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2007 Vol. 27, No. 11
Published: 2007-11-26
 
       光谱学与光谱分析
2145 Physical Meaning of Temperature Measured by Spectral Line Intensity Method
ZHAO Wen-hua, TANG Huang-zai*,SHEN Yan, SHI Yong, HOU Ling-yun
The difference between electron temperature and excitation temperature is analyzed in the aspect of statistics thermodynamics. It is presented clearly that the temperature acquired by spectral line intensity method is not free electron temperature, but internal electronic excitation temperature of heavy particle. Under thermal equilibrium condition, the excitation temperature is equal to the electron temperature, while under non-thermal equilibrium condition, the excitation temperature is not equal to the electron temperature. In the study of arc jet plume in vacuum chamber，spectral line intensity method was employed to measure the apparent excitation temperature of arc jet plume, and Langmuir probe was employed to measure the electron temperature of arcjet plume. The big difference between the excitation temperature and the electron temperature proved that the temperature acquired by spectral line intensity method is not free electron temperature.
2007 Vol. 27 (11): 2145-2149 [Abstract] ( 1191 ) PDF (1194 KB)  ( 545 )
2150 Study on Exploring for Gas Based on Analysis of Spectral Absorption Features
XU Da-qi1,2,NI Guo-qiang1,JIANG Li-li1,LI Ting1,GE Shu-le1,SHU Xian-biao1
Reflectance spectra in the visible and near-infrared wavelength region provide a rapid and inexpensive means for determining the mineralogy of samples and obtaining information on chemical composition. Hydrocarbon microseepage theory establishes a cause-and-effect relation between oil and gas reservoirs and some special surface anomalies. Therefore the authors can explore for oil and gas by determining the reflectance spectra of surface anomalies. This determination can be fulfilled by means of field work and hyperspectral remote sensing. In the present paper, based on the analysis of reflectance spectra determined in the field of Qinghai ×× area, firstly, a macroscopic feature of the reflectance spectra of typical observation points in the gas fields is presented. Secondly, absorption-band parameters of spectra such as the position, depth, width, and asymmetry are extracted. Based on the spectral absorption features of the spectra of 144 samples collected from the field, a spectral library for the Qinghai ×× area is built to make the detection of the mineral alterations more rapid and reliable. Thirdly, two methods are improved and proposed to detect hydrocarbon microseepage using hydrocarbon absorption bands of reflectance spectra determined from the field. Finally, a linear unmixing model is studied based on the spectra of 144 samples so as to semi-quantitatively determine the abundance fractions of main minerals in the authors’ studied area.
2007 Vol. 27 (11): 2150-2154 [Abstract] ( 1246 ) PDF (1906 KB)  ( 527 )
2155 The Effect of Ethylene Glycol on the Morphology of Cu2O Nanoparticles Synthesized in W/O Microemulsion by γ-Irradiation
YANG Shi-guo,CHEN Qing-de,SHEN Xing-hai*
Cuprous oxide nanocubes were successfully prepared in w/o microemulsions by γ-irradiation in the presence of ethylene glycol (EG). Absorption spectrum, XRD, TEM, HRTEM and SEM were used to characterize the as-prepared nanoparticles. The characteristic peak of Cu2O of absorption spectra of the irradiated microemulsions red-shifts apparently with the EG increasing, showing that the as-prepared Cu2O particle size becomes larger. TEM images verify this point and indicate that Cu2O nanoparticles become uniform with the increase of EG. The results indicated that EG played an important role in the structures of cuprous oxide nanoprticles. Firstly, EG increased the viscosity of water-pools of microemulsions which affected the reactivity of hydrated electrons and finally influenced the reduction of Cu2+ and the precipitation of Cu2O. Secondly, EG reduced the rigidity of the interface of microemulsions and enhanced the mass exchange among water pools which impacted the nucleation and precipitation of Cu2O. Thirdly, EG adsorbed certain crystal faces of Cu2O and influenced the final morphology of Cu2O.
2007 Vol. 27 (11): 2155-2159 [Abstract] ( 1441 ) PDF (1409 KB)  ( 523 )
2160 Estimation of Spectral Reflectance Using Color Scanner
SHEN Hui-liang1,MOU Tong-sheng2,YANG Dong-xiao1
To obtain accurate and device-independent color, the scanner needs to be characterized. Considering that the behavior of color scanner always deviates from linear reflectance model and that the color distribution of training samples has considerable effect on the color estimation accuracy, a new spectral characterization method is proposed. This method can estimate accurate high-dimensional spectral reflectance from low-dimensional scanner responses, based on limited sample selection and weighted training. Experimental results indicate that the performance of the proposed method is obviously better than that of previous method, in both color difference error and spectral reflectance error.
2007 Vol. 27 (11): 2160-2163 [Abstract] ( 1746 ) PDF (669 KB)  ( 499 )
2164 VUV Spectral Properties of GdPO4∶Tm3+ and Sr3Gd(PO4)3∶Tm3+
LI Xin,HE Da-wei*,HOU Tao,ZHOU Dan,LU Peng-zhi
GdPO4∶Tm3+ and Sr3Gd(PO4)3∶Tm3+ samples were prepared by solid state reaction. The properties of structure, VUV excitation and luminescence under VUV excitation were studied. GdPO4∶Tm3+ belongs to the monoclinic space group, and the crystal structure does not change as the crystal lattice is doped with Tm ions. The excitation spectra of GdPO4∶Tm3+ show strong absorption at 164 and 210 nm due the to host and the 8S7/2—6GJ transition of Gd3+,respectively. The emission spectra of GdPO4∶Tm3+ reveal two intense and sharp emission peaks (453 nm and 363 nm) under 166 nm VUV excitation. The chief emission is at 453 nm from the typical Tm3+ 1D2→3H4 (22, 123 cm-1) transition. The emission spectra of Sr3Gd(PO4)3∶Tm3+ at 363 nm is weakened, while the blue emission at 453 nm is strengthened because the excitation spectra of Sr3Gd(PO4)3∶Tm3+ at 166 nm are higher than that of GdPO4∶Tm3+.
2007 Vol. 27 (11): 2164-2166 [Abstract] ( 1545 ) PDF (701 KB)  ( 532 )
2167 Study on Spectral Properties of Ca2B5O9Cl∶Eu Prepared with Hydrothermal Method and Solid Method
DONG Hong-jun,CHANG Shu-lan*
Effects of preparation methods (hydrothermal method and high temperature solid method), excitation condition, and Eu ions concentration on spectral properties of Ca2B5O9Cl∶Eu phosphor were studied. The effects of preparation condition on crystal photographs were also discussed. The result showed that the Ca2B5O9Cl∶Eu phosphors prepared with hydrothermal method had mainly 5D0→7FJ(J=1,2,3,4) emission of Eu3+ with 254 nm excitation and 4f65d1→8S7/2 emission of Eu2+ with 365 nm excitation, the one prepared with high temperature solid method had mainly 4f65d1→8S7/2 emission of Eu2+ with 365 nm excitation and very weak emissions of Eu2+ and Eu3+ with 254 nm excitation. Eu ions concentration hardly affected spectral properties, but the preparation method and excitation conditions had remarkable influence on the properties. SEM revealed that the products prepared both in the air and reductive atmosphere had consummate crystal, slippery surface and appropriate size (0.82-1.06 μm).
2007 Vol. 27 (11): 2167-2170 [Abstract] ( 1534 ) PDF (799 KB)  ( 492 )
2171 Morphology Determination of Ionization Region in Multi-Needle-to-Plate Negative Corona Discharge
SU Peng-hao,ZHU Yi-min*,CHEN Hai-feng
Based on the former work on the current-voltage characteristics of a multi-needle-to-plate negative corona discharge at atmospheric pressure, the present work uses the method of OES (optical emission spectrum) for measuring N2 emission spectrum, and the morphology determination of the ionization region has been investigated. According to the distribution of N2 second positive band’s intensity ISPB, the highest of all bands, the outline of the ionization region was drawn fairly accurately. The relationship between ISPB and discharge current I can be obtained through the volume integral of the ISPB. The experimental results show that the size of the ionization region enhances with the rise of the applied voltage U, and the electron avalanche begins at about 1 mm off the tips of needle electrode and multiplies only in the range of several millimeters, indicating that, the range of the ionization region is at the magnitude of mm. The electron avalanche along the axis of the needle develops farther than that along the radial direction of needle, and the shape of the ionization region looks like a bullet. The integral of ISPB is second-order linear to I, with a very second order coefficient, meaning that the main excited substance is N2. Energetic electrons mainly exist in ionization region while ions are the main charged particles to form discharge current in the transfer region.
2007 Vol. 27 (11): 2171-2174 [Abstract] ( 1857 ) PDF (891 KB)  ( 494 )
2175 Study on Plasma Temperature in Dielectric Barrier Discharge at the Middle Value of pd
DONG Li-fang, QI Yu-yan, GAO Rui-ling, LIU Feng, LI Xue-chen
The optical emission spectra of Ar/air dielectric barrier discharge (DBD) scanned from 300-800 nm near atmospheric pressure were obtained. Electron excitation temperature (Texc) and molecule vibrational temperature (Tv) in Ar/air DBD at the middle value of pressure-distance (pd) product (about 6.4×103 Pa·cm) were studied. The ArI 763.51 nm(2P6→1S5) and 772.42 nm(2P2→1S3) lines were chosen to estimate Texc. Tv was measured by the N2 second positive band (C 3Πu→B 3Πg). It was found that Texc and Tv increase with increasing applied voltage. And the varying rate of Texc with increasing voltage is bigger than that of Tv.
