustering is ideal. When tested with the blind samples (which were picked out from the chosen samples) the accuracy of clustering reaches up to 90%. In order to increase the clustering accuracy, the number of the samples should be increased and also these samples should be more characteristic. On the whole, with the combination of the fingerprint spectrum and the clustering analysis, the compound recipe can be distinguished rapidly.
2008 Vol. 28 (02): 327-330 [Abstract] ( 1552 ) PDF (1339 KB)  ( 621 )
331 Study on FTIR Spectra of Finger Nails of Normal People and Patients of Esophagus Cancer
WANG Hong-yan1,Lü Yin1,WANG Fan1*,MA Xiao-dong2,JIANG Shi-ping2,WANG Wei2,LI Cheng-xiang2
DOI: 10.3964/j.issn.1000-0593.2008.02.025
To investigate the application of human finger nails in the diagnosis of cancer, Fourier transform infrared (FTIR) spectroscopy was employed to study the finger nails from some normal people and some with esophagus cancer and others with an operation for curing esophagus cancer five months ago. The results showed that there are obvious differences between FTIR spectra in them in spectral parameters such as frequency, intensity and band shape etc. The changes in the phosphate symmetric stretching vibration νs(PO-2) and asymmetric stretching vibration νas(PO-2) modes are uniform, the νs(PO-2) and νas(PO-2) absorption peaks of cancerous ones shift to high wave number compared with those of normal people, while those with operation shift to low wave number compared with those of cancerous ones. The C—O stretching vibration mode of protein located at 1 164 cm-1 is composed of three absorption peaks located at 1 173.3,1 158.0 and 1 151.1 cm-1 respectively, meanwhile, the intensities and the wave numbers of the three peaks of cancerous ones all increase compared with normal people. The wave numbers of amide Ⅰ and amide Ⅱ of cancerous ones are both lower than those of normal people, while those with operation are between the cancerous ones and normal people, which suggest that the contents of protein and α-helix in finger nails of normal people, cancerous ones and the ones with operation are discriminative. The peak of bending vibration δ(CH2)mode of CH2 groups of protein lipid of cancerous ones shifts to high wave number slightly and the intensity of the peak weakens compared with that of normal people, which indicate that the methylene chain in the finger nails membrane lipids of cancerous ones is more ordered than that of normal people. Nevertheless, the peak of stretching vibration νs(CH2)of cancerous ones is lower than that of normal people, while that of the ones with operation is between cancerous ones and normal ones. As a result, the pathological changes in viscera can induce the changing of framework structure of phosphate in nucleic acid molecule of finger nails, and destroy the hydrogen bond of C—O(H) group in amino acid remnant group in finger nails. Furthermore, it also can decrease the C—O bond in keratin which participates in the action of hydrogen bond, and prompt the changing of content of keratin in finger nails, nevertheless the content of keratin in finger nails of cancerous ones can be resumed to level of normal people by operation.
2008 Vol. 28 (02): 331-334 [Abstract] ( 1284 ) PDF (1234 KB)  ( 557 )
335 Study on Crystal Growth and Vibrational Spectra of Ybx∶KY1-x(WO4)2
LIU Jing-he1,ZHANG Ying1,ZHANG Li-jie1,ZENG Fan-ming1,WANG Cheng-wei2,ZHANG Xue-jian3
DOI: 10.3964/j.issn.1000-0593.2008.02.026
Ybx∶KY1-xW(x=0.05)and KYbW crystals were grown by TSSG method. Both of the structure and spectral properties were compared. The condition for the crystal growth is:the rotation rate 10-15 r·min-1,the pulling speed 1-2 mm·d-1,the growing period 10-15 d,cooling growing speed 0.05-0.1 ℃·h-1,and the cooling speed 20 ℃·h-1. X-ray powder diffraction analysis was performed for the crystal powder. They belong to β-KYW structure with low thermal phase. The cell parameters of the two crystals were calculated, and they are respectively a1=1.063 nm,b1=1.034 nm,c1=0.755 nm,β1=130.75°,Z1=4 and a2=1.061 nm,b2=1.029 nm,c2=0.749 nm,β2=130.65° and Z2=4. The infrared spectrum and Raman spectrum of crystal were measured. The sample of Ybx∶KY1-xW(x=0.05) had stronger infrared absorption peaks at 925,891,840,777 and 749 cm-1,which were caused by stretching vibration. The sample of KYW had stronger infrared absorption peaks at 484 and 437 cm-1 caused by bending vibration. The vibration modes were analysed and vibrational frequencies of vibratory activity was assigned. The two crystals had strong Raman activity. The vibration of WOOW and WOW exists from 200 to 1 000 cm-1.
2008 Vol. 28 (02): 335-338 [Abstract] ( 506 ) PDF (1531 KB)  ( 591 )
339 Surface Enhanced Raman Spectrum of Rat Serum in the Novel Silver Colloid
LIU Kun, WU Shi-fa, CHEN Mao-du, PAN Shi
DOI: 10.3964/j.issn.1000-0593.2008.02.021
In the present article, the high signal-to-noise ratio surface enhanced Raman spectrum of rat serum was analyzed. To be high efficient substrate of SERS, the novel silver colloid was synthesized by microwave method. The characteristic peaks of the rat Raman spectrum were assigned. The mechanism of “hot spot” which was formed by aggregated silver particles was explained by electromagnetic fields enhancements theory, i.e. the excitation of plasmons in the metallic nanoparticles created greatly enhanced local electromagnetic fields, contributing to the major component of the SERS effect. The field distribution at novel silver aggregates exhibits a dramatic enhancement. These strongly localized fields provide an important mechanism for surface enhanced Raman scattering. The surface enhanced Raman spectrum of low quality of component in rat serum was acquired so that the change of body could be known in time. A new method for acquiring abundant information of macro-biomolecule by spectrum means was brought out. It is hopeful to be a novel technique to diagnose diseases in the early stage with serum.
2008 Vol. 28 (02): 339-342 [Abstract] ( 310 ) PDF (1235 KB)  ( 530 )
343 Study on the Surface-Enhanced Raman Spectrum of Phenylalanine on Silver Sols
LIU Wen-han1,YANG Wei1,ZHANG Dan1,2
DOI: 10.3964/j.issn.1000-0593.2008.02.027
The surface enhanced Raman scattering (SERS) of L-phenylalanine solution system was studied in the present paper. The enhancement effect is obvious. Compared to the conventional Raman spectra of solid phenylalanine, the frequency deviations of some peaks in the SERS spectra were observed, and the relative strengths of some peaks were certainly changed. The influence of three different laser sources on the intensity of SERS spectra is discussed. The 514.42 nm of laser source is the best among the 514.42, 632.81 and 785.18 nm. The intensity of SERS spectra can be changed with the concentration of L-phenylalanine. It does not benefit the formation of SERS spectra when the concentration is too high or too low. When the concentration of bottom solution is 1×10-3mol·L-1,the enhancement effect of SERS is the strongest. The pH value of system also has obvious effect on the SERS, and when the pH value is 8, the enhancement effect of SERS is the best. It is the total influence of the pH on the coacervation of the silver sol and existent form of the phenylalanine.
