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2007 Vol. 27, No. 12
Published: 2007-12-26
 
       光谱学与光谱分析
2385 Spectral Power Distribution and Quantum Yield of Sm3+-Doped Bismuth Tellurite Glass under the Excitation of Violet LED
WANG Xue-ying1,LIN Hai1*,LI Chang-min1,YANG Dian-lai1,Setsuhisa Tanabe2
A new method for measuring the spectral power distribution in Sm3+-doped bismuth tellurite glass with higher refractive index and lower phonon energy by using integrating sphere was introduced and designed for the first time. Fluorescence measurement system was constituted by integrating sphere of 10-inch diameter, which was connected to a DDC detector. A standard halogen lamp was used to calibrate the measurement system and the auxiliary standard halogen lamp was employed for collating inner change in integrating sphere. The total radiant flux, total luminous flux and total quantum yield were calculated by luminous flux distribution and photon distribution, which were derived from spectral power distribution, and the values were 55 μW, 0.02 lm and 4.07%, respectively. In the present paper, the integrating sphere-method was applied to measure the luminescence parameters of the multichannel transition emissions in Sm3+,and it was considered as an accurate way to characterize luminescence parameters for luminescence and laser material.
2007 Vol. 27 (12): 2385-2388 [Abstract] ( 2534 ) PDF (1061 KB)  ( 511 )
2389 Spectral Characteristics of Optical Storage Material CaS∶Eu, Sm
JIANG Wei-wei1,XU Zheng1,ZHANG Xi-yan2
As a typical optical storage material, CaS∶Eu, Sm powders were prepared by wet method in a reduced atmosphere. XRD，emission spectrum, excitation spectrum, photostimulated spectrum, thermal spectrum, and decay curve were measured. The XRD indicates that the lattice of CaS∶Eu, Sm was formed at 1 050 ℃. Spectra analysis results show that UV can excite the sample as an information input source. When excited by ultraviolet lamp and then stimulated by 980 nm laser, the same luminescence with peaks at 635 nm. The photostimulated emission decayed rapidly at first and then slowly. The trap level is deep and can make electrons stable in the trap. The optical storage mechanism of CaS∶Eu, Sm is discussed.
2007 Vol. 27 (12): 2389-2392 [Abstract] ( 98 ) PDF (1136 KB)  ( 458 )
2393 Mixing and Quenching of Rb 5PJ States Induced by Collisions with He Atoms and N2 Molecules
MENG Fan-xin1,2,QIN Chen1,DAI Kang1,SHEN Yi-fan1*
The collisional energy transfer process Rb(5PJ)+M, where M=He, N2,under gas cell conditions has been investigated. The Rb(5P3/2) state was excited by a diode laser. The direct 5P3/2→5S1/2 fluorescence and the sensitized 5P1/2→5S1/2 fluorescence as a function of quenching gas pressure were measured. The 5P3/2 and 5P1/2 states are separated by 238 cm-1. The closest other states are >6 500 cm-1 or >28 KT. Neglect of these other states should be an excellent approximation. In the experiment the Rb density was 4.5×1011cm-3. Using radiation trapping theory the effective radiative rate=Γe5P3/2→5S1/2 2.47×107 s-1 was obtained. For quenching by He only electronic to translational energy transfer is possible. However, in the N2 case, electronic to vibrational or rotational transfer is important. The Rb(5P3/2) state is 13 cm-1 lower than the N2[X′Σ+g(V=5, J=11)]state; this energy gap is near resonant. The authors have not attempted to directly observe this possible E-R quenching channel. Using a two-state rate equation model the transfer rate coefficients from Rb(5PJ) were obtained. The rate coefficient (kHe21) for 5P3/2→5P1/2 transfer in collision with He is 2.61×10-12 cm3·s-1. By comparing the direct and sensitized fluorescence intensities for He and N2 case, and fitting the experimental results to the rate equation analysis, the authors estimate that the rate coefficient (kN221) for 5P3/2→5P1/2 transfer in collision with N2 is 2.36×10-11 cm3·s-1. The E-V quenching rate coefficient (kN2) of the 5PJ state is 1.44×10-11 cm3·s-1. The authors found find that the rate coefficient kＮ２ is about 6 times larger than the kN221. The assumption that the Cs-N2 energy transfer occurs primarily in collinear collision geometry is supported. The results are discussed in relation to those of other experiments.
2007 Vol. 27 (12): 2393-2395 [Abstract] ( 456 ) PDF (487 KB)  ( 516 )
2396 Spectrum Studies of Ignition Characteristic in Quick Reaction of Benzene
WU Jin-he1,2,YAN Zheng-xin1,2,YE Song1,HU Dong2,YANG Xiang-dong1*
A new optical spectroscopy system consisting of a monochromator, photomultiplier tubes (PMT), piezoelectric pressure sensor and digital phosphor oscilloscope was established to study spectrum and ignition delay time of benzene in quick reaction in a high temperature shock tube. A new method of determining ignition delay time of energetic materials behind incident shock wave is proposed. Several important products, such as H, C2 and CH, were determined in sequence of emergence time. The reaction mechanism of formation of carbon was introduced when benzene was driven under shock compression. The results indicate that in spite of the variety of Mach number, atom H always emerged first, indicating that the pyrolysis of benzene started with C—H bond instead of C—C bond. The results show that applying spectrum techniques can preferably study the ignition characteristic of benzene in quick reaction. Measuring ignition delay time by means of a prior emerged intermediate product (atom H) is more accurate than that with white color technique widely used home and abroad, and furthermore, can obviously reduce the times of experiment.
2007 Vol. 27 (12): 2396-2398 [Abstract] ( 1575 ) PDF (532 KB)  ( 521 )
2399 Synthesis and Characterization of Broadband IR-to-Visible Upconversion Material CaS∶Ce, Sm by Low-Temperature Combustion Synthesis Method
ZHANG Xi-yan,LU Li-ping,BAI Zhao-hui,WANG Xiao-chun,LIU Quan-sheng,MI Xiao-yun
Broadband IR-to-visible upconversion material CaS∶Ce, Sm was synthesized for the first time by the low-temperature combustion synthesis (LCS) method. The effect of the rare earth dopant concentration on the upconversion properties was studied. XRD analysis shows that the sample features the cubic CaS crystal structure. The excitation spectrum of the sample is in the range of 200-500 nm, i.e. ultraviolet light or the visible light can excite the sample effectively to complete the “charged” process, and the excitation effect of the visible light is dominant. The IR sensitivity spectrum of the sample is in the range of 800-1 400 nm, indicating that CaS∶Ce, Sm possesses the broadband IR-to-visible upconversion effect. The IR-to-visible upconversion spectrum of the sample is a broadband spectrum in the range of 450-650 nm, with two adjacent emission peaks at 513.4 and 572 nm, resulting from the transitions of Ce3+ 2T2g(5d)→2F5/2(4f) and the transitions of Ce3+ 2T2g(5d)→2F7/2(4f), respectively.
2007 Vol. 27 (12): 2399-2402 [Abstract] ( 1444 ) PDF (949 KB)  ( 529 )
2403 Measurement and Analysis of Discharge Current in Dielectric Barrier Glow Discharge at Atmospheric Pressure
LI Xue-chen1,YIN Zeng-qian2,PANG Xue-xia1,LI Yong-hui1,GAO Rui-ling1
Dielectric barrier discharge has become a hot issue in low temperature plasma research field because of wide prospect for its application in industry. In the present paper, an uniform glow discharge was realized in atmospheric pressure helium with a parallel planar dielectric barrier discharge device and an uniform plasma was generated in helium at atmospheric pressure. Electrical method was used to separate the discharge current from the total current signal and the waveform of discharge current could be obtained. The relations among the discharge current, applied voltage, gap voltage and wall charge during the uniform glow discharge were used to analyze the dynamical behavior of wall charges during their accumulation. The results show that the wall charges were mainly accumulated during the existence of discharge current pulse, while the quantity of wall charges continued to increase until the gap voltage changed its polarity after the disappearance of discharge current pulse, and finally the quantity of wall charges decreased until the next breakdown. These experimental results are important for the further study of wall charges’ effect in the dielectric barrier glow discharge and its application in industry.
2007 Vol. 27 (12): 2403-2405 [Abstract] ( 541 ) PDF (828 KB)  ( 455 )
2406 Measurement of N+2 Rotational Temperature in Air Dielectric Barrier Discharge
DONG Li-fang, LI Yong-hui, CHEN Wen-jun,LI Xue-chen
The rotational lines of the first negative band system of N+2 were observed in air dielectric barrier discharge by using liquid electrodes. The rotational temperature was estimated by the J number of the lines with the maximum intensity in rotational spectrum. The rotational temperature was kept at a constant with increasing the applied voltage when the gas pressure was in the range of 10.133-60.795 kPa. The results are of great importance to the model foundation and the application of dielectric barrier discharge in air.