2007 Vol. 27 (11): 2175-2177 [Abstract] ( 211 ) PDF (575 KB)  ( 495 )
2178 Photoluminescence Investigation of InAs Bimodal Self-Assembled Quantum Dots State Filling
JIA Guo-zhi1, YAO Jiang-hong1*, ZHANG Chun-ling1, SHU Qiang1, LIU Ru-bin1, YE Xiao-ling2,WANG Zhan-guo1，2
Self-assembled InAs quantum dots were prepared on GaAs(100) substrate in a solid source molecular beam epitaxy system. The distribution and topographic images of uncapped dots were studied by atomic force microscope. The statistical result shows that the quantum dots are bimodal distribution. The photoluminescence spectrum results shows that the intensity of small size quantum dots dominated, which may be due to: (1) the state density of large quantum dots lower than that of small quantum dots; (2) the carriers capture rate of large size quantum dots is small relative to that of small ones; (3) there is a large strain barrier between large quantum dots and capping layer, and the large strain is likely to produce the defect and dislocation, resulting in a probability of carriers transferring from large quantum dots to small dots that is very small with temperature increasing.
2007 Vol. 27 (11): 2178-2181 [Abstract] ( 1211 ) PDF (636 KB)  ( 489 )
2182 Preparation of CeO2∶Eu3+ Powders by Sol-Gel Method and Their Photoluminescence Properties
WANG Xiao-dong, LIU Xiao-hua*,CHEN Shao-jun, LI Ming, LIU Min
CeO2∶Eu3+ phosphor powders with various Eu3+ concentrations have been prepared by the sol-gel method. Upon excitation with UV light, the CeO2∶Eu3+ powders showed bright orange red emissions due to the 4f—4f transitions of Eu3+ ions. X-ray diffraction (XRD), TG-DTA and Photoluminescence (PL) measurements were used to characterize the samples. XRD analysis showed that the powders with pure cubic fluorite-type CeO2 phase at an up to 10at.% concentration of Eu3+ was obtained at the sintering temperatures from 500 to 1 250 ℃. The large solubility for doping Eu3+ ions in CeO2 is due to the nearness of ionic radius between Ce4+ and Eu3+. It was also found that an increase in sintering temperature promotes the grain growth of CeO2 and improves its crystallinity. The excitation spectra of the CeO2∶Eu3+ powders were dominated by a broad band at 300-390 nm, suggesting the efficient energy transfer from the O2-—Ce4+ charge-transfer state to the doping Eu3+ in the CeO2∶Eu3+ powders. The CeO2∶Eu3+ phosphor powders with a 6at.% concentration of Eu3+ sintered at 1 250 ℃ revealed the strongest photoluminescence and then in abruptly decreased with increasing the doping concentration indicating the concentration quenching. The mechanism of concentration quenching could be explained as the result of the dipole-quadrupole interaction of neighboring Eu3+.
2007 Vol. 27 (11): 2182-2185 [Abstract] ( 1892 ) PDF (1106 KB)  ( 522 )
2186 Difference-Frequency Generation in PPLN and Water Vapor Detection in Air
DENG Lun-hua1, 2,GAO Xiao-ming1, 2,CAO Zhen-song1, 2,YUAN Yi-qian1,ZHANG Wei-jun2,GONG Zhi-ben1
The continuously tunable laser source has been realized in a periodically poled LiNO3 crystal based on difference frequency generation and quasi-phase-matching technique. The pump laser is an 1 W tunable Ti: Sapphire laser with a tunable region from 770 to 870 nm. The signal laser is an 1 W diode-pumped monolithic Nd∶YAG laser. When the grating period is 20 μm and the temperature is tuned between room temperature and 200 ℃, the generated wavelength of idler laser is around 2.8 μm with the general power of 1-2 μW. The direct absorption spectra of (001←000) band of water in laboratory air were measured based on the laser source. The concentration of water vapor in the laboratory air was estimated with an absorption optical path of 8.5 cm in open air
2007 Vol. 27 (11): 2186-2189 [Abstract] ( 1243 ) PDF (745 KB)  ( 514 )
2190 Near Infrared Diffuse Reflectance Spectroscopy for Rapid Analysis of Soluble Solids Content in Navel Orange
LIU Yan-de1,OUYANG Ai-guo2, LUO Ji1, CHEN Xing-miao1
The potential of using visible and near infrared diffuse reflectance spectroscopy to assess soluble solids content (SSC) of intact navel orange was examined. A total 40 samples were used to develop the calibration and prediction models. NIR spectral data were collected in the spectral region between 350 and 2 500 nm and their second derivative spectra were used for the present study. Different scattering correction algorithms (no preprocessing and multiplicative scattering correction (MSC)) were compared. Camibration models based on different spectral ranges, different derivatives and different kinds of statistical models including partial least square (PLS) and principal component regression (PCR) were also compared. The best results of PLS models with the second derivative spectra are r=0.929, RMSEC=0.517 and RMSEP=0.592 in the wavelength range of 361-2 488 nm. The results show that this method is feasible for non destructive assessing of SSC of the navel orange.
2007 Vol. 27 (11): 2190-2192 [Abstract] ( 1146 ) PDF (622 KB)  ( 533 )
2193 Principal Component Extraction Used for the Interpretation of RS-FTIR Spectra
HU Lan-ping1,2,ZHANG Lin1,LI Yan1,ZHANG Li-ming1,REN Yi-bo1, YU Bai-hua1,WANG Jun-de1*
A method for interpretation of remote sensing FTIR spectra was set up based on ANN model. Considering long training time and over-fitting problem of ANN, two methods, partial least squares (PLS) and principal component analysis (PCA), were utilized to extract principal components of spectra, process time decrease from about 30 minutes to a few seconds. Meanwhile, the idea of calibration transfer was used to overcome the limitation of calibration model in remote sensing FTIR spectra analysis. With the optimization of ANN model, four-component mixtures of acetone, benzene, chloroform and methanol were predicted in a remote sensing and real-time way while the calibration model was built with EPA data. The best performance was yielded with PLS-ANN model, and the root mean square error (RMSE) of acetone, benzene, chloroform and methanol were 0.043，0.031，0.034 and 0.051 respectively, which confirm the real-time, correct and quick analysis of remote sensing FTIR in air monitoring.
2007 Vol. 27 (11): 2193-2196 [Abstract] ( 1286 ) PDF (511 KB)  ( 573 )
2197 Effect of Humidity on Detection of Near-Infrared Spectra
ZHOU Ying,FU Xia-ping,YING Yi-bin*
Spectral performance would be affected by many factors such as temperature, equipment parameters and so on. Humidity fluctuations may occur in practice because of varying weather conditions. The objective of the present research was to find out whether the change in humidity would influence the near infrared spectrum. In this trial, an airproof, humidity-controllable test-bed was established to change the humidity of the mini environment. At 40%, 50%, 60%, 70% and 80% degrees of humidity, each sample’s final spectrum was obtained by removing the background’s spectrum from the sample’s. As whether the influences of the sample’s spectrum and the background’s are equal wasn’t known, this trial was divided into two groups: detecting background and sample at each degree of humidity (group 1) and background’s detecting just performed at 40% degree of humidity (group 2). This research was based on the hardware of NEXUS intelligent FTIR spectrometer, made by Nicolet instrument company U.S.A, using fiber optic diffuse reflectance accessory. The final spectrum was analysed using single variance analysis and Mahalanobis distance methods. The result shows that neither in group 1 nor in group 2, humidity had little influence on NIR.
2007 Vol. 27 (11): 2197-2199 [Abstract] ( 1218 ) PDF (537 KB)  ( 563 )
2200 Spectral Analysis of Ball Pen Script by FTIR Microscope with ATR Objective
HUANG Tao-hong1,WU Tian-ming2
Inspection of ball pen script is very important in public security and justice field. It is difficult to get a good spectrum directly by infrared microscope reflectance mode because of low reflectivity of paper and dark gray in color. The best way to measure low reflectivity sample is by infrared microscope with ATR objective method. Measurement with the microscopic ATR method involves bringing the trace of ball pen ink into contact with the prism.By this method, some mixed spectra of ball pen ink and paper fiber were obtained from one of the actual sample. The spectrum of the paper was subtracted from those mixed spectra and a pure spectrum of the ball pen ink was obtained. In this spectrum, three strong peaks were found 1 581，1 361 and 1 172 cm-1 respectively, all from crystal violet, a typical triphenylmethane pigment. Another strong peak at 1 724 cm-1 is contributed by carbonyl vibration from oil reagent alkyd. A 3D graph, showing the distribution of peak 1 581 cm-1 in this area, was set up by using mapping software. In the 3D distribution graph, the figure of ball pen trace vividly appeared. This infrared microscope ATR method makes it available to nondestructively inspect original ball pen script.
