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2004 Vol. 24, No. 12 Published: 2004-12-26

光谱学与光谱分析

	1489	The Key Technology of Picosecond Time-Correlated Single Photon Counting Spectrometer
		ZHANG Xiu-feng^{1, 3}, SONG Ke-fei², YU Tao³, HAN Bing-dong^{1, 3}, SHENG Cui-xia⁴, LIN Jiu-ling^{1, 5*}
		The picosecond time-correlated single photon counting spectrometer developed uses the TCSPC technique and grating splitter technique that can compensate the time spread dynamically and statically. The time spread caused by the conventional optical system can be eliminated completely. The multichannel analyzer is used to measure the fluorescence decay curves and the time-resolved spectrum by opening the time windows. The method for multi-exponential fitting to the fluorescence decay is also used to deal with the data. The system theory and design of the spectrometer are presented in detail, and the process of operation is introduced with the integration of the system. Many standard samples have been measured, and the data have been analyzed and contrasted. Experimental results show that the fluorescence life-span scaled by the spectrometer reaches picosecond distinction, and the spectrometer’s sensitivity is single photon counting. Time resolution of the spectrometer is 8.8 ps.
		2004 Vol. 24 (12): 1489-1493 [Abstract] ( 1624 ) PDF (1132 KB) ( 831 )

	1494	Laser Resonance Ionization Spectroscopy of Even-Parity Autoionization States of Cerium Atom
		LI Zhi-ming, ZHU Feng-rong, ZHANG Zi-bin, REN Xiang-jun, DENG Hu, ZHAI Li-hua,ZHANG Li-xing
		This paper describes the investigation of even-parity autoionization states of cerium atoms by three-step three-color resonance ionization spectroscopy (RIS). Twenty-seven odd-parity highly excited levels, whose transition probability is high, were used in this research. One hundred and forty-one autoionization states were found by these channels with the third-step laser scanning in the wavelength range of 634-670 nm. The ionization probabilities of different channels, which had higher cross sections, were compared. On the basis of this, eight optimal photoionization schemes of cerium atom have been given.
		2004 Vol. 24 (12): 1494-1498 [Abstract] ( 1107 ) PDF (1003 KB) ( 350 )

	1499	Investigations of Transient Time-Dependent Spectral Multi-Channel Measurement for Shocked KCl Crystal
		CHENG Juan¹, HE Ying-hong¹, ZUO Hao-yi¹, RAN Rui-jiang¹, XUE Kang¹, YANG Jing-guo^1*，TAN Hua², HU Shao-lou², WANG Xiao-song²
		In this paper, the authors reported a new method for measuring transient time-dependent spectra using multi-fiber delay coupler and optical multi-channel analysis technique. The fiber delay coupler consists of five fibers with different lengths and its time-delay between two fibers is determined by the different fiber lengths. The light beams that came from the fiber coupler were coupled by a lens system into the slit of a spectrograph and formed a spectral pattern on the focus plane of the spectrometer. A two-dimensional CCD detector convested the optical pattern into an electrical pattern, and then the transient time-dependent spectra were obtained by a personal computer. The experimental setup was constructed, and the transient time-dependent spectra were measured for KCl crystal shocked by a high speed pill. The time resolution was 20 ns, and the spectral intensity resolution reached 1/18 bit.
		2004 Vol. 24 (12): 1499-1501 [Abstract] ( 631 ) PDF (1056 KB) ( 347 )

	1502	Study on Visible Chemiluminescence from Reaction of Microwave Discharge of CF₄/Ar with Carbon Disulfide
		ZHANG Xian-yi^1,2, LUO Xiao-lin¹, KONG Xiang-lei¹, ZHANG Wei¹,LI Hai-yang^1*
		Using crossed molecular beam-chemiluminescence apparatus，visible chemiluminescence in the region of 300-900 nm was measured from the gas-phase reaction of microwave discharge of CF₄ diluted in Ar with carbon disulfide at various pressures. The geometries and frequencies of possible reaction products were respectively investigated at the B3LYP/6-311++G(3df,2pd) and MP2/6-311+G(d,p) levels. Chemiluminescence spectrum was assigned to emission spectrum of the electronically excited states of F₂S₂. From the analyse of spectrum and reaction mechanism, it is proposed that carbon disulfur was dissociated by metastable Ar generated from microwave discharge. The electronically excited state of F₂S₂ was obtained from multistage reactions of the dissociative products with atoms F generated from microwave discharge.
		2004 Vol. 24 (12): 1502-1505 [Abstract] ( 1058 ) PDF (964 KB) ( 342 )

	1506	Effect of Eu³⁺ Molar Ratio on the Spectra of Y₂O₂S:Eu³⁺, Mg²⁺ and Ti⁴⁺ Red Phosphor
		YANG Zhi-ping, GUO Zhi, ZHU Sheng-chao, WANG Wen-jie
		Synthesis of Y₂O₂S:Eu³⁺, Mg²⁺ and Ti⁴⁺red phosphor by flux fusion method was presented. The decay curve of Y₂O₂S:Eu³⁺, Mg²⁺ and Ti⁴⁺ red phosphor was measured and the afterglow time was over one hour. The emission spectra and excitation spectra were measured, and the effect of Eu³⁺ molar ratio on the emission spectra and excitation spectra were also discussed. The emission spectra showed that Y₂O₂S:Eu³⁺, Mg²⁺ and Ti⁴⁺ had narrow emission peaks. The emission peaks ascribed to Eu³⁺ ions transition from ⁵D_J (J＝0, 1, 2, 3,) to ⁷F_J (J＝0，1，2，3，4，5) were found. With the increase of Eu³⁺ molar ratio, the emission peaks 513.6, 540.1，556.4，587.3 and 589.3 nm ascribed to the energy transition ⁵Ｄ₂，⁵Ｄ₁ to ⁷Ｆ_J(J＝0, 1, 2, 3, 4) deteriorated gradually relative to the main emission peak at 627.0 nm. The emission peaks ascribed to energy transition ⁵Ｄ₀ to ⁷Ｆ_J(J=0, 1, 2, 3, 4) didn’t weaken relative to the main emission peak. It was probably due to the so-called true activator saturation effect. This function on the higher activated states ⁵D₂ and ⁵D₁ was more distinct. The excitation spectra of Y₂O₂S:Eu³⁺, Mg²⁺ and Ti⁴⁺ showed that it had excitation peaks at 350 nm nearby, which was ascribed to the absorption of charge transfer (Eu³⁺-O^2-, Eu³⁺-S^2-). The excitation peaks at 468, 520 and 540 nm were ascribed to the representative energy transition 4f-4f of Eu³⁺ ions. With the increase of Eu³⁺ molar ratio, the excitation peaks 468, 520 and 540 nm strengthened relative to the main absorption peak at 350 nm nearby.
		2004 Vol. 24 (12): 1506-1510 [Abstract] ( 960 ) PDF (1031 KB) ( 325 )

	1511	Emission Mechanism in the Tb Complex Doped PVK System
		XU Deng-hui¹, DENG Zhen-bo^1*, ZHANG Zhi-feng¹, ZHANG Meng-xin¹, LIANG Chun-jun¹,WANG Rui-fen²
		Excitation and photoluminescence(PL) spectra of the mixture terbium complex and PVK were investigated. The excitation spectrum of Tb complex dispersed PVK film is very similar to that of the pure PVK film, indicting that energy transfer occurs from PVK to Tb complex. For the overlap between the excitation spectrum of Tb complex dispersed PVK film and the PL spectrum of PVK film is very little, the ratio of occurrence for Frester energy transfer is very little. The emission of Tb³⁺ mainly comes from the excited ligand，which comes from the ligand capture of electron-hole pairs. In the electroluminescence(EL) spectra, the emission of PVK is completely restrained and only emission of Tb³⁺ is occured, which origins from the different mechanism in comparison with photoluminescence.
		2004 Vol. 24 (12): 1511-1513 [Abstract] ( 977 ) PDF (972 KB) ( 338 )

