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2006 Vol. 26, No. 05 Published: 2006-05-26

光谱学与光谱分析

	785	A Measurement of Optical Emission from the Rear Surface with Solid Targets Irradiated by Ultrashort Pulse Laser
		WANG Guang-chang^{1, 2，3},ZHENG Zhi-jian³,YANG Xiang-dong^2*,GU Yu-qiu³,LIU Hong-jie³,WEN Tian-shu³, GE Fang-fang³,JIAO Chun-ye³,ZHOU Wei-min³, ZHANG Shuang-gen^2，3, WANG Xiang-xian^2，3
		The integrated image spectrum and scattering light spectrum of optical emission at normal direction from rear-side of a metallic foil were measured, employing optical CCD camera and OMA optical multi-channel spectrometer. The integrated image spectrum shows that it presents a ring-shape, and in the near margin of the ring-shape a bright localized signal is shown, which is optical transition radiation (OTR) generated by hot electrons transport through solid targets. The scattering spectrum shows that it presents a series of nonperiodic sharp spikes between 300-500 nm, and the sharp spike is ascribed to the coherent transition radiation (CTR) generated by bunches of hot electron beams generated in v×B acceleration mechanism near 400 nm(2 ω). The intensity of transition radiation decreases with the increase of the target thickness.
		2006 Vol. 26 (05): 785-789 [Abstract] ( 1566 ) PDF (1047 KB) ( 444 )

	790	Optical and Morphological Investigation on the Interaction of Dual Dopants in Poly(N-Vinylcarzole)
		ZHANG Ting¹, XU Zheng^{1, 2}, TENG Feng¹, QIAN Lei¹, WANG Yong-sheng¹, XU Xu-rong^1*
		The effect of optical and electrical properties of poly(N-vinylcarzole) (PVK) doped with two dyes, i.e. 8-tris-hydroxyquinoline (Alq₃) and 4-(dicyanomethylene)-2-tert-butyl-6 (1, 1, 7, 7-tetramethyljulolidyl-9-enyl)-4H-pyran (DCJTB), on the energy transfer and charge trapping processes was investigated. The phase separation in blends film at different doping concentration was also studied. More homogeneous dispersion of dyes in PVK with increasing doping concentration was showed. The results indicate that there is a certain interaction of Alq₃ and DCJTB in this dual-doped system. It is the incorporation of DCJTB that untangled the aggregation of Alq₃ owing to the interaction of DCJTB and Alq₃. But for higher doping concentration, DCJTB results in an isolated charge transport channel that decreases the electroluminescence (EL) operating voltage.
		2006 Vol. 26 (05): 790-793 [Abstract] ( 1630 ) PDF (1119 KB) ( 453 )

	794	Study on the Nonlinear Raman Lidar Monitoring the CO₂ Gas
		ZHAO Yue-feng,ZHANG Yin-chao,HONG Guang-lie,LIU Xiao-qin,CAO Kai-fa,FANG Xin,TAO Zong-ming,YU Shi-hua,QU Kai-feng,SHAO Shi-sheng
		It is a new skill to use SRS rays as emitting waves for the lidar monitoring CO₂ gas, and the nonlinear Raman lidar based on the SRS process was devised. The third harmonic Nd:YAG laser wave (354.7 nm) was injected into the Raman cells filled with higher pressure gases, CO₂ and N₂. The first Stokes (S1) line 371.66 nm (CO₂) and 386.7 nm (N₂) were generated by stimulated Raman scattering. The variable S1 energy was measured by changing the gas pressure in the Raman cell and the Nd:YAG laser system output energy. The optimum pressures of the CO₂ and N₂ in the Raman cell were achieved. Moreover, the principles of this physical process were put forward. This skill has been applied to the lidar for monitoring the CO₂ gas.
		2006 Vol. 26 (05): 794-797 [Abstract] ( 1783 ) PDF (906 KB) ( 449 )

	798	Enhancement Effect of Argon Atmosphere at High Pressure on Radiation Intensity of Laser-Induced Soil Plasmas
		SHI Jin-chao, CHEN Jin-zhong^*, WEI Yan-hong, GUO Qing-lin, HUI Su-fang
		In the present paper, the effects of argon atmosphere at high pressure(0.2-1.1 MPa) on the radiation intensity of the plasma induced by a high energy neodymium glass laser (energy ～30 J, pulse width 0.7 ms) were studied by recording the photograph and spectra of the plasma as well as measuring the ablated mass. The experimental results show that the volume of the plasma was compressed, the temperature increased, and the lightness enhanced significantly when pressure was raised. Under our experimental condition, the radiation intensities of the plasmas were enhanced with the increase in the gas pressure; but the ablated mass of the sample decreased. The measured results are discussed, combined with the process of the experiment.
		2006 Vol. 26 (05): 798-801 [Abstract] ( 1099 ) PDF (956 KB) ( 505 )

	802	Measurement of Molecular Vibrational Temperature in Dielectric Barrier Discharge in Argon/Air at Atmospheric Pressure
		DONG Li-fang,LIU Feng,LI Shu-feng,RAN Jun-xia, HE Ya-feng, LI Xue-chen, PANG Xue-xia
		Vibrational temperature of N₂(C ³Π_u) molecules in dielectric barrier discharge (DBD) in argon/air at atmospheric pressure，in which the water electrodes were employed，was measured by using a method of spectrum diagnosis. Emission spectral lines of the N₂ second positive band system(C ³Π_u→B ³Π_g) and the sequences of vibrational bands with Δｖ＝-1，Δｖ＝-2 and Δｖ＝-3 were used in the calculation. The experiment results show that the molecular vibrational temperature of N₂ is in the range from 1 938 K to 2 720 K，and it increases almost linearly with increasing the air content in gas mixture. These results are of great importance to the study of plasma dynamics of DBD.
		2006 Vol. 26 (05): 802-804 [Abstract] ( 2040 ) PDF (911 KB) ( 572 )

	805	Structure and Luminescence Properties of Eu³⁺ Complexes with Benzoic Acid and 1,10-Phenanthroline Incorporated in SiO₂,SiO₂-B₂O₃ and SiO₂-B₂O₃-Na₂O Matrices
		WANG Xi-gui¹, WU Hong-ying¹, ZHAO Si-qin¹, WENG Shi-fu², WU Jin-guang²
		Eu³⁺ Complexes with benzoic acid and 1,10-phenanthroline incorporated in SiO₂, SiO₂-B₂O₃ and SiO₂-B₂O₃-Na₂O matrices were prepared via the sol-gel method. Eu-doped SiO₂, SiO₂-B₂O₃ and SiO₂-B₂O₃-Na₂O luminescence materials were synthesized. The luminescence of Eu³⁺ was studied with excitation spectra and emission spectra. Different forms of dopants could influence the luminescence properties. The structure of Eu-doped glass was studied by comparing IR, TEM and XRD. The results showed that after the materials were annealed at 1 000 ℃ the structure was very stable because ingredient was already removed totally. The emission spectrum showed that the typical optical spectrum of Eu³⁺ is ⁵D₀→⁷F_j(j=1, 2) at 588 nm and 614 nm. Comparing EuCl₃ with Eu³⁺ complexes with benzoic acid and 1,10-phenanthroline as dopant, the latter has strong luminescence property though it has small mass fraction. The luminescence intensity of Eu³⁺-doped SiO₂-B₂O₃ glass material was weaker than that of Eu³⁺-doped SiO₂ glass material, and the former’s spectrum showed that there were Si—O—B bonds. The luminescence intensity of Eu³⁺ was quenched by this kind of structure. The luminescence intensity of Eu³⁺-doped SiO₂-B₂O₃-Na₂O glass material was greatly increased, and the infrared spectrum illustrated that there was not vibration absorption of Si—O—B bonds. Probably Na replaced B, and Si—O—Na bonds formed. This kind of structure could enhance luminescence intensity of Eu³⁺ to some extend.
		2006 Vol. 26 (05): 805-808 [Abstract] ( 639 ) PDF (984 KB) ( 623 )

