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2005 Vol. 25, No. 04 Published: 2005-04-26

光谱学与光谱分析

	481	Magnetic Properties and Transport Behaviors in Double Doped La_0.67+1.33xSr_0.33-1.33xMn_1-xMg_xO₃ System
		CAI Zhi-rang¹，TONG Wei²，ZHANG Meng²，ZHANG Bei²，LIU Ning^1，2，ZHANG Yu-heng²
		The M-T curves, M-H curves, ESR curves, infrared spectrum, Raman spectrum, ρ-T curves and MR-T curves of La_0.67+1.33xSr_0.33-1.33xMn_1-xMg_xO₃(0.00≤x≤0.25) were studied. The experiment pointed out that all samples exhibit a paramagnetic-ferromagnetic(PM-FM) transition associated with metallic-insulating(MI) transition in the low doping region, which does not occur in the heavy doping zone. The authors suggest that this behavior is attributed to the difference between the Jahn-Teller distortion of the Mn³⁺ ion neighboring Mg²⁺ and that of the Mn³⁺ ion non-neighboring Mg²⁺, which is confirmed by the IR and Raman spectra. The anomalous transport behavior is dominated by the differerent Jahn-Teller distortion.
		2005 Vol. 25 (04): 481-486 [Abstract] ( 1581 ) PDF (808 KB) ( 344 )

	487	Fabrication and Study of Sputtered NbN Thin Films
		PENG Song, XIAO Bin-ping, HAO Jian-kui, XIE Da-tao^*
		In this work the authors discussed the fabrication of NbN thin films deposited using two methods: reactive magnetron sputtering system and DC bias-voltage sputtering system. The thickness and the surface morphology of the thin films were measured and observed by SEM. The crystalloid structure was analyzed by X-ray diffraction(XRD). The authors also measured the critical temperature(T_c) of the thin films. The authors compared the characters of NbN thin films that the authors prepared through two methods. The results showed that the films the authors prepared were uniform, compact, well constructed and sing-phase FCC δ-NbN. It is shown that the deposition temperature and the flux of N₂ have a strong effect on the preferred orientation, while the critical temperature of the films is influenced by the quality of the original vacuum.
		2005 Vol. 25 (04): 487-490 [Abstract] ( 1004 ) PDF (662 KB) ( 370 )

	491	Energy Pooling Collisions for K(4P)+Cs(5D) in a K-Cs Mixture
		Pulati·AIHEMAITI, DAI Kang, LU Xin-hong, SHEN Yi-fan^*
		The rate coefficients for energy-pooling collisions K(4P)+Cs(5D)→Cs(6S)+K(4D, 6S) in the K-Cs vapor mixture were measured relative to a known energy-pooling rate coefficient of a homonuclear reaction [i.e., Cs(6P)+Cs(5D)→Cs(6S)+Cs(7D_J)]. Populations of the Cs(6P, 5D) and K(4P) states were produced by photodissociation of K₂ and Cs₂ molecules through the use of a dye laser radiation. The resulting fluorescence included the direct components emitted in the decay of the excited states produced by photodissociation and the induced components arising from the collisionally populated states. By combining relative intensities of the components with the effective lifetimes of Cs(6P) and K(4P) states, the rate coefficients (in units of 10^-9 cm³·s^-1) for the heteronuclear energy-pooling were found to be 2.6 and 3.6, respectively. The contribution to the rate coefficients from other processes are discussed.
		2005 Vol. 25 (04): 491-493 [Abstract] ( 961 ) PDF (280 KB) ( 356 )

	494	Mean Temperature of Electron Determined by Atomic Hydrogen Emission Line in EACVD
		SHANG Yong, DONG Li-fang^*, WANG Zhi-jun
		The process of atomic hydrogen emission in CH₄/H₂ gas mixture in EACVD is simulated by Monte Carlo method. In the simulation the collision between electron and H₂ molecule has two basic types: elastic collision and inelastic collision. Four types of inelastic processes have been considered, namely vibrational excitation, dissociation, electron excitation and ionization. For e-CH₄ collision, elastic momentum transfer, vibrational excitation, dissociation, ionization and dissociation ionization are considered. The relationship between the ratio of atomic hydrogen emission line intensity and mean temperature of electron under different CH₄ concentration in the gas mixture is investigated. A method of determining the mean temperature of electron in situ in the process of diamond film deposited by EACVD is given. The result is of great importance to depositing high quality diamond films by controlling the conditions of technology efficiently.
		2005 Vol. 25 (04): 494-496 [Abstract] ( 924 ) PDF (250 KB) ( 330 )

	497	Studies on the Relation between the Temperature of KTP and the Secondary Harmonic Output
		ZHANG Hui¹, PENG Yue-xiang², SHEN Nai-zheng¹
		Using the Nd:YVO₄-KTP ring frequency-doubled laser designed by the lab, and controlling the laser power current and the crystals temperature accurately, the authors obtained the relation between the temperature changes of KTP crystal and the secondary harmonic output wavelength while the temperature of YVO₄ was constant.
		2005 Vol. 25 (04): 497-498 [Abstract] ( 1501 ) PDF (240 KB) ( 321 )