2008 Vol. 28 (02): 343-346 [Abstract] ( 1286 ) PDF (1556 KB)  ( 692 )
347 Three-Dimensional Fluorescence Fingerprint for Source Determination of Dissolved Organic Matters in Polluted River
ZHONG Run-sheng1,ZHANG Xi-hui2*,GUAN Yun-tao2,MAO Xian-zhong2
DOI: 10.3964/j.issn.1000-0593.2008.02.029
Fluorescence fingerprint technique was used to characterize dissolved organic matter (DOM) in river from different sources. The results showed that two types of DOM fluorescence signals were observed in river water: a humic-like fluorescence with three maxima at λexem=250/460 nm(A1),220/400 nm(A2) and 325/420 nm(C); and a protein-like fluorescence with two maxima at λexem=230/360 nm(T2) and 285/357 nm(T1). The intensity of both of protein-like fluorescence distinctly increased because of the domestic wastewater drainage in the tributary stream. After the tributary converges into the main stream, the Fe3+ concentration in the main stream is 30 times as much as that of tributary stream, and the visible blue-shift of humic-like fluorescence occurred while the others didn’t occur. The intensity of all types of fluorescence decreased from source to estuary resulting from different solute chemistry. However, the intensities of humic-like fluorescence C, A1 and protein-like fluorescence T2 at the longer excitation wavelength decreased significantly because of dilution from main river stream and complexation of humic-like with Fe3+,thus the peaks disappeared at the estuary while the fluorescence peaks at the shorter excitation wavelength were relatively stable on which the river solute chemistry had little effect. Therefore, the fluorophores at the shorter excitation wavelength of 220-230 nm area potential tool to determine the sources of DOM in polluted river.
2008 Vol. 28 (02): 347-351 [Abstract] ( 2296 ) PDF (2178 KB)  ( 701 )
352 Time Resolved UV-Vis Absorption Spectra in Synthetic Process of Quercetin Complex with Al3+
LI Hui-feng1,LI Ping1*,LI Ying1,YANG Xiao-zhan2,WU Da-cheng2,LI Rui-xia2
DOI: 10.3964/j.issn.1000-0593.2008.02.024
With a deuterium light source was used to provide the continuous light, the time resolved UV-Vis absorption spectra in the synthetic process of quercetin complex with Al3+ were measured by using an intensified ICCD spectroscopic detector. The measuing system was controlled synchronously by using a digital delay generator DG535. A total of 50 spectra with the exposure time of 1 μs for each spectrum and the time interval of 20 ms between two successional spectra were acquired. Results showed clearly that the typical bands centered at 254 and 374 nm of quercetin disappeared at 40 ms after the reaction started; at the same time, an absorption band centered at 384 nm of a transitional product appeared, and the typical absorption band centered at 300 nm of Al3+ still existed; with the reaction progressing, the bands of the transitional product and Al3+ disappeared, and the new bands centered at 267 and 436 nm of the complex of quercetin with Al3+ appeared and became stronger gradually; at 980 ms, the typical absorption band of Al3+ disappeared completely and the two typical absorption bands of the complex increased to the strongest. The synthetic reaction of quercetin complex with Al3+ finished within one second. The process of Al3+ being scavenged is shown in the spectra obviously. The prensent results provide experimental evidence for the Al3+ scavenging ability of quercetin.
2008 Vol. 28 (02): 352-355 [Abstract] ( 1842 ) PDF (1442 KB)  ( 728 )
356 Study on the Basic Characteristics of Bohai Sea Ice Reflectance Spectra
LI Ning,XIE Feng,GU Wei*,CUI Wei-jia,HUANG Shu-qing,LIU Zhen
DOI: 10.3964/j.issn.1000-0593.2008.02.028
For monitoring sea ice in Bohai Sea, the present paper performed a field observation experiment on sea ice reflectance spectrum in Bohai Sea by control experiment. In the experiment, three groups of sea ice samples from the Bayuquan in Liaodong Gulf were collected, which were clean even ice of different thickness, sea ice covered by melt snow layer and sea ice with sands. According to the series of observation data during the two years, the reflectance spectrum curve of clean even ice has double peaks (a big one and a small one) when the ice thickness is less than 30 cm. The principal reflection peak is in good relation to the thickness of the sea ice. The principal reflection spectral peak of ice covered by melt snow layer is obviously higher than that of the spectrum of clean even ice without the snow layer with the same ice thickness. The principal reflection spectral peak of the sea ice with sands increases sharply, and the spectrum curve arises slightly in the wavelength rang between 675 and 725 mm and then declines. Covering snow and sands are the key factors to result in the fact that the same ice thicknesses present different spectrum characteristics and the same spectrum characteristics present different thicknesses.
2008 Vol. 28 (02): 356-360 [Abstract] ( 2165 ) PDF (1245 KB)  ( 615 )
361 Synthesis, Structure and Surface Photovoltage Spectrum of Coordination Supramolecule: [Cu(phen)(H2O)2·SO4]
KOU Jin
DOI: 10.3964/j.issn.1000-0593.2008.02.030
A novel transition metal coordination supramolecule [Cu(phen)(H2O)2·SO4] has been synthesized by hydrothermally method. The single crystal structure was determined by X-ray diffraction, and the complex was characterized by IR and UV-Vis-NIR spectra. The structure analysis indicates that there are a lot of hydrogen bonds in the crystal, which make the complex form a 1D double chain coordination supramolecule. Surface photovoltage spectroscopy (SPS) technique was applied to detect surface electron behavior and study the photoelectric conversion capability of the complexes. SPS is a useful tool for surveying the charge change of solid material surface. Its sensitivity comes to 108 q·cm-2,which exceeds that of conventional spectroscopy such as XPS and Auger spectroscopy by many orders of magnitude. But long time, the study of SPS has mainly focused on inorganic semiconductor and organic semiconductor. There are seldom reports about the coordination polymers and supramolecules. The results of surface photovoltage spectrum (SPS) indicate that the complex exhibit positive surface photovoltage responses in the range of 300-800 nm. The induced surface photovoltage spectrum (FISPS) proved that the complex possesses the characteristic of p-type semiconductor.