	1514	Study on the Relationships between Chemiluminescent Properties and Molecular Structures of Some Biacridine Probes
		ZHUANG Hui-sheng¹, WANG Qiong-e², CHEN Guo-nan³, HUANG Jin-ling³
		The chemiluminescent(CL) properties of biacridine probes, such as 10,10’-dimethyl-3,3’-disulfo-9,9’-biacridine(DMDSBA), 3,3’-disulfo-9,9’-biacridine dinitrate(DSBADN), 10,10’-diethcarboxyl-9,9’-biacridine dinitrate(DEBADN), 10,10’-dimethyl-3,3’-diamino-9,9’-biacridine (DMDABA)，and 10,10’-di(4-aminobutyl)-9,9-biacridine dinitrate(DABADN)，were studied in this paper, and the relationships between properties and molecular structures were obtained. A new theory and some valuable experimental data have been provided for the investigation and exploitation of the new CL probes for biomacromolecules.
		2004 Vol. 24 (12): 1514-1517 [Abstract] ( 1065 ) PDF (1257 KB) ( 352 )

	1518	A Study on Europium Sensitized Chemiluminescence of Pipemidic Acid
		LI Xia¹，QIANG Hong¹，WANG Xiao-li²，CHEN Shi-lü²，ZHAO Hui-chun²
		A flow injection chemiluminescence method for the determination of Pipemidic acid (PPA) was developed. It is based on luminescence produced with KMnO₄-Na₂S₂O₄ CL system sensitized by Eu³⁺-PPA. The familar excipients such as starch and dextrine do not cause interference. The several kinds of affect on chemiluminescence were studied. The linear range and detection limit for PPA are 7.00×10^-9-9.00×10^-7 mol·L^-1 and 4.09×10^-9 mol·L^-1, respectively. This method have successfully been applied to the determination of PPA in tablet and urine. And the mechanism of chemiluminescence is proposed.
		2004 Vol. 24 (12): 1518-1520 [Abstract] ( 1542 ) PDF (1262 KB) ( 341 )

	1521	Determination of Phloroglucinol by a New Flow Injection Chemiluminescence Method
		XIE Cheng-gen，LI Huai-fen
		Abstract Chemiluminescence reaction of phloroglucinol with potassium permanganate in the presence of formaldehyde as an enhancer was investigated. A new chemiluminescence method for the determination of phloroglucinol with flow injection technique was developed. The linear range for phloroglucinol is 5.0×10^-9-5.0×10^-5 mol·L^-1 with a detection limit of 3.0×10^-9 mol·L^-1. The relative standard deviation is 2.5% for 1.0×10^-6 mol·L^-1 phloroglucinol in 11 repeated measurements. The method has been used to determine the content of phloroglucinol in simulated water with satisfactory results.
		2004 Vol. 24 (12): 1521-1523 [Abstract] ( 1000 ) PDF (1263 KB) ( 500 )

	1524	Preparation and Characterization of 2(8-Hydroxyquinoline)-2(Phenol)Zirconium Thin Film
		HAO Yu-ying¹, HAO Hai-tao², WANG Hua², ZHOU He-feng², LIU Xu-guang², XU Bing-she²
		In this paper, the new emitting material zirconium complex with 8-hydroxyquinoline and phenol (Zr(OPh)₂q₂), which can form high quality nano-scale amorphous thin films at glass substrates cleaned by vacuum evaporation, was synthesized. Its crystallization，thermal stability，the structure of energy band and PL mechanism were investigated respectively by FTIR spectra, DTA-TG analysis , SEM, XRD spectra, UV-Vis absorption spectra and fluorescence spectra. Results show that the Zr(OPh)₂q₂ is a thermally stable material, whose melting point is 381.2 ℃, decomposition temperature is 467.1 ℃, whose film can emits intense yellow-green fluorescence with peak wavelength at 525 nm and a full width at half-maximum of 107.6 nm under UV excitation(390 nm), powder has intense yellow fluorescence, therefore it may be a excellent electroluminescent material.
		2004 Vol. 24 (12): 1524-1527 [Abstract] ( 1001 ) PDF (1761 KB) ( 459 )

	1528	Research on the Infrared Spectrometry of Aging Silk Fabrics
		ZHANG Xiao-mei,YUAN Si-xun
		The detection of deterioration degree of ancient silk fabrics will be helpful to the selection and developing of conservation methods. This paper caried out some research on the deterioration extent and mechanism of silk fabrics by means of infrared spectrometry. The samples artificially aged and excavated from Hubei, Innermongolia and Qinghai province, were analyzed. The artificially aging was done by simulating three main natural aging factors: light, heat and hydrolysis. The infrared spectrometric analysis results show that although the infrared spectrometry is a half-quantitative analysis method, for the hydrolysis-aged silk fabrics, it can give good qualitative and better half-quantitative analysis results because of the increase of carboxyl. So the infrared spectrometric analysis is of practical value for the conservation state and aging mechanism studies of ancient silk.
		2004 Vol. 24 (12): 1528-1532 [Abstract] ( 1474 ) PDF (1308 KB) ( 479 )

	1533	Structural Characterization of Rare-Earth Stearate and It’s Thermal Stability Mechanism for PVC
		ZHENG Yu-ying, CAI Wei-long, FU Ming-lian, SUN Rui-qing
		Structural characterization of rare-earth stearate was conducted by FTIR and XRD. The results show that the bonds between the stearate and rare-earth metal ions in rare-earth stearate are main ionic character and have the stratified crystalline structure with the crystal layer formed from a plane layer of rare-earth ions combined with two layers of fully extended zigzag chains of stearic acid radicals arranged parallelly to each other on its both sides, and the rare-earth ions axes are inclined to the crystal layer planes in it. Congo red test showed that the stabilizing time increased when the stabilizers’ concentration increased. The order of stability of this four rare-earth stearates is Last＞Ndst＞Yst＞Dyst. Furthermore, the thermal stability mechanism of rare earth stearate for PVC has been presumed by FTIR. The results indicate that Last and Ndst can bate the chain reaction and exchange the labile functional groups in the backbone chains for other more stable substituents derived from the stabilizer and change the framwork, while Yst and Dyst’s effect is not clear.
		2004 Vol. 24 (12): 1533-1536 [Abstract] ( 1792 ) PDF (996 KB) ( 431 )

	1537	Oil Spill Identification by Near-Infrared Spectroscopy
		WANG Li¹，ZHUO Lin¹，HE Ying^{1, 2*}，ZHAO Ying¹，LI Wei¹，WANG Xiao-ru²，Frank Lee²
		Petroleum oil spill happens occasionally at sea. It’s important to differentiate the exact products in order to carry out following actions to decrease harmfulness. In the present study, a rapid oil spill identification method by near infrared spectroscopy coupled with pattern recognition techniques is proposed. 56 simulated spilled oils of gasoline, diesel fuel and lubricating oil in marine were chosen to develop the method. Organic reagent of CCl₄ was used to extract the oil. Pattern recognition techniques were established by principal component analysis (PCA) coupled with Mahalanobis’ distance with the multiplicative signal correction (MSC) and Norris first derivative pretreatment. The study shows that PCA technique is a useful method to extract the main characteristics, and Mahalanobis’ distance is an ellipsoidal boundary that circumscribes a data cluster. And oil spill samples with concentration above 0.4 μL·mL^-1 can be successfully identified by the method. The developed technique could be further applied to the identification of spilled oil in marine.
		2004 Vol. 24 (12): 1537-1539 [Abstract] ( 1859 ) PDF (971 KB) ( 925 )