	499	Photoluminescence Spectra of Trivalent Neodymium Doped TiBa Glass Microspheres
		WANG Ji-you¹，HAO Wei¹，ZHAO Li-juan², LU Ying³
		In this work, TiBa glass microspheres doped with Nd³⁺ for morphology-dependent resonances of emission were designed and prepared. The emission spectra of TiBa glass plate and TiBa glass microspheres (45 and 13 μm in diameter) under 514 nm excitation were measured. The authors observed many regularly spaced, sharp peaks in the emission spectra of a Nd³⁺-doped glass microsphere. Based on the Mie scattering theory, the wavelength separation between the adjacent resonant peaks for the 45 μm sphere was calculated to be 3.0 for 810 nm. This value agrees well with the observed peak separation (3.1 nm), which indicates the contribution of the whispering gallery modes. The emission intensities of a Nd³⁺-doped TiBa glass microsphere (13 μm in diameter) in the 901.69 nm region were plotted against the excitation laser power. The emission intensities of the microsphere exhibit the linear dependence at the low excitation power (＜2 mW). The 901.69 nm emission intensity of the microsphere steeply increases at the excitation power of 2 mW, which can be ascribed to the laser operation.
		2005 Vol. 25 (04): 499-501 [Abstract] ( 389 ) PDF (311 KB) ( 374 )

	502	Study on Multi-Photon Excited Fluorescence Combined with Capillary Electrophoresis
		SUN Yun-xu, ZHU Feng, MA Wan-yun^*
		This paper describes a new method, multiphoton excitation fluorescence detection combined with capillary electrophoresis separation. The excitation source was a self mode-locked femtosecond titanium-sapphire laser (Spectra-physics Inc.), producing a stream of pulses with a pulse duration of about 100 fs at 82 MHz repetition rate. Its average power was about 200 mW at 750 nm. The laser beam was focused into a thin wall flow cell of capillary electrophoresis. A high numerical aperture objective (100×NA 1.25) was chosen to focus the laser beam and to collect the fluorescence emitted by detecting molecules. Then the fluorescence was detected by a fast response PMT. All data were acquired and processed by a microcomputer. For three biological molecules, 5HT, FAD and NADH, it was demonstrated that they can be separated and detected efficiently by this method with three-photon and two-photon excitation respectively using only one 750 nm laser beam. The detection limits were 1.0×10^-６ mol·L^-1 for 5HT, 7.4×10^-７ mol·L^-1 for FAD and 9.8×10^-７ mol·L^-1 for NADH using the criterion of three standard deviations above background. The results are much better than those with UV absorption detection by one or two magnitudes.
		2005 Vol. 25 (04): 502-505 [Abstract] ( 1021 ) PDF (404 KB) ( 350 )

	506	Photoluminescence of Nano-SiC Annealed by Pulse Laser
		YU Wei，HE Jie，SUN Yun-tao，HAN Li, FU Guang-sheng
		Nanocrystalline silicon carbon (nc-SiC)from amorphous silicon carbon films was obtained through XeCl excimer laser annealing. The photoluminescence (PL) of the nc-SiC was analyzed at different annealing laser energy density. It was observed that PL presented a wide luminescence band from 300-600 nm in the nc-SiC films. The two main luminescence bands, situated at 398 and 470 nm respectively, are attributed to band to band and defect recombination in the 6H-SiC based on the structure changes of the nc-SiC films. The relative PL intensity of these two bands was determined by the surface state density in the nc-SiC films and their irradiative life time.
		2005 Vol. 25 (04): 506-508 [Abstract] ( 1019 ) PDF (449 KB) ( 382 )

	509	Multiple Emissions in Organic Electroluminescent Device Using a Mixed Layer as an Emitter
		ZHU Wen-qing, WU You-zhi, ZHENG Xin-you, JIANG Xue-yin, ZHANG Zhi-lin, SUN Run-guang, XU Shao-hong
		A organic electroluminescent device has been fabricated by using a mixed layre as an emitter. The configuration of the device is ITO/TPD/TPD: PBD(equimole)/PBD/Al, in which TPD (N, N′-diphenyl-N, N′-bis(3-methylphenyl)-1, 1′-biphenyl-4, 4′-diamine) and PBD(2-(4′-biphenyl)-5-(4″-tert-butylphenyl)-1, 3, 4-oxadiazole) are used as hole transport material and electron transport material, respectively. Broad and red-shifted electroluminescent spectra related to the fluorescence of constituent materials were observed. It is suggested that the monomer, exciplex and electroplex emissions are simultaneously involved in EL spectra by comparison of the EL with the PL spectra and decomposition of the EL spectrum. The type of exciplex is the interaction between the excited state TPD(TPD^) and PBD in the ground state, and the type of electroplex is a (D⁺-A^-)^ complex by cross-recombination of hole on the charged hole transport molecule(D⁺) and electron on the charged electron transport molecule(A^-). All types of excited states show different formation mechanisms and recombination processes under electric field. The change of emission strengths from monomer and excited complexes lead to a blue-shift of the emissive spectra with an increasing electric field. The maximum luminance and external quantum efficiency of this device are 240 cd·(cm²)^-1 and 0.49%, respectively. The emissions from exciplex or electroplex formation at the organic solid interface generally present a broad and red-shifted emissive band, providing an effective method for tuning of emission color in organic electroluminescent devices.
		2005 Vol. 25 (04): 509-511 [Abstract] ( 1660 ) PDF (342 KB) ( 356 )

	512	Research on Noninvasive Blood Glucose Measurement with Simulate Sample by NIR Spectroscopy
		ZHANG Yue¹，Lü Li-na²，XU Ke-xin^2*
		The article puts milk forward as simulate sample for blood glucose measurement. With the new simulate sample, the authors make deep researches on measuring method and wavelength choice in the field of noninvasive blood glucose measurement by near-infrared diffuse reflectance spectroscopy. Depending on the absorption coefficient of lactose, the authors choose the two wavebands from 1 560 to 1 750 nm and form 2 090 to 2 190 nm. The model was built by partial least-squares(PLS), several pretreatment methods (including multiplicative scatter correction，first derivative and vector normalization) and different spectral regions were compared. The best correlation values for lactose were 0.99 and the best RMSEP values for lactose were 0.045. The results provide us with valuable theory reference and practical experiences and lead us to next research on noninvasive blood glucose measurement.
		2005 Vol. 25 (04): 512-515 [Abstract] ( 1738 ) PDF (452 KB) ( 406 )