2008 Vol. 28 (02): 361-365 [Abstract] ( 1237 ) PDF (1843 KB)  ( 572 )
366 Study on the Interactions of Eu(Ⅲ) Complex of O-(Thioxanthone-[2]-yl)-Oxyacetic Acid with DNA
YANG Wu,GAO Qi-kuan,LU Xiao-lin,WU Jin-xiu
DOI: 10.3964/j.issn.1000-0593.2008.02.031
The interaction of the Eu(Ⅲ) complex of O-(thioxanthone-[2]-yl)-oxyacetic acid and calf thymus DNA was studied using fluorimetric, UV-Vis and CD(circular dichroism) methods. It was found that the ultraviolet absorption intensity of Eu(Ⅲ) complex of O-(thioxanthone-[2]-yl)-oxyacetic acid decreased as the concentration of DNA increased under the physiological condition of pH 7.10, and the compound remarkably influenced the negative peak in CD spectra of DNA when Eu(Ⅲ) complex of O-(thioxanthone-[2]-yl)-oxyacetic acid interacted with DNA. The emission intensity of the Eu(Ⅲ) complex evidently increased in the presence of DNA. The emission intensity of the DNA-EB system decreased as the concentration of the complex increasesd. And the presence of EB also led to the decrease in the emission intensity of the DNA-complex system. These changes observed here are often characteristic of intercalation. The above results strongly suggest that the complex can bind to DNA mainly by intercalation.
2008 Vol. 28 (02): 366-369 [Abstract] ( 1246 ) PDF (1380 KB)  ( 654 )
370 Preparation of N-Doped Nanosize TiO2 and Spectral Analysis
JIN Zhen-xing1,HUANG Hong-yan1,LIU Shou-xin2
DOI: 10.3964/j.issn.1000-0593.2008.02.032
Nitrogen-doped nanosize TiO2 was prepared by sol-gel method with TBT and EDA as forerunner body,ethanol as solvent and glacial acetic acid as inhibitor. The crystalline structure and spectrum character were characterzed. According to the curves of differential thermal gravimetric analysis(TG/DTA), the crystal transformation temperature and the best calcining temperature of the obtained samples were determined. According to the ultraviolet-visible diffuse reflection spectrum(UV-Vis/DRS), the spectral absorption characteristic of the obtained samples was characterized; According to the X-ray diffraction spectrum (XRD), the particle size and crystalline phase structure of the prepared samples were determined; and according to the X-ray photoelectron spectrum(XPS), the superficial composition of the prepared samples was analyzed. The relations between the red shift degree of absorption band and the proportion of EDA/TBT and calcining temperature were investigated in this experiment. The results indicate that the crystal phase of the obtained nitrogen-doped TiO2 is anatase, and the absorption band has a red shift obviously. Both the proportion of EDA/TBT and the calcining temperature have an evident effect on the spectral absorption of the prepared samples . When the mol proportion of EDA/TBT is 1∶10 and the calcining temperature is 600 ℃, the spectral absorption of the prepared samples is the strongest.
2008 Vol. 28 (02): 370-373 [Abstract] ( 1738 ) PDF (1414 KB)  ( 614 )
374 Synthesis of Sulfur-Contained D(+)-Glucosamine Metal Complexes and Interaction with DNA and Serum Albumin
WU Shan-shan1,ZHANG Yin-feng2,DU Jin-feng1,ZHANG Qi1*, YUAN Wen-bing1,GU Hai-bo1
DOI: 10.3964/j.issn.1000-0593.2008.02.034
Four sulfur-contained D(+)-glucosamine metal complexes were synthesized (M-GLUS,M = Co, Cu, Ni and Zn)and characterized by elementary analysis, molar conductance, and proton nuclear magnetic resonance. The yield of the complex was about 70%, and it dissolved easily in water. The ligand coordinates with metalions mainly between sulphur and metalions, the coordination molar ratio of the ligand to metalion was 2∶1, and the molar conductivity indicated that all the complexes are nonelectrolyte. The mechanism of the interaction between metal complexes and calf thymus (ct) DNA in Tris buffer (pH=7.08), was studied by ultraviolet absorption and fluorescence spectroscopy. The results from varied experiments showed that the intensity of the maximal absorption peaks increased with gradual addition of metal complexes, but the metalions can decrease the maximal absorption and the ligand has no effect on it. Meanwhile, metal complexes could remarkably quench the emission intensity of the DNA-EB system, and the metal complexes could be bound to ct DNA. The quenching mechanism was discussed by Stern-Volmer’s equation, the figure showed that it is influenced by static quenching and dynamic quenching, so the partial interaction of the complexes and ct DNA was the major mode. Under physiological pH condition, this study was designed to examine the effect of complexes on human serum albumin and bovine serum albumin by fluorescence. The binding constants and sites of the interaction with SA were analyzed by the Scatchard’s equation, the results indicated that there was a strong interaction between the four metal complexes and serum albumin and the binding force was Co-GLUS>Zn-GLUS>Cu-GLUS>Cu-GLUS, and the binding site is only one.
2008 Vol. 28 (02): 374-379 [Abstract] ( 2619 ) PDF (19665 KB)  ( 513 )
380 Quenching Effect of Gold Nanoparticles for Fluorescein Sodium
GUO Yan-li,YAN Hong-tao,PEI Ruo-hui
DOI: 10.3964/j.issn.1000-0593.2008.02.033
The spectroscopic characteristic of interaction of fluorescein sodium and gold nanoparticles with different sizes was investigated via UV-Vis and fluorescence spectrophotometry. It was shown that fluorescein sodium adsorbed respectively onto the different sized gold nanoparticle surface suffers different extent of quenching of their fluorescence. The quenching efficiency is different for different sized gold nanoparticles. It was found that smaller gold nanoparticles are more efficient quenchers due to their larger surface areas. The quenching mechanism was discussed. It was a dynamic quenching.
2008 Vol. 28 (02): 380-383 [Abstract] ( 1804 ) PDF (1319 KB)  ( 677 )
384 Determination of the Proteins in Serum Albumins by Synchronous Fluorescence Technique with 3-(2-Cyanoethyl) Cytosine as a Probe
CUI Feng-ling,WANG Jun-li,CUI Yan-rui,QU Gui-rong, LU Yan,FAN Jing
DOI: 10.3964/j.issn.1000-0593.2008.02.035
Under simulative biological conditions and upon the interactions between 3-(2-cyanoethyl) cytosine (CECT) and human serum albumin (HSA) or bovine serum albumin (BSA), the authors studied the characteristics of synchronous fluorescence spectra of CECT-protein system with CECT as a molecular spectral probe. The spectral characteristics and intensity of synchronous fluorescence were related to the value of Δλ, reaction medium, reaction temperature and so on. On the basis of these, the new method for the determination of proteins in serum albumin was developed with CECT as a molecular spectral probe. Under the optimum experimental conditions, the synchronous fluorescence intensities of CECT-HSA and CECT-BSA systems were in good proportion to the concentrations of HSA and BSA in the ranges of 0-441.4 and 0-351.0 μg·mL-1,respectively. The detection limits were 0.023 and 0.035 μg·mL-1,respectively. Relative standard deviations located between 12% and 3.3%, and the addition standard recovery was 97.2%-100.4% for all elements. The results suggested that the method features easy of implementation, rapidity, high sensitivity, broad linear range, and better RSD and recovery etc., and was employed directly to determine the total proteins in serum albumin samples with satisfactory results.