	1540	A Novel Method for the Determination of Inorganic Ions in Complex Plant Samples by Near Infrared Spectroscopy
		WANG Guo-qing, WANG Fang, CHEN Da, SU Qing-de, SHAO Xue-guang^*
		Inorganic ions in plant samples can be determined by near-infrared (NIR) spectral technique, because they are combined with organic groups with NIR absorption. A method for the determination of inorganic ions in complex plant samples was established based on the combination of discrete wavelet transform (DWT) and NIR technique. In the proposed method, the raw NIR data and their wavelet coefficients are used for modeling and prediction of the contents of potassium in tobaccos by partial least square method (PLS). It is shown that there is almost no loss of spectral information with the NIR data compressed to 3.3% of its original size. The model based on wavelet coefficients is better than that based on the full NIR spectral range. With the improved method, accurate prediction can be achieved.
		2004 Vol. 24 (12): 1540-1542 [Abstract] ( 1479 ) PDF (966 KB) ( 499 )

	1543	FTIR Study on the Finger Nail with Carcinoma of Nasopharynx
		DONG Qin¹, LIU Gang²,LIU Tian-hui³
		Finger nails from twenty normal people and three with carcinoma of nasopharynx were studied by Fourier Transform Infrared (FTIR) technique. The results showed that there are obvious differences between FTIR spectra of them in spectral parameters such as frequency, intensity and band shape etc. The most striking differences in the spectra were observed in the change of amide Ⅱ, the disappearance of δ_ｓ(CH₃) peak, and at 874.0 cm^-1 whether appeared an absorption peak. The changes involving the phosphate symmetric stretching ν_{s, PO^-₂} and asynmmetric stretching ν_{as, PO^-₂} modes, the CH₃ and CH₂ groups stretching (ν_{s, CH₂}, ν_{as, CH₃}) bending (δ (CH₃)) modes and the C—O stretching ν (C—O) mode were discussed. In addition, the changes of structure of hydrogen-bonding of nucleic acid and cell proteins and the packing and the conformational structure of the membrane lipids were analysed. The average wave number of band of ν_s (PO^-₂) shifted from 1 080.0 to 1 077.6 cm^-1 and that of ν_as (PO^-₂) shifted from 1 239.4 to 1 238.4 cm^-1, which indicated that the degree of hydrogen-bonding formed by oxygen atom of the phosphodiester groups of nucleic acids was weakened. The average wave number of band of δ (CH₂) of membrane lipids shifted from 1 453.1 to 1 453.7 cm^-1, and its peak intensity was slightly enhanced, which suggested that the conformational structure of the methylene chains of membrane lipids is more disordered than in normal nail.
		2004 Vol. 24 (12): 1543-1545 [Abstract] ( 1485 ) PDF (972 KB) ( 359 )

	1546	Influence of Smooth，1st Derivative and Baseline Correction on the Near-Infrared Spectrum Analysis with PLS
		ZHENG Yong-mei¹, ZHANG Tie-qiang¹, ZHANG Jun², CHEN Xing-dan², SHEN Xuan-guo¹
		This paper studied the influence of using pre-procession such as smooth, 1st derivative and baseline correction on the analyｓis of near-infrared spectrum. Comparing the analysis results by the pre-procession methods, and using PLS arithmetic, the best pre-procession was determined. In smooth pre-procession method, the best smooth points were proposed for regression using PLS. The analysis result is satisfactory.
		2004 Vol. 24 (12): 1546-1548 [Abstract] ( 1569 ) PDF (956 KB) ( 761 )

	1549	Wavelet Denoising and Optimization of Two-Dimensional Correlation IR Spectroscopy
		ZHAN Da-qi, SUN Su-qin^*, ZHOU Qun，QIN Zhu
		Wavelet analysis and wavelet denoising was applied to analyse the data of two dimensional correlation IR spectroscopy of traditional Chinese medicine for the first time in this article. The results showed that, after denoising, the authors can decrease the interference to the synchronous spectra of two dimensional correlation IR spectroscopy effectively, and tone up the signal peaks and separate the peaks which overlap together before denoising. In this way, the authors can not only improve the spectral revolution, but also get more spectral informations.
		2004 Vol. 24 (12): 1549-1552 [Abstract] ( 1392 ) PDF (1080 KB) ( 384 )

	1553	Identification of an Unknown Assistant Blowing Agent in AC Blowing System
		HE Wen-xuan¹, Robert Shanks²
		Recently it has become a trend to modify AC by adding different additives in AC system. In the modification, it is a key question to know what kind of additives should be added. So, qualitatively deformulating the additives will certainly help the research on and development of modifying AC a lot. In this paper, TLC (Thin Layer Chromatograph) was used to separate and purify the unknown assistant blowing agent in AC blowing system. After that, FTIR-Microscope was used to indicate the functional group in the uncommon unknown compound. Through combination of FTIR analysis, elemental analysis and other physical and chemical analysis, the molecular structure of the unknown was deduced. Finally, by explaining the unknown compound’s MS spectra, the molecular structure of the unknown was confirmed further. The method can be extended to analyze other additives in AC blowing agent system whose various standard spectra are absent.
		2004 Vol. 24 (12): 1553-1555 [Abstract] ( 958 ) PDF (987 KB) ( 322 )

	1556	A DRIFTS Study of SO₂ Oxidation on the Surface of CaCO₃ Particles
		LI Lei, CHEN Zhong-ming^*, DING Jie, ZHU Tong, ZHANG Yuan-hang
		CaCO₃ is an important component of mineral dust aerosols in the atmosphere, but its role in atmospheric heterogeneous chemistry is still unclear. In this paper, the oxidation of SO₂ on CaCO₃ particles was studied using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Formation of sulfite and sulfate was identified on the surface, and the role of O₃ on the oxidation process is determined by comparing the experiments in different conditions. DRIFTS is proved as a useful tool for studying heterogeneous reactions on CaCO₃ particles. The results show that in the presence of O₃, SO₂ can be oxidized into sulfate on the surface of CaCO₃ particles. A two-step mechanism that involves adsorption of SO₂ followed by oxidation is presented.
		2004 Vol. 24 (12): 1556-1559 [Abstract] ( 1358 ) PDF (1033 KB) ( 365 )

	1560	Extraction and Analysis of Sargassum Hemiphyllum Polysaccharides
		MENG Qing-yong, LIU Zhi-hui, XU Mei-yi, DONGYE Guang-zhi
		Sargassum hemiphyllum polysaccharides(SHP) was extracted by thermal water method and the physical and chemical characters, the extraction rate, contents, compositions of SHP was studied. The result showed that SHP was ashen powder, water-soluble, insoluble in organic solvents. The reaction of iodide-potassium iodide was negative to evaluate that SHP was nonstarch polysaccharides. Extraction rate was 7.04% and the content of polysaccharides was 82.9%. Ultraviolet spectrum showed that there were little DNA and protein. Infrared spectroscopy showed that SHP was main pyrano polysaccharides and had β-linked glycopolysaccharides in molecule structure of SHP. Thin layer chromatography traced that SHP could be xylan. The results indicated that the extract was not only polysaccharides but also higher purify and the method was high efficiency.
		2004 Vol. 24 (12): 1560-1562 [Abstract] ( 1483 ) PDF (1332 KB) ( 536 )

	1563	Preprocessing of Near Infrared Spectroscopic Data
		GAO Rong-qiang¹, FAN Shi-fu^1*, YAN Yan-lu², ZHAO Li-li²
		Spectroscopic data of samples recorded by spectroscopic instruments are confused by a series of noises, and interferences, therefore the proper data preprocessing is the basis of the following spectroscopic calibration, model establishment and transference, which is very important for the achievement of accurate analytical results. This paper reports our research work, combined with NIR spectroscopic analyses of the protein contents of wheat, that is the preprocessing of NIR spectral data recorded for 66 different wheat samples by a NIR grating spectrophotometer and a NIR Fourier transform spectrometer, respectively. The preprocessing algorithm is wavelet transform with the Gaussian first and second order derivatives. Compared with the result of preprocessing by normal first order difference algorithm, the wavelet transform algorithm by Gaussian derivatives was proved to be very effective and applicable, the spectra were smoothed perfectly, noises were eliminated obviously, and the spectral sections, which include all useful information for spectral analyses, were displayed clearly. So, it is very beneficial to the following spectral calibration, model establishment and transference.
		2004 Vol. 24 (12): 1563-1565 [Abstract] ( 1434 ) PDF (998 KB) ( 880 )