	516	Near Infrared Spectra (NIR) Analysis of Octane Number by Wavelet Denoising-Derivative Method
		TIAN Gao-you¹, YUAN Hong-fu¹,CHU Xiao-li¹, LIU Hui-ying², LU Wan-zhen¹
		Derivative can correct baseline effects and also increase the level of noise. Wavelet transform has been proven an efficient tool for de-noising. This paper is directed to the application of wavelet transfer and derivative in the NIR analysis of octane number (RON). The derivative parameters, as well as their effects on the noise level and analytic accuracy of RON, have been studied in detail. The results show that derivative can correct the baseline effects and increase the analytic accuracy. Noise from the derivative spectra has great detriment to the analysis of RON. De-noising of wavelet transform can increase the S/N and improve the analytical accuracy.
		2005 Vol. 25 (04): 516-520 [Abstract] ( 1448 ) PDF (456 KB) ( 415 )

	521	Identification of Rhubarb Samples Based on IR Spectra by Using Takagi-Sugeno Fuzzy Systems
		TANG Yan-feng¹, ZHANG Zhuo-yong^1*, FAN Guo-qiang²
		Takagi-Sugeno fuzzy system is composed of several back-propagation neural networks (BP-NNs), and has some fuzzy logic properties. In this paper, the Takagi-Sugeno fuzzy logic system is applied to identifying official and unofficial rhubarb samples based on their infrared spectra. The effects of the number of hidden neurons and the momentum parameters on the prediction were investigated. The results obtained by using Takagi-Sugeno fuzzy system were better than those by commonly used BP-networks. With a proper network training parameter, 100% correctness can be obtained by using Takagi-Sugeno fuzzy system. This method is more accurate than the common methods, and is more scientific than traditional methods. So it is applied to identifying rhubarb easily and rapidly.
		2005 Vol. 25 (04): 521-524 [Abstract] ( 556 ) PDF (468 KB) ( 354 )

	525	Detrended Correspondence Analysis of Phenetic Relationships of Bryophytes Based on FTIR Spectra
		GUO Shui-liang^{1, 2}, CAO Tong²，CHENG Cun-gui¹
		Bryophytes are important high plants. However, the plants of bryophyte are small in size with few identification characters. The identification of plant samples using Fourier transform infrared spectrometer with OMNI collector is simple, convenient，fast and accurate. In the present paper, Fourrier transform infrared spectrometer with OMNI collector was applied to gain the infrared spectra of 30 samples belonging to 26 bryophyte species. Based on the indices of wave number-absorbance, the differences of the 30 infrared spectra were compared by the method of Detrended Correspondence Analysis (DCA). The results showed that there is good correspondence between the position relationship of DCA two-dimensional plot of the samples based on the indices of wave number-absorbance of FTIR spectra and their classification relationship. Therefore, it is practical to apply the infrared spectra to identifying the false sample from the true one in medicine bryophytes.
		2005 Vol. 25 (04): 525-528 [Abstract] ( 975 ) PDF (472 KB) ( 319 )

	529	Structure Analysis on Growth Solid-Liquid Boundary Layer of BSO Crystal at Real Time
		QIU Huai-li¹, WANG Ai-hua¹, YOU Jing-lin², CHEN Hui²，YIN Shao-tang¹
		The micro Raman spectra of solid-liquid boundary layer, the melts and crystal side, were measured at real time, concerning BSO crystal grown with zone-melting method. The structure characters in boundary layer, melts and crystal were analyzed. The process, of which the growth unit structure changed while they transited from melts through boundary layer to crystal lattice, was analyzed. The results show that, there exists Bi₃O₄ and [SiO₄] bonding structure in the melts of BSO crystal.While in the solid-liquid boundary layer, the Bi₃O₄ molecular units converge into [BiO_７] octahedron monomer of polymer in form,the monomer or the polymer converge with the [SiO₄] structure units, then all these converged structure enter into crystal lattice sites.
		2005 Vol. 25 (04): 529-531 [Abstract] ( 653 ) PDF (392 KB) ( 366 )

	532	Raman Spectroscopy Studies on the Aqueous Solutions of Sodium Formate and Lithium Formate
		SU Jing^{1, 2}, YU Xi-ling^{1, 2}, YOU Jing-lin³, YIN Shao-tang^{1, 2}
		The structures of the aqueous solutions of sodium formate and lithium formate are studied according to the growth conditions of the crystals under different supersaturations and temperatures by Raman spectroscopy. The effects of temperature, concentration, supersaturation and cation on the structures of solutions and the structure difference between lithium formate solution and lithium formate monohydrate crystal are analyzed. The result shows that the concentration，temperature and supersaturation effect the structures of the solutions slightly and the cation effects the frequency of the bands greatly.
		2005 Vol. 25 (04): 532-536 [Abstract] ( 1448 ) PDF (558 KB) ( 478 )

	537	Spectral Study on Intermolecular Coupling Interaction and Relation to Microstructure in Polyester/Inorganic Hybrid Materials
		NIE Kang-ming^{1, 2}, PANG Wen-min¹, WANG Yu-song¹, LU Fei¹, ZHU Qing-ren¹
		The coupling form of the polymeric-inorganic component and the relation between intermolecular special hydrogen bonding interaction and the microstructure of crystallizable polymer, as well as micro-phase separation scale in non-covalently coupled poly(ε-caprolactone) (PCL)/silica (SiO₂) hybrid materials were investigated by means of Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible (UV-Vis) spectroscopy, wide angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC). The results show that the coupling form between PCL and SiO₂ mainly depend on a strong intermolecular hydrogen bonding interaction in the hybrid system. The hydrogen bonding strength increases with increasing TEOS content, while the crystallization of PCL decreases, and the optical transparency of hybrid materials increases. In addition, it affects the scale of micro-phase separation in hybrid materials.
		2005 Vol. 25 (04): 537-540 [Abstract] ( 1503 ) PDF (524 KB) ( 330 )