2008 Vol. 28 (02): 384-388 [Abstract] ( 1604 ) PDF (1597 KB)  ( 596 )
389 Fluorescence Quenching Reaction of Tetracaine Hydrochloride with Erythrosine and Their Analytical Applications
QIN Ming-you,LIU Shao-pu,LIU Zhong-fang,HU Xiao-li*
DOI: 10.3964/j.issn.1000-0593.2008.02.038
In Britton-Robinson (BR) buffer solution at pH 4.0, erythrosine(ET) reacts with tetracaine hydrochloride (TA·HCl) to form an ion association complex that quenches the fluorescence of erythrosine and has a compound ratio of 1∶1. The measurement wavelength of fluorescence quenching was located at λexem=525 nm/556 nm. The linear range for TA·HCl is from 0.28 μg·mL-1 to 4.8 μg·mL-1,and its detection limit is 0.083 μg·mL-1. The influence of coexisting substance was also inspected, and the result shows that this method has a better selectivity. Therefore, a new fluorospectrophotometry, being high sensitive, sample and rapid, was developed to determinate TA·HCl at trace amounts. The method has been applied to the determination of TA·HCl in human serum and urine samples with satisfactory results. In this study, the spectral characteristics and the optimum reaction conditions were discussed with quantum chemistry AM1 method.
2008 Vol. 28 (02): 389-393 [Abstract] ( 1611 ) PDF (1554 KB)  ( 578 )
394 Thermal Coagulation of Human Benign Prostatic Hyperplasia Tissues Induced Changes in the Absorption and Scattering Properties in Spectral Range from 590 to 1 064 nm in vitro
WEI Hua-jiang1,XING Da1*,HE Bo-hua2,WU Rong-hai3,GU Huai-min1,WU Guo-yong4,CHEN Xue-mei5
DOI: 10.3964/j.issn.1000-0593.2008.02.036
The optical properties and their differences of native and coagulated human benign prostatic hyperplasia (BPH) tissues were studied in the spectral range from 590 to 1 064 nm in vitro. The measurements were performed using a spectrophotometer with an integrating sphere attachment, and the absorption and scattering properties were assessed from these measurements using the inverse adding-doubling method. The results of measurement showed that the thermal coagulation of BPH tissues induced obviously the decrease in the absorption coefficients in the spectral range from 590 to 1 064 nm. The peaks in the absorption coefficients for native and coagulated BPH tissues were respectively 0.438 and 0.416 mm-1 corresponding to the same wavelength of 990 nm, the maximum difference in the absorption coefficients of native and coagulated BPH tissues is 86.79% at 1 064 nm, and the minimum difference is 4.74% at 920 nm. The thermal coagulation of BPH tissues induced an increase in the reduced scattering coefficients in the spectral range from 600 to 1 064 nm obviously, and induced a decrease in the reduced scattering coefficients at 590 nm obviously. The peaks in the reduced scattering coefficients for native and coagulated BPH tissues were respectively 1.090 and 1.449 mm-1 corresponding to the same wavelength of 970 nm, and other peaks in the reduced scattering coefficients for native and coagulated BPH tissues were respectively 1.116 and 1.627 mm-1 corresponding to the same wavelength of 1 050 nm, the maximum difference in the reduced scattering coefficients of native and coagulated BPH tissues is 47.73% at 1 064 nm, and the minimum difference is 4.86% at 600 nm.
2008 Vol. 28 (02): 394-398 [Abstract] ( 629 ) PDF (1196 KB)  ( 503 )
399 Study on the Interaction of Carbaryl and ctDNA by Resonance Light Scattering Spectra and Its Application
RAO Zhen-hong, LIU Shi-lu, SUN Ying*,MIN Shun-geng, ZHAO Hui-yu
DOI: 10.3964/j.issn.1000-0593.2008.02.037
Interaction modes of carbaryl and DNA were studied by resonance light scattering (RLS) spectra and absorption spectra. Experiments show that at pH 1.97, there are two interaction modes between carbaryl and ctDNA, namely surface assembly mode and intercalative mode. Interaction mode has a relation with the concentration ratio of carbaryl to ctDNA. Under this condition, the RLS intensity of carbaryl and ctDNA is proportional to the concentration of ctDNA. According to this, one new simple and rapid method of determining ctDNA was set up. The linear ranges of the concentration of ctDNA were 0.02-3 μg·mL-1,the linear regression equation was I=200.77c(μg·mL-1)+118.91, and the correlation coefficient was r=0.998 9. This method has successfully been used to determine the synthetic samples.
2008 Vol. 28 (02): 399-402 [Abstract] ( 2558 ) PDF (1375 KB)  ( 559 )
403 Linear and Nonlinear Optical Properties of Zinc Phthalocyanines
ZHEN Xiao, FENG Miao, ZHENG Chan, HUANG Juan, ZHAN Hong-bing*
DOI: 10.3964/j.issn.1000-0593.2008.02.039
Linear and nonlinear optical properties of five kinds of zinc phthalocyanines (ZnPcs) were investigated using UV-Vis absorption spectra, fluorescence spectra and Z-scan measurements. The influence of concentrations on the optical properties of zinc phthalocyanine (ZnPc) was also studied. Linear optical results show that the five investigated ZnPcs are fluorescent, while nonlinear optical results show that they are effective reverse saturable absorption materials. The concentrations have drastically influenced the linear and nonlinear optical properties of ZnPc.
2008 Vol. 28 (02): 403-406 [Abstract] ( 1770 ) PDF (1592 KB)  ( 578 )
407 Study on the Interaction of Tetra-Sulfonated Phathalocyanine Cobalt with Bovine Serum Albumin
HUANG Yan1,3,XU Guo-xing2*,PENG Yi-ru4*,WENG Jia-bao4,5
DOI: 10.3964/j.issn.1000-0593.2008.02.040
The tetra-sulfonated phathalocyanine cobalt(CoPcS4)was synthesized by using 4-sulfonic phthalic acid as raw material, CoCl2 as template agent and (NH4)2MoO4 as catalyst. CoPcS4 was demonstrated to be C4h mono-isomer by elementary analysis, IR, NMR and HLPC. Depolymerization of CoPcS4 was found in DMSO. The depolymerization increased with the pH value raising. The interaction of tetra-sulfonated phathalocyanine cobalt with bovine serum albumin (BSA) was studied by UV-Vis and fluorescence spectra. The number of binding sites and binding constant were determined at equal pace of the order of magnitude 105 L·mol-1. CoPcS4 binds with BSA at SiteⅠ and SiteⅡ. In conclusion, CoPcS4 binds with BSA commendably and albumin plays a role of storage and transport.