	809	Luminescence Properties of Ba₂MgSi₂O₇∶RE
		SHI Yan-ning, HE Da-wei^*, LIANG Zhong-yi
		In the present paper, alkaline earth silicates Ba₂MgSi₂O₇∶RE were prepared under a reducing atmosphere by solid-state reaction. Under UV light excitation, Ce³⁺ doped pyrosilicates phosphors emit efficient bluish violet light. The emission spectra of Eu²⁺ doped pyrosilicates phosphors showed that Eu²⁺ ions could occupy two types of sites in Ba₂MgSi₂O₇ host. The energy transfer from Ce³⁺ to Eu²⁺ in Ba₂MgSi₂O₇ is efficient, as there is a large overlap between Ce³⁺ emission bands and Eu²⁺ excitation bands. Analysis of the spectra of Ce³⁺ and Tb³⁺ co-doped phosphor indicated the existence of energy transfer from Ce³⁺ to Tb³⁺ in Ba₂MgSi₂O₇ under UV excitation.
		2006 Vol. 26 (05): 809-811 [Abstract] ( 552 ) PDF (885 KB) ( 429 )

	812	The Emission Mechanisms of Two Kinds of Tb Complexes Doped in PVK System
		XU Ying¹, DENG Zhen-bo^1*, XU Deng-hui¹, XIAO Jing¹, WANG Rui-fen²
		Two kinds of new rare earth complexes Tb(p-MBA)₃phen (sample Ⅰ) and Tb(p-ClBA)₃phen (sample Ⅱ) were synthesized, and photoluminescence (PL) and electroluminescence (EL) characteristics of the terbium complex and PVK blended system were investigated. As to the sample Ⅰ, the emission of PVK was completely restrained in the EL spectra of the blended film; while in the PL spectra, obvious emission of PVK appeared besides the emission of Tb³⁺. But as to the sample Ⅱ, only the green emission from Tb³⁺ can be observed in both PL and EL spectra of the doping system. So there are two processes that occur in sample Ⅰ, one is the incomplete Frster energy transfer process from PVK to the Tb complex, and the other is the carrier charge trapping process. The main mechanism of sample Ⅱ is the energy transfer process.
		2006 Vol. 26 (05): 812-815 [Abstract] ( 1485 ) PDF (922 KB) ( 518 )

	816	Recent Progress in Flow-Injection Chemiluminescence for Pharmaceutical Analysis
		XUE Bing-chun, WANG Tao, LIU Er-bao^*
		Flow-injection chemiluminescence(FI-CL) analysis has made great progress in analytical chemistry for its high sensitivity with a wide linear range，simple instruments，rapidity and reproducibility in signal detection，and being appropriate for on-line analysis. A review with 74 references dating from 2002-early 2004 is given of the application of FI-CL method in the determination of drugs.
		2006 Vol. 26 (05): 816-820 [Abstract] ( 212 ) PDF (886 KB) ( 527 )

	821	Depth Profiles of High-Density Polyethylenes Filled with Different Inorganic Fillers during Natural Photo-Oxidation by Infrared Microscopy
		YANG Rui¹, WANG Kun-hua¹, YU Jian¹, SONG Yuan-yuan^２, WANG Hong-kai^２
		The natural photo-oxidation degradation of HDPE filled with different inorganic fillers was carried out, and the depth profiles of the standard samples were characterized by infrared microscopy (IM) and scanning electron spectroscopy (SEM). The results show that HDPE filled with different inorganic fillers show different depth profiles. For HDPE and CaCO₃-filled HDPE, there are no cracks on the cross sections, and the carbonyl indexes remain nearly zero from the surface to the interior. For HDPE filled with black mica, mica, kaolin and diatomite, there are more or less parallel, comb-like cracks on the cross sections, and the carbonyl indexes show decreasing trends from the surface to the interior. Furthermore, the transition points in CI curves are basically consistent with the formation of cracks in these samples. The UV absorbances of these inorganic fillers demonstrate the relationship between the photo-oxidation of HDPE and the relative absorbances of inorganic fillers. This implies that the UV absorbance of the inorganic filler may be responsible for the occurrence of cracks and oxidation in the standard samples.
		2006 Vol. 26 (05): 821-824 [Abstract] ( 587 ) PDF (1141 KB) ( 493 )

	825	FTIR Investigation of Organic Phase Containing Rare Earth Ion in Naphthenic Acid-Phosphonate Ester-Heptane System
		YIN Wen-xuan^{1, 2}, LIU Yu-feng¹, ZHANG Yuan-fu¹, WENG Shi-fu¹, WU Jin-guang^1*
		Naphthenic acid (NA) was mixed with PC88A in heptane, and 10 moL·L^-1 KOH aqueous solution was used to saponify the solution subsequently. The transparent and clear appearance of the obtained solution indicated the formation of w/o micell and microemusion. In the present study, micell with high saponification percentage (80%) was used to extract neodymium. The organic phase structure was characterized using FTIR spectroscopy in the extraction process. IR spectra indicate that the characteristic peaks of ν(COOH), ν_s(COO^-) and ν(PO) shift to lower wavenumbers as the loading of Nd in organic phase increases. The results demonstrated that Nd(Ⅲ) are coordinated to PO and COO^- groups simultaneously, and the supramolecules with self-assembly structure was formed containing PC88A and NA, which were binding with Nd(Ⅲ) in the extracted organic phase.
		2006 Vol. 26 (05): 825-827 [Abstract] ( 1731 ) PDF (893 KB) ( 410 )