	541	Study on the Method to Adjust Optical Fiber’s Spectrum Attenuation with the Fourier Transform
		MENG Xian-jiang¹，ZHANG Tie-qiang²，SHI Wei-jie³，SHEN Xuan-guo¹
		A method based on Fourier transform to compensate the non-linear attenuation of optical fiber used as a probe in a spectrum-collecting system was proposed. First the output electric currents of photoelectric tube with and without fiber were transformed to the frequency field. So a adjustable function in frequency field was obtained, and the adjustable function was transformed to the spectrum field, so the final adjustable function was obtained. A photoelectric system was designed for testing. With visible light, this method can make the error rate of fiber transmission as low as less than 1.54%. It is proved that the method is fit for adjusting some optical fiber spectrum attenuation.
		2005 Vol. 25 (04): 541-543 [Abstract] ( 306 ) PDF (329 KB) ( 330 )

	544	Hydrogen-Bond State Analysis of CellobiohydrolaseⅡ Molecule from Trichoderma Viride
		YU Duo-wei，YUAN Sheng
		Hydrogen-bond states on cellobiohydrolase Ⅱ (CBHⅡ) of trichoderma viride were analysed by laser Raman spectroscopic method used to reveal molecular normal modes of vibration character. The results indicated that hydrogen-bond ability of carbonyl oxygen-atom of amideⅠ was raised in two types of aqueous solution samples(6.0 and 8.0 of pH value) compared to the solid sample. The variation trend of β structure modes was similar between amideⅡ and amideⅠ. As far as the ability of hydrogen-bond forming is concerned, tryptophan (Trp) and tyrosine (Typ) residues are strong hydrogen proton donor in pH 6.0 and solid sample，thus proving the results of previously spatial structure analysis. By analysis of free S—H character，the —S—S— construction in trichoderma viride mature paptide has been proved to be the same as that of trichoderma reesei.
		2005 Vol. 25 (04): 544-547 [Abstract] ( 211 ) PDF (486 KB) ( 345 )

	548	Ion Solvation and Ion Association in High-Concentration of NaBF₄ /DMF Solutions
		XUAN Xiao-peng^{1, 2}, TANG Jun-ming¹, WANG Jian-ji^1*, WANG Han-qing²
		Ion solvation and ion association in solutions of NaBF₄/DMF were studied by infrared and Raman spectroscopy and ab initio quantum chemistry. It was found that the sodium cation interacts on oxygen atom of CO group in DMF molecules. The solvation number of Na⁺, four, was obtained according to the change analysis of CH₃ rocking band. The splitting of the ν₁ mode of BF^-₄ anion indicates the presence of contact ion pairs. Ionic association degree increases with increasing molality of the salt. The solvated structure of Na⁺ and the geometry of Li⁺BF^-₄ ion pair were also suggested based on the ab initio calculations.
		2005 Vol. 25 (04): 548-552 [Abstract] ( 1528 ) PDF (596 KB) ( 356 )

	553	Synthesis of Ag₂S Nanoparticles at Room Temperature and Their Characterization with XPS
		YE Yin, SHAO Ming-wang^*, WU Zheng-cui, NI You-bao
		Nanocrystalline silver sulfide was successfully synthesized at room temperature and ambient pressure via a novel, safe, convenient and inexpensive redox reaction, using silver oxide, sulfur and polyformaldehyde as reactants and ethylenediamine as solvent. The products were characterized with XPS, XRD and TEM. XRD spectrum demonstrates a monoclinic Ag₂S; TEM shows the products are rod-like nanoparticles with average diameter of 100 nm, its corresponding SAED reveals clear diffraction spots indexed as (120) and (3-03); XPS confirms the formation of Ag₂S and indicates the sample’s surface stoichiometry of Ag∶S=1∶0.453. The control experiments show polyformaldehyde and ethylenediamine are both important in the formation of products. Ethylenediamine accelerates the reactions via dissolving silver oxide and sulfur and neutralizing the by-product formic acid.
		2005 Vol. 25 (04): 553-555 [Abstract] ( 1649 ) PDF (437 KB) ( 362 )

	556	Direct Determination of Nb in Titanium Oxide Using Slurry Sample Introduction by Axial Viewing Inductively Coupled Plasma Optical Emission Spectrometry
		WANG Zheng^{1, 2}, CHEN Tian-yu¹, TAO Guang-yi¹，YANG Peng-yuan^2*
		By using dispersant polyacrylate amine (NH₄PAA) to disperse TiO₂, effects of different dispersants, pH value and the amount of dispersant on TiO₂ slurry were investigated. The pH value of the medium and the dispersant amount were optimized, and a stable and homogeneous suspension was prepared. Nb in TiO₂ was determined by an axial viewing ICP-OES spectrometer. At the same time, the performance of the axial viewing ICP-OES using solid powder analysis was discussed. Under the optimum experimental conditions, the detection limit of the present method is 3.0 μg·L^-1 and the RSD is 3.1%(n=3, c=0.3 mg·L^-1).
		2005 Vol. 25 (04): 556-559 [Abstract] ( 1053 ) PDF (473 KB) ( 362 )