2007 Vol. 27 (11): 2200-2202 [Abstract] ( 2595 ) PDF (996 KB)  ( 543 )
2203 Rapidly Determination of Compositions of Animal Manure Compost Using Near Infrared Reflectance Spectroscopy
HUANG Guang-qun1,2,HAN Lu-jia1,2*,YANG Zeng-ling1,2
Composting is a process of aerobic thermophilic microbial degradation or an exothermic biological oxidation of various wastes by many populations of the indigenous microorganisms, which lead to a stabilized, mature, deodorized and hygienic product, free of pathogens and plant seeds, rich in humic substances, less volume, easy to store and marketable as organic amendment or fertilizer. Compared to the conventional wet chemical method, near-infrared reflectance spectroscopy (NIRS), a rapid, nondestructive, cost-effective technique, has been extensively used for qualitative and quantitative analysis in the field of agriculture. This study was to explore the capability of NIRS to analyze the compositions of Chinese animal manure compost. A representative population of 120 animal manure compost samples from 22 provinces in China was selected as research object, and this study explored the feasibility of analyzing animal manure compost compositions, which included moisture (Moist), volatile solid (VS), total organic carbon (TOC), total nitrogen (TN), C∶N, pH and Electronic conductivity (EC) using NIRS. Original samples were scanned with a SPECTRUM ONE NTS (Perkin Elmer, New Jersey, USA) from 10 000 to 4 000 cm-1. NIRS calibrations of a series of chemical parameters were developed by means of partial least-squares (PLS) regression. Results showed that the determination coefficient of calibration (r2) and the standard error of estimate (SEE) were Moist(0.981 6, 21.98), VS(0.936 5, 37.29), TOC(0.961 0, 16.46), TN(0.987 4, 1.61), C∶N(0.741 0, 2.29), pH(0.788 0, 0.48) and EC(0.870 4, 1.74), respectively. The determination coefficient of validation (r2V) and the standard error of prediction (SEP) were Moist(0.983 2, 20.99), VS(0.938 1, 35.07), TOC(0.912 8, 26.34), TN(0.973 5, 3.96), C∶N(0.830 8, 2.01), pH(0.615 8, 0.60) and EC(0.895 3, 1.87), respectively. The value of RPD (SD/SEP) for Moist, VS, TOC, TN and EC were all greater than 3.0, 2.39 for C∶N and 1.63 for pH. Together, results showed the feasibility and efficiency of NIRS to determinate compositions of animal manure compost.
2007 Vol. 27 (11): 2203-2207 [Abstract] ( 1677 ) PDF (844 KB)  ( 536 )
2208 Study on the Detection of Gray Mold of Tomato Leave Based on Vis-Near Infrared Spectra
WU Di1,FENG Lei1,ZHANG Chuan-qing2,HE Yong1*
Visible and near-infrared reflectance spectroscopy (Vis/NIRS) technique was applied to the detection of disease level of grey mold on tomato leave. Chemometrics was used to build the relationship between the reflectance spectra and disease level. In order to decrease the amount of calculation and improve the accuracy of the model, principal component analysis (PCA) was executed to reduce numerous wavebands into several principal components (PCs) as input variables of BP neural network. The loading value of PC1 was applied to qualitatively analyze which wavebands were more important for disease detection. Prediction results showed that when the number of primary PCs was 8 and the hidden nodes of BP neural network were 11, the detection performance of the model was good as correlation coefficient (r) was 0.930 while standard error of prediction (SEP) was 0.068 7. Thus, it is concluded that spectroscopy technology is an available technique for the detection of disease level of grey mold on tomato leave based on chemometrics used for data analysis.
2007 Vol. 27 (11): 2208-2211 [Abstract] ( 1237 ) PDF (703 KB)  ( 547 )
2212 Discrimination of Adulterated Traditional Chinese Medicines by Infrared Spectroscopy-Two Dimensional Correlation Analysis
LI Shu1,LE Jian2,CHEN Gui-liang2,CHAI Yi-feng1,LU Feng1*
A new method was established, based on infrared spectroscopy-two dimensional (2D) correlation analysis, for the discriminative analysis of adulteration in traditional Chinese medicines (TCM). Fenfluramine hydrochloride (FH) and sibutramine hydrochloride (SH) were taken as examples of synthetic drugs (adulterant), and the correlative peaks of their synchronous 2D correlation spectra were found. Then the characteristics of the synchronous 2D correlation spectrum of the suspected TCM were compared with those of FH. Since the correlative peaks in the synchronous spectrum of the suspected TCM coincide well with those of FH, a positive conclusion could be drawn after further investigation of the asynchronous spectra of TCM, which could provide the information about the source of correlative peaks. On the contrary, the dissimilarity of the synchronous spectra of SH and TCM directly implies that the suspected TCM is not adulterated with SH. The method can be used for a correct discrimination on whether the TCM is adulterated with the synthetic drugs, it does not rely on sample separation, and provides a new simple and cost-effective alternative to test the adulteration of TCM.
2007 Vol. 27 (11): 2212-2215 [Abstract] ( 1861 ) PDF (1136 KB)  ( 560 )
2216 Multicomponent Quantitative Analysis Using Near Infrared Spectroscopy by Building PLS-GRNN Model
LIU Bo-ping1,2,QIN Hua-jun3,LUO Xiang2,4,CAO Shu-wen3,WANG Jun-de1*
The present paper introduces an application of near infrared spectroscopy(NIRS) multi-component quantitative analysis by building partial least squares (PLS)-generalized regression neural networks (GRNN) model. The PLS-GRNN prediction model for chlorine, fibre and fat in 45 feedstuff samples was established with good veracity and recurrence. Eight peak values in principal components compressed from original data by PLS and four in original spectra were taken as inputs of GRNN while 4 predictive targets as outputs. 0.1 was chosen as smoothing factor for its good approximation and prediction with the lowest error compared with 0.2, 0.3, 0.4 and 0.5. Predictive correlation coefficient and Standard error of the estimate of three components by the model are 0.984 0, 0.987 0 and 0.983 0, and 0.015 89, 0.154 1 and 0.115 1，while the Standard deviations of an unknown sample scanned 8 times are 0.003 26, 0.065 5 and 0.031 4. The results show that PLS-GRNN used in NIRS is a rapid, effective means for measuring chlorine, fibre in the fat in feedstuff powder, and can also be used in quantitative analysis of other samples. A settlement in the high error of prediction of other samples with lower contents was also shown.
2007 Vol. 27 (11): 2216-2220 [Abstract] ( 2393 ) PDF (1081 KB)  ( 560 )
2221 The IR Spectra of Complexes of N-(Phenyl, Ferrocenyl)Methyl-β-Hydroxyethylamine with Ni(Ⅱ), Cu(Ⅱ), Zn(Ⅱ), Cd(Ⅱ) and Hg(Ⅱ)
WANG Xiao-li1,2,BIAN Zhan-xi1*,WANG Xi-gui2
The reaction of ferrocenylphenylcarbinol with the ethereal solution of boron trifluoride in dichloride methane resulted in the relevant ferrocenylphenylmethyl carbocation .Without separation from the reaction mixture, the ion reacted with ethanolamine to from N-(phenyl,ferrocenyl) methyl-β-hydroxyethylamine(FcY). A series of coordinate complexes-FcY-Ni(Ⅱ), FcY-Cu(Ⅱ), FcY-Zn(Ⅱ), FcY-Cd(Ⅱ) and FcY-Hg(Ⅱ) were obtained through coordination of this ligand with MCl2(M=Ni, Cu, Zn, Cd, Hg). The complexes and ligand were taken for FTIR in the range of 4 000-400 cm-1. Their major bonds were assigned and compared. The results showed that in all the complexes some bands(νO—H,νN—H,δO—H,δN—H) showed a certain shift to lower wave number, and bands(νC—N,νO—N) exhibited a certain shift to higher wave number. The aminoalcohol groups and metal ions were bonding with coordinated bond.