	1566	Adopting the Method of Principal Components Analysis Combined with Correlation Coefficient to Increase the Predicted Concentration’s Accuracy of Benzene and Its Homology Mixture
		WU Zhong-chen¹, XU Xiao-xuan¹, YANG Ren-jie¹, YU Gang², ZHANG Cun-zhou¹
		The concentrations of benzene and its homology mixture were measured by near infrared spectra, and the emphasis was put on the character of the principal component and its physical significance. It is pointed out that the anterior principal components are very similar to the correlation coefficient of the multi-component solution and the theoretical proof for the right condition is given. The high frequency noise of the system can be checked out by principal component combined with the correlation coefficient. Removing the noise can greatly increase the accuracy of the prediction model.
		2004 Vol. 24 (12): 1566-1570 [Abstract] ( 1665 ) PDF (1065 KB) ( 444 )

	1571	Study on the Synthesis, Characterization of Structure and Fluorescence Properties of the Solid Complex of Europium Ion with 1,10-Phenanthroline and 2-Thiopheneglyoxylic Acid
		YU Bin¹, SUN Bo^1*, ZHAO Ying², YAN Xiao-qi¹
		The complex of europium with 1, 10-phenanthroline and 2-thiopheneglyoxylic acid (HL) was synthesized. Its chemical formula was determined to be [EuL₂·phen·(H₂O)₃]NO₃ by elemental analysis, electrical conductivity, IR and ¹H NMR. It was found that the europium ion coordinated to the O atoms of 2-thiopheneglyoxylic acid and H₂O, and to the N atoms of 1,10-phenanthroline. Its fluorescence property was determined by the excitation and emission spectra at room temperature, the emission peaks at 592 and 618 nm were assigned to the ⁵D₀-⁷F₁ and ⁵D₀-⁷F₂, respectively. It was also observed that the title complex emits strong red fluorescence under ultraviolet light at room temperature. In the IR spectrum, the characteristic absorptionν_CO(1 719cm^-1)，ν_C—O(1 232 cm^-1)，δ_O—H(909 cm^-1) of 2-thiopheneglyoxylic acid disappeared in the complex, the ν_as and ν_s of —COO^- appeared at 1 642 and 1 408 cm^-1 in the complex respectively. In ¹H NMR, the signals of 2-thiopheneglyoxylic acid were shifted upfield, and those of 1,10-phenanthroline downfield. It is proved by the TG curve that the complex is stable from ambient temperature to 250 ℃.
		2004 Vol. 24 (12): 1571-1574 [Abstract] ( 1077 ) PDF (1022 KB) ( 393 )

	1575	Study of the Factors Effecting Surface-Enhanced Raman Scattering Reporter-Labeled Immunogold Colloids
		LI Shu-jin，QIU Li-qun，CAO Pei-geng，GU Ren-ao^*
		The applications of the high sensitivity of Surface-Enhanced Raman Spectroscopy (SERS) in labeled immunoassay have proved to be very useful. In the sandwich structure of “immobile antibody-antigen-labeled antibody”, the authors prepareｄ the labeled antibody by attachｉｎｇ gold nanoparticles，which ｗａs first labeled with moleculｅ that haｄ SERS signal, to the antibody. In this article, colloids were labeled with Raman reporter thiophenol through S—Au bond on gold and formed surface-enhanced Raman scattering (SERS) reporter-labeled gold colloids. Then, goat anti-rat antibody ｗａｓ adsorbed onto the reporter-labeled gold colloids and formed reporter-labeled immunogold colloids. This paper studied factors ａｆｆｅｃｔｉｎｇ FＴ-SEＲS ｒｅｐｏｒｔｅｒ-ｌａｂｅｌｅｄｉｍｍｕｎｏｇｏｌｄ colloids such as the sizes of gold particles, the amount of thiophenol in gold colloids and processing time, and whether goat anti-rat antibody would influence the SERS of reporter-labeled gold colloids.
		2004 Vol. 24 (12): 1575-1578 [Abstract] ( 1117 ) PDF (2566 KB) ( 442 )

	1579	*Raman Spectroscopy Study of 1,3-Dimethyluracil and It’s ab initio* (DFT) Calculation**
		LIU Yang-tao¹, Lü Xuan-zhong^1*, YU Zhou², HEI Xiao-ming¹, SONG Qin-hua¹
		The Raman spectrum of polycrystal 1,3-dimethyluracil(DMU) was obtained and investigated. Ab initio (DFT) calculation (B3PW91/6-31G method) of DMU was performed. And the vibration modes of DMU molecular were analyzed. The results suggest that DMU molecular, as a model compound of bio-base, has some advantages in Raman analysis, such as stronger intensity of marker bands and sharper, clearer bands of double band stretching than uracil’s. The ultima goal of this research is to get large quantity of Raman spectral information of DMU and it’s cyclobutane dimmers, use them as model compounds to research on the Raman characteristics of DNA’s or RNA’s photodamage. And this work is also an essential supplement to the 1,3-dimethyluracil’s Raman study.
		2004 Vol. 24 (12): 1579-1583 [Abstract] ( 378 ) PDF (981 KB) ( 314 )

	1584	Raman Spectroscopic Studies on Methanol under High Pressure
		QIAO Er-wei，ZHENG Hai-fei^*，SUN Qiang
		This paper studies Raman spectra of methanol at pressures from 169.2 MPa up to 713.8 MPa and at ambient temperature. The result shows that the spectral profile of stretching vibrational modes of CH and OH gradually changes and Raman shift moves to higher and lower frequency respectively with increasing pressure, which indicates that the energy of C—H bonding increases with pressure, and the influence of hydrogen bonding on O—H function group is greater than that of pressure. In addition, the relative peak area of O—H stretch band decreases with pressure, showing that the total intensity of O—H bonding is weaker compared with C—H bonding.
		2004 Vol. 24 (12): 1584-1587 [Abstract] ( 1009 ) PDF (1008 KB) ( 463 )

	1588	Theoretical Study on the Structure and Spectra of C₇₂O₃
		WANG Hong-xia, MI Wei-hong,GAO Yan,LIU Yi-jing, ZHAO Wen-juan,HAO Ce^*
		The optimized geometries and stability of eight different isomers of C₇₂O₃, the five-membered ring derivatives of C₇₀ fullerenes, were investigated by using AM1 method. According to the optimized geometries of eight different isomers, AM1 and ZINDO／CI method were employed to study the vibrational spectra and electronic spectra, respectively. The calculated results indicate that the —C₂O₃ groups are added preferably to the seats of C_Ⅰ—C_Ⅱ and C_Ⅲ—C_Ⅲ bond to form the isomers of A and B. The additive C—C bond is elongated to become primarily a single bond. The stability of isomer B is very similar to that of isomer A that has been prepared experimentally. The calculated vibrational spectra of isomer A, similar to those of isomer B, are consistent well with the results from the experiment. The electronic transitions of isomers of C₇₂O₃ were assigned and the red shift of electronic spectra was discussed. The spectra of other isomers were predicted theoretically.
		2004 Vol. 24 (12): 1588-1593 [Abstract] ( 1600 ) PDF (1004 KB) ( 320 )