2008 Vol. 28 (02): 407-411 [Abstract] ( 2151 ) PDF (1637 KB)  ( 599 )
412 Spectrophotometric Determination of Deoxyribonucleic Acid by Its Quenching Effect for Acridine Orange
SI Wen-hui1,2,ZI Yan-qing3,TU Yi-feng1*
DOI: 10.3964/j.issn.1000-0593.2008.02.041
Based on the reaction of acridine orange with deoxyribonucleic acid(DNA), and under the optimized condition, a novel method to determine the DNA was developed with the spectrophotometry. The absorbance of acridine orange at the maximum absorption wavelength of 444 nm responded to the concentration of DNA negatively with excellent linearity. It has an upper linear limit concentration of 8.0 μg·mL-1 and a detection limit of 0.12 μg·mL-1 with the correlation coefficient of 0.999 8. The method is simple, rapid and sensitive, and could be applied to sample assay satisfactorily. Finally, the reaction mechanism is discussed.
2008 Vol. 28 (02): 412-414 [Abstract] ( 2693 ) PDF (1285 KB)  ( 734 )
415 Determination of Aniline in Water by Flow Injection Spectrophotometry
HUANG Jin1,2,ZHANG Xin-shen1*,YUAN Dong3,XIE Yong-hong1
DOI: 10.3964/j.issn.1000-0593.2008.02.044
A new flow injection analysis spectrophotometric method for the determination of aniline in water sample was introduced. It is based on the chromogenic-reaction of diazotization-coupling with 1-naphthol in basic media, and coupled with the flow injection analysis for the determination of aniline. The absorbance intensity was registered in this reaction solution at 495 nm. The volume of the sample loop, the length of the reacting coil and chromogenic coil, the flow rate of reagent, the reagent concentrations of H2SO4,NaNO2,NaOH and 1-naphthol, and the effect of coexistence ions were studied. The calibration graph is linear in the range of 0.005-2.0 mg·L-1. The detection limit is 0.001 mg·L-1,and the RSD was 0.7% (c=0.25 mg·L-1, n=11). The proposed method is simple, accurate, sensitive and rapid, and was successfully applied to the determination of aniline in tannery wastewater with the recoveries in the range of 98.0%-103.0%.
2008 Vol. 28 (02): 415-417 [Abstract] ( 1762 ) PDF (1034 KB)  ( 603 )
418 Determination of Physiological Indices in Albizzia Julibrissin Durazz Seedlings under Alkaline Stress with Visible Spectrophotometry
ZHOU Jian1,ZHANG Lin2,YUAN De-yi2,QI An-guo1
DOI: 10.3964/j.issn.1000-0593.2008.02.045
There is a large area of saline-alkali soil in our country, and soil alkalization is always a problem affecting urban gardening. To examine the capacity of alkaline resistance of Albizzia julibrissin Durazz seedlings, the contents of MDA, soluble sugar and proline, and the activity of POD and SOD in Albizzia julibrissin durazz tree body were measured by means of visible spectrophotometry. Also, the change patterns of the five indexes with different treatment concentration and time were analyzed. Attempts were then made to elucidate the physiological mechanism of how alkaline stress affects the growth of the Albizzia julibrissin durazz tree, which could provide theoretical foundation for planting and gardening and an approach to dealing with the difficulties in planting and gardening in saline and alkaline area. The results showed that with the increase in Na2CO3 concentration, the contents of MDA and soluble sugar in the leaves slowly ascended when the treatment concentration was lower than 75 mmol·L-1,and then rapidly increased when the treatment concentration was higher than 75 mmol·L-1; There were significant differences between different treatments. Proline content exhibited the same change pattern with MDA and soluble sugar. It slowly ascended when the treatment concentration was lower than 100 mmol·L-1,whereas it sharply increased when the treatment concentration was above 100 mmol·L-1; The changes in SOD and POD were similar, showing a unimodal pattern. However, the treatment concentration corresponding to the maximum of SOD and POD was 50 and 75 mmol·L-1,respectively. With the changes in stress time, in addition, the contents of MDA treated with the same concentration increased gradually. However, praline, soluble sugar, SOD and POD changed irregularly. These results indicated that Albizzia julibrissin Durazz could resist the alkaline stress by modulating values of physical indexes such as the contents of MDA, soluble sugar and proline and the activity of POD and SOD.
2008 Vol. 28 (02): 418-421 [Abstract] ( 552 ) PDF (1434 KB)  ( 604 )
422 Spectrum Properties of Thulium Bisphthalocyanine Langmuir-Blodgett Films
LIU Yun-long,WANG Wen-jun*,GAO Xue-xi,LI Shu-hong
DOI: 10.3964/j.issn.1000-0593.2008.02.046
The configuration state and spectral properties of sandwiched thulium bisphthalocyanine (TmPc2) molecule in Langmuir films and Langmuir-Blodgett (LB) films were investigated by using the surface pressure-area (π—A) isotherm and UV-Vis absorption spectra. The experimental results indicated that the sandwiched thulium bisphthalocyanine molecules form well-ordered stable monolayer films on the water/air interface,and the sandwiched thulium bisphthalocyanine molecules take the face to face orientation for the macrocycles and edge-on configuration in pure films, with the collapse pressure being 56 mN·m-1. But the sandwiched thulium bisphthalocyanine molecules take the face-on configuration in the sandwiched thulium bisphthalocyanine films mixed with arachidic acid (AA), and the collapse pressure is more than 60 mN·m-1. The sandwiched thulium bisphthalocyanine molecule could form well stable Langmuir films on sub-phase surface. The mixed TmPc2/arachidic acid not only could form well stable Langmuir films, but also could be transferred to solid substrate and deposited LB multilayers. In the chloroform solution and LB films of sandwiched thulium bisphthalocyanine,the UV-Vis absorption spectra have two absorption bands, namely Soret-bands and Q-bands. The electron orbit of sandwiched metal bisphthalocyanines was calculated by using absorption spectra VEH (Valence effective Hamiltonian) theory, and the electron transition orbit corresponding to the absorption peaks was analyzed. The Soret absorption band has two absorption peaks that are correlated with the electron orbital transitions of 184—187* and 178—186, and four absorption peaks of the Q absorption band are correlated with the electron orbital transitioned of 186—189*,190* and 185—187*,188*. In the LB films, the absorption peaks were red-shifted compared with those in the solution because of the interaction of molecules. The interaction of intra-layer molecules was stronger than that of interlayer molecules.