2007 Vol. 27 (12): 2406-2408 [Abstract] ( 556 ) PDF (616 KB)  ( 526 )
2409 Luminescence Characteristics of Terbium-Doped Nanocrystalline Zinc Oxide
SONG Guo-li
It is known that zinc oxide is a kind of important functional and novel material of Ⅱ-Ⅵ wide bandgap semiconductor(Eg=3.37 eV), and has excellent microstructural, chemical and physical properties. The intensity of photoluminescence, luminescence peak positions and other kinds of luminescence properties of ZnO∶RE3+ nanocrystalline are strongly dependent on the annealing temperature and time, and the concentration of the doping rare earth ions. Terbium-doped zinc oxide nanocrystalline were successfully prepared by sol-gel process at different annealing temperature. Photoluminescence spectrum (PL), photoluminescence spectrum excitation(PLE) and X-ray diffraction pattern(XRD) of nanocrystalline ZnO∶Tb3+ with excitation wavelength 368 nm were measured at room temperature. The emission from 5D4→7F6(485 nm), 5D4→7F5(544 nm), 5D4→7F4(584 nm) and 5D4→7F3(620 nm) of Tb3+ ions, and the wide visible band of ZnO were observed. Photoluminescence intensity of nanocrystalline ZnO∶Tb3+ on the doping concentration and annealing temperature was given, and it was found that the optimal dopant concentration and annealing temperature were 4 at% and 600 ℃, respectively. The luminescence process of Tb3+-doped zinc oxide nanocrystalline was investigated by using PL and XRD. The photoluminescence mechanism suggests that there is energy transfer between ZnO nanocrystalline hosts and the doping Tb3+ centers.
2007 Vol. 27 (12): 2409-2412 [Abstract] ( 1256 ) PDF (835 KB)  ( 526 )
2413 Thermal Decomposition of 2-H-Heptafluoropropane at Different Temperatures
HU Yong-hua,LI Shu-fen*
The thermal decomposition processes of 2-H-heptafluoropropane were investigated during a 30 second reaction time and at temperatures of 400, 500, 600, 700 and 800 ℃ using fast pyrolysis method and Fourier transform infrared spectra (FTIR) and gas chromatography/mass spectrometry (GC/MS) analytical techniques. The results indicate that the reaction temperatures have the obvious effects on the thermal decomposition of 2-H-heptafluoropropane. The 2-H-heptafluoropropane is steady at first three temperatures, whereas starts to obviously decompose at 700 ℃ and undergoes intense decomposition at 800 ℃. At the same time, coke formation was observed on the surface of the reactor at 800 ℃. Moreover, three cyclocompounds, 1,2-bis(trifluoromethyl)perfluoroindane, perfluoro(1-ethylideneindane) and octafluoronaphthalene, were for the first time discovered in the products of thermal decomposition at 800 ℃. This demonstrates that 2-H-heptafluoropropane experiences not only simple decomposition, but also cyclization and the polymerization reactions under high temperature thermal decomposition conditions.
2007 Vol. 27 (12): 2413-2416 [Abstract] ( 1187 ) PDF (1248 KB)  ( 485 )
2417 Effects of Thermostress on the Plasma Membrane Permeability of Desert Moss Tortula desertorum Examined by In-Situ Micro-FTIR Analysis
XU Shu-jun1,CHEN Wei-hong2,CHEN Ying-wen1,HE Ming3,WANG Yan1*
A technique based on Fourier transform infrared microscope (FT-IRM) was developed to detect the corresponding changes in chemical composition associated with thermostress among aging tissues of the desert moss Tortula desertorum. The results indicated that wild leaves could accelerate the rate of carbohydrate synthesis and decrease the permeability of plasma membrane during heating at 45 ℃ for 1 h. Those biological responses can alleviate the damage of heat stress, so called thermotolerance. And the ability has a positive relation to the leaf age among various wild leaves. However, the secondary protonema and leaves, cultivated in artificial incubator, were unable to adapt the change of temperature immediately and the permeability of cellular membranes was increased.
2007 Vol. 27 (12): 2417-2421 [Abstract] ( 2209 ) PDF (1445 KB)  ( 475 )
2422 FTIR Spectroscopic Explorations of Freshly Resected Thyroid Malignant Tissues
ZENG Xiang-tai1,3,XU Yi-zhuang2,ZHANG Xiao-qing1,XU Zhi1,ZHANG Yuan-fu2 , WU Jin-guang2,ZHOU Xiao-si1,LING Xiao-feng1*
In the present paper, 17 cases of freshly resected malignant thyroid tissue samples and 23 cases of benign thyroid tissue samples were characterized using FTIR spectroscopy with an ATR probe. Statistic analysis indicated that the FTIR spectra of cancerous tissue were significantly different from those of benign tissue. In comparison with normal tissues, the FTIR spectra of malignant thyroid tissues possess the following features: (1) Variation of bands related to protein: Amide Ⅰ band shifted to lower wave number significantly (P<0.01), while amide Ⅱ band shifted to higher wave number(P<0.05), and the ratios of I1 640/I1 460 and I1 640/I1 550 were raised(P<0.01). The authors can conclude that the amounts and the secondary structure of protein in malignant tissue changed. (2)The peaks at 2 955, 2 920, 2 870, 2 850 and 1740 cm-1 appeared less frequently suggesting that the relative quantity of lipid in malignant tissue decreased significantly; (3) Variation of bands related to nucleic acid: The band of 1 241 cm-1shifted to (1 238.29±2.87)cm-1,and the ratios of I1 080/I1 460 were raised significantly(P<0.05). The most possible reason for the changes was that the mutation of DNA and the amounts of nucleic acid had increased in malignant neoplasms. Experimental results show that the malignant thyroid tissues can be distinguished from the benign tissues by their infrared spectra. This approach proves that FTIR spectroscopy is a reliable and practicable method for thyroid cancer diagnosis in operations. The authors have expanded their research on detecting the thyroid cancer FTIR spectra via percutaneous and in vivo, and have achieved a positive result which is going to be reported in another paper.
2007 Vol. 27 (12): 2422-2426 [Abstract] ( 2231 ) PDF (796 KB)  ( 499 )
2427 Application of Fourier Transform Infrared Spectroscopy to Non-Invasive Detection of Pleomorphic Adenoma of Salivary Gland in vivo
WANG Bing-bing1,2,PAN Qing-hua2,ZHANG Yuan-fu2,XU Yi-zhuang2*,WU Qi-guang3,ZHOU Feng-shan1, YU Guang-yan3,SUN Kai-hua3,PENG Xin3,WU Jin-guang2
In the present work, 20 patients with salivary pleomorphic adenoma were recruited for FTIR spectroscopic measurement. These obtained FTIR spectra were analyzed and compared. It was found that there were significant differences in the spectral features of the skin covering normal salivary gland, pleomorphic adenoma, and carcinoma change of pleomorphic adenoma，such as the changes in peak position, band shape and relative intensity of the bands in the ranges of 1 000-1 800 cm-1 and 2 800-3 000 cm-1. Pathological diagnosis demonstrated that 2 of the 20 patients suffered actually carcinoma change of pleomorphic adenoma, which is in good agreement with the result of FTIR spectroscopic measurement. FTIR spectroscopic method suggested that pleomorphic adenoma is the intermediate between normal salivary gland and carcinoma change of pleomorphic adenoma.
2007 Vol. 27 (12): 2427-2431 [Abstract] ( 1769 ) PDF (1147 KB)  ( 512 )
2432 The First and Second Cluster Analysis of Dual Index Grade Sequence of IR Fingerprint Spectra of Guifudihuang Pill and Jinkuishenqi Pill Samples and Their Quality Evaluation
ZOU Hua-bin1,HAN Zhi-feng1,ZHAI Hong2,WEI Ying-qin3,WANG Fei1
In the present paper a method for identifying and evaluating traditional Chinese medicine(TCM) Jinkuishenqi pill and Guifudihuang pill samples is proposed. Mathematical statistics was applied to analyze the dual index sequences of infrared fingerprint spectra of components extracted from Jinkuishenqi pill and Guifudihuang pill samples with water, then the grade sequences were determined and the first and second clusters were performed based on these grade sequences. As a results, the most similar sample groups of different samples were also obtained. The Jinkuishenqi pill and Guifudihuang pill samples can be distinguished accurately with the most similar sample groups. The method put forward is new and effective to identify and evaluate combinational TCM quantitatively.
2007 Vol. 27 (12): 2432-2436 [Abstract] ( 1510 ) PDF (712 KB)  ( 595 )
2437 Recognition of Plant Parts of Tobaccos Based on Infrared and Near Infrared Spectra
ZHANG Xin,GUO Jia,NI Li-jun*,ZHANG Li-guo
In the present paper, an IR/NIR spectrometry based on the pattern recognition using Mahalanobis distance method in the principal component analysis (PCA) space was established for the discrimination of plant parts of tobaccos. Effects of the type of IR/NIR spectrometers, calibration region of the spectra, model parameters and pretreatment of the spectra on the accuracy of discrimination were investigated using tobaccos cultivated in Yunan Province in 2003 and 2005 as case study. The recognition model shows the internal relationships between the information of spectra and the plant parts of tobaccos. The results indicate that both IR and NIR could be successfully used to recognize plant parts of the tobaccos, but the latter was better because it involves more sample information. It was found that the highest recognition accuracy, 94.11%, was obtained by using apparatus A with the second derivative spectra, while recognition accuracy of 88.24% and 82.35% was respectively given by apparatus B with with the first derivative SNV spectra and IR spectrometer with first derivative spectra. For the same spectrometer, the optimal calibration region and principal component number were changed with samples and the spectral pretreatment method.