	1594	Investigation of Electron Paramagnetic Resonance Spectrum in Ni²⁺:RbMgF₃
		XU Chang-tan
		The optical spectra, the zero-field splitting parameter D and the g-factor of transition-metal ions in crystal are related to the crystal structure. A method，which can be used to calculate accurately the optical spectra, the zero-field splitting parameter D and the g-factor, was founded by using the parametriｚation d orbital for Ni²⁺, the energy matrix elements of strong-field coupling scheme for d²(d⁸) electron configuration in trigonal crystal field and by adopting the method of complete diagonalization. In the calculation, all spin singlet states and spin triplet states have been considered, and then the result is exact. The present theory shows that g_∥>g_⊥, D<0 or g_∥<g_⊥, and D>0 are due to the different distortion of ligands along C₃ axis. The electron paramagnetic resonance spectrum in Ni²⁺:RbMgF₃ with C_3v and D_3d symmetry was calculated by using the theory. The relationship between the EPR spectrum in Ni²⁺:RbMgF₃ and the crystal structure were investigated. The agreement of the theory with the experiment shows that the present theory is reasonable.
		2004 Vol. 24 (12): 1594-1596 [Abstract] ( 1566 ) PDF (951 KB) ( 336 )

	1597	The Medium Effects of Fluorescence of Eosin-5-Isothiocynate as a Luminescent Marker
		WU Ya-lan¹，LI Long-di^1*，LIU Jia-ming²，ZHU Guo-hui²
		In this paper，the medium (pH，organic solvent and surfactant) effects on fluorescence of eosin-5-isothiocynate(eosin-ITC) have been studied in detail. The results show that the pH and polarity of system studied are two great important influence factors on fluorescence of eosin-ITC. The fluorescence intensity of eosin-ITC in weak acidic medium is higher obviously than that of in weak basic medium， but it is sensitive to change of pH， be careful to use. The reaction between surfactant and eosin-ITC shows a good electric selectivety，and the effect of CTMAB on fluorescence of eosin-ITC can be classified as two stages: monomer quenching (below cmc) and micelle sensibilization (above cmc). In the presence of micelle of CTMAB， the fluorescence intensity of eosin-ITC in weak basic medium is even higher than that of in weak acidic medium. In the presence of high organic solvent content，the fluorescence intensity of eosin-ITC is also increased obviously. These properties are available for use.
		2004 Vol. 24 (12): 1597-1600 [Abstract] ( 390 ) PDF (998 KB) ( 331 )

	1601	Study of Solid-Phase Time-Resolved Fluorescence Label Immunoassay
		PAN Li-hua¹, ZHOU Shi-hong¹，SUN Wen-wei²，XIE Wen-bing¹，ZHAO Chao¹
		This paper describes optimal conditions for HBsAbIgG labeling with a new fluorescence probe, 4,7-bis-chorosulfophenyl-1,10-phenanthroline-2,9-dicarboxylic acid(BCPDA)for the solid phase time-resolved fluorimmunoassay (TRFIA). The result of experiment under states clearly that BCPDA may react with protein under relative mild condition. The relative bioactivity of reacted protein was more than 80%. The labeling molar ratio of BCPDA for HBｓAbIgG was 45-70. The recovery was higher than 80%. Protein-BCPDA-Eu³⁺ complex is stable. It can emit very high fluorescence intensity with very long fluorescence life times. The fluorescence of Protein-BCPDA-Eu³⁺ complex has a very large stokes shift (270 nm). The emission band at 611.2 nm is very narrow. The research provides the base for developing non-isotopic immunoassay technique and clinical medical diagnosis.
		2004 Vol. 24 (12): 1601-1604 [Abstract] ( 1052 ) PDF (1289 KB) ( 385 )

	1605	Ion Fluorescence Probe Detecting the Formation of Triplex DNA
		ZHOU Wen-jun, SHEN He-bai^*, YANG Yong-tao, YUAN Lian-qun
		The fluorescence of Tb³⁺ is not quenched after the rare earth ion is combined with DNA. The fluorescence intensity is related not only to the kinds of bases of DNA but also to the kinds of DNA. The rare earth ion Tb³⁺ was used as the fluorescence probe to detect the formation of triplex DNA. The results show that the fluorescence intensity of Tb³⁺ combined with polydA is much stronger than that of Tb³⁺ combined with polydT，which testifies that the fluorescence intensity is related to the kinds of bases combined with Tb³⁺. The results also demonstrate that the rare earth ion can be used to detect those three forms of DNA though their fluorescence peak positions are similar when Tb³⁺ as a fluorescence probe is combined with single strand DNA (ssDNA), double helix DNA (dsDNA)，and triple helix DNA (tsDNA)，respectively. However，their intensities are quite different. The fluorescence intensity of Tb³⁺ combined with ssDNA-Tb³⁺ is the largest. And the fluorescence intensity of Tb³⁺ combined with tsDNA-Tb³⁺ takes the second place. The minimum peak intensity belongｓ to the contribution of Tb³⁺ coupled with dsDNA-Tb³⁺. The reason is that the capability of energy transference of ssDNA, dsDNA and tsDNA is different. The different degree of energy transference influences the intensities of Tb³⁺. The influences of pH and the metal ion on the formation of triplex DNA were also studied. The authors found that the neutral pH and high valence metal ion are beneficial to the formation of ts-DNA.
		2004 Vol. 24 (12): 1605-1608 [Abstract] ( 1036 ) PDF (1291 KB) ( 301 )

	1609	Fluorescence Spectra Characters of Nanostructured Gold Thin-Film
		ZHAO Jun-wu, WANG Yong-chang, ZHU Jian
		Gold colloid was prepared via electrochemical method. Nanostructured gold thin-films were deposited on glass by using self-assembled technique. UV-visible spectra and fluorescence emission spectra were measured at room temperature. The absorption spectrum features show two peaks and the longer wavelength one at 610 nm corresponds to linear aggregated gold nanochains. The fluorescence emission peaks at about 375 nm and 700 nm are due to the local field enhancement via coupling to the transverse and longitudinal surface plasmon resonance from gold nanochains. Both the intensity and number of the fluorescence emission peaks increase with increasing excited light and the layers number. It is indicated that the nanostructured gold thin-films formed a disordered particles system. Further more, multiple scattering takes place in these self-organized random micro-cavities.
		2004 Vol. 24 (12): 1609-1611 [Abstract] ( 1405 ) PDF (986 KB) ( 519 )

	1612	Fluorescence Reaction of Terbium(Ⅲ) Ion and Norepinephrine and Its Analytical Application
		TONG Shang-lun, XIANG Guang-hong, CHEN Ping-ping
		Experiments indicated that terbium(Ⅲ) ion could form complex with norepinephrine, then emitted its characteristic fluorescence. In the present paper, the fluorescence reaction of terbium(Ⅲ) ion with norepinephrine was studied in detail. Thus a new method for the determination of norepinephrine was propsed. The fluorescence intensity was measured in a 1 cm quartz cell with the excitation and emission wavelengths of 300 and 545 nm, respectively. The result showed that the fluorescence intensity of the system presented a linear relationship with the concentration of norepinephrine in the range of 0.01-50 μg·mL^-1, and the detection limit(S/N=3) was 1.0 ng·mL^-1. The method was used to determine pharmaceutical sample which contained norepinephrine, and the result was satisfactory.
		2004 Vol. 24 (12): 1612-1614 [Abstract] ( 1380 ) PDF (1257 KB) ( 300 )