2008 Vol. 28 (02): 422-425 [Abstract] ( 636 ) PDF (1288 KB)  ( 569 )
426 Probe of the Effect of Asp44 on the Stability of Myoglobin by Circular Dichroism Spectropolarimeter
WANG Jing-yun1,LIU Dan1,TANG Qian1,2,BAO Yong-ming1,ZHENG Xue-fang2,AN Li-Jia1
DOI: 10.3964/j.issn.1000-0593.2008.02.042
To characterize the roles played by surface-charged residue Asp44 in the structure stability of horse heart myoglobin, the code of Asp44, GAT, in the gene of horse heart myoglobin was changed into AAA for Lys by PCR site-directed mutagenesis. The mutant gene was ligated into PstI/BamHI-cut pGYM and the resulting plasmid was transformed into E.coli BL21. The mutant protein(D44K) was expressed in BL21 successfully. The bacteria containing mutant myoglobin were treated with lysozyme. Then the mutant protein was purified by ammonium sulfate precipitation, ion-exchange chromatography and gel filtration. Circular dichroism spectra were employed to monitor the kinetic behaviors of wild-type and mutant myoglobins’ denaturation at different pHs or upon heating, and the “two-state” model was used to simulate the kinetic process of wild-type and mutant myoglobins’ denaturation upon heating to determine the unfolding thermodynamic parameters of Mb and its mutant(D44K). The results show that the mutation of the surface-charged residue Asp44 to Lys44 can increase the protein’s stability on its resistance to heat, resulting in the increase in the protein’s denaturing mid-temperature by about 4 ℃, from 71.9 to 75.1 ℃, but shows little effect on its resistance to acid denaturation.
2008 Vol. 28 (02): 426-429 [Abstract] ( 1957 ) PDF (1387 KB)  ( 995 )
430 Purification of Growth-Inhibitor Formed by Isochrysis Galbana
SUN Ying-ying1,WANG Chang-hai1,2*,CHEN Jing2
DOI: 10.3964/j.issn.1000-0593.2008.02.043
The objective of the present study is to isolate and purify the anti-cell bioactive fraction-cell growth-inhibitor from the old cultured liquid of Isochrysis galbana. By means of extraction with ethyl acetate, ultraviolet scan, Sephadex G-15 column chromatography, preparative thin-layer chromatography and high-performance liquid chromatography, the bioactive component was purified. The growth-inhibitor, a kind of crude ethyl acetate extract isolated from the cell-free supernatant of the old culture liquid of Isochrysis galbana, obviously inhibited the cell growth. It was showed that the growth-inhibitor existing in the old cultured liquid of Isochrysis galbana was efficiently extracted with ethyl acetate. The characteristic absorption of the growth-inhibitor was determined by ultraviolet scan and the wavelength of characteristic absorption for the growth-inhibitor was 235 nm. The residue of crude ethyl acetate extract was dissolved in diluted aqueous NaOH, and then was loaded onto Sephadex G-15 column chromatography and eluted with distilled water. Five-mL fractions were collected and monitored by UV absorption at 235 nm. The crude ethyl acetate extract was fractionated by gel filtration on Sephadex G-15 to obtain three fractions. And the three fractions inhibited the growth of Isochrysis galbana. Those active fractions were adjusted to the pH value 2-3, and extracted with ethyl acetate. And then the extracts were concentrated to the befitting volume under reduced pressure at 40 ℃, and were separated by preparative thin-layer chromatography on silica gel with chloroform. Bands visualized under UV-light (254 and 365 nm) were scraped off and extracted with ethyl acetate, and monitored as well as inhibitory activity against Isochrysis galbana. The extracts were separated into four bands on a preparative thin-layer chromatography plate with chloroform, but only the band at Rf 0.63 was active. This active fraction was finally purified by high-performance liquid chromatography on ODS with aqueous acetonitrile to produce 4 prominent peaks. The selected optimum chromatographic conditions were ZORBAX Eclipse XDB C18 with aqueous acetonitrile at a flow rate of 0.3 mL·min-1,and UV detection at 235 nm. This paper would afford very well condition for further isolation and preparation by HPLC and identification of growth-inhibitor formed by Isochrysis galbana.
2008 Vol. 28 (02): 430-435 [Abstract] ( 2194 ) PDF (1914 KB)  ( 581 )
436 Determination of the Trace Elements in Shengmai San Decoction by ICP-AES
LI Ming-fang1,2,LIU Ying-xia1,WAN Yi-qun1*
DOI: 10.3964/j.issn.1000-0593.2008.02.048
The method for the determination of the trace elements in Shengmai San by inductively coupled plasma atomic emission spectrometry(ICP-AES) was presented. The contents and solubility of the trace elements in Shengmai San with different ginseng were compared. The recovery rates of the procedure were between 95.2% and 112.4%, and the RSDs were between 0.70% and 5.9%. When the ginseng was western genseng in the Shengmai San, the solubility of trace elements was the highest. The couple of Shengmai San was proved reasonable. The method was simple,rapid,precise,convenient and suitable for traditional Chinese medicine.
2008 Vol. 28 (02): 436-440 [Abstract] ( 2560 ) PDF (1005 KB)  ( 598 )
441 Evaluation of the Uncertainty in the Determination of Arsenic in Cosmetics by ICP-AES
DAI Qi,ZHU Xiao-yu,CHEN Xiao-mei
DOI: 10.3964/j.issn.1000-0593.2008.02.047
A mathematic model for evaluating the uncertainty of the determination procedure for arsenic in cosmetics by ICP-AES was established. The uncertainty sources for each of the parameters in the model were analyzed. The uncertainties of type A (based on the calculation of the statistical distribution of the determination results) or type B (based on the estimation by experience and the probability distribution of other information) were evaluated. According to the international general method, the component uncertainties were synthesized and extended respectively to obtain the uncertainty evaluation. The results showed that the preparation of standard solutions, the fitted linear regression equation for the calibration curve and the volume of sample solution were the main sources of uncertainties.The proposed method was also suitable for application to the evaluation of the uncertainty of the results obtained by using the method of linear regressive standard curve.