	828	Monitoring Cerebral Oxygenation Using Near Infrared Spectroscopy during Cardiopulmonary Bypass Surgery
		TENG Yi-chao¹, DING Hai-shu^1*, GONG Qing-cheng², JIA Zai-shen², HUANG Lan¹, WANG Pei-yong¹
		To avoid cerebral hypoxia caused by the imbalance between cerebral oxygen supply and consumption, regional cerebral oxygenation of patients need to be monitored at real time during cardiopulmonary bypass (CPB) surgery, and the physiological parameters can be regulated and emergent treatment can be used according to it. Using the near infrared (NIR) instrument developed by our group, cerebral oxygenation of the patients under cardiac surgery was monitored. The instrument consists of a two-wavelength near infrared light source and two near infrared detectors. Hemoglobin concentration changes of regional cerebral tissue were calculated, and by steady-state spatially resolved spectroscopy (SRS) algorithm, regional cerebral oxygen saturation (rSO₂) was also calculated. Physiological parameters of patients, such as mixed venous oxygen saturation (SvO₂), were measured by another monitor during CPB. Hemoglobin concentration changes were easily disturbed, but the anti-disturbance ability of rSO₂ was good. The value of rSO₂ could be detected all over the surgeries, but SvO₂ could be detected only during CPB. There were positive correlations between rSO₂ and SvO₂ in most of the patients, but the correlation coefficients were not very high. This was because SvO₂ reflects the saturation of the main venous, but rSO₂ reflects regional cerebral oxygenation. So the physiological meaning of rSO₂ and SvO₂ is different. The results indicate that cerebral oxygenation of patients can be reflected by rSO₂ during CPB, while only monitoring SvO₂ is not enough.
		2006 Vol. 26 (05): 828-832 [Abstract] ( 1732 ) PDF (917 KB) ( 484 )

	833	The PLS Calibration Model Optimization and Determination of Rice Protein Content by Near-Infrared Reflectance Spectroscopy
		LI Jun-xia^{1, 4},MIN Shun-geng², ZHANG Hong-liang¹, YAN Yan-lu³, LUO Chang-bing³, LI Zi-chao^1*
		A hundred and ninety one representative brown rice samples from the Chinese Rice Genebank and the DH population derived from the cross of japonica upland rice IRAT109 with paddy rice Yuefu were selected for this study. Their protein content range was 5.90%-14.50%. Near-infrared diffusive spectroscopy (NIDRS) and partial least square (PLS) were used to determine protein content with different wavelength ranges and data preprocessing methods for regression and information extraction. The object function [R/(1+RMSECV)] of quantitative model was defined, and the samples of calibration and validation tests were classified by projective distribution of PLS loadings. These methods were applied to the optimization of the calibration model. It is demonstrated that the calibration model developed by the spectral data pretreatment of the first derivative + standard vector normalization with the same spectral region (5 000-9 000 cm^-1) resulted in the best determination of protein content in brown rice when the maximum values of the object function were reached. The maximum values of the object functions of calibration and validation sets were 0.701 and 0.687, respectively. Projective distributions of PLS loadings were used to validate the models, and the result was the same as that of validating model by object function [R/(1+RMSECV)].
		2006 Vol. 26 (05): 833-837 [Abstract] ( 2064 ) PDF (925 KB) ( 580 )

	838	Temperature Effect on the Noninvasive Measurement of Human Blood Glucose by NIR
		CUI Hou-xin, XU Ke-xin, CHEN Min-sen, AN Lin
		During the noninvasive measurements of body blood glucose, the result will be effected by many factors, such as the measuring conditions including temperature, contact pressure and so on, and in addition the change of body’s state also will induce some error. However, among so many factors the temperature is very important and should be discussed. To find the quantitative value of the result bias caused by temperature in the wavelength range from 1 100 to 1 700 nm, the aqueous glucose with the concentration ranging from 10 mg·dL^-1 to 200 mg·dL^-1 and 10 mg·dL^-1 interval was detected at temperature of 15, 20, 25, 30, 35 and 40℃. Then six different models at different temperature were founded and predicted one another. The maximum RMSEP result of models is 11.227 9 mg·dL^-1 and the minimum is 3.298 8 mg·dL^-1. The correlation is about 0.98. The authors have also found that 1 ℃ change of temperature will induce Δc＝2.662(mg·dL^-1·℃^-1)change of the prediction result, so these show that the detect error will be minimal when the temperature of measuring is the same as that of modeling. Moreover, the authors put forward two approaches to decreasing or compensating the error induced by the temperature.
		2006 Vol. 26 (05): 838-841 [Abstract] ( 590 ) PDF (942 KB) ( 865 )

	842	The Effects of Noise on NIR Analysis and Related Mathematic Pretreatments and Models
		ZHAO Huan-huan¹, YAN Yan-lu²
		The feasibility of using a relatively high noise NIR spectrometer for analysis was examined by using maize powder samples. The results showed that with four-time averaged NIR spectrum data without more pretreatments, PLS mathematic models and CAU-NIR software, the relative high noise scan NIR spectrometer could be used to get satisfied prediction results compared with other low noise NIR spectrometers. The prediction coefficient could reach 98% and the CV(variation coefficient) was 6.2%. It was proved that when the S/N of NIR spectrometer was lower than 10⁵, it still could be used for quantity analysis with the help of some mathematic pretreatments and models.
		2006 Vol. 26 (05): 842-845 [Abstract] ( 528 ) PDF (884 KB) ( 572 )

	846	A Study of Preparation and Infrared Absorbency of La₂O₃ Nanocrystals
		WANG Chun-xiu,LI Fu-li
		Nanocrystals were prepared by stearic acid gel method. The structure and morphology of nanocrystals were characterized by X-ray powder diffraction (XRD), transmission electron microscope(TEM) and infrared spectra. Experimental results show that the absorption peaks of La₂O₃ extendwith their blue shift or red shift. The absorption of La₂O₃ nanocrystals is good in the wavelength range of 1 000 to 1 700 nm, where La₂O₃ nanocrystals may serve as a kind of absorbent of laser camouflage material.
		2006 Vol. 26 (05): 846-849 [Abstract] ( 1091 ) PDF (992 KB) ( 498 )

	850	Discrimination of Varieties of Apple Using Near Infrared Spectra Based on Principal Component Analysis and Artificial Neural Network Model
		HE Yong, LI Xiao-li, SHAO Yong-ni
		A new method for the discrimination of varieties of apple by means of near infrared spectroscopy(NIRS) was developed. First, principal component analysis (PCA) was used to compress thousands of spectral data into several variables and describe the body of spectra, the analysis suggested that the cumulate reliabilities of PC1 and PC2 (the first two principle components) were more than 98%, and the 2-dimentional plot was drawn with the scores of PC1 and PC2. It appeared to provide the best clustering of the varieties of apple. The loading plot was drawn with PC1 and PC2 through the whole wavelength region. The fingerprint spectra, which were sensitive to the variety of apple, were obtained from the loading plot. The fingerprint spectra were applied as ANN-BP inputs. Seventy five samples from three varieties were selected randomly, then they were used to build discrimination model. This model was used to predict the varieties of 15 unknown samples; the distinguishing rate of 100% was achieved. This model is reliable and practicable. So the present paper could offer a new approach to the fast discrimination of varieties of apple.
		2006 Vol. 26 (05): 850-853 [Abstract] ( 1203 ) PDF (899 KB) ( 1022 )