	560	*Determination of Constant and Trace Elements in Ranunculus Ternatus Thunb* by ICP-AES**
		CHEN Jun¹，YAO Cheng^1*，OUYANG Ping-kai²
		The determination of twenty one kinds of constant and trace elements in Chinese herb Ranunculus ternatus thunb was performed by ICP-AES. The results show that K, Fe, Ca, Cr, Mg, Mn, Zn, Co, Cu, Ni, Se and Sr are relatively rich in Ranunculus ternatus and the content of Pb, Cd and As are very low. The ratio of the content of Zn to that of Cu is about 3, which is consistent with the relative content level of Zn and Cu contained in many anticancer Chinese traditional plants.
		2005 Vol. 25 (04): 560-562 [Abstract] ( 1858 ) PDF (293 KB) ( 343 )

	563	Comparison of Different Digestion Methods Used for the Decomposition of Plant Samples in Elemental Quantification by Using ICP-AES
		WANG Xiao-ping
		Four digestion methods were used for the decomposition of plant samples. The contents of Al, B, Ba, Ca, Cu, Fe, K, La, Mg, Mn, Na, P, Pb, Sr, Ti and Zn in the two Standard Reference Materials 1573a (Tomato Leaves) and 1575(Pine Needles) were determined by using ICP-AES and the determined values were compared with the certified ones. It was demonstrated that hydrofluoric acid is of vital importance in the decomposition of plant samples, because it can remove silicious materials from the matrix. Appropriate selection of digestion methods can improve greatly the accuracy of elemental quantification in plant samples.
		2005 Vol. 25 (04): 563-566 [Abstract] ( 1040 ) PDF (376 KB) ( 354 )

	567	GFAAS Determination of Trace Amount Cadmium in Chitosan by Micro Wave
		WENG Di，ZHAI Guo-qing
		In this work, a method had been developed for determination of cadmium in chitosan by means of graphite furnace atomic absorption spectrometry with micro wave digestion, a systematic study was carried out by selection of the most appropriate working conditions and optimization of the sample mass. The samples were digested by micro wave with mixed acid of HF-HClO₄(1∶2). Trace amount cadmium has been determined by Graphite Furnace Atomic Absorption Spectrometry(GFAAS) with Pd(NO₃)₂ as a matrix modifier. If appropriate working conditions are chosen, the method finally proposed shows interesting features for the determination of the analytics in the samples such as: suitable precision values (R.S.D-2.8%) and the recover rate by standard addition is 97.0%-106.3%. The method is simple, rapid and with accurate results.
		2005 Vol. 25 (04): 567-569 [Abstract] ( 1598 ) PDF (347 KB) ( 345 )

	570	Direct Determination of Trace Lead in Chestnut by Graphite Furnace Atomic Absorption Spectrometry with Slurry Sampling
		SONG Guang-sen
		A method for the direct determination of trace lead in chestnut by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) with slurry sampling was developed in the present paper. Ammonium ortho-phosphate was used as a matrix modifier. The effects of slurry preparation, particle size of sample, matrix modifier, ashing temperature, atomization temperature, and common coexisting components on the determination of lead were studied. Under the optimized operating conditions, the detection limit, the relative standard deviation (RSD), and the recoveries of standard addition for this method were 0.47 ng·mL^-1, 6.1% (n=11) and 90%-106%, respectively.
		2005 Vol. 25 (04): 570-572 [Abstract] ( 1022 ) PDF (339 KB) ( 331 )

	573	Determination of Pb and Al in Blood and Hair of Child Using Transverse Heated Graphite Furnace Atomic Absorption Spectroscopy
		NIU Feng-lan¹，XIE Wen-bing²，LI Chen-xu¹，DONG Wei-yan¹
		Pb and Al in blood and hair of child were determined by transverse heated graphite furnace atomic absorption spectrometry with NH₄H₂PO₄ and Mg(NO₃)₂ as a modifier，which enhanced the temperature of ashing, eliminated the matrix interference and memorial effect. The method is rapid, simple and accurate. The characteristic mass of the method was 2.3×10^-11 g and 2.2×10^-11 g for Pb and Al respectively. The relative standard deviation of Pb and Al was 3.0% and 11.4%, respectively, and the recovery was 96%-102%.
		2005 Vol. 25 (04): 573-575 [Abstract] ( 1984 ) PDF (304 KB) ( 333 )

	576	Determination of Trace Cobalt in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point
		ZHANG Yuan, LUO Wen-hong^*, LI Hui
		In buffer solution of citric acid monohydrate-disodium hydrogen phosphate at pH 5-7.5, cobalt water samples were chelated by 1-(2-pyridylazo)-2-naphthol(PAN) to form Co-PAN. After water-bath at 66 ℃ for two hours, Co-PAN is extracted into Triton X-100 nonionic surfactant phase and separated from bulk water. Extracted cobalt content was measured by graphite furnace atomic absorption spectrometry. The surfactant phase separated was treated with 0.5% HNO₃-0.1% Pd(NO₃)₂ to remove background interference at 1 200 ℃ temperature. The pre-concentration of cobalt in water samples permitted the detection of 0.003 μg·L^-1(10σ) with the enhancement factor of 100. The recoveries were 90.5%-106%. The proposed method was applied to the determination of cobalt in water samples and satisfactory results were obtained.
		2005 Vol. 25 (04): 576-578 [Abstract] ( 981 ) PDF (393 KB) ( 363 )