	1615	The Fluorescence Characteristics of Norfloxacin and Its Application
		XU Li-ying, YU Wen-qing
		The fluorescence characteristics of norfloxacin in different pH media have been studied by spectrofluorimetry. It was found that in the neutral and alkalescent media the fluorescence signal of norfloxacin was weak, while in the acidity media the signal was very strong. The maximum fluorescence signal of norfloxacin could be obtained at pH 3.04, and the norfloxacin fluorescence emission wavelength has red-shifted 30 nm compared with the other condition. Based on this, a spectrofluorimetric method of the determination of norfoxacin in pharmaceuticals is proposed. The linear range was 0.016-0.96 μg·mL^-1, the detection limit was 0.016 μg·mL^-1, the RSD was 1.65%-2.86%, and the recovery was within the range of 99.7%-100.94%. At pH 3.04, norfloxacin in human urine can be well resolved by Synchronization-1st derivative fluorescence spectroscopic techniques with Δλ=90 nm, and the interference from urine blank can also be eliminated. The linear range was 0.096-3.19 μg·mL^-1 for determining norfloxacin in human urine sample. The detection limit was 0.096 μg·mL^-1, the recovery was within the range of 96.24%-104.4% and RSD was 0.71%-2.60%. Pharmacokinetic study of norfloxacin showed that norfloxacin reached its peak concentration in urine samples two hours after a healthy man took capsules. The method is simple, rapid and accurate with high sensitivity and good selectivity, and suitable for the determination of norfloxacin. The method was applied to analysis of norfloxacin in drugs and biological samples.
		2004 Vol. 24 (12): 1615-1617 [Abstract] ( 1618 ) PDF (1264 KB) ( 400 )

	1618	Study on the Interaction of Cystine and Polyphenol Oxidase from Nicotian Tobaccum
		XIAO Hou-rong，XU Xiao-long，XIE Yong-shu，ZHANG Yan-ge，PENG Dun-geng，LIU Qing-liang^*
		The interaction of cystine and polyphenol oxidase(PPO) from nicotian tobaccum has been studied. The results show that cystine has an inhibitory effect on the enzymatic activity, the mechanism of which might be that the thiolether in cystine coordinates with Cu²⁺ in the active site of PPO, and the inactivation constant value of PPO by cystine is 0.633 min^-1, while the substrates or the products inhibit their combination. Cystine can also be combined with the products of enzymatic reaction to form a colourless compound. Cystine can inhibit the enzymatic activity completely when the molar ratio of cystine to PPO approaches 16 000∶1. The effect of cystine on the fluorescence changes with the molar ratio of cystine to the PPO. However, when the molar ratio gets to 75∶1, cystine has no longer the effect on either the fluorescence spectra or the synchronous spectra. Microenvironment of trp residue in PPO is more hydrophobic than that of free trp in water.
		2004 Vol. 24 (12): 1618-1622 [Abstract] ( 100 ) PDF (1317 KB) ( 362 )

	1623	Fluorescence Spectroscopy Determination of Lomefloxacin by Charge Transfer Complex Formation with Chloranilic Acid
		DU Li-ming, ZHOU Jing, YUAN Jian-mei
		Charge-transfer complex was formed between LMX as the donor and Chloranilic Acid(CL) as the acceptor has been studied by fluorimetry. It was shown that the n-π complex can be formed at ambient temperature, which can emit，which strong fluorescence. Different variables and parameters affecting the reactions were studied and optimized. Based on this, a simple and reliable fluorescence spectroscopy method for the determination of Lomefloxacin (LMX) has been developed. Interference from some co-formulated drugs was also studied. No interference was observed due to additives commonly present in the pharmaceutical preparations. The proposed methods could be applied successfully to the investigated pure compounds and pharmaceutical dosage forms with good accuracy and precision. The linear range is 0.04-0.8 mg·L^-1, the detection limit is 0.04 mg·L^-1，the recoveries of LMX are 97.4%-99.3%, and RSD is 1.3%-2.6%. Finally, the charge-transfer reaction mechanism was discussed. The composition of the change-transfer complex was found to be 1∶1 by Bent-French and curved intersection methods. This ratio may be due to the presence of the fluorine atom acting as an electron drawing group in the molecule of lomefloxacin. The benzene ring has lower electron density, but nitrogen atom in 4′ of piperazingl has higher electron density and is less sterically hindered. So n-πcharge transfer complexes were formed.
		2004 Vol. 24 (12): 1623-1625 [Abstract] ( 1044 ) PDF (959 KB) ( 402 )

	1626	Photobleaching Properties of GFP Expressed in Human Lung Cancer Cells
		JIN Ying，XING Da^*
		The characteristic properties of GFP make this protein a good candidate for use as a molecular reporter to monitor patterns of protein localization, gene expression, and intracellular protein trafficking in living cells. In this study, the dicistronic expression vector (pEGFP-C1) was used to be transfected into human lung cancer cell line(ASTC-a-1)and a positive clone which stably expressed GFP in high level was obtained. The results showed that the green fluorescent protein expressed in tumor cells was also photobleached under intense irradiation (-488 nm) and the degree of photobleaching varied with the intensity of the excitation. In order to analyze the effect of low temperature on the fluorescent sample, the photobleaching of tumor cell slice stored at -20 ℃ was observed additionally.
		2004 Vol. 24 (12): 1626-1629 [Abstract] ( 980 ) PDF (1157 KB) ( 298 )

	1630	Absorption Spectra Study of Cation Surfactant-[AuI₄]^- Association Particle System and Its Analytical Application
		LUO Yang-he，JIANG Zhi-liang^*
		In 0.01 mol·L^-1 HCl medium, there is an absorption peak at 350 nm for [AuI₄]^-. The association particle system of CTMAB-[AuI₄]^- exhibits violet-red color. It has a new absorption peak at 520 nm. The CTMAB concentration c_CTMAB in the range of 0-7.0×10^-5mol·L^-1 is linear to the A_{520 nm} value. Its regression equation is A_{520 nm}=0.989×10⁴c_CTMAB+0.013 8，regression coefficient is 0.999 5，and the mole absorption coefficient is 1.059×10⁴ L·mol^-1·cm^-1. A new spectrophotometry has been proposed for the determination of cation surfactant. The resonance scattering spectra show that the CTMAB^＋ and [AuI₄]^- combine to form(AuI₄-CTMAB) association molecule with hydrophobicity by means of attraction forces. The association molecules automatically aggregate to form(AuI₄-CTMAB)_n association particles. So, the particles exhibit two resonance scattering peaks at 580 and 470 nm, and the system exhibits violet-red.
		2004 Vol. 24 (12): 1630-1633 [Abstract] ( 987 ) PDF (976 KB) ( 384 )

	1634	Spectral Properties of the Association Particle System of Quinine-[PtI₆]^2- and Its Analytical Application
		JIANG Zhi-liang¹，ZOU Jie-ming²，KANG Cai-yan¹，WANG Li-sheng²
		In 0.01 mol·L^-1 HCl medium, red color [PtI₆]^2- and quinine combine to form association molecule. The molecules aggregate automatically owing to strong hydrophobic and molecular forces. And PtI₆-quinine association particles with violet-red color formed. It exhibits three resonance scattering peaks at 310 nm, 400 nm and 610 nm, and a Rayleigh scattering peak at 470 nm. The absorption values all increase in the wavelength range of 350-740 nm, and the fluorescence peak at 450 nm was quenched. Under the conditions chosen, the quinine concentration in the range of 0-40×10^-6 mol·L^-1 is linear to the A_{620 nm} value. The mole absorption coefficient ε_{620 nm} is 1.31×10⁴ L·mol^-1·cm^-1. The results show that the association particles produce the resonance scattering effect, fluorescence quenching and the violet-red color.
		2004 Vol. 24 (12): 1634-1636 [Abstract] ( 1040 ) PDF (962 KB) ( 375 )