	854	Study on Vibrational Spectra and Structure of 4-Mercaptopyridine Monomer and Dimer Using Density Functional Theory
		CHENG Jian-bo^{1, 2},XU Wei-qing¹,ZHAO Bing^1*, ZHANG Gang³,GONG Bao-an²
		The optimized molecular structure and vibrational frequencies of 4-mercaptopyridine monomer and dimer were studied by density functional theory using B3LYP method with the 6-311++G(d, p) basis set. On the basis of the calculations, the assignments of vibrational spectra were performed on monomer and dimer, and the change in structure and vibrational spectrum of dimer as well as the intermolecular force of forming dimer were investigated. It was found that the two pyridine ring planes are vertical to each other, and the dimer was formed through H-bonding, which is between the nitrogen on one ring and the hydrogen of SH moieties on another. Furthermore, the structure and vibrational spectrum of the dimer have some changes with respect to those of the monomer.
		2006 Vol. 26 (05): 854-857 [Abstract] ( 1443 ) PDF (878 KB) ( 572 )

	858	Surface Enhanced Raman Scattering Spectra of Phytic Acid in the Sol Silver Oxide
		FENG Jie, SUN Xiao-jing, ZHU Jun, XIA Wei, LIU Hong, YANG Hai-feng^*
		Surface enhanced Raman scattering spectra of phytic acid were recorded in the sol oxide silver. Based on ab-initio/STO-3 quantum calculations results, assignments to the vibrational modes of phytic acid were carried out. On the basis of the mechanism of SERS, the adsorption modes were suggested that phytic acid chemically adsorbed on the oxide silver surface through four phosphate bonds.
		2006 Vol. 26 (05): 858-860 [Abstract] ( 1160 ) PDF (888 KB) ( 417 )

	861	Raman Scattering Spectra of Ca₃NbGa₃Si₂O₁₄(CNGS) Crystals
		LAN Jian-hui¹, LU Gui-wu^1*, WANG Zeng-mei², YUAN Duo-rong³, XIA Hai-rui³
		The CNGS crystal belongs to the trigonal system, the 32 point group and the P321 space group, which is the same as the LGS crystal. Its lattice constants are a=0.808 73 nm and c=0.497 98 nm. The primitive cell of the CNGS crystal contains only one formula unit (23 atoms). The vibration modes were measured with Raman spectroscopy technique, assigned with ab initio molecular orbit calculation method. In order to model the crystal, two clusters Ca₃NbGa₂SiO₁₂ and Ca₃NbGaSi₂O₁₂ were designed, and calculations were carried out on them. Their configurations were optimized, and the vibration frequencies were calculated with UHF method. By investigating the force constants and activities of the assigned Raman spectra, the structure of CNGS crystal was analyzed, and its layer structure and piezoelectric properties were confirmed. It is concluded that CNGS crystals have more excellent anisotropy and piezoelectric properties than LGS crystals.
		2006 Vol. 26 (05): 861-864 [Abstract] ( 1115 ) PDF (952 KB) ( 375 )

	865	Influence of Different Light Source on the Laser Raman Spectra in Determination of Sodium Glutamic Acid
		LIU Wen-han, ZHANG Dan, ZHENG Jian-zhen, WU Xiao-qiong, LI Zu-guang, MA Chun-an
		The influences of different laser source and different light power on laser Raman spectra were studied for the sodium glutamic acid. The results show that some influences existed using different wavelength and power of light source the peak shifting 6 cm^-1. As UV laser has great light power, the samples were destroyed, making the Raman spectra reduce or disappear. The attenuation of light was needed. The linear relation existed between the Raman intensity and the power of laser light source, and the correlation coefficient was more then 0.999. The Raman intensity per light power unit was related to the wavelength, and was not related to the power of laser source.
		2006 Vol. 26 (05): 865-868 [Abstract] ( 1530 ) PDF (944 KB) ( 506 )

	869	Confocal Raman Microspectroscopic Study of Human Breast Morphological Elements
		YU Ge¹, XU Xiao-xuan², Lü Shu-hua³, ZHANG Cun-zhou², SONG Zeng-fu4, ZHANG Chun-ping²
		Breast tissue sections were examined by means of confocal Raman spectroscopy with an excitation wavelength of 633 nm. Acquired using a microscopic mapping approach with the sample volume of ～2 μm³, these spectra were compared with the ones of the commercially available actin, DNA, collagen (type Ⅰ), triolein etc. Some spectra were distinguished and identified and characterize the morphological elements like cell cytoplasm, extracellular matrix etc. The cell nucleus spectrum was also obtained by K-means cluster analysis. The correlation analysis showed that the spectrum from a morphological element is highly correlated with that from the corresponding purified chemical. The spectroscopic characterization of these morphological elements was then investigated. This study is helpful to understanding the chemical/morphological basis of the Raman spectrum and designing the Raman microspectroscopic model of human breast tissue.
		2006 Vol. 26 (05): 869-873 [Abstract] ( 1629 ) PDF (938 KB) ( 588 )

	874	SEM, XRD and FTIR Investigation on Crystal Growth of Calcium Oxalate Modulated by Sodium Tartrate
		ZHENG Hui¹, CHEN Cun-yuan¹, OUYANG Jian-ming^{1, 2*}
		Crystallization of calcium oxalate (CaOxa) was investigated in the presence of sodium tartrate (Na₂tart) of different concentration in a gel system by scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. It was found that in the presence of a low concentration of Na₂tart (0.01 mol·L^-1), calcium oxalate monohydrate (COM) is the dominant crystal phase. The percentage of calcium oxalate dihydrate (COD) is less than 5%. In the XRD pattern the main diffraction peaks are (101), (020), and (202) planes of COM crystals. In the FTIR spectrum, the main asymmetric carbonyl stretching band ν_as(COO^-) and the metal-carboxylate stretch ν_s(COO^-) of COM occur at 1 618 and 1 317 cm^-1, respectively. With the concentration of Na₂tart increasing to 0.10 and 0.50 mol·L^-1, the percentage of COD crystals increases to 10% and 50%, respectively, and the surface area of COM crystals decreases. The diffraction peaks that assigned to the (200), (211), (411), and (213) planes of COD crystals become stronger and stronger. The temperature can influence the modulation of Na₂tart in terms of the phase composition and morphology of CaOxa crystals. As the temperature decreases, the percentage of COD increases. At a higher temperature beyond 47 ℃, COM is the dominant phase; but COM is dominant when the temperature is lower than 27 ℃. The ν_as(COO^-) and ν_s(COO^-) of COD crystals occur at 1 647.6 and 1 327.7 cm^-1, respectively.
		2006 Vol. 26 (05): 874-878 [Abstract] ( 1637 ) PDF (1274 KB) ( 780 )