	579	Spectroscopic Studies on Different Chemical Composition between the Shell and Core of Radix Notoginseng
		LIU Zhi, LI Sai-jun, TIAN Hong-bo, XU Yi-zhuang, WU Jin-guang^*
		Notoginseng(Sanqi) is one of the most important components of famous Chinese recipe(Yunan Baiyao) and possesses a wide variety of applications in clinical practice. It has been found that Sanqi of different size exhibits different curative effects. Such a phenomenon may be attributed to that the chemical constituent from shell region is different from that of core region. To prove the above-mentioned hypothesis, Ultraviolet-Visible(UV-Vis), FTIR, fluorescence spectroscopy, together with high performance liquid chromatography(HPLC) and electrospray ionization mass spectroscopy(ESI-MS) were utilized to study the variation of chemical compositions from shell and core regions of Sanqi. The results demonstrate that the chemical compositions of Sanqi from shell and core regions are different. In summary，differences in chemical composition between Sanqi shell and core were manifested from versatile aspects. Such differences shed a light on the different curative effects of Sanqi.
		2005 Vol. 25 (04): 579-583 [Abstract] ( 562 ) PDF (758 KB) ( 351 )

	584	Fluorescence Spectra and Protonation of Ofloxacin
		LIU Cui-ge^{1, 2}, XU Yi-zhuang^1*, WEI Yong-ju², QI Jian¹, XU Zhen-hua¹, YE Fang³, WU Jin-guang¹
		Fluorescence spectra, ultraviolet spectra and protonation of Ofloxacin (OFL) at different pH values have been studied. In strong acidic solutions, OFL molecule might accept two protons to exist as ternary acid H₃L²⁺ with a maximum emission wavelength (λ_max) at 505 nm. Along with the increase in pH value, fluorescence spectrum of OFL changed, an iso-fluorescence point at 352 nm was found in the fluorescence excitation spectra, and at the same time, isosbestic points were found in its UV absorption spectra. This spectral feature reveals that H₃L²⁺ gradually lost hydrogen ion combined on C-4 keto oxygen. In the range of pH 2.5 to pH 4, OFL exists as H₂L⁺ with λ_max at 499 nm. When pH＞4, the fluorescence emission peak at 499 nm gradually blue-shifted to 455 nm as pH was increasing, and an iso-fluorescence emission point was formed at 484 nm，indicating the dissociation of hydrogen ion of carboxylic acid at C-3. At about pH 7.0, OFL exists in the dipole ion form HL with λ_max at 455 nm, which is the strongest fluorescence form. When pH＞8, λ_max red-shift from 455 to 475 nm as pH increases, meanwhile, fluorescence intensity decreases, indicating that HL lost hydrogen ion combined on N-4 of piperazinyl group. When pH＞10, OFL exists in anion ion form L^-，and fluorescence intensity decreases with pH increasing, but λ_max remains essentially constant, indicating that medium environment influences the fluorescence property of OFL.
		2005 Vol. 25 (04): 584-587 [Abstract] ( 2489 ) PDF (526 KB) ( 376 )

	588	Simultaneous Determination of Aspirin and Salicyclic Acid by Synchronous Fluorescence Spectrometry
		WEI Yong-feng, LI Xiao-hua，MA Dong-mei
		A simple, rapid and inexpensive fluorimetric method for simultaneously determining ASA and SA in a single scan of the co-existing specimen had been established. When the wavelength interval(Δλ) is 80 nm for scaning, the amounts of ASA and AS could be quantitatively determined respectively. The fluorescence intensity was linearly related to the aspirin concentration in the range of 4.0×10^-6-1.0×10^-4 mol·L^-1 with correlation coefficient 0.994 9; the fluorescence intensity was linearly related to the salicyclic acid concentration in the range of 8.0×10^-7-1.0×10^-4 mol·L^-1 with correlation coefficient 0.997 5, the determination limit was 4.0×10^-7 mol·L^-1. The method is simple, rapid and inexpensive, it can be used for medicament analysis.
		2005 Vol. 25 (04): 588-590 [Abstract] ( 390 ) PDF (371 KB) ( 344 )

	591	Study on the Inclusion Interaction of Water-Soluble p-(N,N-Dimethylamino)-Calix[8]Arene with Diphenylamine-4-Sulfonic Sodium Salt
		HUANG Zhi-bing, LI Lai-sheng^*, WANG Yu-xiao, WU Yu-mei
		The inclusion interaction of water-soluble p-(N,N-dimethylaminomethyl)-calix[8]arene with diphenylamine-4-sulfonic acid sodium salt was investigated by fluorimetric method. When diphenylamine-4-sulfonic acid sodium salt was added into the p-(N,N-dimethylaminomethyl) -calix[8]arene solution, the emission spectrum of diphenylamioe-4-sulfonic acid sodium salt occurred to a blue shift with the enhancement of the fluorescent intensity. The results show that the formation of the inclusion complex of the p-(N,N-dimethylaminomethyl)-calix[8]arene with diphenylamine-4-sulfonic acid sodium salt. The influence factors such as the pH value of solutions, solvents on the emission and excitation spectra of the inclusion complex were studied. It indicates that diphenylamine-4-sulfonic acid sodium salt penetrated the cavity of the calix[8]arene via the static action between the sulphonyl group of diphenylamine-4-sulfonic acid sodium salt and nitrogen atom of p-(N,N-dimethylaminomethyl)-calix[8]arene and the hydrophobic interaction of the aromatic rings.
		2005 Vol. 25 (04): 591-593 [Abstract] ( 986 ) PDF (389 KB) ( 346 )

	594	Synthesis of Purpure-18-Imide and Study on Its Interaction with Bovine Serum Albumins by Fluorescence
		WANG Jin-jun，LIU Yong-ming, LI Li
		Purpure-18-imide was synthesized based on the porphyrin’s special affinity for cancer cells and the antitumor activity of pyrrolidine compound. The binding reaction between purpure-18-imide and bovine serum albumins (BSA) in aqueous was studied by fluorescence and UV-Vis absorption spectra. The research results indicated that the combination reaction of them was a single static quenching process. In aqueous, purpure-18-imide strongly bound BSA with molar ratio of 1∶1. The binding constant K_０ was 5.386×10⁵ L·mol^-1. The shortest binding distance (r=3.54 nm) and energy transfer efficiencies (E=0.26) between donor (BSA) and acceptor (purpure-18-imide ) were obtained by Frster’s nonradiative energy transfer mechanism.
		2005 Vol. 25 (04): 594-597 [Abstract] ( 1052 ) PDF (493 KB) ( 349 )