2007 Vol. 27 (12): 2437-2440 [Abstract] ( 512 ) PDF (869 KB)  ( 498 )
2441 Preliminary Study on Identification of Heroin from Different Route with Clustering Analysis by Fourier Transform Infrared Spectroscopy
CAI Xi-lan,WU Guo-ping
In the present paper, using Fourier transform infrared (FTIR) absorption spectrometry, the characteristic peaks of fingerprint infrared spectra of heroin samples from different routes were identified with clustering analysis successfully. It is a very fast, simple and reliable method. That is to say, a new method for the discrimination of heroin seizured from different routes is provided.
2007 Vol. 27 (12): 2441-2444 [Abstract] ( 1100 ) PDF (1070 KB)  ( 481 )
2445 Study on Quantitative Analysis of Cross Linked Copolymer by IR
SHAO Qiong-fang1,2,DONG Ming1,CHEN Shuai-hua2,WEI Chao2,XIE Xiao-hong2
Cross linked copolymer silicon oil-Co-lactide(Si-co-LA) was analyzed quantitatively by IR. Potassium sulfocyanate(KSCN) was chosen as an inside mark material, because it has only one strong absorption peak at 2 100 cm-1 and the peak was chosen as its quantitative peak. The peak at 1 750 cm-1 is the characteristic absorption of carbonyl and was chosen as the quantitative peak of lactide(LA). The ratio of the two absorbencies is I, and I=ALA/AKSCN. KSCN and LA were mixed according to a certain mass ratio C=MLA/MKSCN to prepare standard samples. The curve of C versus I is the quantitative work curve. The result of the experiment indicates that the work curve has good linearity in the range of 2/5＜MLA/MKSCN＜8/5. The formulas calculating the proportion of every component in the cross linked copolymer were established: MKSC/Mp=B，MLA/MKSCN=C, and (MLA/Mp)×100%=BC×100%. Cross Linked Copolymer is hard to be analyzed quantitatively, because of its no dissolving and no melting. A convenient method of determining the component of the cross linked copolymer or other copolymer has been provided.
2007 Vol. 27 (12): 2445-2447 [Abstract] ( 1881 ) PDF (536 KB)  ( 491 )
2448 FTIR and XRD Analysis of Hydroxyapatite from Fossil Human and Animal Teeth in Jinsha Relict, Chengdu
HUANG Cheng-min1,ZHANG Qing2,BAI Song1,WANG Cheng-shan3*
Diagenetic effect during burial on the hydroxyapatite in enamel and dentin from fossil human and animal teeth was examined, using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). For the enamel and dentin of all fossil teeth, XRD patterns exhibit bulge line and overlap between major reflections of hydroxyapatite, and the crystallinity of hydroxyapatite is low. For each infrared spectrum, H2O and OH- have distinct peaks of absorbance, and PO3-4and CO2-3 ions have intensive infrared vibration modes at the fundamental wave numbers. The component of hydroxyapatite of all fossil teeth is similar to the modern biological hydroxyapatite. Furthermore, the index (PCI) which reflects the hydroxyapatite crystallinity of each sample ranges from 2.4 to 4.0 while the index (BPI) reflecting the amount of type B carbonate to phosphate indicates that the values of CO2-3 content in hydroxyapatite are rather high, accordingly the crystallinity of all fossil hydroxyapatites are poor. It could be concluded that little alteration of hydroxyapatites from fossil human and animal teeth occurred in the process of diagenesis in Jinsha Relict, Chengdu, China.
2007 Vol. 27 (12): 2448-2452 [Abstract] ( 2488 ) PDF (549 KB)  ( 528 )
2453 Identification of Pericarpium Citri Reticulatae from Different Regions Using FTIR
ZHOU Xin1,SUN Su-qin2,HUANG Qing-hua1*
The essential oil of Pericarpium Citri Reticulatae from seven different regions were identified by Fourier transform infrared spectroscopy (FTIR) in the present paper. The result indicated that it’s easy to find a fingerprint character of 2-methyaminomethyester benzoic acid in the FTIR spectra of essential oil of the Pericarpium Citri Reticulataes collected from Guangdong and Guangxi, but it can’t be seen in the FTIR spectra of the samples from other regions, and especially, there is a obvious difference between Xinhui and non-Xinhui regions at 1 690 and 1 644 cm-1 in the FTIR spectra. Therefore, the simple, fast and accurate property of FTIR is a good foundation for the identification of Pericarpium Citri Reticulatae using its fingerprint character.
2007 Vol. 27 (12): 2453-2455 [Abstract] ( 1114 ) PDF (715 KB)  ( 560 )
2456 Study on the Multicomponent Quantitative Analysis Using Near Infrared Spectroscopy Based on Building Elman Model
LIU Bo-ping1,2,QIN Hua-jun3,LUO Xiang2,CAO Shu-wen3,WANG Jun-de1*
The present paper introduces an application of near infrared spectroscopy(NIRS) multi-component quantitative analysis by building a kind of recurrent network(Elman)model. Elman prediction model for phenylalanine(Phe), lysine(Lys), tyrosine(Tyr) and cystine(Cys) in 45 feedstuff samples was established with good veracity. Twelve peak value data from 3 principal components straight forward compressed from the original data by PLS were taken as inputs of Elman, while 4 predictive targets as outputs. Forty seven nerve cells were taken as hidden nodes with the lowest error compared with taking 43 and 45 nerve cells. Its training iteration times was supposed to be 1 000. Predictive correlation coefficients by the model are 0.960, 0.981, 0.979 and 0.952. The results show that Elman using in NIRS is a rapid, effective means for measuring Phe, Lys, Tyr and Cys in feedstuff powder, and can also be used in quantitative analysis of other samples.
2007 Vol. 27 (12): 2456-2459 [Abstract] ( 1115 ) PDF (697 KB)  ( 542 )
2460 Application of PCA-SVR to NIR Prediction Model for Tobacco Chemical Composition
LIU Xu1,2,CHEN Hua-cai3*,LIU Tai-ang4,LI Yin-ling4,LU Zhi-rong4,LU Wen-cong1,2
Near infrared diffuse reflectance spectra of 50 tobacco samples were pretreated with PCA. The calibration models of determination of the main components in tobacco were developed with support vector regression (SVR). The models were tested with leave-one-out (LOOCV) method and optimized with parameters of kernel function, penalty coefficient C and insensitive loss function. The root mean square errors (RMSE) with leave-one-out cross validation of the optimal models of nicotine, and total sugars, reductive sugar, and total nitrogen were 0.313, 1.581, 1.412 and 0.117 respectively. Based on the comparison of RMSE of the SVM model with those of the partial least square (PLS), multiplicative linear regression (MLR) and back propagation artificial neuron network (BP-ANN) models, it was found that the SVR model was the most robust one. This study suggested that it is feasible to rapidly determine the main components concentrations by near infrared spectroscopy method based on SVR.
2007 Vol. 27 (12): 2460-2463 [Abstract] ( 1817 ) PDF (869 KB)  ( 530 )
2464 High Temperature Raman Spectroscopy Techniques and Its Applications
CHEN Hui,JIANG Guo-chang*,YOU Jing-lin,WU Yong-quan
Based on the frequency and time domain characters of heat radiation, high temperature Raman spectroscopy techniques were aralyzed and summarized. Thereby, two high temperature Raman systems were set up. One is an accumulated time-resolved macro-Raman spectroscopy system, and the other is an accumulated time-resolved and confocal coupled micro-Raman spectroscopy system. Finally, their applications in the study of high temperature processes such as melt structure and phase transformation, crystallization as well as samples with high fluorescence were intrtoduced.
2007 Vol. 27 (12): 2464-2467 [Abstract] ( 1131 ) PDF (995 KB)  ( 528 )
2468 Raman Spectra of Fossil Dinosaurs from Different Regions
YANG Qun,WANG Yi-lin
Raman microscopic spectra in the higher wave number region were obtained from 7 fossil dinosaurs specimens from different regions. The specimens of fossil dinosaurs are different parts of bone. The Raman spectra of fossil dinosaurs indicate the high similarity among peak positions of different fossil dinosaurs; but important differences exist in the spectral peak figures. In the wave number region of 1 000-1 800 cm-1 the Raman spectra of the same bone part fossils from different regions are very similar, example similarities between spectra of Lufeing backbone head and Yua nmou backbone head; Lufeng limb bone and Wuding limb bone. There are relations between the same bone part spectra of different fossil dinosaurs. The characteristic does not relate to regions. Raman spectra of fossil dinosaurs cannot be used to distinguish fossil source, although the part of bone can be used as an indicator to narrow the range of possible geographical origins.
2007 Vol. 27 (12): 2468-2471 [Abstract] ( 2337 ) PDF (903 KB)  ( 452 )
2472 Raman Scattering Studies on 0.5PZN-0.5PZT Piezoceramics
CHANG Li-min,HOU Yu-dong*,ZHU Man-kang,YAN Hui
PZT based multi-system has shown super piezoelectric properties when the composition was located at morphotropic phase boundary (MPB), which divided the regions into rhombohedral and tetragonal structures equally. In the present paper, the diffuse phase transition and phase coexistence of rhombohedral and tetragonal phases of 0.5PZN-0.5PZT ceramics were investigated by Raman scattering spectroscopy in detail. The results revealed that compared with pure PZT, the width of Raman bands of 0.5PZN-0.5PZT was quite broad, indicating that the system has strong relaxor feature. According to the temperature dependence of dielectric permittivity, the indicator of degree of diffuseness, γ, was calculated and the values were as high as 1.71. Through the separation by Gauss fitting of the Raman bands, the intensities of different Raman vibration modes, such as the tetragonal E(3TO), A1(3TO), E(4LO) and A1(3LO) modes, as well as the rhombohedral R1 and Rh modes, were determined. The results indicated that for 0.5PZN-0.5PZT system, the fraction of rhombohedral phase was equal to the tetragonal phase, which has also been affirmed by XRD results and suggested that the system was close to the MPB. Excellent piezoelectric properties, such as kp (0.66) and d33 (425 pC/N), were found in 0.5PZN-0.5PZT system, showing a great promise of this system as practical materials for piezoelectric actuators.