	879	Study on Structures of Blattela Germanica Allergen, Bla g 2 Expressed by Eukaryotic and Prokaryotic Vectors Using Fluorescence and CD Spectra
		LIU Zhi-gang¹, ZHU Jian-qi¹, HUANG Hai-zhen², XU Hong¹
		The recombinant allergen, Bla g 2, was expressed by prokaryotic vector E.coli and eukaryotic vector P.Pastoris. The different structures and configurations of the Bla g 2 from E.coli and P.Pastoris were studied by fluorescence and circular dichroism. The secondary structures of Bla g 2 in solution, and the composition besides the type of its tertiary structure were proposed. These studies help understand the differences between prokaryotic and eukaryotic expression systems, reveal the relationship between the structure and the function of Bla g 2, and improve the production of this significant allergen.
		2006 Vol. 26 (05): 879-883 [Abstract] ( 222 ) PDF (972 KB) ( 452 )

	884	Study of Red Tide Spectral Characteristics and Its Mechanism
		CUI Ting-wei^{1, 2}, ZHANG Jie^{2, 3}, MA Yi^{2, 3}, SUN Ling²
		In situ spectral data of different red tide, whose dominant species are leptocylindrus danicus, chattonella marina, skeletonema costatum, and mesodinium rubrum, were acquired by above water method utilizing spectrometer manufactured by FieldSpec^® Dual VNIR(USA). It is emphasized that the characteristic reflectance peak lying between 687 and 728 nm can be used to distinguish between red tide and normal sea water. Also the spectral discrepancy between different dominant species of red tide is pointed out, which could be utilized to identify certain red tide species by remote sensing technique. Mechanisms of phytoplankton red tide spectra peaks and vales are given. Spectral characteristics of mesodinium rubrum, a kind of protozoan, may be related to its symbiotic alga in its body and phytoplankton pigment crumb. So, research on ingestion preference, symbiotic property with algae, and fluorescence emission character of such symbiotic algae under normal temperature may be helpful for the deep understanding of mechanism of mesodinium rubrum spectra.
		2006 Vol. 26 (05): 884-886 [Abstract] ( 462 ) PDF (930 KB) ( 724 )

	887	New Method and Instrument to Diagnose Crop Growth Status in Greenhouse Based on Spectroscopy
		ZHANG Xi-jie,LI Min-zan^*,CUI Di, ZHAO Peng, SUN Jian-ying, TANG Ning
		Spectral reflectance of cucumber leaves in greenhouse was measured using an ASD FieldSpec Pro VNIR spectrometer with natural illumination. Two sensitive wavelengths, 527nm and 762 nm, were selected to evaluate the nitrogen content of the cucumber leaves. A model was established and validated using normal difference color index(NDCI) with the correlation coefficient of 0.881. Based on the above efforts, a handheld spectral instrument was developed to diagnose the growth status of the crop in greenhouse using fiber optics. The instrument was mainly composed of four parts: reflected light acquisition system, light intensity measurement unit, signal conditioning unit, and data acquisition system. The sunlight reflected by the crop was transmitted by the fiber, and passed through the light filter to obtain light at the sensitive wavelengths. Finally it was transformed into electronic signal by the photoelectric transistor, and was used to diagnose the growth status of the crop according to the evaluation model. The result showed that the developed instrument was practical.
		2006 Vol. 26 (05): 887-890 [Abstract] ( 1154 ) PDF (1031 KB) ( 486 )

	891	Preparation of Adsorbent Made from Sewage Sludge and Its Spectrum Properties
		YU Lan-lan,ZHONG Qin^*,FENG Lan-lan
		Biochemical sludges of sewage and petrochemistry and surplus sludge were taken as raw materials to prepare adsorbents for flue gas desulfurization by pyrolysis. To compare with active carbon, the abilities of adsorbents made from different sludges were studied by SEM, X-ray diffraction diagram, TG and DTA, pore characteristics and elements analysis, and the adsorption mechanisms of systems of SO₂-O₂-N₂ and SO₂-O₂-H₂O_(g)-N₂ were studied by FTIR. Results indicated that the desulfurization performance of adsorbent made from surplus sludge was better, subsequent was petrochemical sludge, and the adsorbent made from biochemical sludge of sewage was worse. The desulfurization efficiency of adsorbent made from surplus sludge was slightly lower than active carbon. In the system of SO₂-O₂-N₂, physical adsorption was primary, but in the condition of water, chemical adsorption was primary, where catalysis and oxidation of SO₂ took place in sludge-derived adsorbent. In adsorption process, the adsorption depends on micropore structure.
		2006 Vol. 26 (05): 891-894 [Abstract] ( 1155 ) PDF (1168 KB) ( 446 )

	895	Spectroscopy Study of the Immobilized Cellulose of Magnetic Nanoparticles Fe₃O₄
		WANG Mei¹,SONG Fang¹,WANG Shi-long^2*,WU Qing-sheng¹
		Fe₃O₄ magnetic nanoparticles were synthesized by chemical coprecipitation method using ammonia as the precipitator in the present paper. And then cellulase was immobilized on Fe₃O₄ magnetic nanoparticles via carbodiimide activation, which was testified by FTIR and lots of repeating catalysis experiments. The morphology of nanoparticles immobilized by cellulase was characterized by TEM, and the activity of cellulase was measured by DNS spectrophotometry. The optimum temperature(60 ℃) and pH value (3.94-5.50) for the catalysis ablility of immobilized cellulose were studied. The result showed that compared with the native enzyme the cellulase immobilized on Fe₃O₄ magnetic nanoparticles has the advantages of thermal stability, storage stability, and more extensive optimum pH value.
		2006 Vol. 26 (05): 895-898 [Abstract] ( 430 ) PDF (1017 KB) ( 536 )

	899	Nonlinear Kalman Filter Simultaneous Determination of Mixture of Phenol and 2-Chlorophenol
		WANG Qiang^{1, 2}, MA Pei-sheng¹,TANG Hong-mei^{1, 2},JIA Qing-zhu¹
		An analysis method of nonlinear absorbance for binary composition mixture was proposed. The nonlinear absorbance was composed of the contributions from both themselves and the change in their contributions due to mixing, as well as the contribution from their interaction. The mixture of phenol and 2-chlorophenol was simultaneously determined using nonlinear Kalman filter UV spectrophotometry. UV absorption spectra were obtained with 32 standard solutions (range 1-15 mg·L^-1) and 71 wavelengths(250-290 nm). Standard work matrix of extended Kalman filter was performed from partial least-squares method. The vectors function Jacobi matrix was obtained by linearization of Taylor series for nonlinear absorbance formula. The recovery experiment showed that the extended Kalman filter simultaneous determination of mixture of phenol and 2-chlorophenol that is not only exact, but also stable.
		2006 Vol. 26 (05): 899-903 [Abstract] ( 1473 ) PDF (902 KB) ( 429 )