2008 Vol. 28 (02): 441-443 [Abstract] ( 1660 ) PDF (1057 KB)  ( 510 )
444 Determination of Gold in Geological Sample by Inductively Coupled Plasma Mass Spectrometry after Carbon Nanofibers Separation and Preconcentration
XIAO Ming-fa,CHEN Shi-zhong*,LU Deng-bo,ZHAN Xi-lin
DOI: 10.3964/j.issn.1000-0593.2008.02.050
A novel method for the determination of Au by inductively coupled plasma mass spectrometry (ICP-MS) is described. Au can be separated and preconcentrated with a micro-column packed with carbon nanofibers as an adsorption material. The adsorption and elution behaviors of Au3+ on carbon nanofibers were systematically investigated under dynamic conditions. The experimental results showed that the studied ions can be adsorbed quantitatively at pH 2.0, and the analytes adsorbed on the column can be eluted with H2NCSNH2-HCl solution at pH 1.0. Under the optimum conditions, the detection limits for Au is 0.15 ng·mL-1,and the relative standard deviation (RSD) is 8.5% (n=6). The proposed method has been applied to the determination of trace Au in geological standard material with satisfactory results.
2008 Vol. 28 (02): 444-446 [Abstract] ( 1252 ) PDF (996 KB)  ( 559 )
447 Determination of Meconium Lead Level of Newborn by Graphite Furnace Atomic Absorption Spectrometry
LI Yan, XU Xi-jin, LIU Jun-xiao, ZHENG Liang-kai, CHEN Gang-jian, CHEN Song-jian, HUO Xia*
DOI: 10.3964/j.issn.1000-0593.2008.02.049
To establish a method for the determination of lead in meconium from 144 samples of newborn through nitric acid digestion by means of graphite furnace atomic absorption spectrometry. Methods: after being baked for at least 12 h at 60 ℃, 0.3 g of meconium was digested by nitric acid and hydrogen peroxide in turn at 80 ℃ under water-bath condition for 1h and then metered to the whole volume of to 2 mL. After correcting the background with D2 lamp, specimen basal corpuscle matched standard curve was used to detect the lead content. Results: The mean lead content of 93 experimental samples was 1.934 μg·g-1 with the standard deviation (SD) of 1.551, and that of the 51 control samples was 1.012 μg·g-1,with the SD of 1.084. There was a significant difference in lead levels of in meconnt between the experimental group and control group (p=0.000). Conclusion: The lead content of the experimental was significantly higher than that of the control group detected by this method. This method was stable and efficient.
2008 Vol. 28 (02): 447-449 [Abstract] ( 1229 ) PDF (1002 KB)  ( 543 )
450 Spectrometric Determination of Trace Elements in Tricholoma Giganteum Massee
LI Tao1,WANG Yuan-zhong2,LIU Hong-gao3*
DOI: 10.3964/j.issn.1000-0593.2008.02.052
The eight trace elements in Tricholoma giganteum Massee, including K, Ca, Na, Mg, Fe, Zn, Mn and Cu, were determined simultaneously by flame atomic absorption spectrometry. The relative standard deviation of the method is 0.1%-2.2%, and the recovery is 98.1%-106.4%. The analytical results were satisfactory. The results showed that some elements essential to human such as Zn, K, Ca, Mg and Mn in Tricholoma giganteum Massee are abundant, implying that the nutritive value of Tricholoma giganteum Massee is high.
2008 Vol. 28 (02): 450-452 [Abstract] ( 2268 ) PDF (989 KB)  ( 592 )
453 Determination of the Contents of Trace Elements in Chinese Herbal Medicines for Treating Respiratory System Diseases
HAN Li-qin, DONG Shun-fu, LIU Jian-hua
DOI: 10.3964/j.issn.1000-0593.2008.02.051
There is an intimate connection between trace elements and body healthiness, trace elements and organism depend on each other, and each trace element exists with certain proportion, which preserve physio-function. If the balance is of maladjustment, diseases may occur or develop. The trace elements were determined in 16 kinds of Chinese herbal medicines by atomic absorption spectrometry. The medicines include lilium brownii, herba houttuyniae, licorice root, radices isatidis seu baphicacanthi, Sehizandra sinensis Bail, Scutellaria baicalensis Georgi, Beimu, Polygonum multiflorum Thunb, Lithospermum officinalel, Rhizoma acori gramjnoi, Pinellia ternate Breit, Salisburia adiantifolia, Lonicera japonica, Radices puerarire, Bupleurum falcatum and Ligusticum wallichii, all of which could be bought on the market. Sixteen kinds of Chinese herbal medicines commonly used to treat respiratroy system diseases in clinic were selected, dried and powdered, completely mixed, 1.000 0 g was weighed accurately with analytical balance, and 3 portions were used for each kind of sample. The atomic absorption spectrometry was used to determine the contents of trace elements (Cu, Zn, Fe, Cr, Ni and Mn), and the content discrepancy of the trace elements in different medicines was observed the results shows that the contents of the trace elements were rich in the 16 kinds of Chinese herbal medicines, there were more contents of Fe, Zn and Mn, but they were different in different medicines. And there were more trace elements in Salisburia adiantifolia, Polygonum multiflorum Thunb, Bupleurum falcatum, Sehizandra sinensis Bail, Pinellia ternate Breit and Lithospermum officinalel, and lower trace elements in Radices puerarire, Rhizoma acori gramjnoi and Radices isatidis seu baphicacanthi. The analytic results provided useful data for using Chinese herbal medicines and provided theoretical basis for studying Chinese herbal medicines theory.
2008 Vol. 28 (02): 453-455 [Abstract] ( 228 ) PDF (934 KB)  ( 681 )
456 Determination of Trace Gold by Flame Atomic Absorption Spectrometry after Separation and Preconcentration with Load Nanometer Titanium Dioxide
LIU Zheng-hua1,ZHOU Fang-qin1*,JIANG Fang-ming2,HUANG Rong-hui1,YANG Liu1,ZHOU Le-zhou1
DOI: 10.3964/j.issn.1000-0593.2008.02.054
A new method for the determination of trace gold by flame atomic absorption spectrometry (FAAS) after preconcentration with p-dimethylaminobenzylidenerhodanine (DMABR) loaded with nanometer TiO2 was developed. The method is convenient, highly precise and linear in a wide range. Under dynamic condition, the optimum pH of solution, flow rate, elution conditions were obtained for preconcentration of trace gold. And the effect of interfering ions was also investigated. It was found that the studied gold could be quantitatively preconcentrated on loaded nanometer TiO2 at pH=3.5, and the flow rate of sample solution was 0.6 mL·min-1,and the flow rate of eluting solution with 0.1 mol·L-1 HCl-0.5 mol·L-1 thiourea was 0.5 mL·min-1,sufficient for complete elution. The dynamic adsorption capacity of gold on load nanometer TiO2 was 23.19 mg·g-1. The linear range for gold was 0-0.40 μg·mL-1,correlation coefficient was 0.999 3,detection limit(3σ, n=11) for gold was 2.34 ng·mL-1,and the relative standard deviation was 2.9% (n=6, c=0.10 μg·mL-1), the recovery was in the range of 96.7%-101.7%. The method has been applied to the determination of trace gold in water samples with satisfactory results.