2007 Vol. 27 (11): 2221-2223 [Abstract] ( 1780 ) PDF (513 KB)  ( 537 )
2224 Optimizing Spectral Region in Using Near-Infrared Spectroscopy for Donkey Milk Analysis
ZHENG Li-min1,ZHANG Lu-da3,GUO Hui-yuan2,PANG Kun2,ZHANG Wen-juan1,REN Fa-zheng2*
Donkey milk has aroused more attention in recent years since its nutrition composition shows a higher similarity to human milk than others. Due to the composition difference between cow milk and donkey milk, the present models available for cow milk analysis could not be applied to donkey milk without modifications. A rapid and reliable analysis method is required to measure the nutrition composition of donkey milk. Near infrared spectroscopy is a newly developed method in food industry, but no literature report was found regarding to its application in the analysis of donkey milk. Protein, fat, ash contents and energy value are the major nutrition factors of milk. In the present paper, these factors of donkey milk were investigated by Fourier transform near-infrared (FT-NIR) spectroscopy. The ranges of protein, fat and ash contents, and energy value in donkey milk samples were 1.15%-2.54%, 0.34%-2.67%, 0.28%-0.57% and 355.87-565.17 cal·kg-1, respectively. The IR spectra ranged f from 3 899.6 to 12 493.4 cm-1,with a 1 cm-1 scanning interval. When the principal least square (PLS) regression algorithm is used for spectral regions information extraction, the additional constraint makes the principal components of matrix X to be related with the components of Y which is to be analyzed. Various spectral regions and data pretreatment methods were selected for principal least square (PLS) regression model development. A comparison of the whole and optimized spectral region NIR indicated that the models of selecting optimum spectral region were better than those of the whole spectral region. It was shown that the protein, fat and ash contents, and energy value in donkey milk obtained by chemical methods were well correlated to the respective values predicted by the NIR spectroscopy quantitative analysis model (α=0.05). The RMSEP values were 0.18, 0.117, 0.040 6 and 23.5 respectively, indicating that these predicted values were reliable. These results suggested that FT-NIR spectroscopy could be used for the rapid detection of the composition of donkey milk by establishing NIR spectroscopy quantitative analysis models. Selecting an optimum spectral region and establishing a special NIR analysis model accordingly are key steps during the data pretreatment. The models of the optimum spectral region were better than the models of the whole spectral region. When irrelevant information was included in the models, it would interfere with the analysis and give less reliable results. Therefore, the selection of a right spectra region plays an important role in the set-up of quantitative analysis models. The accuracy and reliability of the standard data used in model settings are also critical to the final results. In order to improve the reliability and accuracy of the NIR methods, a wide range of component contents and more accurate standard data are definitely required.
2007 Vol. 27 (11): 2224-2227 [Abstract] ( 2365 ) PDF (484 KB)  ( 528 )
2228 Research Progress of Terahertz Wave Technology in Quality Measurement of Food and Agricultural Products
YAN Zhan-ke1,2,ZHANG Hong-jian1,YING Yi-bin2*
The quality concern of food and agricultural products has become more and more significant. The related technologies for nondestructive measurement or quality control of food products have been the focus of many researches. Terahertz (THz) radiation, or THz wave, the least explored region of the spectrum, is the electromagnetic wave that lies between mid-infrared and microwave radiation, which has very important research and application values. THz spectroscopy and THz imaging technique are the two main applications of THz wave. During the past decade, THz waves have been used to characterize the electronic, vibrational and compositional properties of solid, liquid and gas phase materials. Recently, THz technology has gained a lot of attention of researchers in various fields from biological spectral analysis to bio-medical imaging due to its unique features compared with microwave and optical waves. In the present paper, the properties of THz wave and its uniqueness in sensing and imaging applications were discussed. The most recent researches on THz technology used in food quality control and agricultural products inspection were summarized. The prospect of this novel technology in agriculture and food industry was also discussed.
2007 Vol. 27 (11): 2228-2234 [Abstract] ( 725 ) PDF (1555 KB)  ( 589 )
2235 Determination of the Monomers in Phenylethylene-Butyl Acrylate-Vinyl Triethoxy Siloxane Terpolymer for Solid Phase Microextraction Coating by Combining IR and UV
SHEN Shu-chang1,LIU Cai-yun1,FU Shuang1,ZHANG Wei-bing2,WANG Wen-bo1
In the present paper, phenylethylene-butyl acrylate-vinyl triethoxy siloxane terpolymer, as SPME coating, was synthesized. Combining infrared spectrum and ultraviolet spectrum, the contents of the monomers were determined. The two monomers’ mole ratio of phenylethylene to butyl acrylate was obtained by IR. The content of phenylethylene was obtained by UV. Then the contents of butyl acrylate and vinyl triethoxy siloxane were calculated from the phenylethylene quantity and the mole ratio. For the determination of the mole ratio of phenylethylene to butyl acrylate, the standard curve was Ar=0.114mr+0.032 (A: absorptance ratio, mr: mole ratio), and the corre lation efficient(r2) was 0.999 3; for the determination of the content of phenylethylene, the standard curve was ΔA=0.078 6c+0.081 2(ΔA: absorptance difference, c: concentration of phenylethylene), and the correlation efficient(r2) was 0.998 9. The relative standard deviation (RSD) for phenylethylene was 0.41%, and recoveries were 97.8%-104%. The relative standard deviation (RSD) for butyl acrylate was 0.39%, and the recoveries were 97.1%-99.6%.
2007 Vol. 27 (11): 2235-2238 [Abstract] ( 1107 ) PDF (527 KB)  ( 452 )
2239 Application of Comparison Method with Correlation Coefficient Array in Identification of Chinese Herbs
XU Yong-qun1,DENG San-yao2,LI Xing-wang3,CHEN Xiao-kang1
The infrared spectrum of Chinese herbs possesses the character similar to fingerprint .The purpose to identify Chinese herbs can be achieved by way of comparing these spectra. The software of comparing correlation coefficient array of FTIR spectra was designed in Visual Basic 6.0. It established an infrared spectrum database including more than 300 kinds of Chinese herbs. The FTIR spectra of unknown herb can be compared with those of Chinese herbs in the database, and this method can identify the suitable herbs according to the similar herbs in the database. The study shows that within the spectral database of herbs, the factors of spectral interference, such as H2O, CO2,etc., can be avoided through assigning threshold values of correlation coefficients and comparing spectra with characteristic peak bands, and the comparison result is credible and correct. This method was expected to be a common method in identifying Chinese herbs.
2007 Vol. 27 (11): 2239-2242 [Abstract] ( 2370 ) PDF (765 KB)  ( 498 )
2243 Investigation on the Change in C—F Stretching Vibration of FTIR Spectrum by 1H NMR Method
LIU Hua-qing,JIANG Feng-chi
FTIR spectroscopy and 1H NMR method were used to investigate three organic compounds—1,2-di[-β-(α-methyl-α′-p-substitutephenyl) thiophene]hexafluorocyclo pentene. After assigning all main infrared spectrum peaks，it was observed that the stretching vibration frequency(ν) of C—F band in cyclopentene is rised gradually, and it was found that for compound Ⅰ：νas C—F=1 332.21 cm-1,νs C—F=1 231.91 cm-1 and δC—F=1 159.9 cm-1；for compound Ⅱ：νas C—F=1 338.18 cm-1,νs C—F=1 254.31 cm-1 and δC—F=1 179.22 cm-1；and for compound Ⅲ：νas C—F=1 360.99 cm-1,νs C—F=1 263.29 cm-1 and δC—F=1 194.00 cm-1. The reason for ν change is discussed not only using infrared absorption theory qualitatively but also using 1H NMR method quantitatively. It was also found that for compound Ⅰ H-1=7.503, H-2=7.484；for compound Ⅱ H-1=6.896, H-2=7.465; and for compound Ⅲ：H-1=6.728, H-2=7.413, proveing that the substitution group —F，—OCH2CH3，—N(CH3)2 influences the C—F stretching vibration by the conjugative effect and the inductive effect. The result is satisfactory and it shows that 1H NMR is a powerful tool for infrared spectrum analysis.
2007 Vol. 27 (11): 2243-2245 [Abstract] ( 274 ) PDF (531 KB)  ( 527 )
2246 Determination of Constituents of Polysaccharide and the Content of Saccharide in Mongolian Medicine Garidi-15
CUI Yi1,BAI Hai-quan2,ZHAO Yu-ying1*,Wulangerile1,SONG Juan-juan1,XU Xiu-ting1
The present paper introuduces the method, with which the water-soluble polysaccharide was extracted with hot water from Garidi-15, the products were further purified with column chromatography on SephadexC-25, and the contents of water soluble polysaccharide were determined by phenyl hydrate-sulfuric acid method. The average recovery was 100.50%, and RSD was 0.82%. The components of water soluble polysaccharide were identified by gas chromatography as xylose, mannose, galactose and glucose in the molar ratio of 1.03∶1.26∶0.77∶2.30. The water soluble polysaccharide was identified by IR spectrum and UV(200-400 nm) scanning spectrum. The IR spectrum indicates that there are characteristic absorption peaks of polysaccharides at 3 417.46, 2 928.65, 1 742.86, 1 643.69, 1 149.78, 1 078.19, 1 022.56 and 834.57 cm-1, of which there are absorption peaks of pyranose at 1 078.19 and 1 022.56 cm-1,and contain one characteristic absorption peak of α-pyranose indican band at 834.57 cm-1. The UV scanning spectrum shows the obvious polysaccharide absorption peak at 280 nm, and indicates the existence of CO bond.
2007 Vol. 27 (11): 2246-2248 [Abstract] ( 440 ) PDF (555 KB)  ( 553 )
2249 Raman Spectra of PAN-Based Carbon Fibers during Graphitization
LI Dong-feng1,2,3,WANG Hao-jing1,WANG Xin-kui1
Laser Raman spectroscopy was employed to characterize the structure of PAN-based carbon fibers during graphitization (2 000-3 000 ℃), and the spectra of the surface and the cross section of the fibers were compared. The results show that the Raman spectra of the fibers after graphitization can be separated as three bands (D, G and D′). The degree of disorder of the fibers can be measured by Raman spectra parameter, such as the full-widths at half maximum (FWHM) of D and G bands, Raman shift of G band, and the integrated intensity ratio in the form of R(ID/IG). Further investigation demonstrated that the FWHM of D and G bands, Raman shift of G band and the value of R decrease with increasing heat treatment temperature (HTT). The D band can be seen and the value of R is 0.19 even after being heat treated at 3 000 ℃, indicting that the fibers still have disordered carbons. In addition, the value of R is linearly related to the reciprocal of the basal plane length of the crystallites (La). The spectra of the surface and the cross-section of the fibers after graphitization show obvious difference. So the degree of graphitization and preferred orientation of carbon fibers can be quantitatively characterized by laser Raman spectroscopy.