	1637	The Spectroscopic Behaviour and Extraction Separation of Cu(Ⅱ), La(Ⅲ), U(Ⅵ) and Ce(Ⅳ) in Two-Phase Aqueous Systems
		DENG Fan-zheng, WEI Ying, CHEN Ying, SHI Ying
		In polyethylene glycol 2000(PEG)-(NH₄)₂SO₄-extractant(sodium diethyldithiocarbamate, DDC) two-phase aqueous systems, spectroscopic behaviour of complexes of Cu(Ⅱ), La(Ⅲ), U(Ⅵ) and Ce(Ⅳ) with DDC as the extractant in PEG phase and general water phase was investigated. Comparing to DDC spectrophotometry, the new method has the advantage that the maximum wavelength of complex of Cu(Ⅱ) shifts to red wavelength. Extraction mechanism and existing form of complexes of metal ions in PEG phase were studied. Effects of different acidity, quantities of DDC and salt, different surfactant on the extraction efficiency of copper(Ⅱ), lanthanum(Ⅲ), uranium(Ⅵ) and cerium(Ⅳ) were discussed. Experimental results show that Cu(Ⅱ) was almost completely extracted in PEG phase at pH 5-8, U(Ⅵ) was partly extracted at pH 1-11, while La(Ⅲ) and Ce(Ⅳ) were not extracted at pH 3-6 buffer solution. So, extraction separation of Cu(Ⅱ)-La(Ⅲ) and Cu (Ⅱ)-Ce (Ⅳ) was carried out by control ling the solution acidity.
		2004 Vol. 24 (12): 1637-1639 [Abstract] ( 978 ) PDF (1254 KB) ( 361 )

	1640	Absorption Spectra Study of the Association Nanoparticle System of Berberine-[AuI₄]^- and Its Analytical Application
		WANG Li-ｓheng¹，ZOU Jie-ming¹，JIANG Zhi-liang^2*，LIAO Zu-he²，PAN Hong-cheng²
		In 0.008 mol·L^-1 HCl medium, [AuCl₄]^- and I^- combine to form [AuI₄]^-. [AuI₄]^- reacts with berberine(BB) to form (AuI₄-BB) association molecule. The molecules aggregate automatically owing to strong hydrophobic and molecular forces. And (AuI₄-BB)_n association nanoparticles with orange-yellow color were observed. It exhibits a resonance scattering peak at 520 nm. The absorption peak for the nanoparticle system and the [AuI₄]^- is at 350 nm. However, the absorbance values for the nanoparticle system increased in the visible light region. Under the conditions chosen, the BB concentration in the range of 0.8×10^-6 mol·L^-1-20×10^-6 mol·L^-1 is linear to the A_{450 nm} value. The results show that the formation of (AuI₄-BB)_n nanoparticles produces the resonance scattering effect and the orange-yellow color.
		2004 Vol. 24 (12): 1640-1642 [Abstract] ( 954 ) PDF (1276 KB) ( 403 )

	1643	Extraction Catalytic Spectrophotometric Determination of Trace Chromium by Synergetic Catalytic Effect
		SUN Deng-ming，YOU Yong-li
		In this paper, a new synergetic extraction catalytic spectrophotometric method for the determination of trace chromium was studied. The method is based on the iron(Ⅲ) and chromium(Ⅵ) synergetic catalyzed oxidation of o-aminophenol by hydrogen peroxide in weak acidic medium at pH 5.5. The reaction time, concentration of o-aminophenol in aqueous phase，and degree of reaction were controlled by extraction equilibrium. The absorbance of organic phase was measured at 424 nm. The linear range of the method is 0.001 0-0.90 mg·L^-1. The detection limit for chromium(Ⅵ) is 5.0×10^-6 g·L^-1. The relative standard deviation (n=11) for 0.20 μg·mL^-1 level of Cr(Ⅵ) is 2.0%. The method has been applied to the determination of chromium in tap water and waste water with satisfactory results.
		2004 Vol. 24 (12): 1643-1645 [Abstract] ( 1028 ) PDF (1255 KB) ( 358 )

	1646	A Catalytic Kinetic Spectrophotometric Method for Determination of Trace Zinc(Ⅱ) in Mongolian Medicine and Hair Sample
		SHA Ren, BAO Di, WU Di, Erdengsang
		A new catalytic kinetic spectrophotometric method for the determination of trace zinc(Ⅱ) was developed, which is based on the decolour reaction of H₂O₂ with calcon catalyzed by zinc(Ⅱ) in weak acid medium. The optimum condition and kinetic property of the reaction were also studied. The detection limit in this method is 0.68 μg·L^-1. The apparent activation energy Ea and the apparent rate constant R are 45.1 kJ·mol^-1 and 5.80×10^-3 s^-1 respectively. The range of determination is 0.80-40.00 μg·L^-1. The method has been applied to the determination of zinc(Ⅱ) in Mongolian medicine and hair sample with satisfactory results.
		2004 Vol. 24 (12): 1646-1648 [Abstract] ( 912 ) PDF (947 KB) ( 698 )

	1649	Study on Spectral Properties of Chinese Herbal Medicines Additives in Cosmetic
		HUANG Chong¹, OUYANG Yan-dong^1*, FANG Yi-wen², YU Yun-peng¹, LIN Shun-hui¹
		Chinese herbal medicines as additives in cosmetic can both keep the properties of cosmetic and have maintaining, health protection and remedial effect. Some of the Chinese herbal medicines can absorb ultraviolet and cure sunburn. This article mainly studies the spectral properties of several kinds of Chinese herbal medicine additives in cosmetic by ultraviolet and visible spectrophotometer, and analyses the ultraviolet absorption of the Chinese herbal medicine additives. It was shown that gynostemma pentaphyllum can absorb ultraviolet very well. It can be a promising natural additive in the health protection cosmetic. Codonopsis pilosula, floss chrysanthemum indicum, radix scutellariae and radix glycyrrhizae can absorb ultraviolet. They can also be the additives, while ligusticum wallichii can’t absorb ultraviolet, so it can not be used as the sunburn protection additive.
		2004 Vol. 24 (12): 1649-1651 [Abstract] ( 325 ) PDF (957 KB) ( 421 )

	1652	Determination of Trace Manganese in Mongolian Medicine by Methylthymol Blue-Mn(Ⅱ)-H₂O₂ Catalytic System
		WU Yun, LI Jing-feng, Garidi
		A new catalytic kinetic spectrophotometry method for the determination of trace manganese based on the oxidation reaction of H₂O₂ with methylthymol blue in Na₂B₄O₇-NaOH medium has been developed. The range of the determination range was 0.20-40.00 μg·L^-1. The apparent activation energy and apparent rate constant were 73.24 kJ·mol^-1 and 5.62×10^-4·s^-1, respectively, and the detection limit was 6.4×10^-10 g·mL^-1. The method has been used to determine trace manganese in Mongolian medicine with satisfactory result.
		2004 Vol. 24 (12): 1652-1654 [Abstract] ( 1327 ) PDF (949 KB) ( 423 )

	1655	Study on Optimizing the Analysis Condition for Active Compound in Eucommia Olive
		PENG Mi-jun^1,2，ZHOU Chun-shan^2*，LIU Jian-lan¹，ZHANG Min¹，LEI Qi-fu²
		The absorption spectroscopic determination of aucubin by condensation with p-dimethylaminobenzaldehyde was optimized in this paper. A high sensitive method was established and the linearity range of the method was from 4.5 to 45 μg·mL^-1. The influences of the factors, such as the dosage of coloring agent, reaction time, heating temperature and the dose of acid etc., on the system were studied. And the result indicated that all of the factors had obvious effects on the system. The method has been applied to determining the content of aucubin in the extract of Eucommia olive with satisfactory results.
		2004 Vol. 24 (12): 1655-1658 [Abstract] ( 1368 ) PDF (1262 KB) ( 356 )