2007 Vol. 27 (12): 2472-2474 [Abstract] ( 2026 ) PDF (832 KB)  ( 538 )
2475 Using Hyperspectral Derivative Index to Monitor Winter Wheat Disease
JIANG Jin-bao1,2,CHEN Yun-hao1*,HUANG Wen-jiang3
The canopy reflectance of winter wheat that infected different severity stripe rust was measured through artificial inoculation, the disease index (DI) of the wheat corresponding to the spectra was acquired in the field, and the parameters of biochemistry and biophysics were measured indoors. The 1st derivatives were analyzed. The results show that the 1st derivative values increase at the green edge (500-560 nm), while decrease at the red edge (680-760 nm) with DI increasing. The ratio of the sum of derivatives within the red edge (SDr′) to the sum of derivatives within the green edge (SDg′) has a higher negative linear correlation with DI, with a coefficient of determination r2=0.921 0(n=28), and that can be use to identify the healthy and disease crops 12 days before symptoms appearing. Therefore, the derivative vegetation index SDr/SDg can be used to monitor crops disease information. The conclusion is significant and may find application in acquiring crops disease information using hyperspectral remote sensing, and has a important meaning for increasing yields of crops and ensuring security of food supplies.
2007 Vol. 27 (12): 2475-2479 [Abstract] ( 241 ) PDF (1037 KB)  ( 655 )
2480 Study on the Spectrum of the Flocculent Conformation of Polymer Ferric Sulfate Flocculants
ZHENG Huai-li1, 2,PENG De-jun1,HUANG Xiao-hong1,LIU Hong1
In the present paper，the flocculent conformation and qualities of polymer ferric sulfate flocculants were studied by the ultraviolet-visible spectrum. The spectra of polymer ferric sulfate flocculants at different pH values, the microcosmic flocculent conformation of polymer ferric sulfate flocculants corresponding to some peaks in the spectrum, the reaction mechanism and the effects of different pH value on turbidity and colour removal and described. The absorbance of peaks in the wavelength range of 200-1 100 nm all increased with pH value rising from 1.0 to 2.5. The absorbance of peaks in the wavelength range mentioned above did not continuously increased with pH value rising above 2.5, and some of them are even decreased apparently. The flocculent effects of turbidity and colour removal on stimulant waste water is optimum at pH 2.0. When pH value is in the range of 1.5 to 2.0 and 2.0 to 2.3, the flocculent effects are also better. However, the flocculent effect is decreased apparently when pH value is over 2.5. The change in the spectral curve of the different pH polymer ferric sulfate flocculants is corresponding to the flocculent effects of turbidity and colour removal on stimulant waste water to some extent. The research method has potential application prospect for the better flocculation conformation analysis and identification of the polymer ferric flocculants. And it can provide some easy and actable methods for the flocculation conformation analysis and identification of high polymer ferric flocculants.
2007 Vol. 27 (12): 2480-2484 [Abstract] ( 1548 ) PDF (1148 KB)  ( 558 )
2485 Spectroscopy Study on the Interaction of Colchicine and Human Serum Albumin
MA Jun-yan1,CHEN Ke-hai1,ZHENG Xue-fang1,2*,GUO Ming2,MA Jing1,TANG Qian1,WANG Yu-lian1, HU Jie-han2,3
The binding reaction of colchicine with human serum albumin(HSA) was studied by UV-Vis absorption, fluorescence and circular dichroism spectrometry. The results indicated that colchicine led to the increase in UV absorption and the quenching of intrinsic fluorescence of HSA. As the temperature increased, the quenching constant KSV decreased. The binding constants and the numbers of the binding sites of the interaction between colchicine and HSA at different temperatures were obtained. The thermodynamic parameters, enthalpy change (ΔH) and entropy change (ΔS), were calculated to be -11.66 kJ·mol-１ and 51.507 J(mol·K)-１ respectively according to Van’t Hoff equation, which suggested that the main binding force between colchicine and HSA was static interaction. The protein conformation was altered(CD date) with decreasing of α-helices in the presence of colchicine. The results showed that the quenching mechanism of the combination of colchicine with human serum albumin was a static quenching procedure.
2007 Vol. 27 (12): 2485-2489 [Abstract] ( 1689 ) PDF (1004 KB)  ( 595 )
2490 Spectrometric Study on the Interaction of Doxepin Hydrochloride and Fast Green and Its Application
WU Cheng-ke,FENG Su-ling*,FAN Jing
The characteristics of resonance light scattering and absorption spectra of doxepin hydrochloride with fast green were investigated, and a new analytical method for doxepin hydrochloride was described. In the buffer solution of pH 4.0, doxepin hydrochloride can strengthen the signal of resonance light scattering of fast green. The effective factors, including the order of addition of the reagents, acidity and kinds of the buffers, and concentration of fast green were investigated. Under the optimum conditions, the scattering peaks of the system are at 344 and 486 nm，while the maximum is at 344 nm. The enhanced intensity of RLS is proportional to the concentration of doxepin hydrochloried in the range of 8.75×10-3-4.88×10-2 mg·mL-1. The detection limit for doxepin hydrochloried is 1.72×10-5 mg·mL-1. The relative standard deviation obtained from eleven determinations for a 0.025 mg·mL-1 standard solution of doxepin hydrochloried is 1.4%. The method was applied to the determination of doxepin hydrochloric in pharmaceutical preparations. The results were compared with those obtained by the reference method, and t-test showed no significant difference between the two methods.
2007 Vol. 27 (12): 2490-2493 [Abstract] ( 2128 ) PDF (794 KB)  ( 454 )
2494 Study of LCD Tricolor Spectrum Characteristic
HUANG Chong1,JIANG Yan-sen1,OUYANG Yan-dong1,WU Yong-jun2
The electro-optical characteristic of TB3639 liquid crystal light valve under both voltage-drive and frequency-drive modes was measured using spectrophotometer, and the change in tricolor transmissivity with the two methods was analyzed. The result shows that the changes in tricolor transmissivity with these two methods are not identical, and color cast will appear, which will influence display quality. The change in tricolor transmissivity becomes more obvious with the changes in voltage in voltage-drive mode, in which the maximum difference is 11% and the minimum is 0. The change in tricolor transmissivity has better uniformity in frequency-drive mode and the difference of transmissivity is relatively small with the maximum difference of 4% and the minimum of 2.5. The color should be adjusted and compensated in order to get exact hue and color saturation, and this will help to study further for improving the performance of liquid crystal display.
2007 Vol. 27 (12): 2494-2497 [Abstract] ( 1599 ) PDF (1006 KB)  ( 520 )
2498 Study on the Interaction between Fangchinoline and Bovine Serum Albumin
WU Qiu-hua,WANG Chun,WANG Zhi*,MA Jing-jun,ZANG Xiao-huan,QIN Na-xin
The binding reaction of fangchinoline with bovine serum albumin was studied at different temperatures by fluorescence quenching spectra, synchronous fluorescence spectra and ultra-violet spectra. It was shown that fangchinoline has a strong ability of quenching the fluorescence of BSA. The Stern-Volmer curve of the fluorescence quenching of BSA by fangchinoline indicated that the quenching mechanism of fangchinoline to BSA was a static quenching. According to the Frster theory of non-radiation energy transfer, the binding distances (r) at different temperature were 2.51 nm (27 ℃), 2.72 nm (37 ℃) and 2.89 nm (47 ℃), respectively, while the binding constants (KA) were 1.05×105 L·mol-1 (27 ℃), 3.31×105 L·mol-1 (37 ℃), and 7.24×105 L·mol-1 (47 ℃), respectively. The thermodynamic parameters showed that the interaction of fangchinoline and BSA was mainly driven by hydrophobic force. Synchronous spectrum was used to investigate the conformational changes of BSA.
2007 Vol. 27 (12): 2498-2501 [Abstract] ( 1228 ) PDF (731 KB)  ( 603 )
2502 Preparation and Study on the Spectra of Conductive Nano-Silver Film
MO Li-xin1,LI Lu-hai1*,LI Ya-ling1,HAO Ya-ling1,MENG Tao1,WANG Yan-hui2
The preparation and study on the spectra of conductive nano-silver film were done under mild conditions. The silver citrate emulsion coating on the surface of PET was reduced by ascorbic acid (Vc) aqueous solution to prepare a silver film. The morphology, crystal structure, surface roughness and conductivity of the silver film were measured by FTIR, UV-Vis spectrum, X-ray diffraction (XRD), scanning electron microscope, scanning probe microscope system and so on. It was found that the silver citrate emumsion has a homogenous particle distribution from 60 nm-150 nm. The UV-Vis spectrum of the silver film shows a peak at 430 nm, and the silver thin film was considered to have a typical nano-scale structure. By the comparison of the XRD patterns of the films treated and untreated with water, it was concluded that the further deoxidization of silver citrate could be accelerated by water. The crystal structure of the silver film was improved and the surface resistance of the silver film was decreased greatly. The effect of ethanol on the decrease in the resistance of the silver film is much less than that of water.