	598	Determination of Ascorbic Acid by Indirect Fluorimetry
		TONG Chang-lun, XIANG Guang-hong, LIU Wei-ping
		Experiments indicated that cerium(Ⅳ) ion which could not emit fluorescence was deoxidized by ascorbic acid to cerium(Ⅲ) ion which could emit its characteristic fluorescence in water solution, while sodium hexametaphosphate added could greatly enhance the fluorescence intensity of the system. From this, an indirect sensitive method for determining ascorbic acid was developed. The fluorescence intensity of the system was measured in a 1 cm quartz cell with the excitation and emission wavelengths of 303 and 340 nm, respectively. The results showed that the fluorescence intensity of the system presented a linear relationship with the concentration of ascorbic acid in the range of 1.0×10^-7-8.0×10^-6 mol·L^-1, the correlation coefficient r was 0.999 7, and the detection limit(S/N=3) was 1.6×10^-8 mol·L^-1. The presented method was used to determine ascorbic acid sample and vitamin C tablet, and the results were satisfactory.
		2005 Vol. 25 (04): 598-600 [Abstract] ( 1479 ) PDF (346 KB) ( 335 )

	601	A Study on the Ultraviolet Spectra of Halogenated Benzoylferrocenes
		FAN Rui-lan, BAO Feng-rong, WANG Yong-sheng
		The ultraviolet spectra of all of the o, m, p-halogenated benzoylferrocenes have been studied the following rules obtained: 1. The λ_max of the ultraviolet spectrum R band and K band for the isomers is λ_max(m-X)＞λ_max(p-X)＞λ_max(o-X). 2. With the same substituted positions of the different halogen on the benzene ring, the λ_max of the ultraviolet spectrum K band is λ_max(C1)＞λ_max(Br)＞λ_max(I)＞λ_max(F), then, the λ_max of ultraviolet spectrum R band is λ_max(I)>λ_max(Br)>λ_max(Cl)>λ_max(F).
		2005 Vol. 25 (04): 601-603 [Abstract] ( 1481 ) PDF (391 KB) ( 351 )

	604	The Study of Protoporphyrin Ⅸ Metabolism in Cell Proliferation Using Yolk as the Target Samples
		WANG Rong, ZHENG Rong-er^*, LI Ying, MA Jun，MENG Ji-wu
		In order to find the better target sample to investigate protoporphyrin Ⅸ metabolism in the cell proliferation process in chick embryos, the emission spectra of egg white, yolk and urine from non-incubated and incubated eggs were measured under the excitation at 405 nm. It was observed that, among the three components investigated, only yolk sample was possible to get in pureness almost through the whole incubation process. Furthermore, compared with the egg white, the yolk had more obvious characteristic emission of protoporphyrin Ⅸ and lower background spectra and turned to be the better target sample for the investigation. The relative characteristic emission intensity of PpⅨ of yolk samples was used to determine the level of PpⅨ metabolism. It was found that the relative emission intensity increases during the first 10 days of proliferation process, indicating an increase in the concentration or in the metabolism level of protoporphyrin Ⅸ. The relative emission intensity, hence the PpⅨ metabolism level, then decreased gradually during the rest days of proliferation process. These results are similar to those obtained on human malignant tumors as they develop. The result testifies the point of view further that the abnormity of PpⅨ metabolism is correlative to the rapid limitless cell proliferation.
		2005 Vol. 25 (04): 604-607 [Abstract] ( 1538 ) PDF (508 KB) ( 350 )

	608	Study on the Mechanism of the Interaction of Methylene Blue and Sulfation Pachymaran
		GAO Gui-zhen^{1, 2}, JIAO Qing-cai¹, DING Yi-lei¹，CHEN Lei¹
		In order to understand the mechanism of the interaction of sulfate polysaccharides and small molecules at molecular level, the structure of pachymaran was decorated by Wolfrom, and sulfation pachymaran(SP) was prepared. The maximum binding number(N=54) and the binding equilibrium constant(K=1.563×10⁶) of the sulfation pachymaran and methylene blue (MB) were obtained by the exoterica model. The influence of the molar ratio of MB/SP，ethanol，hydroxypropyl-β-cyclodextrin，Triton X-100 and NaCl on the spectra of MB-SP complex was investigated. The mechanism of the color changes of methylene blue and sulfation pachymaran reaction system has been discussed. The authors draw the conclusion that the color changes result mainly from the hydrophobic interaction between methylene blue molecules binding on sulfation pachymaran on the base of the electrostatic interaction of methylene blue and sulfation pachymaran.
		2005 Vol. 25 (04): 608-612 [Abstract] ( 1390 ) PDF (590 KB) ( 367 )

	613	Instant Effect of Temperature on the Oxygen Carrying Capacity of Single Living Intact Red Blood Cell
		YAO Cheng-can¹, LI Xiao-kun¹, HUANG Yao-xiong^2*
		The instant effect of temperature on the absorption spectra of the hemoglobin in single living intact red blood cells was investigated, by employing a highly sensitive fast multi-channel micro-spectrophotometer system to perform non-invasive, in situ, real time measurements on the cells. It was found that both the heights and position of the specific peaks in the absorption spectra of intercellular hemoglobin were changed with temperature, indicating that the oxygen carrying capacity of red blood cells varies with temperature. The correlations of the structure and concentration as well as the function of hemoglobin, and the molecular mechanism were also discussed.
		2005 Vol. 25 (04): 613-616 [Abstract] ( 1553 ) PDF (597 KB) ( 332 )