2007 Vol. 27 (11): 2249-2253 [Abstract] ( 2346 ) PDF (1223 KB)  ( 591 )
2254 Research on Raman Spectra of 2-Methylpentaneat at Pressure of 0-1.5 GPa and Temperature of 26 ℃
LIU Jun-jie,ZHENG Hai-fei*
The present paper investigates the Raman spectral character of liquid 2-methylpentane by an experiment at the pressure of 0-1.5 GPa and the temperature of 26 ℃, and defines the relation between the pressure and the Raman peak of 2-methylpentane at ambient temperature. The result shows that there are five characteristic Raman peaks in 2-methylpentane defined as ν(CH2) and ν(CH3), and all of them move to high position as the system pressure increases. The relation between the system pressure and peaks positions is given as following: νas(CH3)=0.013 1p+2 960.1, νs(CH3)=0.008 8p+2 871.0, νas(CH2)=0.008 9p+2 930.2, νas(CH2)’=0.007 0p+2 903 and νs(CH2)=0.007 9p+2 844.7. On the other hand, 2-methylpentane is reliable as a liquid pressure gauge for high pressure experiment. The equation applied to demarcate system pressure is also showed: p(MPa)=76.2(Δνp)2 960+21.65(r2=0.995 8). This is probably the first organic liquid gauge, especially for systems not expected to emergence of Si, Al and hydroxyl matter.
2007 Vol. 27 (11): 2254-2257 [Abstract] ( 605 ) PDF (1224 KB)  ( 524 )
2258 Carotenoid Levels Measured by Resonance Raman in Vivo
SHAO Yong-hong1,HE Yong-hong1,MA Hui1*,NAN Nan2,QIAN Long-sheng2,WANG Shu-xia1
Carotenoid molecules are powerful antioxidants which can act as scavengers for free radicals, singlet oxygen, and other harmful reactive oxygen species in human body. Studies have shown an inverse correlation between the level of carotenoid and the risk of cancers, cardiovascular diseases, and degenerative diseases. High-performance liquid chromatography is used for measuring carotenoid levels as a standard method, but it is not noninvasive and real-time detecting. The authors have developed a novel noninvasive optical technology to measure carotenoid level in vivo by detecting the resonance Raman spectra, which can be used for high sensitivity and real-time detecting. When a low noise 473 nm laser with power less than the exposure limit set by ANSI Z136.1-2000 standards, a clearly distinguishable low resonance Raman spectra superimposed on a strong fluorescence background is produced. The carotenoid level is assessed by measuring the resonance Raman intensity. Using penetrating tissue technology, the authors improved the signal-to-noise ratio in the setup. The experimental results from different volunteers confirmed that the carotenoid level is proportional to the intake of it. The technology provided important values for clinic applications and science research.
2007 Vol. 27 (11): 2258-2261 [Abstract] ( 570 ) PDF (1014 KB)  ( 526 )
2262 Differentiating Gastric Cancer Cell from Normal Cell by Laser Raman Spectrum
HUANG Ying1,TAO Jia-you1,LIN Rong2,LI Yi1,HOU Xiao-hua2,YI Xin-jian1
The gastric cancer cell and normal cell were comparatively detected by means of laser Raman spectrum in the present paper. The special Raman spectrum wave crest of gastric cancer cell was inquired. It was found that the special Raman spectrum wave crest of gastric cancer cell differs from the one of normal cell. After the sample at concentration of 1.25×105 individual· mL-1 was cultivated for several days, a few special Raman spectrum wave crests of sample at 583, 633 and 656 nm respectively were detected. This is a few new special Raman spectrum wave crests rarely reported. Whether at the special Raman spectrum wave crests or at the same several Raman spectrum wave crests 674, 707, 773 and 799 nm for both canner cell and normal cell, the Raman spectrum intensity increases with the cancer cell concentration. As a result, the laser Raman spectrum analyse is considered truly a kind of rapid and effectual method to check cancer cell.
2007 Vol. 27 (11): 2262-2265 [Abstract] ( 1718 ) PDF (879 KB)  ( 526 )
2266 The Relationship between Structure and Oxygen Storage Capacity of CexZr1-xO2 Solid Solution
ZHAN Ying-ying,CAI Guo-hui,XIAO Yi-hong,ZHENG Qi*,WEI Ke-mei
Heating reflux aging technology was applied to prepare a series of CexZr1-xO2(0.25≤x≤1) solid solution. The effects of the CexZr1-xO2 composition on the structure and oxygen storage capacity were characterized using N2 physical adsorption, X-ray diffraction (XRD), FT-Raman, UV-Vis diffuse spectroscopy techniques. The texture, structure and thermal stability of ceria-zirconia mixed oxides are closely related to the ratio of cerium to zirconium in the solid solution, with increasing the zirconium content, the specific area increases, and the structure undergoes a change of order→disorder→order. Among them, Ce0.4Zr0.6O2 sample possesses the maximum OSC and Ce0.25Zr0.75O2 sample possesses the best thermal stability.
2007 Vol. 27 (11): 2266-2269 [Abstract] ( 618 ) PDF (1237 KB)  ( 541 )
2270 Study on Components in Shengli Viscous Crude Oil by FTIR and UV-Vis Spectroscopy
GUAN Run-ling,ZHU Hong*
The asphaltenes and resins in the Shengli viscous crude oil were studied by FTIR, UV-Vis spectrophotometry and synchronous fluorescence spectrometry in order to find out the polarity and the distribution of the number of the aromatic ring in the asphaltenes and resins. The results of FTIR spectrum showed that the molecules of the asphaltene and resin include hydroxy, amido, carboxyl and carbonyl, all of which can make up hydrogen bonds. This accounts for that there is the strong hydrongen bond interaction between the molecules of asphaltenes and those of resins. The structures of resins and asphaltenes were studied by synthetic analysis of the UV absorption spectrum and synchronous fluorescence spectrometry of asphaltenes and resins and by comparison with the model compounds. The results show that the aromatic sheet is the basic unit of the asphaltene and resin. The structures of resins and asphaltenes have similarity. The conjugated aromatic rings in the unit sheet are generally three rings and four rings, whose connection is linear order, namely cata-condenesed. The difference between asphaltenes and resins is that resins have generally less than five aromatic rings in conjugated aromatic unit, while asphaltenes have more than five aromatic rings. The asphaltenes have more conjugated aromatic units than the resins and their aromatic rings are plane order, namely peri -condensed approximate structure model for resins and asphaltenes was obtained by experiment.
2007 Vol. 27 (11): 2270-2274 [Abstract] ( 1257 ) PDF (1258 KB)  ( 566 )
2275 Study on Dynamic Spectral Characteristics of Humic Acid in Municipal Solid Wastes Composting
WEI Zi-min1,2,XI Bei-dou1,ZHAO Yue2*,WANG Shi-ping3*,LIU Hong-liang3,HE Lian-sheng1,JIANG Yong-hai1, HUO Shou-liang1
In the present study, the compost consisted of residual MSW with metal, plastic and glass removed. The composting process was assisted using industrial technology. During the composting, humic acid (HA) was extracted and purified. The spectroscopic characteristics of the HA were determined by using UV, FTIR, and fluorescence spectroscopy. During the composting process, the HA fluorescence spectra exhibited a sharp reduction in relative fluorescence intensity at the short wavelength region, and the primary peak shifted from 335 nm at the initial stage to 458 nm at the final stage of composting, thereby approaching the main peak at 460-480 nm for HA in soil. The FTIR spectra exhibited a reduction in polysaccharides and aliphatic components, and a relative increase in aromatic components; while the HA UV spectra revealed an increase in conjugation and the degree of humification. However, compared with the E4/E6 value and the spectroscopic characteristics of HA in soil, the HA in the MSW compost has a relatively low molecular weight, a simpler structure and a relatively low degree of aromatic condensation, which also implies that the HA in compost is highly active.
2007 Vol. 27 (11): 2275-2278 [Abstract] ( 1808 ) PDF (753 KB)  ( 562 )
2279 Spectral Properties of the Hemoporphyrin Derivative Interacting with Hemoglobin
FENG Shang-yuan1,2,CHEN Rong2*,YANG Wen-qin1,LI Yong-zeng2,HUANG Zu-fang2,LIAO Xiao-hua2
The quenching reaction of hemoporphyrin derivative with hemoglobin (Hb) was studied by using fluorescence spectra and absorption spectra.It was shown that HpD has a powerful ability to quench the Hb fluorescence via a nonradiative energy transfer mechanism. The formation constants of them were analyzed at different temperature according to Stern-Volmer equation and double-reciprocal equation，which are bigger at high temperature than at low temperature. The critical binding site was calculated (R0＝3.22 nm) by Fster energy transfer mechanism, and the thermodynamic parameters were obtained.