	904	Study on the Method of Rapid Quality Control of Aqueous Solution of Flos Lonicerae Japonicae Extraction in the Preparation of Qingkailing Injection
		GAO Xiao-yan, LI Na, FAN Qiang, WANG Yun, QIAO Yan-jiang^*
		To establish a rapid and accurate on-line quality control method for aqueous solution of Flos Lonicerae Japonicae extraction (ASFLJE) in the preparation of Qingkailing injection, the wavelength of UV original spectrum and its first derivative spectrum of ASFLJE were scanned. The most suitable spectrum type and wavelength correlated with the chlorogenic acid content in ASFLJE determined by RP-HPLC were chosen to build a regress model. The UV equation for predicting chlorogenic acid content in ASFLJE was established. Other 10 batches of ASFLJE were used for testing the on-line prediction results by comparison of the values of chlorogenic acid content determined by HPLC and predicting equation respectively. The most suitable wavelengths correlated with chlorogenic acid content were 294 nm(r=0.991 9, n=28) in the original UV spectrum and 316 nm(r=0.995 9，n=28)in the first derivative spectrum respectively. The predicting equation of chlorogenic acid content was: c(mg·mL^-1)=506.254 3×A_{316 nm}＋0.177 1(r=0.995 9，n=28). This predicting equation is credible and accurate, as tested by HPLC method (r=0.991 5，n=10). The prediction results of chlorogenic acid content were: the chlorogenic acid content in probable 90 percent ASFLJE was: 0.4-4.0(mg·mL^-1). This method is rapid, simple and accurate, and can be used for the on-line quality control of ASFLJE in Qingkailing injection preparation.
		2006 Vol. 26 (05): 904-907 [Abstract] ( 1461 ) PDF (961 KB) ( 606 )

	908	Library Search of UV Spectra of Organic Environmental Pollutants Based on Neural Network
		WANG Feng-xia, ZHANG Zhuo-yong^*, WANG Ya-min
		The effects of optimization of network parameters, noise, and impurity on the network were investigated detailedly. To speed up the convergence of the network and enhance the resolution of the library search of UV spectra, the derivative spectra for BP-ANN library search was proposed. The method has a higher tolerance to noise and impurity levels than using ordinary UV spectra, especially to slop background levels. Finally, the resolutions of library search of UV spectra with ANN with optimized parameters were compared with conventional correlation coefficient method. Results showed that the ANN is superior to conventional correlation coefficient method and is an effective method for library search of UV spectra.
		2006 Vol. 26 (05): 908-912 [Abstract] ( 426 ) PDF (1097 KB) ( 455 )

	913	Spectrophotometric Determination of Azithromycinbase by Charge Transfer Reaction
		HUANG Wei¹, LIU Xue-jing¹, ZHAO Feng-lin²
		The charge transfer interactions of Azithromycin and 7,7,8,8-tetracyanoquinodimethane (TCNQ) or chloranilic acid(CL) were investigated by spectrophotometry. The apparent molar absorptivity of TCNQ complex is 2.7×10⁴ L·mol^-1·cm^-1at 743 nm，and 5.0×10⁴ L·mol^-1·cm^-1at 842 nm;and that of CL complex is 2.4×10³ L·mol^-1·cm^-1. Beers law is obeyed in the concentration range of 0-30 mg·L^-1 for TCNQ method, and 5-225 mg·L^-1 for CL method. The relative standard deviations of the two methods are 1.0% and 1.4 % (n=6), respectively. The composition of complex of Azithromycin with 7,7,8,8-tetracyanoquinodimethane or chloranilic acid is 1∶2. This proposed method has been applied to the determination of Azithromycin in tablets with satisfactory results.
		2006 Vol. 26 (05): 913-916 [Abstract] ( 1688 ) PDF (989 KB) ( 431 )

	917	ICCD-Based Fast Fluorescence Micro-Imaging Technique and Preliminary Application in Living Cells
		LIN Dan-ying, SUN Yun-xu, MA Wan-yun^*, HAN Dong
		A fast fluorescence micro-imaging system using mainly intensified charge couple device(ICCD), argon-ion laser, and xenon lamp was set up, and its preliminary application in living cells was presented. Real-time observation and imaging of fast concentration and distribution changing of intracellular Ca²⁺ labeled by Fluo-3, a fluorescent Ca²⁺ indicator, in the proliferation process of rat cerebral micro-vessels endothelial cells(rCMECs) were carried out, and curves of artificial intensity versus imaging sequence of four typical points were obtained. It is shown that the ICCD-based fast fluorescence micro-imaging system is a powerful tool for recording the real-time fast processes in living cells.
		2006 Vol. 26 (05): 917-921 [Abstract] ( 635 ) PDF (1128 KB) ( 791 )

	922	Analysis of the Characters of Organic Matter in Water Using Spectral Fluorescence Signature and Fitting Gaussian
		ZHAO Nan-jing, LIU Wen-qing, CUI Zhi-cheng, ZHANG Yu-jun, LIU Jian-guo, LI Hong-bin, YANG Li-shu
		A sort of analytical method of fast diagnosis of organic matter in water is discussed. The total luminescence spectra (TLS) of water samples in combination with laser induced fluorescence (LIF) measurements using 532 nm wavelength excitation source were measured in the laboratory. The spectra of dissolved organic matter (DOM) and chlorophyll a (Chl a) were pointed out and obtained with spectral fluorescence signature (SFS) technique. The spectrum of water Raman scattering and fluorescence of DOM and Chl a were separated from TLS with fiting Gaussian of the least squares method, and a high correlation coefficient excelling 0.996 4 was obtained. The results indicated the possibilities of water quality monitoring in real time and on line based upon SFS technique and fitting Gaussian of the least squares method.
		2006 Vol. 26 (05): 922-924 [Abstract] ( 1489 ) PDF (923 KB) ( 821 )

	925	Self-Absorption of NO Fluorescence Induced by Two-Photon
		ZHANG Lian-shui,ZHANG Gui-yin,HAN Xiao-feng
		The two-photon LIDFS of NO excited with 452.4 nm output of an optical parameter generator and optical parameter amplifier pumped by a Nd：YAG laser was obtained. The vibration frequency and the inharmonic coefficients of the ground electronic state of NO were calculated from the results of the spectral ascription. They are ω″_e=(1 904.7±7.3) cm^-1,ω″_eχ″_e=(14.2±1.2) cm^-1, and ω″_ey″_e=-(0.021 8±0.009 1) cm-1 respectively. It was found for the first time that the intensity of the spectral lines departs from the Frank-Condon principle due to the self-absorption of NO molecules. The spectral line of A ²Σ(v′＝0)→X ²Π(v″＝0) transition disappears in the fluorescence spectra. But it appears gradually with decreasing the sample pressure and the distance from the laser-gas interaction volume to the receiving window. All of these provide an important reference for monitoring NO by the technique of laser-induced fluorescence.
		2006 Vol. 26 (05): 925-927 [Abstract] ( 1564 ) PDF (905 KB) ( 489 )