2007 Vol. 27 (12): 2502-2505 [Abstract] ( 1733 ) PDF (1112 KB)  ( 556 )
2506 Spectral Diagnosis of Hydroxyl Radical in Multiphase Pulsed Discharge System
WANG Hui-juan1,3,LI Jie2*,QUAN Xie1,WU Yan2,LI Guo-feng2
A gas-liquid hybrid pulsed discharge system with a multi-needle-to-plate electrode geometry was used in the present study. A multiphase (gas-liquid-solid) pulsed discharge system was then formed by adding glasses beads immobilized with TiO2 photocatalyst into the discharge system. In the present paper, ultraviolet light produced during the pulsed discharge process was used as the lamp-house to induce the photocatalytic activity of the TiO2 photocatalyst. The synergistic effect of pulsed discharge and TiO2 photocatalysis was reviewed by the spectral diagnosis of hydroxyl radical (·OH) in the pulsed discharge system. The obtained results showed that the emission spectrum of ·OH could be observed at 306 nm (A2Σ+→X2Π), 309 nm (A2Σ+ (ν′=0)→X2Π(ν″=0)) and 313 nm (A2Σ+(ν′=1)→X2Π(ν″=1) transition). The relative emission intensity of ·OH at 313 nm in the discharge system was the strongest among the three characteristic spectra. The relative emission intensity of ·OH at 313 nm was stronger by adding TiO2 photocatalyst into the pulsed discharge system than that in the sole pulsed discharge system. In the case of experiments that changing the gas bubbling varieties and initial solution pH values, the results revealed that the relative emission intensity of ·OH at 313 nm in the synergistic system was stronger when Ar was used as bubbling gas compared with that when air and oxygen were bubbled into the reaction system. Furthermore, the acidic solution system was favorable for producing more ·OH, and therefore the corresponding emission intensity of ·OH at 313 nm was stronger than that in the neutral and basic solution.
2007 Vol. 27 (12): 2506-2509 [Abstract] ( 277 ) PDF (1483 KB)  ( 540 )
2510 Study on Photocatalytic Decomposition of Azo-Dyes by ZnO/Carbon Nanotubes Composites by UV-Vis Spectroscopy
XU Jing,SONG Xiao-jie,WEI Xian-wen*
ZnO/carbon nanotubes composites were prepared by hydrothermal treatment of the mixture of zinc nitrate and acid-treated multiwalled carbon nanotubes and characterized by transmission electron microscope (TEM) and X-ray powder diffraction (XRD). The TEM image indicated that ZnO nanoparticles with a diameter about 28 nm covered the carbon nanotubes. The XRD pattern shows that ZnO nanoparticles attached to the MWNTs exhibit a hexagonal phase. The diffraction peaks can be assigned to (100), (002), (101), (102), (110), (103), (200), (112) and (201) planes of the crystalline ZnO, respectively. The average size of the crystalline ZnO, calculated from the half-width of the (100) diffraction peak by the Scherrer equation, is 27.8 nm, which accords with the TEM observation. The ZnO/carbon nanotubes composites were used as a photocatalyst under sunlight for the decomposition of azo-dye, which was studied by UV-Vis spectroscopy. The effects of the illumination time, catalyst amount, initial dye concentration and the different structures of the dye on the photocatalytic process were investigated. It was noted that the intensity of the absorption peak corresponding to the azo-dye decreased rapidly at 400 nm during the photolysis process and the decomposition of azo-dye was a quasi-first order reaction. The decomposition rates for azo-dyes such as acid orange, Acid bright red, Acid light yellow are 0.09, 0.28 and 0.22 mg·L-1·min-1,respectively, which maybe resulted from their different functional groups. It can be stated that the complete removal of color, after selection of optimum operation parameters, can be achieved in relatively short time by using ZnO/carbon nanotubes composites. After recycling 5 times, the catalyst still has more than 50% efficiency.
2007 Vol. 27 (12): 2510-2513 [Abstract] ( 1827 ) PDF (1079 KB)  ( 581 )
2514 Comparative Research on Determination of Water Integrated Organic Pollution Index with Three Dimensional Excitation-Emission Fluorescence Spectroscopy and Traditional Wet Chemical Methods
WANG Zhi-gang1,2,LIU Wen-qing2*,ZHANG Yu-jun2,LI Hong-bin2,ZHAO Nan-jing2，LIU Jian-guo2, SIMA Wei-chang2,YANG Li-shu2
Three dimensional excitation-emission fluorescence spectra, chemical oxygen demanding (COD) and dissolved organic carbon (DOC) for water samples from Science Island, Chaohu Lake and Taihu Lake were determined. The COD values of the samples from Chaohu Lake were linearly correlated with the DOC values. Relationships of dissolved organic matter (DOM) concentrations determined by three dimensional excitation-emission fluorescence matrix (3DEEM), observed protein-like fluorescence intensity (Ipro-like) and humic-like fluorescence intensity (Ihum-like) to the chemical oxygen Demanding (COD) for all the samples from different sources were analyzed. Results indicated that DOM concentrations measured by 3DEEM and COD for the water samples from Science Island were well linearly related (r=0.821 72), and the linear relationships also existed between Ipro-like and COD (r=0.846 51), as well as Ihum-like and COD (r=0.836 89). However, for the water samples from Chaohu Lake and Taihu Lake, no linear relationships existed. The cause of the above difference between the water samples from Science Island and those from Chaohu Lake and Taihu Lake, and the feasibility and the limits of the integrated organic pollution measurement using three dimensional excitation-emission fluorescence spectroscopy were further discussed.
2007 Vol. 27 (12): 2514-2517 [Abstract] ( 1162 ) PDF (3506 KB)  ( 567 )
2518 Study of Derivatives of 2,6 -Diaminopyridine as Fluorescence Probe of Transition Metal Ions
ZHOU Yan-mei1,TONG Ai-jun2
Three derivatives of 2,6-diaminopyridine were synthesized with naphthyridine ring and —NH2,—OH and —NHCOCHCH2 groups. They are 2,4-dimethyl-7-hydroxyl-1,8-naphthyridine (DMHND), 2,4-Dimethyl-7-amino-1,8-naphthyridine (DMAND ) and DMAAN. The binding ability of the derivatives of 2,6-diaminopyridine for metal ions in acetonitrile was investigated using UV-Vis and fluorescence spectrometry. The changes of the dyes spectra were observed in the presence of transition metal ions, but were not observed in the presence of K+,Na+,Mg2+,Ca2+ and Pd2+. Except for DMHND that has weak binding ability for Cu2+,two dyes can bind with Cu2+ at the ratios of DMAAN∶Cu2+=1∶1, DMAND∶Cu2+=1∶1. The resulting binding curves were analyzed by nonlinear regression methods, giving the association constant for DMAAN to be about 4.4×105 L·mol-１,and about 6.3×106 L·mol-１ for DMAND. DMAND contains an electron-donating group (amino group) conjugated to an electron-withdrawing group (the pyridine ring), and undergoes intramolecular charge transfer from the donor to the acceptor upon excitation by light. When Cu2+ interacting with the N of the pyridine ring enhances the electron-withdrawing character of this group, the spectrum is thus red-shifted and the intensity is increased. DMAND displayed a high sensitivity among the three derivatives of 2,6-diaminopyridine as the fluorescence probe of transition metal ions.
2007 Vol. 27 (12): 2518-2522 [Abstract] ( 1601 ) PDF (1096 KB)  ( 550 )
2523 The Analysis of Sinusoidal Modulated Method Used for Measuring Fluorescence Lifetime
FENG Ying,HUANG Shi-hua*
This paper has built a system with a sinusoidal modulated LED as the excitation source. Such exciter was used upon the sample Eu2L′3·nH2O(L′=C4H4O4). Both the excitation light and the 5D0—7F2 emission of Eu3+ ion were measured. Fluorescence lifetime, which approximate to 0.680 ms, can then be obtained from the measured excitation and fluorescence waveforms by non-linear least square curve fitting based on the principle of phase-shift measurement of fluorescence lifetime. Data processing methods considering respectively the high order harmonics in the modulation and multi-exponential decay of the fluorescence were discussed. A method of utilizing Fourier series expandedness to amendatory the result was put forward. Accordingly, the applicability for phase-shift method was expanded as well as a more exact result was acquired.