2007 Vol. 27 (11): 2279-2282 [Abstract] ( 1592 ) PDF (710 KB)  ( 532 )
2283 Preparation and Fluorescence Properties of Calix[4]arene Nanoparticle
LIU Chun, XU Hong-wei, YU Hua-peng, LU Qin, WANG Lun, ZHOU Yun-you*
Novel organic nanoparticles of calix[4]arene (CN) were prepared by the reprecipitation method under sonication and vigorous stirring. The nanoparticles showed an average diameter of 40 nm characterized by transmission electron microscopy. It was found that the nanoparticles exhibited better fluorescence compared with that of monomer. In weak acidic medium, the relative fluorescence intensity of these nanoparticles could be quenched remarkably with the addition of appropriate amounts of Fe3+. Based on the obtained results, a novel fluorimetric method has been developed for the rapid determination of Fe3+. Under optimal conditions, the linear range of calibration curves was 1.0×10-6-2.4×10-5 mol·L-1 and the detection limit was 3.0×10-7 mol·L-1. The proposed method was applied to determine Fe3+ in water samples with satisfactory recovery and relative standard deviation.
2007 Vol. 27 (11): 2283-2286 [Abstract] ( 1269 ) PDF (986 KB)  ( 533 )
2287 The Study on the Inueraction of FCLA with Human Serum Albumin with Spectroscopy Techniques
ZHOU Jing,WEI Yan-chun*
It is very important to detect reactive oxygen species (ROS) in biologic and medicinal research. FCLA, the Fluoresceinyl Cypridina Luciferin Analog, is a high sensitivity probe of detecting singlet oxygen and superoxide anions. The FCLA molecule can react with ROS and, after a series of reactions that result in the release of additional chemical energy, releases photons. Depending on the probe used, the photons are typically in visible wavelength range and easily measurable with conventional optical detectors. The binding reaction of FCLA with human serum albumin (HSA) was studied with spectroscopy techniques. It was found that HSA fluorescence was partially quenched by FCLA. The binding constants were obtained with quenching results. According to the Fōrster energy transfer mechanism, the energy efficiency and the distance between FCLA and HSA were calculated. Then it was found that static quenching was the main binding reaction between FCLA and HSA, and the energy transfer caused the HSA fluorescence quenching and the FCLA fluorescence producing. By studying the binding reaction of FCLA with HSA by spectroscopy techniques, this research proved the transfer style of FCLA and the interaction mechanism in the body. The results will offer some good advises about the ROS detection with the chemiluminesence probe in vivo. Meanwhile, it will also provide a new means to study pharmacokinetics and some basic theories about the medicine transfer in the body.
2007 Vol. 27 (11): 2287-2290 [Abstract] ( 1983 ) PDF (863 KB)  ( 450 )
2291 Photostability and Optical Limiting Cycling Behavior of Chloroindium (Ⅲ) Phthalocyanine
ZHEN Xiao, FENG Miao, ZHENG Chan, HUANG Juan, ZHAN Hong-bing*
Optical limiting (OL) cycling behavior of chloroindium (Ⅲ) phthalocyanine (InPcCl) solution was investigated by repeating Z-scan measurement up to 150 times, while photostability was characterized by changes in the UV-Vis absorption spectra during the process of laser irradiation and daylight illumination. The results show that InPcCl is stable against laser irradiation, leading to its good OL cycling behavior, although it features poor stability against daylight illumination. The possible mechanism behind this difference in photostability is proposed.
2007 Vol. 27 (11): 2291-2293 [Abstract] ( 1744 ) PDF (719 KB)  ( 543 )
2294 Study on the Binding Mode of Sulfated Chitosans with Nucleic Acids Using Spectral Analysis
ZHANG Hai-rong1,2,GUO Si-yuan2,LI Lin2,CAI Miao-yan2,ZHENG Bi-sheng2
The interaction of two kinds of sulfated chitosans with DNA was investigated using fluorescence spectra，absorption spectra, alkaline denaturation curves, ionic strength, fluorescence quenching etc. The results showed that there were two modes of the interaction between sulfated chitosans and DNA/ ethidium bromide(EB): intercalative and electrostatic binding. Hyperchromic and bathochromic effects in the absorption spectra were observed when sulfated chitosans with a low degree of substitution (CT-L) or a high degree of substitution (CT-L) were bound to herring sperm DNA. The stability of DNA/EB was increased with the increase in alkaline denaturation pH in the presence of CT-H and CT-L. Meanwhile, a weak interaction of cationic Mg2+ and phosphate groups of DNA by electrostatic force binding was observed. The fluorescence was efficiently quenched in the presence of a micro-amounts of sulfated chitosans, which confirmed that there was a strong competitive binding interaction among EB, CT-H or CT-L and DNA. All of these demonstrated that different sulfated chitosans can be used as a type of hopeful target-pointed molecule of gene therapy.
2007 Vol. 27 (11): 2294-2298 [Abstract] ( 1706 ) PDF (1047 KB)  ( 506 )
2299 Development of Fluorescence Polarization Immunoassay for Determination of Pesticides and Veterinary Drugs
WANG Zhan-hui1,ZHANG Su-xia1,SHEN Jian-zhong1*,Sergei A Eremin2
Fluorescence polarization immunoassay (FPIA) is a fast screening technique based on immune competition and fluorescence polarization principle and is most used in the determination of small molecular substance (antigen). FPIA is based on the increase in polarization of the fluorescence of small fluorescent-labeled antigen when bound by specific antibody. FPIA is a homogeneous technique and not affected by solution color and the sensitivity of instrument. No separation step is required for FPIA. Simplifying the assay and minimizing the analysis time are the most notable advantages of FPIA over other immunoassays and FPIA is suitable to screening a large number of samples. The technique has been applied to the determination of pesticides and veterinary drugs in environment and food samples, while no studies have been reported in the correlative field in China. The present paper presents the principle and history of FPIA and its application in the screening determination of pesticides and veterinary drugs.
2007 Vol. 27 (11): 2299-2306 [Abstract] ( 1129 ) PDF (1289 KB)  ( 471 )
2307 Study on the Characters of Phytoplankton Chlorophyll Fluorescence Excitation Spectra Based on Fourth-Derivative
LU Lu1,SU Rong-guo1,2,WANG Xiu-lin1,2*,ZHU Chen-jian1,2
Chlorophyll fluorescence excitation spectra of six phytoplankton species, belonging to Bacillariophyta and Dinophyta, were dealt by fourth-derivative analysis with the Matlab program. The results show that between 350 nm and 550 nm six fluorescence peaks were found in the fourth-derivative spectra, which are representatives of non-pigments, chlorophylls and carotenoides respectively. The method makes Bacillariophyta and Dinophyta more distinguishable when the fourth-derivative spectra are compared with the chlorophyll fluorescence excitation spectra. It can be used not only to discriminate the two groups of algaes, but also to reduce the effect of noise. The fluorescence peaks in the fourth-derivative spectra are proved to be stable.
2007 Vol. 27 (11): 2307-2312 [Abstract] ( 1224 ) PDF (2743 KB)  ( 590 )
2313 Fluorometric Determination of Fructose in the Presence of Glucose Using Zirconyl Chloride-Ammonium Chloride
TONG Lei1,WANG Yan-xin1,ZHAO Zhong-yi2,JIN Ji-hong2,GUO Xiao-hui2
According to the principle that Zn(OH)+ produced by ZrOCl2 upon hydrolysis in water can react to form a fluorescent derivative with fructose, a method for the quantitative determination of fructose has been proposed. The fluorescence of the derivative enhanced at 408 nm in NH4Cl medium has a direct ratio with fructose in the linear range of 0.5-25 μg·mL-1. When reaction conditions such as a temperature of 70 ℃ and a time of 15 min are used, the detection limits is 0.071 mg·mL-1. The proposed method was also applied successfully to the determination of fruit, satisfaction with high accuracy and good reproduction.
2007 Vol. 27 (11): 2313-2316 [Abstract] ( 1746 ) PDF (902 KB)  ( 465 )
2317 Study on the Interaction of Nimodipine and Bovine Serum Albumin by Fluorescence Quenching Method
WU Qiu-hua,WANG Chun,WANG Zhi*,SONG Shuang-ju
The interaction of Nimodipine and bovine serum albumin (BSA) was studied using fluorescence spectroscopy (FS) and ultraviolet spectroscopy (UV). The apparent binding constants (KA) between Nimodipine and BSA were 5.01×104(26 ℃) and 4.46×104(36 ℃), and the binding sites (n) were 1.08±0.01. According to the Frster theory of non-radiation energy transfer, the binding distances (r) were also obtained. The experimental results showed that Nimodipine could quench the inner fluorescence of BSA by forming the Nimodipine-BSA complex. It was found that both static quenching and non-radiation energy transfer led to the fluorescence quenching. The process of binding was a spontaneous molecular interaction in which entropy increased while Gibbs free energy decreased. The thermodynamic parameters indicated that the interaction of Nimodipoine and BSA was driven mainly by static electrical force.