	617	Determination of Chinese Traditional Medicine Activity Eliminating Superoxide Anion Radical by Kinetics Spectrophotometry
		TIAN Yi-ling¹, CHEN Guan-hua², CUI tong¹
		A new method to determine Chinese traditional medicine activity eliminating superoxide anion radical by kinetic spectrophotometry was developed. It is shown that the optimum determination condition may be obtained when wavelength is 520 nm, the concentration of enzyme is 4×10^-3 μg·mL^-1, the reaction time is between 2-7 min. Vitamin C activity eliminating superoxide anion radical was determined under the condition, and the results were identical with literature. The method is used to determine IC₅₀ of Cortex Magnoliae Officinalis and Cortex Eucommia, and they are 7.580 and 323.800 mg·L^-1 respectively.
		2005 Vol. 25 (04): 617-619 [Abstract] ( 1367 ) PDF (400 KB) ( 326 )

	620	Ratio Spectrophotometry and Its Application to Assay of Compound Pharmacy Preparations
		HUANG Xi-ru¹, CAI Yong-mei², TAI Yan¹, CAO Dong¹
		The present paper is to study ratio spectrophotometry for its application to the assay of compound pharmacy preparations. According to the feature of ratio spectra, the wavelength pair was selected at the peak point or valley point of ratio spectra to establish ratio spectrophotometry for the determination of Co-Chlorzoxazone tablet and injection of caffeine and sodium benzoate. The average recoveries and relative standard deviations for Chlorzoxazone and paracetamol were 100.0% and 1.28%, and 100.0% and 0.84%, respectively; the average recoveries and relative standard deviations for caffeine and sodium benzoate were 99.98% and 0.70%，and 99.91% and 0.78%, respectively. It is concluded that as long as the ratio spectra exhibit at least one peak and one valley, the results are satisfactory.
		2005 Vol. 25 (04): 620-623 [Abstract] ( 1301 ) PDF (371 KB) ( 324 )

	624	Comparison of Non-Protected Fluid Room Temperature Phosphorescence and Micellar-Stabilized Room Temperature Phosphorescence Properties of Indole-3-Butyric Acid
		LONG Wen-qing
		For indole-3-butyric acid (IBA), the non-protected fluid room temperature phosphorescence (NP-RTP) and the fluid room temperature phosphorescence with polymeric dispersant polyethyleneglycol-200 (PEG-200), PEG-400 or non-ionic surfactant Tween-20, Tween-40, Tween-80, Tween-85, Brij35 and emulsifier OP as a medium have been studied in detail. When the surfactants or polymeric dispersants were added to the NP-RTP system, the profile of RTP spectrum was not changed, but the RTP intensity and the pre-irradiation time required to attain a stable RTP signal were increased. Whether the surfactants or polymeric dispersants were added to the system or not, no RTP signal was observed when TlNO₃ was used as a heavy atom perturber (HAP), but intense RTP emissions were observed when KI was present as HAP. Recoveries of 95.2%-104% with relative standard deviations of 2.4%-4.0% were obtained in spiked water and soil samples.
		2005 Vol. 25 (04): 624-627 [Abstract] ( 1345 ) PDF (462 KB) ( 370 )

	628	Research Development of Spectroscopic Probes of Protein
		YU Ying^1，2，ZHOU Zhen-tao¹
		A review on the recent research progress in spectroscopic probes of protein was presented and discussed. The review included categories of spectroscopic probes of protein, interaction models of protein and spectroscopic probes, interaction force of protein and spectroscopic probes, and protein conformation research. Future research direction of spectroscopic probes of protein was forecast.
		2005 Vol. 25 (04): 628-632 [Abstract] ( 978 ) PDF (634 KB) ( 312 )

	633	Optical Detection System for Micro Biochemical Analyses
		LI Feng, WU Yi-hui^*, ZHAO Hua-bing, JU Hui
		For the need of biochemical chip, which consumes fewer specimens and is easy to integrate with micro-fluid chip, two kinds of spectrophotometric analysis methods are described in the present paper. Both the direct detection method and evanescent wave detection method are used in the experiments with visible light(460-800 nm). The experimental results proved that the direct detection is simple and evident; on the other hand the evanescent wave detection method consumes much less reagent and is easy to integrat with microchips.
		2005 Vol. 25 (04): 633-636 [Abstract] ( 2036 ) PDF (670 KB) ( 359 )

	637	Analysis of Spectral Properties of Novel Holographic Transmission Notch Filter
		HUANG Chong¹, OUYANG Yan-dong¹, WU Jian-hong², YU Yun-peng¹, LIN Shun-hui¹
		Optical filter has extremely important applications in spectroscopy, optical measurement and laser physics. Holographic filter, especially the transmission volume holographic notch filters using dichromate gelatin (DCG), is a new kind of filter with the main characteristic of a very narrow bandwidth. In this paper, measurements were carried out on the spectral properties of this transmission volume holographic notch DCG filter using an ultraviolet-visible transmittance spectrometer. The experimental results show that the relative transmittance of main spectrum of this filter is less than 2% in the visible region between 400 and 800 nm, and the relative transmittance of other spectra are more than 85%. Moreover, the filter has a narrow bandwidth with a half-bandwidth less than 12 nm, and a 1/10 width of the bandwidth less than 15 nm. These results indicate that this new kind of filter has an excellent filter characteristic to the main spectrum of Ar⁺ laser at the wavelength of 514.5 nm.
		2005 Vol. 25 (04): 637-638 [Abstract] ( 1545 ) PDF (222 KB) ( 389 )

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