	928	Synthesis, Characterization and Luminescence Properties of Coordination Compounds of Rare Earth with p-Tert-Butyl-Calix[8] Arene
		YAN Lai¹, ZHAO Yong-liang^1*, ZHAO Feng-ying², WANG Ling-xuan³, YE Jian-ping³
		Fourteen solid coordination compounds of rare earth(Sm³⁺, Eu³⁺, Tb³⁺ and Dy³⁺ and Ln³⁺(La³⁺, Gd³⁺ and Y³⁺)-doped Tb³⁺ with p-tert-butyl-calix[8] arene (LH₈) have been synthesized and characterized. Elemental analysis, rare erth complexometry, ¹H NMR spectra and TG-DTA have been studied. The results suggest that the complexes have the composition of [RE₂(LH₂)(DMSO)₅]DMSO，[RE₂(LH₂)(DMF)₅]2DMF，[LnTb(LH₂)(DMSO)₅]DMSO and [LnTb(LH2) (DMF)₅]2DMF respectively. Fluorescence spectrum suggests that the Tb³⁺ complexes have characteristic luminescence, and its fluorescence intensity is enhanced after doping with La³⁺, Gd³⁺ and Y³⁺. The influence of the doping ions and two neutral ligands(DMSO and DMF) has also been discussed. In addition, the fluorescence lifetime of some complexes has been investigated.
		2006 Vol. 26 (05): 928-932 [Abstract] ( 1129 ) PDF (925 KB) ( 459 )

	933	Synthesis and Spectral Characterization of Rare-Earth-Ortho-Amino Phenylbenzoate-2,2’-Bipyridine Complexes
		WANG Shao-ting, YANG Yong-li, ZHU Hui-ju, NIE Feng-mei, ZONG Rui-fa, DENG Yu-heng^*
		The solid rare-earth complexes were synthesized using rare-earth ions (RE=Tb, Nd, Sm, La) reacting with ortho-amino phenylbenzoic acid (L) and 2,2’-bipyridine (bipy). Their compositions were confirmed and the spectral properties were characterized by element analysis, infrared and ultraviolet absorption spectra, and DTA-TGA. The fluorescent properties of complexes TbL₃ and TbL₃·bipy·3H₂O were also measured and discussed. The result shows that the fluorescence intensity of TbL₃·bipy·3H₂O is stronger than that of TbL₃.
		2006 Vol. 26 (05): 933-935 [Abstract] ( 1180 ) PDF (869 KB) ( 647 )

	936	Plasma Glutathione of Patients with Coronary Heart Disease Measured by Fluorospectrophotometer
		HUANG Yan-sheng¹, ZHI Yan-fang¹, KONG Shen-yan², WANG Qiu-lin¹, XU Bo-shi³ , WANG Shu-ren^1*
		The standard samples of reduction form glutathione (GSH) and oxidization form glutathione (GSSG) were scanned with full-wavelength range to determine the excitation wavelength λ_ex 334.4 nm，the emission wavelength λ_em 424 nm, and the spectral bandwidth 5 nm respectively. Phosphate buffer saline (PBS) of pH 8.3 served as buffer solution. GSH was incubated for 30 min with 100 μL o-phthaldehyde (OPA) of 10 mmol·L^-1 methyl alcohol solution for derivatization, and then fluorescence intensities were measured. With standard glutathione concentration being independent variable and fluorescence intensity being dependent variable，the linear equations for GSH and GSSG were deduced: Y_GSH=6.9+8.6X (r²=0.994) and Y_GSSG=6.2+17.2X (r²=0.999). Standard curves were done hereby. The plasma glutathione of three groups was then measured, and GSH/GSSG redox potential was calculated according to Nernst equation. The results indicated that, from normal control group to prophase coronary heart disease group, then to coronary heart disease group, the GSH and GSH/GSSG ratio gradually reduced, GSSG and GSH/GSSG redox potential gradually increased (more positive) (all P＜0.05), and the redox potential shifted to oxidization direction along with the development of coronary heart disease. This fluorospectrophotometry method showed simple operation, and fine precision and accuracy.
		2006 Vol. 26 (05): 936-940 [Abstract] ( 1500 ) PDF (985 KB) ( 797 )

	941	Studies on the Interaction of the Metal Complex of Hydrazide of Podophyllic Acid with DNA
		WANG Ping-hong¹, ZHANG Qi^1*, WANG Liu-fang², SONG Yu-min³, QU Jian-qiang², LIU Ying-qian²
		The interaction between the metal complex of hydrazide of podophyllic acid and calf thymus (CT) DNA was studied by using absorption spectra, fluorescence spectra and DNA heat denaturation. It was found that the intensity of the maximal absorption peaks from absorption spectra is weakened in the presence of the metal complex of hydrazide of podophyllic acid compared with that in the absence of the metal complex. All the experimental results show that the intercalation mode was proved to exist between HDPP-Ni complexes and CT DNA.
		2006 Vol. 26 (05): 941-943 [Abstract] ( 1783 ) PDF (945 KB) ( 436 )

	944	Determination of Calcium Concentration in Water Solution by Laser-Induced Plasma Spectroscopy
		LI Jing¹, LIN Chang-he¹, LI Sheng-li²
		With the experiment setup the calcium concentration in water solution was measured, based on a Nd:YAG Q-switched solid laser as the exciting light. The experiment results show that the concentration of calcium has a good linear relationship with its spectral intensity, the maximum relative errors of measurement are 3.79%, and the linear regression coefficients are 0.992 87. In addition, laser induced plasma spectroscopy (LIPS) demonstrated convenient operation, and reliable and higher precision measurement of calcium concentration in water solution.
		2006 Vol. 26 (05): 944-946 [Abstract] ( 1511 ) PDF (887 KB) ( 640 )

	947	Determination of Trace Elements in Sika Bone Powder by Inductively Coupled Plasma Mass Spectrometry with Microwave Digestion
		LIU Yan-ming¹, CHEN Zhi-yong¹,HAN Jin-tu¹, WANG Hui¹ , WANG Zhi-wen²
		Contents of trace elements in sika bone powder were determined with microwave digestion and inductively coupled plasma mass spectrometry. Under the optimum conditions, the detection limits (3σ, n=11) are in the range of 0.000 6-1.498 ng·mL^-1 with relative standard deviations of 1.7%-6.8%. The recoveries are between 91% and 109%. The analytical results of national certified reference demonstrated the applicability of the proposed method.
		2006 Vol. 26 (05): 947-949 [Abstract] ( 1095 ) PDF (866 KB) ( 518 )

	950	Direct Determination of Lead and Cadmium in Soil by Slurry-Sampling Graphite Furnace Atomic Absorption Spectrometry Using Matrix Modification Technique
		SUN Han-wen,WEN Xiao-hua,LIANG Shu-xuan
		A method for the direct determination of lead and cadmium in soil by slurry-sampling graphite furnace-atomic absorption spectrometry using NH₄H₂PO₄ as matrix modifier was developed. The effects of slurry stability, particle size of sample, matrix modifiers, ashing temperature, atomization temperature and common coexistent components on the signal intensities of lead and cadmium were investigated. The apparent activation energies of lead and cadmium were measured based on the linear relationship between the logarithm value of atomization peak time and atomization temperature. The mechanism of matrix modification was discussed. Under optimized conditions, the detection limit was 9.05×10^-10 g·mL^-1 for Pb and 1.76×10^-11 g·mL^-1 for Cd. The recoveries were in the range of 91%-97% for Pb and 93%-109% for Cd. The relative standard deviations were in the range of 4.2%-7.8%.
		2006 Vol. 26 (05): 950-954 [Abstract] ( 1663 ) PDF (918 KB) ( 590 )