	1659	Resonance Light Scattering of Rhodamine B
		WEI Yong-ju¹, KANG Zhi-min², LIU Cui-ge¹, LAN Rui-jia¹, WANG Hui-ying¹
		The characteristic and mechanism of resonance light scattering (RLS) of Rhodamine B (RhB) were studied. In acidic solutions with pH from -0.38 to 4.10, the intensity of RLS increases with an increase in pH and reaches a maximum at nearly neutral pH. The change in RLS intensity with the wavelength was not accordant with Rayleigh scattering law. The fluorescence excitation and emission spectra of RhB overlap partly, and the RLS peak lies between the fluorescence excitation and emission peaks. In the three-dimensional fluorescence contour spectra of RhB, Rayleigh scattering line intersects fluorescence contour. In light polarization experiment, the polarization of RLS was measured to be P≈0.1. All the above experimental facts reveal that the RLS of RhB is mainly resonance fluorescence. The mechanism of RLS enhancement by the increase in pH is that the formation of fluorescence species occurs in acid-base equilibrium. The RLS peak of RhB appears within the envelop of absorption, and light scattering is affected by light absorption, so, the relationship between RLS intensity and RhB concentration is not strictly linear.
		2004 Vol. 24 (12): 1659-1662 [Abstract] ( 1084 ) PDF (1013 KB) ( 437 )

	1663	Study on the Determination of Metal Elements in Wild Jujube Seed Decoction by ICP-AES
		ZHANG Sheng-bang，GUO Yu-sheng
		The determination of metal elements in Chinese medicine wild jujube seed decoction was studied by ICP-AES after HNO₃-H₂O₂ digestion. The average recoveries of the method for Ca，Cr，Al，Fe，K，Mg，Mn and Zn in wild jujube seed decoction were found to be 95.5%-106.8%，while RSD (n=5) was found to be 1.7％-3.9% for these metal elements. The method was applied to the analysis of some practical samples and the results obtained were satisfactory.
		2004 Vol. 24 (12): 1663-1665 [Abstract] ( 1044 ) PDF (1240 KB) ( 354 )

	1666	Studies on the Determination of Silicon and Phosphorus in Ferromanganese by ICP-AES
		MO Qing-jun¹, SONG Lan-hui¹, WANG Xiu-yan²
		An ICP-AES method for the determination of silicon and phosphorus in ferromanganese was studied. Digesting samples by microwave and all kinds of parameters of the analytical method were optimized, which included selecting the acid and controlling the temperature and pressure of dissolving the sample, confirming analytical spectrum, considering the effect of sample matrix, analytical pH and disturbing elements on the determination results. By optimizing and choosing all kinds of condition parameters, the simultaneous determination of silicon and phosphorus was realized and satisfactory results were obtained. The linear correlation coefficients of Si and P were 0.999 8 and 0.999 6, respectively. The detection limit for silicon was 0.006 0% with recovery of 97.0%-101%. The detection limit for phosphorus was 0.030%. This method is accurate and quick with less reagent dosage and broad linear range. The way of this determination is fit for the determination of silicon and phosphorus with low, middle and high carbon contents.
		2004 Vol. 24 (12): 1666-1668 [Abstract] ( 1301 ) PDF (1239 KB) ( 341 )

	1669	Spectral Determination of the Contents of Mineral Elements in Polygonum Cuspidatum
		ZHANG Min，YU Hua-zhong，CAO Yong，BU Xiao-ying，LU Cheng-ying，DU Ya-tian，HUANG Rong-fang
		The present paper reports the determination of mineral elements by FAAS, including K, Ca, Na, Mg, Fe, Zn, Mn and Cu. The best condition for the determination was investigated. The best ionization inhibitor and acidity media were confirmed. The experiment used CsCl to prevent ionization interference, and the concentration of HCl was controlled below 2%. At the same time SrCl prevented interference of P to Ca. So the value of absorbance was stable. The results were obtained by calibration curve method. The analysis method is simple, rapid, accurate and fiting to the determination of mineral elements in plants. The recoveries of the method are 90.5%-108.2%. The relative standard deviations are 0.3%-0.7%. The result show that large amounts of mineral elements are embodied in polygonum cuspidatum. The contents of K and Ca are in conformation with the medical effects of polygonum cuspidatum, and each element is related closely to its growing.
		2004 Vol. 24 (12): 1669-1671 [Abstract] ( 350 ) PDF (1242 KB) ( 353 )

	1672	Determination of Trace Zinc，Manganese，Cadmium and Lead in Aloe by Microwave-Digestion Atomic Absorption Spectrometry
		YANG Yi¹, HOU Xiang-yan¹, WANG Shu-jun¹, JIA Qian-ling¹, LI Zhi¹, GUO Zhen-ku²
		A microwave digestion procedure was developed for the determination of trace Zn，Mn，Cd and Pb in aloe-leaf cuticle and aloe-leaf gelatin, using the obturated vessel microwave digestion system with a pressure controlling part, and the amounts of these trace metallic elements were determined by atomic absorption spectrometry after microwave digestion. The effects of the composition of digestion solution, the ratio of the sample to digestion solution, and the digestion time were studied. It is satisfactoty to apply the microwave digestion procedure to the determination of Zn, Mn, Cd and Pb under the optimized condition with the recovery of 95.0% to 110.0% and RSD of 0.3% to 6.2%. The results show that this method is rapid and simple with low environmental contamination and complete digestion of the sample.
		2004 Vol. 24 (12): 1672-1675 [Abstract] ( 1045 ) PDF (947 KB) ( 502 )

	1676	Recent Advance of Resonance Light Scattering Technique for the Determination of Nucleic Acids
		FENG Shuo¹，LI Zheng-ping^{1, 2*}，ZHANG Shu-hong¹，FANG Zheng¹
		Nucleic acid analysis is one of the most important techniques for the study in biotic field. The spectrophotometry using inherent ultraviolet absorption spectrum of nucleic acids and the spectrofluorimetry based on the interaction of nucleic acids and fluorescence probes were usually used for nucleic acid analysis. However, the spectrophotometry was severely limited by its low sensitivity, and the spectrofluorimetry suffered from the disadvantages of high cost and toxic reagents. Recently, resonance light scattering has emerged as a new nucleic acid analysis technique. The resonance light scattering analysis is becoming increasingly important because high sensitivity can be obtained with a common spectrofluorimeter by using inexpensive and safe reagents. In this paper, the principle of resonance light scattering was briefly stated and the recent advances of the nucleic acid analysis by resonance light scattering were reviewed with 57 references. The resonance light scattering probes for nucleic acid analysis were divided into four groups: organic dyes; cation surfactants; metal ions and their complexes; and drugs. The light scattering analysis for nucleic acids based on the formation of large particles was also stated.
		2004 Vol. 24 (12): 1676-1680 [Abstract] ( 1045 ) PDF (977 KB) ( 420 )

	1681	The Application of Variable Theoretical α Influence Coefficent to the Matrix Correction in Cr-Fe-Ni Stainless Steel
		YING Xiao-hu，WANG Qian，CAO Guo-zhou，YU Ming-fang
		X-ray fluorescence analysis software Spectra Plus was used to calculate theoretical α influence coefficents of other elements to Cr in seven stainless steel standard samples, theoretical α influence coefficients of elements, by which Cr signal was enhanced, varied largely with the change of elements content. Variable theoretical α influence coefficients, which varied with elements content, were used to correct the matrix effects in stainless steel, the secondary excitation of Cr by other elements were corrected, and Cr (0.3%-20.8%) in stainless steel and low alloy steel could be analysed in accordance with one calibration curve. The matrix effects in samples can be corrected by variable theoretical α influence coefficients, so the measurable content range of calibration curve was enlarged. The contents of fifteen elements Al, Si, P, S, Ti, Cr, Mn, Co, Ni, Cu, As, Mo, Sn, W and Pb in stainless steel were measured by X-ray fluorescence spectrometer, variable theoretical α influence coefficients were used to correct the matrix effects, and the analysis results are comparable to those obtained by wet chemical method.
		2004 Vol. 24 (12): 1681-1683 [Abstract] ( 1874 ) PDF (959 KB) ( 364 )

	1684	《光谱学与光谱分析》2004年(第24卷)总目次(第1～12期)
		光谱学与光谱分析

		2004 Vol. 24 (12): 1684-0 [Abstract] ( 711 ) PDF (1341 KB) ( 326 )

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