2007 Vol. 27 (12): 2523-2526 [Abstract] ( 1137 ) PDF (901 KB)  ( 450 )
2527 Enhancement Effect on Fluorescence of Tm3+ Mixed Dysprosium Perchlorate in Phenyl-Phenacyl Sulfoxide
GUO Lei,LI Wen-xian*,SHI Xiao-yan
Nine different proportional complexes of different nuclear rare earth perchlorate (Dy3+ and Tm3+ are mixed) with phenyl-phenacyl sulfoxide (L=C6H5COCH2SOC6H5) have been synthesized and characterized. Element analysis and coordination titration studies suggest that the complexes have the composition of (DyxTmy)L5(ClO4)3·2H2O(x∶y=1.000∶0.000, 0.999∶0.001, 0.995∶0.005, 0.990∶0.010, 0.900∶0.100, 0.800∶0.200, 0.700∶0.300, 0.600∶0.400, 0.500∶0.500). IR studies indicate that the ligand is bonded with RE(Ⅲ) through one oxygen atom in sulfoxyl group，and the oxygen atom in carbonyl group did not bond.The molar conductivities measured in the DMF solution indicate that three inorganic anions ClO-4 are non-coordinated. The fluorescence emission intensity of Dy3+ complexes would be enhanced strongly by mixing Tm3+. Tm3+ has the best sensitization to the fluorescence of Dy3+ in the ratio of 0.990∶0.010. The fluorescence intensity can be increased to 246%.
2007 Vol. 27 (12): 2527-2530 [Abstract] ( 170 ) PDF (487 KB)  ( 470 )
2531 Effect of Glucose Concentration in Human Serum on Fluorescence Intensity
ZHU Wei-hua1,2,ZHAO Zhi-min1*,ZHENG Min1,XIN Yu-jun1,WANG Le-xin1,GUO Xin1
Blood plays an important role in the clinical diagnosis and treatment; many diseases may lead to changes in the blood composition or characteristic properties. Therefore, the analysis of blood sugar will be of great importance. The present paper studies the difference of fluorescence intensity stimulated by light wave between normal blood serum and hyperglycemia blood serum. The result shows that the average grey level of fluorescence image at 365 nm increases obviously with the changes in the concentration of glucose; however, the average grey changes little at 353, 369 and 405 nm. This shows that the main effect of serum glucose on the fluorescence intensity peak appears at 365 nm. Because the fluorescence intensity has something to do with the concentration of the fluorescence material, the blood glucose concentration influences directly the fluorescence intensity at 365 nm. Therefore, it is possible to judge blood sugar content, and to make sure whether the content exceeds the normal value or not by comparing the fluorescence intensity of the blood serum measured at 365 nm. This technique of optical measurement provides an experimental basis for the diagnosis of blood diseases.
2007 Vol. 27 (12): 2531-2533 [Abstract] ( 1084 ) PDF (628 KB)  ( 555 )
2534 Nanosilver Sensitized Fluorescence and Second-Order Scattering of Tb(Ⅲ)-Norfloxacin and Its Application
YANG Zhi-jie1,2,ZHAO Hui-chun1*,DING Fen1,LI Ai-yun1,WANG Xiao-li1
Norfloxacin (NFLX) can form complex with Tb(Ⅲ) ion, and the intramolecular energy transfer from NFLX to Tb(Ⅲ) takes place when excited. And thus the characteristic fluorescence of Tb(Ⅲ) ion is enhanced and the maximum fluorescence peak locates at 545 nm. The second-order scattering (SOS) peak at 545 nm also appears for the Tb(Ⅲ)-NFLX complex with the excitation wavelength of 272 nm. When the silver nanoparticles were added to the Tb(Ⅲ)-NFLX binary system, the luminescence intensity at 545 nm greatly increased. And the relative intensity is proportional to the amount of NFLX. Based on this phenomenon, a novel method for the determination of NFLX has been developed by using a common spectrofluorometer to measure the intensity of fluorescence and SOS. The calibration graphs for NFLX are linear in the range of 6.0×10-9-1.0×10-5 mol·L-1,and the detection limit is 4.4×10-9 mol·L-1. This method was applied satisfactorily to the determination of NFLX in capsule and eye drop samples. The experimental results showed that it is the certain size and certain concentration of silver nanoparticles that can greatly enhance the fluorescence-SOS intensity.
2007 Vol. 27 (12): 2534-2537 [Abstract] ( 1645 ) PDF (744 KB)  ( 547 )
2538 Fluorescence and Visible Spectroscopic Studies on Interaction of β-Cyclodextrin-Thionine Inclusion Complex with DNA
TONG Xiao-qing1,2,Lü Jian-quan1*,SUN Juan1,GONG Zhong-hong1
The inclusion of β-cyclodextrin (CD) for thionine (TH) and the interaction of DNA with CD-TH inclusion complex were investigated by fluorescence and visible absorption spectrometry. TH with β-CD formed a 1∶1 inclusion complex with the stability constant of 527 L·mol-1 (visible spectrometry)/444 L·mol-1 (fluorescence) in the pH 7.2 PBS buffer solutions. The addition of DNA makes the absorbance of the inclusion complex decrease and the absorption spectrum shift toward long wavelengths. The fluorescence experiments indicated that the presence of DNA makes the emission peak of CD-TH shift toward short wavelengths and the fluorescence of inclusion complex quench, and the quenching constant was calculated to be 6.12×104 L·mol-1 by Stern-Volmer method. All the data confirmed that CD-TH reacted with DNA in intercalative mode, and the binding numbers and the binding constant were estimated to be 1 and 3.47×104 L·mol-1 by spectrophotometry.
2007 Vol. 27 (12): 2538-2541 [Abstract] ( 2120 ) PDF (1010 KB)  ( 486 )
2542 Study on the Binding Reaction Features Between Naphthol Green B and Bovine Serum Albumin by Fluorescence Spectrophotometry
YAN Cheng-nong1,XIE Ze-yu1,MEI Ping1,LIU Yi2
At different temperatures, the binding of naphthol green B(NGB) to bovine serum albumin (BSA) was studied by the fluorescence spectroscopy, three-dimensional fluorescence spectrum, synchronous fluorescence spectrum and ultra-violet spectrum. It was shown that this compound has a quite strong ability to quench the fluorescence from BSA. After analyzing the fluorescence quenching data according to Sterm-Volmer equation and Lineweaver-Burk equation, it was found that BSA had reacted with naphthol green B and formed a new compound, the quenching action was due to static fluorescence quenching, and the action force was electrostatic interaction. According to the Lineweaver-Burk equation and thermodynamic equation, the average value of the binding constant(KLB：1.411×105 L·mol-1)，the thermodynamic parameters(ΔHθ：-5.707 kJ·mol-1,ΔGθ：-30.25 kJ·mol-1 and ΔSθ：79.95 J·K-1) and the amounts of binding sites(1.258) were obtained, providing important information for the research on the configuration modification of BSA because of the added naphthol green B, biological effects in a living body, and the coloration mechanism of naphthol green B.
2007 Vol. 27 (12): 2542-2545 [Abstract] ( 1914 ) PDF (1209 KB)  ( 525 )
2546 Determination of Terbium(Ⅲ) with EHPG-Tb(Ⅲ) System by Fluorescence Spectroscopy
ZHAO Chun-gui,LI Xiao-li,YANG Bin-sheng
The fluorescence of terbium was sensitized after addition of terbium to the ethylene-N, N’-bis (o-hydioxyphenylglycine) (EHPG) solution. A novel and simple method used for the determination of Tb(Ⅲ) was developed by means of fluorescence spectroscopy in the presence of EHPG. It was showed that the relative fluorescence intensity is proportional to the concentration of terbium ions, while the molar ratio of terbium to EHPG is less than 1.0 in the system. The maximum wavelengths of excitation and emission are 295 and 547 nm respectively. The optimal range of pH is 7-9. The linear range of detection of the concentration of terbium is from 1.0×10-8mol·L-1 to 1.0×10-5 mol·L-1,with a detection limit of 1.18×10-9 mol·L-1. The relative standard deviation is still within ±3% in the presence of other lanthanide ions. The method was applied to the determination of the recoveries of synthetic samples and a rare earth sample with satisfactory results.
2007 Vol. 27 (12): 2546-2549 [Abstract] ( 1685 ) PDF (727 KB)  ( 552 )
2550 Study on the Interaction between Fe3(CO)12 and DNA by Electronic and Fluorescence Spectrophotometry
WANG Ping-hong1,ZHANG Yin-feng2,ZHANG Qi1*,CHEN Shang-wen1,YUAN Wen-bing1,WU Shan-shan1
The interaction between Fe3(CO)12 and DNA was investigated by absorption and spectra, fluorescence spectra. The absorption of EB-DNA system in the presence of Fe3(CO)12 showed that Fe3(CO)12 could partly sustain the place of EB. The result of fluorescence spectra suggested that Fe3(CO)12 could enhance the fluorescence intensity of DNA sharply. All the experimental results indicated that the intercalative binding mode was the major model for the interaction of Fe3(CO)12 cluster complex with DNA.
2007 Vol. 27 (12): 2550-2552 [Abstract] ( 1797 ) PDF (604 KB)  ( 444 )
2553 Fluorescence Spectrum Analysis System for Protoporphyrin IX in Serum Based on Wavelet Transform
ZHU Dian-ming1,2,YANG Hong-peng3,LUO Xiao-sen2*,LIU Ying2,SHEN Zhong-hua2,LU Jian2,NI Xiao-wu2
Protoporphyrin IX is an important kind of organic compound for vital movement, and can be used as the sign of tumour blood. Human protoporphyrin IX content in serum is very low, and affected by various factors. The serum fluorescence spectrum analysis system based on wavelet transform was used to discriminated the protoporphyrin IX weak signals. The protoporphyrin IX fluorescence spectrum was obtained by a multi-function spectrum measuring system, and decomposed several times by wavelet transform to distinguish the noise and spectrum signals. The fluorescence spectrum can be divided into corresponding discrete approximations signals (a1-a6) and discrete details signals (d1-d6) by six times of decomposition, showing the signal frequency decreasing with decomposition times increasing and the protoporphyrin IX fluorescence character peak appears here. The weak signals were discriminated and the exactly component and quantity can be acquired for further analysis. So it can be analysed quantitatively. The researches in the present paper provide the potential application in the diagnosis of incipient tumous using the serum fluorescence spectrum.