2007 Vol. 27 (11): 2317-2320 [Abstract] ( 1200 ) PDF (852 KB)  ( 444 )
2321 Study on the Detection of Organic Pesticides by Fluorescence Spectra
WANG Zhong-dong1,LI Dong-ming1,WANG Yu-tian2
In the present paper the basic theory that organic molecules can emit fluorescence as they are excited by ultraviolet rays is described, the molecular structures of a few common pesticides, such as carbamate, benzoylurea and fungicide, are analyzed, and the mechanism of fluorescence generation is also ascertained. Consequently, the theoretic basis for further detection of pesticides by means of fluorescence methods is provided. Moreover a steady-state fluorescence spectrograph was applied to conduct fluorescence spectrum experiments with standard solutions of these pesticides, the fluorescence spectra were obtained, and their fluorescence characteristics were also analyzed. The results indicate that carbamate, benzoylurea and fungicide pesticides may emit strong fluorescence when excited by UV rays under the condition of a certain solvent, their fluorescence spectra are distinct, and the resolution is fine. As a result, it is feasible to carry out qualitative and the quantitative analysis of the concerned pesticides by fluorescence spectral analysis.
2007 Vol. 27 (11): 2321-2324 [Abstract] ( 379 ) PDF (1473 KB)  ( 521 )
2325 Resonance Scattering Spectral Study of IgA Immune Complex Particles and Its Analytical Application
LIANG Ai-hui1,WANG Na2,HOU Ming1
Based on the resonance scattering (RS) effect of immune complex particles, a new resonance scattering spectral method for the determination of trace IgA in the human blood serum was developed. It was based on that goat anti-human IgA was combined with the antigen of IgA. It is known that antibody has C-terminal and N-terminal and the N-terminal is binding site of antigen, and it could combine antigen. Because the stereo structure anastomoses and the charge are opposite between goat anti-human IgA and IgA, they could attract and combine each other. The attraction and combination have high idiosyncrasy and they are done by Val der Waals force, hydrophobic force, Coulomb attracting force and hydrogen bond binding force, and aggregate to form immune complex particles that exhibit three resonance scattering peaks at 340，390，420，450，470 and 520 nm respectively, in the pH 6.2 Na2HPO4-citrate buffer solutions and in the presence of polyethylene glycol (PEG) 4000. The laser scattering results indicate that the average diameter of the immune complex particles is about 1 100 nm. The influences of pH, PEG type and its concentration, goat anti-human immunoglobulin A concentration, incubation temperature and incubation time, foreign substance such as glucose, human serum albumin (HSA), urea and L-tyrosine were examined in details. Under the chosen conditions of pH 6.2 Na2HPO4-citrate buffer solutions-60 mg·mL-1 polyethylene glycol(PEG) 4000-0.35 mL anti-human immunoglobulin，the resonance scattering intensity at 340 nm ΔI340 nm and the resonance scattering intensity at 470 nm ΔI470 nm all are both proportional to the concentration of IgA in the range of 0.133-4.67 μg·mL-1. Its regress equation was ΔI340 nm=18.61 cIgA+3.19, ΔI470 nm=18.57cIgA+ 6.51，with a detection limit of 0.068 and 0.072 μg·mL-1,respectively. The assay has been applied to the analysis of IgA in human serum, which was also determined by the immunoturbidimetric method, with satisfactory results. The slope, intercept and correlation coefficient of the linear regress analysis were 1.064, -0.213 and 0.929 9, respectively.
2007 Vol. 27 (11): 2325-2328 [Abstract] ( 671 ) PDF (662 KB)  ( 455 )
2329 Tetrasulfophthalocyaninatozinc-Sensitized Titania Synthesized by a Novel In-situ and Self-Assembly Process and Photocatalytic Activity under Visible-Light Irradiation
ZHONG Chao-yang, PAN Hai-bo*,GUO Long-fa, HUANG Jin-ling
Tetrasulfophthalocyaninatozinc/titanium dioxide (ZnTsPc/TiO2) was synthesized by a novel in-situ and self-assembly process. The prepared products, including pure TiO2 and ZnTsPc, were characterized by XRD, UV-Vis, FTIR, Zeta potential and fluorescence spectroscopic techniques. The results indicated that ZnTsPc was indeed synthesized during the in-situ method and sol-gel process. A chemical bond (—SO2—O—Ti—) was also formed between the sensitizer (ZnTsPc) and the surface of titanium dioxide particles. The photocatalyst of ZnTsPc/TiO2 reveals greatly enhanced activity for the degradation of organic pollutant, Rhodamine B, under visible-light irradiation as compared with pure TiO2 and P25. The sensitization mechanism is that photo-generated charge carriers are separated by the chemical bond between ZnTsPc and TiO2.
2007 Vol. 27 (11): 2329-2332 [Abstract] ( 1720 ) PDF (1021 KB)  ( 501 )
2333 Determination of Trace Elements in Different Human Hair and the Comparison and Research on Living Environment
WANG Ying1,2,KANG Wan-li3,XIN Shi-gang2,XU Peng2
In the present paper, Chemometrics was applied to the determination of 20 kinds of trace elements in human hair by ICP-AES. The method was simple, rapid, highly sensitive and accurate. The determination of many elements could be performed at the same time. The recoveries of the method were in the range of 94.07%-107.6%, and the relative standard deviations were less than 3.49%. According to the results of 1 600 human hair samples with various ages from different regions, the influences of nutrition and environmental pollution upon human health were studied. Thereby, the comparison of and research on the living environment were carried out.
2007 Vol. 27 (11): 2333-2336 [Abstract] ( 529 ) PDF (470 KB)  ( 467 )
2337 Determination of Trace Lead in Traditional Chinese Herbal Medicine Astragalus by Microwave Digestion-CTAB Enhancing-Continual Flow Ingection Hydride Generation-ICP-AES
LIU Dong-lian1,2,KE Shao-ying1,YE Rong2,DING Ming-yu3
A new method using microwave digestion technique was developed for the determination of lead in Astragalus by CTAB enhancing-continual flow hydride generation-inductively coupled plasma atomic emission spectrometry(HG-ICP-AES). The experimental conditions of microwave digestion and hydride generation were optimized. This method shows a linear range of 0.23-800 μg·L-1and the correlation coefficient is 0.999 9. It is satisfactory to apply the microwave digestion procedure to the determination of Pb under the optimized conditions. The detection limit of the method is 0.23 μg·L-1 and the RSD is 1.02%. The recovery obtained is 98.8%-100.1%. The results show that this method is rapid and simple with low environmental contamination and complete digestion of samples.
2007 Vol. 27 (11): 2337-2340 [Abstract] ( 1766 ) PDF (813 KB)  ( 552 )
2341 Study on Determination of Rare Earth La and Ce in Feed by Using ICP-MS
WANG Pei-long,SU Xiao-ou*
An advanced method for the determination of rare earth La and Ce in animal feed by using of inductively coupled plasma mass spectrometry was studied. The operation parameters for ICP-MS was optimized, the effect of pre-mix feed matrix and formular feed matrix for La and Ce was studied by the conventional method and stepwise dilution method, and the suppression of signal intensity of La and Ce by nitric acid was examined. Under the optimum condition, the limit of determination for La and Ce were 2.62×10-2μg·kg-1 and 6.47×10-3μg·kg-1,respectively, the linear coefficient was 1.000 0, the dynamical linear range was of 3 order of magnitudes, and the internal standards were In(115) and Tb(159). The developed method was applied to the determination of rare earth La and Ce in pre-mix feed and formular feed, with the recovery ≥77.8% and the relative standard deviation(RSD) ≤8.5%, and the testing results were satisfactory.
2007 Vol. 27 (11): 2341-2344 [Abstract] ( 1102 ) PDF (950 KB)  ( 519 )
2345 Simultaneous Analysis of Multi-Elements in Vegetation Oils by Inductively Coupled Plasma Atomic Emission Spectrometry
GUO Lan1, 2,XIE Ming-yong1*,YAN Ai-ping2,XIAHOU Jian-yun2
A simple, accurate and sensitive method for the simultaneous analysis of eleven trace elements (Fe, Cu, Co, Ni, Pb, Al, Zn, Cd, Cr, Mn and Mg) in vegetation oils by ICP-AES has been developed. The oils were digested by H2SO4 ashing method. The detection limits (MDLs) of the method for the eleven elements were in the range of 0.1-3.6 μg·kg-1. The average recoveries at three concentrations of 0.1, 0.5 mg·kg-1 were between 70.4% and 113% with the RSD in the range of 1.01%-10.6%. The proposed method has been applied to the determination of the above elements in soy, peanut, sesame, rape, tea and blended oils with satisfactory results.