2008 Vol. 28 (02): 456-459 [Abstract] ( 1879 ) PDF (1108 KB)  ( 729 )
460 Analysis and Characterization of Belamcanda Chinensis with Space Mutagenesis Breeding by X-ray Fluorescence Analysis and X-ray Diffraction
GUAN Ying, DING Xi-feng, WANG Wen-jing, GUO Xi-hua,ZHU Yan-ying
DOI: 10.3964/j.issn.1000-0593.2008.02.055
The contents of various elements in the fourth generation Belamcanda chinensis(L.)DC. with space mutagenesis breeding were analyzed and characterized. X-ray fluorescence spectrum analysis (XRF) and powder X-ray diffraction (PXRD) were applied jointly. It was found that the content of K element in the space flight mutagenesis increases 1.03 and 0.31 times, Mg enhances 1.44 and 0.06 times, but Al reduces 38.5% and 85.5% respectively compared to the contents in the ground group and the comparison group, while those of Ca, Mn and Fe enhance 0.95, 0.30 and 0.29 times respectively contrasted to the ground group. Besides, there was discovered the crystal of whewellite in the Belamcanda chinensis(L.)DC. and the content in the ground group is less than that of the outer space and the outer space group, which in turn is less than that of the comparison group. It is concluded that the contents of mineral elements indispensable to body in the space group are closer or superior to the comparison, group as compared to the ground group. In the present paper, a quick and simple appraising method is offered, which may be of great significance to the popularization of the planting outer space Chinese traditional medicine to filtrate more excellent breed and set up norm of quality appraisal.
2008 Vol. 28 (02): 460-462 [Abstract] ( 1985 ) PDF (1129 KB)  ( 649 )
463 Study on Quantificational Analysis Method for the Non-Crystalline Content in Blast Furnace Slag
YAN Ding-liu, GUO Pei-min*,QI Yuan-hong, ZHANG Chun-xia, WANG Hai-feng, DAI Xiao-tian
DOI: 10.3964/j.issn.1000-0593.2008.02.056
Quantificational analysis method for the non-crystalline and crystalline contents in blast furnace slag was studied by means of X-ray diffraction. The process of quantificational analysis method includes standard samples preparation, samples preparation, X-ray diffraction measurement and data treatment. The data treatment includes integration areas of non-crystalline curve and crystalline peaks in certain diffraction angle range, linear fitting and quantificational coefficient determination. The preparation methods of standard samples for X-ray diffraction of blast furnace slag were proposed, including 100% crystalline sample and 100% non-crystalline sample. The 100% crystalline sample can be obtained by heating blast furnace slag for 12 h at 1 000-1 200 ℃, and the 100% non-crystalline sample can be obtained by quenching the molten slag with enough water. The X-ray diffraction method of quantificational analysis of non-crystalline content in blast furnace slag was proposed with the 100% non-crystalline and 100% crystalline standard samples, and the quantificational coefficient can be obtained by linear regression on the integration areas of non-crystalline curve and crystalline peaks of X-ray diffraction in the 2-theta range 20°-40°. This method is suitable for the blast furnace slag with the non-crystalline content over 80%. The non-crystalline and crystalline contents of original blast furnace slag are obtained by combining the X-ray diffraction results and mathematical treatment, and this method is suitable for the blast furnace slag with the non-crystalline content over 90%, whose process includes preparing the 100% crystalline standard sample by heating blast furnace slag for 12 h at 1 000-1 200 ℃, samples preparation with the 0.02 interval in the 0-0.1 mass ratio range of 100% crystalline to original slag, X-ray diffraction measurement of the samples prepared and data treatment using iterative linear regression. The quantificational analysis method for blast furnace slag can be applied to various kinds of blast furnace slag from different steel plants.
2008 Vol. 28 (02): 463-467 [Abstract] ( 2237 ) PDF (1576 KB)  ( 574 )
468 Spectral Analysis of Effects of Annealing on the Characteristics of Intrinsic SnO2 Polycrystalline Thin Films
ZENG Guang-gen,ZHENG Jia-gui*,LI Bing,CHEN Qi,WU Li-li,LI Wei,ZHANG Jing-quan,LEI Zhi,CAI Ya-ping,CAI Wei,FENG Liang-huan
DOI: 10.3964/j.issn.1000-0593.2008.02.053
In order to improve the conversion efficiency of the CdTe solar cells, it is necessary to decrease the thickness of CdS layer. However, the decrease in CdS thickness may lead to adverse effects on the solar cells. Therefore, a high-resistance transparent layer (intrinsic SnO2) has been used as a buffer layer between the transparent conducting oxide (TCO) and CdS layer. In the present paper, SnO2 polycrystalline thin films were prepared by magnetic reactive sputtering. The properties of the films before and after annealing were studied by XRD and XPS. The results revealed that the films annealed at 550 ℃ for 30 minutes are polycrystalline SnO2 with a single phase of tetragonal structure and have orientation of (110) direction. XPS investigation shows that after annealing the oxygen content of the film increases, O1s peak shifts to lower energies, and SnO is oxidized into SnO2,After annealing the intrinsic SnO2 films of high-resistance as a buffer layer are very suitable for the CdTe solar cells.
2008 Vol. 28 (02): 468-471 [Abstract] ( 624 ) PDF (1617 KB)  ( 598 )
472 The Application of Adaptive Boosting Method in Automated Spectral Classification of Active Galactic Nuclei
ZHAO Mei-fang1,LUO A-li2,WU Fu-chao1,ZHAO Yong-heng2
DOI: 10.3964/j.issn.1000-0593.2008.02.057
Given a set of low-redshift spectra of active galactic nuclei, the wave bands of spectra in the rest frame were intercepted according to the different features of emission lines of broad-line AGNs and narrow-line AGNs, and an adaptive boosting (Adaboost) method was developed to carry out the classification experiments of feature fusion. As a result, the wave band of and [NⅡ] was confirmed to be the main discriminative feature between broad-line AGNs and narrow-line AGNs. Then based on the wave band of and [NⅡ], the Adaboost method was used for the spectral classification. In this method, the “weak classifiers” were increased constantly during training until a scheduled error rate or a maximum cycle times was met, then the classification judgment of the consequent collective classifier was determined by the votes of respective judgments of these “weak classifiers”. The Adaboost method needs not to adjust parameters in advance and the results of “weak classifiers” are only required to be better than random guessing, so its algorithm is very simple. As proved by the experiments, the adaboost method achieves good performance in the classification just based on the wave band of and [NⅡ] so that it could be applied effectively to the automatic classification of large amount of AGN spectra from the large-scale spetral surveys.
2008 Vol. 28 (02): 472-477 [Abstract] ( 247 ) PDF (1563 KB)  ( 550 )