2007 Vol. 27 (12): 2553-2557 [Abstract] ( 2320 ) PDF (1286 KB)  ( 473 )
2558 Fluorescence Spectra Analysis of Papain Treated by Pulsed Electric Field
ZENG Xin-an,YU Shu-juan,XU Ya-li
Tryptophane, tyrosine and phenylalanine are there kinds of fluorescent amino acids and exist in papain, so the structure change of papain can be measured by fluorescence spectra analysis without exterior fluorescence probe. Fluorescence excitation spectrum, emission spectrum and polarization spectrum were used to analyze the possible mechanisms of papain’s activity change after being treated by pulsed electric field (PEF). Results demonstrated that the relative activity of papain was decreased by 56.5％ after PEF treatment under the condition of electric field strength 50 kV·cm-１,frequency 1 500 Hz, pulse width 40 μs and pulse number 19 800. The spectra of fluorescence excitation showed that the relative fluorescence strength of the treated sample was distinctly higher than the untreated one, even at peak position (280 nm) which was 80 and 120 for untreated and treated samples, respectively. The peak position in the fluorescence emission spectrum of treated sample was shifted from the original 342 nm to about 346 nm, and its fluorescence polarization degree was much smaller compared to the untreated sample. These phenomena indicated that the α-helix structure of papain was loosened or broken down after being treated by PEF. This treatment made the amino acid’s residue exposed from inside to outside, and even some fluorescent amino acids such as tryptophane, tyrosine and phenylalanine were decomposed from the α-helix structure of protein and went into the solution which helped increase the fluorescent strength. This effect led to the active site change of the enzyme and finally inactivated it.
2007 Vol. 27 (12): 2558-2561 [Abstract] ( 1574 ) PDF (804 KB)  ( 514 )
2562 New Iron-Porphyrin/Vanadium-Substituted Polyoxometalate Catalyst: Synthesis, Characterization and Catalytic Activity
DONG Xiao-li,ZHANG Zhen-cheng,AN Qing-da*,ZHANG Shao-yin,WANG Shao-jun*
A new kind of iron-porphyrin/vanadium-substituted polyoxometalate coordination compound was synthesized by the ion exchange reaction of FeTTMAPPI and H5PMo10V2O40 in solution. The new catalyst was characterized by IR spectrometry and UV-Vis spectrometry. As an excellent catalyst, its effects on benzene hydroxylation and catalytic capabilities were studied with H2O2 solution as the oxidant. The results indicated that the products contained the conjugated structure of porphyrin and the cage structure of polyoxometalate, the V atom in polyoxometalate is the main centre of catalytic activity, meanwhile the presence of iron-porphyrin could increase its catalytic activity greatly.
2007 Vol. 27 (12): 2562-2565 [Abstract] ( 1234 ) PDF (873 KB)  ( 506 )
2566 Synthesis and Spectroscopic Properties of Tetra-(Dimethylaminophenyl) Porphyrin and Its Metal Complexes
DUAN Cai-hong, MA Hong-min, CHEN Xin, ZHANG Li-na, ZHANG Nuo, LI He, DU Bin, WEI Qin*
Porphyrin and metalloporphyrin distribute widely in nature and they play an important role in the life. Synthesis of porphyrin compounds with special function has been the focus of attention. In the present paper, porphyrin and metalloporphyrin compound were synthesized by the following method: by one-step synthesis, tetra-(dimethylaminophenyl) porphyrin(T(DMAP)P) was synthesized with propionic acid, acetic acid and nitrobenzene as solvent and 4-dimethylaminobenzaldehyde and pyrrole as raw material. The yield was 24.24%. The complexes of T(DMAP)P with Zn2+,Mn2+ and Tb3+ were synthesized by solvent of chloroform-N, N dimethylformamide(1∶1). The effects of solvent, temperature and reaction time on the reaction were discussed. Optimum proportion between porphyrin and metallic salts was studied also and the molar ratios of T(DMAP)P to Zn(CH3COO)2·2H2O, T(DMAP)P to MnCl2·4H2O, and T(DMAP)P to TbCl3 were 1∶1.2, 1∶1.4, 1∶1.5, respectively. The synthesis of metalloporphyrins under mild conditions is simper with high yield (94.2%, 91.7% and 90.5% for T(DMAP)P combined with Zn2+,Mn2+ and Tb3+ respectively) and the unstability of metalloporphyrin could be avoided. The constitution and structures of these compounds were studied by elemental analyses, infrared spectrum (IR), and ultraviolet-visible spectrum (UV-Vis). The conductivity of porphyrin compound with different concentration and temperature was studied. It was found that the molar conductivity of T(DMAP)P-TbCl(74.6 s·cm-2·mol-1) was greater than that of T(DMAP)P-Zn (8.8 s·cm-2·mol-1) and T(DMAP)P-Mn (25.8 s·cm-2·mol-1). So T(DMAP)P-TbCl could be regarded as the 1∶1 electrolyte compound while T(DMAP)P-Zn and T(DMAP)P-Mn were non-electrolyte compounds. The influences of different metal ions on the reaction were investigated. The discussion was concentrated on the molecular spectra of porphyrin and metalloporphyrin. Compared with tetraphenyl porphyrin, the absorption of T(DMAP)P and its metal complexes had red-shifts due to the substituent groups and metal ions. When the porphyrin rings were occupied by metal ions, the number of Q band decreased and the absorption peak intensity decreased. Among these metalloporphyrin compounds, the maximum absorption of T(DMAP)P-TbCl had the biggest red-shifts and could be used as ideal photosensitizer.
2007 Vol. 27 (12): 2566-2569 [Abstract] ( 1717 ) PDF (516 KB)  ( 567 )
2570 Determination of Sb and Bi in 24 International Geological Reference Materials by Using Pressurized Acid Digestion-ICP-MS
HU Zhao-chu1,2,GAO Shan1,2,LIU Xiao-ming2,YUAN Hong-lin2,LIU Ye2,DIWU Chun-rong2
The authors studied in detail the memory effect of Bi, Sb, As and Te in ICP-MS. The produced memory effects of these element were in the order of Bi>Sb>Te>As. Bi was seriously adsorbed by the polypropylene sample storing bottle and the sample introduction system in the low nitric acid medium (0.01%-1% HNO3). The washout effect of 0.1% HF was found to be better than those of 6% HNO3 and 0.1% HClO4. Under the given experiment conditions, the instrumental limit of detection was 0.001 and 0.000 1 ng·mL-1 for Sb and Bi, respectively. The authors report the determination of Sb and Bi in 24 international geological reference materials by using pressurized acid digestion-ICP-MS (including AGV-2, BHVO-2, BCR-2, etc.). Most of the results were found to be in reasonable agreement with the reported values in the literature. The authors’ determined values of Sb for GSR-1(granite; 0.30 μg·g-1) and JP-1(peridotite; 0.045 μg·g-1) are obviously higher than those reported values. This is attributed to the efficient pressurized acid digestion, which is generally much more efficient than conventional wet digestions for insoluble minerals.
2007 Vol. 27 (12): 2570-2574 [Abstract] ( 1590 ) PDF (1257 KB)  ( 498 )
2575 Effects of Soil on the Concentration of Rare Earth in Nanfeng Orange
LIU Ping-hui1,RUI Yu-kui2*,YE Chang-sheng1
Nanfeng orange is a famous fruit in the world, but the content of rare earth in the fruit and its relation to the content in soil were little studied. The present paper studied the contents of rare earth in Nanfeng orange fruit and the effects of soil planting Nanfeng orange on the contents of rare earth in Nanfeng orange fruit by ICP-MS/ICP-AES in order to find the relation of rare earth content in the soil to that in Nanfeng orange fruit. The results showed that ten kinds of rare earths were detected, namely La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho and Yb, whose contents range from 0.63 to 0.01 ng·g-1,while the contents of the ten elements range from 29.36 to 0.07 μg·g-1 in the soil. All data showed that the content of rare earth in fruits is right relative to that in soil. So the authors can conclude that fertilizing with rare earth should be the best way to enhance the content of rare earth in Nanfeng orange fruits.
2007 Vol. 27 (12): 2575-2577 [Abstract] ( 257 ) PDF (307 KB)  ( 441 )
2578 Determination of W, Mo and Other 8 Elements in Powder Metallurgical Materials by ICP-AES
KAI Xiao-ming1,LI Cheng2,WANG Jie2,WANG Yan-qing2
Samples were dissolved using nitric acid, perchloride acid and hydrofluoride acid in the medium of 0.025 mol·L-1 EDTA with a kind of standard solutions, and the element contents of Ni, Cu, V, Mn, W, Mo, Co and Cr were determined by ICP-AES method. After investigating the spectral interfere from matrix element and coexistent elements, optimum spectral lines were selected for each analyzed element, and the analytical precision, detection limits and recoveries were measured. The results show that the detection limits of the method are very low, relative standard deviations (n=10) are less than 1%, and the recoveries range from 98.2% to 101.6%. The proposed method is accurate, reliable, simple, and rapid. The method satisfies.