2007 Vol. 27 (11): 2345-2348 [Abstract] ( 264 ) PDF (501 KB)  ( 587 )
2349 Determination of Trace Barium in Soil and Sediment by Zeeman Graphite AAS with Coated Graphite Tube
JI Hai-bing,LIU Jin-song,PANG Xiao-lu
The sample was decomposed by HNO3-HF-HClO4. Using a tungsten-coated graphite tube, trace barium in soil and sediment was determined by Zeeman graphite AAS. To avoid producing carbide, the graphite tube was coated with tungsten. Tungsten and carbon in the surface layer of graphite tube became tungsten carbide. Tungsten carbide prevented barium and carbon from forming barium carbide, which in turn not only led to a long service life for the tube, but also increased greatly the sensitivity and precision of the determination Ba. Tungsten carbide belongs to internal filled type and can give reduction environment. To some extent, the common interfering elements co-existing in the soil and sediment had little chance to form oxides to interfere the determination of Ba in the atomization period. The method was easy and sensitive. The detection limit of Ba was 4.2×10-10g·g-1. The relative standard deviation (RSD) was in the range of 2.0%-6.5%(n=4). The relative deviations from the certificated values of standard soils were under 5%.
2007 Vol. 27 (11): 2349-2352 [Abstract] ( 1192 ) PDF (638 KB)  ( 538 )
2353 Determination of Lead and Cadmium in Rapeseed and Rapeseed Meal with Microwave Digestion by Graphite Furnace Atomic Absorption Spectrometry
HE Xiao-min1,WANG Min2,WANG Xiao-dong1,XUE Ai-fang1,LI Sheng-qing1,CHEN Hao1*
Comprehensive utilization of rapeseed and rapeseed meal has been increasingly emphasized, and contaminative problems of heavy metal have been attracting great attention, so it is of quite important significance to determine the contents of Pb and Cd. An effective method was developed for the rapid determination of Pb and Cd in rapeseed and rapeseed meal. Digestive dissolvent, time and pressure were discussed for sample preparation by microwave digestion technique, and the optimum condition of determination by GFAAS was studied. The determination limits were 2.172 and 0.243 μg·L-1,and the linear arranges were 0-100 μg·L-1 and 0-8 μg·L-1 for Pb and Cd, respectively. The recoveries were from 80.8% to 110.7%. The RSD of determination was lower than 5.3%. The method offers traits of low detection limit, high sensitivity, speediness and exactness, and was applied to the determination of Pb and Cd in samples with satisfactory results.
2007 Vol. 27 (11): 2353-2356 [Abstract] ( 628 ) PDF (723 KB)  ( 606 )
2357 Speciation Analysis of Zinc in Bunge Pricklyash Seed by AAS
TU Jian-bo1,WANG Si-wang1*,XIE Yan-hua1,LI Ding-chuan2,GAO Shuang-bin1,WANG Jian-bo1
A method was developed for the investigation of the contents and the speciation of zinc in bunge pricklyash seed (BPS) in different habitats by atomic absorption spectrum (AAS). By using 0.45 μm filter membrane and chloroform，four different species of the decoction of BPS, named the suspended，the soluble，the inorganic and organic species, were obtained, and the segregation analysis methods for those species were developed. The octanol-water system was proposed to simulate the distribution of decocted zinc in the stomach and the intestine of the human body. The results showed that the decocted zinc was the main content of the total zinc, and the contents of zinc were different in different habitats, but the percentages of decocted zinc and the organism zinc were similar. The recovery for the method was 97.5%-104.0% and the relative standard deviation was less than 2.36%. The results showed that the sensitivity and reproducibility of this method were excellent.
2007 Vol. 27 (11): 2357-2360 [Abstract] ( 1598 ) PDF (503 KB)  ( 508 )
2361 Determination of Trace Mercury Species in Water and Soil Samples with Atomic Fluorescence Spectrometry
HUANG Zhi-yong1,HUANG Zhi-tao1,ZHANG Qiang1,ZHUANG Zhi-xia2
With hydride generation-cold atomic fluorescence spectrometry (HG-AFS), the method of determining trace mercury species in water and soil samples in Jimei, Xiamen city, China was established. The content of inorganic mercury in water was measured by sample direct injection, while the total mercury was measured after digestion with the reagents of KBrO3-KBr. The soil samples were digested with microwave for total mercury measurement. Sequential extraction procedure was carried out for determining different mercuric species in soil samples. The results indicated that the mercury concentration of wastewater from chemical laboratory exceeded the limit of the integrated wastewater discharge standard of China (GB 8978—1996). It is one of the serious pollution sources of mercury in environment. The mercury contents from soil samples including the sideward soil of highway, the sea sediment and the garden soil were under the limits of relative national standards of China. However, attention should be paid to the accumulation of mercury in garden soil due to the artificial pollution. Meanwhile, the average recoveries for water and soil samples tested with adding standards were 93.7% and 93.8%, respectively. Meanwhile, the detection limits estimated with 3-fold standard deviation were 0.000 8 μg·L-1 for water and 0.072 3 μg·kg-1 for soil, respectively. The results indicated that the established method, with the merits of high sensitivity and precision, was suitable for the measurement of trace mercury species in environmental samples.
2007 Vol. 27 (11): 2361-2366 [Abstract] ( 566 ) PDF (1683 KB)  ( 555 )
2367 Novel Analysis Algorithms for Differential Optical Absorption Spectroscopy for Pollution Monitoring
ZHANG Xue-dian,HUANG Xian,XU Ke-xin*
Differential optical absorption spectroscopy, or DOAS, is a widely used method to determine concentrations of atmospheric species. The principle of DOAS for measuring the concentration of air pollutants is presented in briefly. Using the linear relationship between the area of the measured differential absorbance curve and that of the differential absorption cross-section curve as taken from the literature, an alternative method for calculating the gas concentration on the basis of the proportionality between differential absorbance and differential absorption cross section of the gas under study was developed. The method can be used on its own for single-component analysis or as a complement to the standard technique in multi-component cases. The procedure can be used with differential absorption cross sections measured in the laboratory or taken from the literature. In addition, the method provides a criterion to discriminate between different species having absorption features in the same wavelength range.
2007 Vol. 27 (11): 2367-2370 [Abstract] ( 1685 ) PDF (1225 KB)  ( 522 )
2371 Modulation of Polysaccharide Extracted from Laminaria on Phase Compositions of Urinary Crystal Calcium Oxalate
DENG Sui-ping, OUYANG Jian-ming*
The influence of sulfate polysaccharide (SPS) isolated from marine algae Laminaria japonica aresch on the growth of urinary crystal calcium oxalate (CaOxa) was investigated by means of X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, and atomic absorption spectroscopy. SPS can stabilize thermodynamic metastable calcium oxalate dihydrate (COD) crystals. As the concentration of SPS increases from 0 to 0.60 mg·mL-1,the mass percentage of COD crystals increases from 0 to 100%, and the relative supersaturation of calcium oxalate increases from 1.0 to 19.6. The ability of SPS to stabilize the existence of COD in aqueous solution and to increase the concentration of soluble calcium ions is favorable to the inhibition of CaOxa stone. Indicating that SPS is a potential green drug for prevention and cure of CaOxa urinary stones.
2007 Vol. 27 (11): 2371-2374 [Abstract] ( 1645 ) PDF (1128 KB)  ( 512 )
2375 Development of a High Resolution Simultaneous Microwave Plasma Torch Spectrometer
JIANG Jie1,HUAN Yan-fu1,JIN Wei2,FENG Guo-dong1,FEI Qiang1,CAO Yan-bo1,JIN Qin-han1,2*
A unique high resolution simultaneous microwave plasma torch (MPT) atomic emission spectrometer was developed and studied preliminarily. Some advanced technologies were applied to the spectrometer, such as echelle grating, UV-intensified CCD array detector, adjustable microwave generator, and water cooling system for the generator, etc. The detection limits of the spectrometer for some elements were determined, the spectral resolution and pixel resolution of the spectrometer were calculated, and an analysis of a practical sample was carried out. The preliminary results demonstrate that such simultaneous spectrometer has advantages of saving sample and time, possessing high sensitivity and resolution, and low-cost for the purchase and maintenance. Taking analytical figures of merit into consideration, the high resolution simultaneous MPT spectrometer will have extended application areas and greater competition potential as compared with sequential MPT spectrometers.
2007 Vol. 27 (11): 2375-2379 [Abstract] ( 1165 ) PDF (1428 KB)  ( 521 )
2380 Application of ICP-MS/ICP-AES to Detecting Factors Influencing the Quality of Nanfeng Orange
LIU Ping-hui1,2,RUI Yu-kui3*,ZHANG Fu-suo3
Nanfeng orange is a world famous fruits, but its quality changes remarkably with the producing area. The present paper studied the contents of heavy metal mineral elements and microelements in soil planting Nanfeng orange by ICP-MS/ICP-AES and in order to find the dominant factors that affect the quality of Nanfeng orange in soil. The results showed that the contents of B, P, K, Mg and Ca, especially B, P and K were much higher in soil where the quality of Nanfeng orange is palatable than those where Nanfeng orange is unpalatable; but the contents of Fe, Mn, Si, Cu and Zn were lower in soil where the quality of Nanfeng orange is palatable than those where Nanfeng orange is unpalatable. These data indicate that B, P, K, Mg and Ca, especially B, P and K, affect the quality of Nanfeng orange significantly.
2007 Vol. 27 (11): 2380-2381 [Abstract] ( 2232 ) PDF (266 KB)  ( 594 )

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