	955	Determination of Lead in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction with Dithizone
		XIAO Shan-mei^{1, 2}, CHEN Jian-rong^2*, SHEN Yu-qin²
		Cloud point extraction was used for the preconcentration of lead after the formation of a complex with dithizone in the presence of surfactant Triton X-114, and then the lead was determined by graphite furnace atomic absorption spectrometry. The conditions affecting the separation and detection process were optimized. Separation of the two phases was accomplished by centrifugation for 15 min at 4 000 rpm. Upon cooling in an ice-bath, the surfactant-rich phase became viscous. The aqueous phase could then be separated by inverting the tubes. Later, a solution of methanol containing 0.1 mol·L^-1 of HNO₃ was added to the surfactant-rich phase up to 0.5 mL. The samples were determined by graphite furnace atomic absorption spectrometry with NH₄H₂PO₄ and Mg(NO₃)₂ as a chemical modifier. At pH 8.0, the preconcentration of only 10 mL sample in the presence of 0.05% Triton X-114 and 20 μmol·L^-1 dithizone permitted the detection of 0.089 μg·L^-1 lead. The enhancement factors were 19.1 times for lead. The calibration graph using the preconcentration system for lead was linear with a correlation coefficient of 0.998 from levels near the detection limits up to at least 30 μg·L^-1. The regression equation was A=0.026 1c(μg·L^-1)+0.010 6. The proposed method has been applied to the determination of lead in water samples.
		2006 Vol. 26 (05): 955-958 [Abstract] ( 609 ) PDF (942 KB) ( 556 )

	959	Determination of Trace Copper and Cadmium in Water by Flame Atomic Absorption Spectrometry Coupled with Flow Injection On-Line Preconcentration Using Air Segmentation
		SU Yao-dong, ZHU Wen-ying, QIN Li, CHEN Long-wu
		The flow injection on-line preconcentration with a knotted reactor (KR) system for the determination of copper and cadmium in water by flame atomic absorption spectrometry(FAAS) was described in the present paper. The precipitation preconcentration of trace copper and cadmium was achieved by on-line merging of the sample and ammonia solutions. The resultant precipitates were on-line collected by a knotted reactor (KR) without filtration, and then the authors used a process of air segmentation. A solution of 1 mol·L^-1 HNO₃ was employed to dissolve the collected precipitates and to deliver the analyte into the FAAS system for on-line detection. With a sample loading flow rate of 4.4 mL·min^-1 and a preconcentration time of 90 s, the enhancement factor was 34 (for Cu) and 36 (for Cd) as compared with the conventional FAAS method. The detection limits (3σ) are found to be 1.9 and 0.3 μg·L^-1 for copper and cadmium respectively. The precision (RSD, n=11) was found to be 2.3% at the level of 30.0 μg·L^-1 of Cu (Ⅱ), and 2.6% at the level of 20.0 μg·L^-1 of Cd (Ⅱ). The proposed method has been successfully applied to the determination of Cu (Ⅱ) and Cd (Ⅱ) in water samples.
		2006 Vol. 26 (05): 959-962 [Abstract] ( 1116 ) PDF (966 KB) ( 649 )

	963	Determination of Nine Trace Elements in Dioscorea Opposita Thumb by Flame Atomic Absorption Spectrophotometry
		ZHANG Wei¹, ZHANG Zhuo-yong^1*, SHI Yan-zhi¹, FAN Guo-qiang²
		The contents of the potassium, calcium, sodium, magnesium, copper, zinc, iron, manganese, strontium and nickel in Dioscorea opposita thumb were determined. The relative standard deviation(RSD) of the first eight contents is 0.43%, 1.10％, 4.41％, 0.68％，1.44％，1.88％，1.29％ and 0.03％ respectively, and the percentage recovery is 90.0%-111.0%. The method is convenient and accurate. It can be used to determine the trace elements simultaneousy in Dioscorea opposita thumb.
		2006 Vol. 26 (05): 963-965 [Abstract] ( 516 ) PDF (867 KB) ( 909 )

	966	Adsorption and Coprecipitation of Dissolved Metals with Jarosite under Conditions Simulating Sewage Sludge Bioleaching
		ZHOU Shun-gui, ZHOU Li-xiang^*
		The inoculation of Acidithiobacillus ferrooxidans and the addition of Fe²⁺ as their substrates accelerated the solubilization of Zn, Cu and Cr from sewage sludge. However, a decrease in Cu removal from 91% to 60% with time elapse could be observed in the late process, which appeared simultaneously with the formation of jarosite resulting from hydrolysis of Fe³⁺. The tested jarosite was synthesized by using bacterial oxidation of Fe²⁺ by resting A. ferrooxidans in acid solution (pH 2.5) under conditions stimulating sludge bioleaching. Adsorption edge measurement showed that only less than 9% of Cu²⁺ was adsorbed onto jarosite in the pH range of 2.0-2.5, indicating that adsorption mechanism could not explain fully re-sorption of Cu²⁺ (about 31%) in the anaphase of bioleaching process. In the coprecipitation studies, when jarosite was precipitated in the presence of Cu²⁺ (10 mg·L^-1), a significant amount of Cu (44.6%) was incorporated into the precipitate. Coprecipitation of jarosite with Cu²⁺ was the predominant process by which soluble Cu was partially re-sorpted by jarosite in the anaphase of bioleaching process.
		2006 Vol. 26 (05): 966-970 [Abstract] ( 1793 ) PDF (1001 KB) ( 400 )

	971	The Reflection Spectrometer and Quantitative Analysis Design
		ZHANG Ping, CHEN Yong-heng, YAO Yan
		The reflection spectrometer with optical fibre transmission was designed and used in quantitative analysis. The reflection spectrometry was applied to the determination of reducing sugar in samples based on the reduction reaction of the reducing sugar with Fehling’s reagent. The reduction reaction was carried out in a micro-reaction cell, and the reddish colored Cu₂O produced was settled at the bottom of the reaction cell. The reflectance R_∞, which is directly proportional to the amount of Cu₂O produced, was measured by the reflection spectrometer. The fundamental principle, effect factors, and experimental conditions of the method were discussed. Linear relationship was obtained in the range of 20-120 μg of reducing sugar. The special features of this method were its simplicity in operation, relatively high sensitivity of determination, and the use of small amount of reagent. Satisfactory results were obtained in its application to the analysis of wine and honey samples.
		2006 Vol. 26 (05): 971-973 [Abstract] ( 1554 ) PDF (938 KB) ( 480 )

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