2007 Vol. 27 (12): 2578-2580 [Abstract] ( 1100 ) PDF (315 KB)  ( 551 )
2581 Determination of Cd in Sediment Samples by Flow Injection On-Line Anion Exchange Combined with Vapour Generation-Atomic Fluorescence Spectrometry
WANG Yi-zhuang1,QIU Hai-ou1*,TANG Zhi-yong1,GU Yan-sheng2,ZHANG Shu-qing1
In the present work, a method was developed for the determination of ultra-trace levels of Cd in sediment samples by atomic fluorescence spectrometry (AFS). A flow injection on-line separation and preconcentration technique coupled with an intermittent injection vapor generation technique was employed in the study. The instrument operating parameters and chemical conditions were optimized. In a 2.0 mol·L-1 HCl solution, Cd(Ⅱ) was adsorbed on 717-strong alkaline anion exchange resin, while Cu(Ⅱ) and Pb(Ⅱ) passed throngh. Then Cd(Ⅱ) was eluted by 0.5 mol·L-1 HNO3. The eluting solution was determined directly by intermittent injection vapor generation atomic fluorescence spectrometry. It was showed that Cd(Ⅱ) can be preconcentrated effectively and the interference can be completely eliminated by this improved method. The Cd atomic vapor generation efficiency could be greatly enhanced in the presence of Co(Ⅱ) and 1,10-phenanthroline. The linear range of the determination was 0-12 μg·L-1 with a detection limit of 0.058 μg·L-1. The RSD(5 μg·L-1,n=7) was 1.09%. The method was convenient, rapid and successfully validated by using national water sediment standard reference materials.
2007 Vol. 27 (12): 2581-2584 [Abstract] ( 2192 ) PDF (859 KB)  ( 505 )
2585 Determination of Trace Arsenic in Chinese Traditional Medicine by Hydride Generation Atomic Fluorescence Spectrometry
ZHU Yong-qin1,SHI Jie2
A hydride generation atomic fluorescence spectrometry method was developed for the determination of trace arsenic in CTM. A digestion system using HNO3-H2O2 under high pressure was applied for the pretreatment of the samples. The experimental conditions were optimized. Under the optimum conditions, there was a good linear relationship between the fluorescence intensity and arsenic concentration in the range of 0-80 μg·L-1 with a correlation coefficient of 0.999 9, while the detection limit was 0.069 μg·L-1. Trace arsenic in the standard reference substance (GBW08501) was determined incording this way and the results for six times of analysis were in good agreement with certified value. The authors also studied the arsenic contents in three kinds of CTM by the working curve method and the results were satisfactory.
2007 Vol. 27 (12): 2585-2587 [Abstract] ( 1658 ) PDF (371 KB)  ( 503 )
2588 Determination of Nutrition Elements in Yak Milk Powder by Atomic Absorption Spectrometry
SHI Yan1,ZHENG Wei-wan1,XIAO Wei-wei2,SONG Jian-jun1,LI Xiao-dan1
In the present paper, orthogonal design test was planed by changing cinefaction temperature, cinefaction time, and the concentration of hydrochloric acid. Yak milk powder and milk powder were digested by dry method. The contents of elements Ca, Mg, Fe, Cu, Zn, Mn, K and Na were determined by flame atomic absorption spectrometry. The best conditions for the digestion were obtained as follows: the temperature was 510 ℃, cinefaction time 4 hours, and hydrochloric acid concentration 1∶5. Meanwhile, under the best experimental conditions, the recovery ratio of the method in the range of 95.2%-107.3%, and the relative standard deviations were 0.38%-3.86% (n=6). The experimental results proved that Yak milk powder is valuable and nutritious food, and has rich nutrition elements.
2007 Vol. 27 (12): 2588-2590 [Abstract] ( 529 ) PDF (363 KB)  ( 539 )
2591 Determination and Comparison of Trace Elements in Four Sorts of Bulbus Fritillariae by Microwave Digestion-Atomic Absorption Spectrometry
YU Rui-peng1,CHENG Ze-feng2,GONG Xiao-qing1*
The contents of elements such as Zn, Fe, Mn, Cu, Na, Mg, K, Ca, As, Pb, Cd, Co, Cr, Sr, and Al in four sorts of Bulbus Fritillariae, namaly from Fritillaria thunbergii Miq.(Panan and Ningbo), Fritillaria thunbergii Miq. Var. chekiangensis Hsiao et K. C. Hsia and Fritillaria cirrhosa D. Don, were determined by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) respectively. The effect of different microwave digestion conditions on the analysis results was reviewed, and optimal condition for using atomic absorption spectrophotometry was determined. Principal component analysis (PCA) was applied taking trace elements contents as indexes. The results revealed that microwave digestion was a simple, rapid, digestion complete, and low blank value method, and the measurement result is satisfactory. The experimental results indicated that the linear relationships for different elements within the limits of working curve were good. The RSDs were all smaller than 3.97%. The addition standard rates of the procedure was between 91.0% and 108.7%. Principal component analysis has the application value of reflecting the differences in trace elements contents in various samples.
2007 Vol. 27 (12): 2591-2594 [Abstract] ( 1678 ) PDF (629 KB)  ( 498 )
2595 Exploration of Quality Control of Inorganic Elements in Chinese Herbal Medicines for Stimulating Blood Circulation and Relaxing Muscles and Joints by Atomic Absorption Spectrophotometry
ZHANG Qi-feng1,FAN Mei-mei2,WANG Guan-min1,TU Long-fei1,WANG Cheng1
Researches have shown the close relationships between inorganic elements and curative efficiencies of various Chinese herbal medicines. Yet, in studies of chemical composition and quality control of Chinese herbal medicines for stimulating blood circulation and relaxing muscles and joints, inorganic substances are often overlooked. In order to improve and reestablish the standard of quality control of Chinese herbal medicines, the authors attempted a method that would incorporate the composition of inorganic elements as part of the quality control. In the present study, the authors used atomic absorption spectrophotometry to measure the contents of fifteen inorganic elements, namely, Cu, Ca, Fe, K, Mg, Mo, Ni, Sr, V, Mn, Zn, Na, Cr, Cd, and Hg, in several Chinese herbal medicines, including Da Huo Luo Wan. The authors then discussed the relationship between these inorganic elements and curative efficiencies of these Chinese herbal medicines. By comparing the levels of inorganic elements found in Da Huo Luo Wan with those found in other Chinese herbal medicines used in the study, it was revealed that trace elements, Fe, Cu, Mn, and Zn, contribute to the curative efficiency of Da Huo Luo Wan. The authors’ results showed that the amounts of trace elements Fe, Cu, Mn and Zn found in Chinese herbal medicine Da Huo Luo Wan are related to the following curative effects of Da Huo Luo Wan: relieving rheumatism, rectifying breathing and alleviating phlegm, stimulating blood circulation and relaxing muscles and joints. The measurement and analysis of inorganic elements in Da Huo Luo Wan will also provide evidences and references for the fingerprint establishment of Da Huo Luo Wan in the future.
2007 Vol. 27 (12): 2595-2597 [Abstract] ( 1068 ) PDF (389 KB)  ( 499 )
2598 Determination of Eight Trace Elements in the Swertia Davidii Franch by Flame Atomic Absorption Spectrometry
LI Tao1,WANG Yuan-zhong2,YU Hong2,3*,CAO Yu-juan1,ZHANG Jing-jing1,LIU Qin1
The effects of different sample digestives on the determination of Swertia davidii Franch are compared. Eight trace elements in the Swertia davidii Franch were determined by flame atomic absorption spectrometry. The result shows that the RSD and recovery are better if the Swertia davidii Franch was digested with HNO3-HClO4(5∶1) mixed acid. The experimental results show that the detection limits were all smaller than 0.097 μg·mL-1,the RSDs (n=8) all smaller than 2.34%, and the addition standard recovery (ASR)(n=8) was 89.32%-106.65% for all the elements.
2007 Vol. 27 (12): 2598-2600 [Abstract] ( 817 ) PDF (399 KB)  ( 549 )
2601 Simultaneous Determination of Calcium and Magnesium by Calculative Spectrophotometric Complexometric Titration
LIAO Li-fu1,XIAO Xi-lin1,2,YANG Ming-hui2,YANG Jing1
A new spectrophotometric complexometric titration method coupled with chemometrics for the determination of mixtures of metal ions has been developed. In the method described here, the titrant is a mixture of EDTA and two indicators. In the process of titration, both the volumetric addition of titrant and the progress of titration reaction can be characterized simultaneously by chemometric calculation with the absorption spectra, and then the titration curves can be obtained. With the titration curves, a matrix equation can be established, and thus the concentration of each component in the mixture of metal ions can be calculated with principal component regression. The method only needs the information of absorption spectra to obtain the analytical results, and is free of volumetric measurements. So the method is simple, convenient and precise, and has been applied to the simultaneous determination of mixtures of calcium and magnesium using malachite green and Cu-PAN as indicators with satisfactory results.
2007 Vol. 27 (12): 2601-2604 [Abstract] ( 1809 ) PDF (698 KB)  ( 467 )

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