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2004 Vol. 24, No. 09 Published: 2004-09-26

光谱学与光谱分析

	1025	Discrimination of Normal and Malignant Gastric Tissues with FTIR Spectroscopy and Principal Component Analysis
		Peter R Griffiths¹, YANG Hu-sheng¹，LI Qing-bo², LING Xiao-feng², WANG Jian-sheng³, YANG Li-min², XU Yi-zhuang², WENG Shi-fu², WU Jin-guang^2*
		In this paper, the identification of normal and malignant gastric tissues, including 11 cases of cancerous tissues and 10 cases of normal tissues, was investigated using mid-IR spectroscopy and principal component analysis (PCA). The results indicated that the difference between cancerous and normal tissues was found in the first principal component. The IR detection and PCA results are in agreement with the biopsy results. The combination of these two methods might provide a new opportunity for clinical application.
		2004 Vol. 24 (09): 1025-1027 [Abstract] ( 1048 ) PDF (888 KB) ( 484 )

	1028	Synthesis and Luminescence Properties of Reactive Ternary Europium Complexes
		GUO Dong-cai^{1, 2}，SHU Wan-gen¹，ZHANG Wei²，LIU You-nian¹，ZHOU Yue²
		In this paper, five new reactive ternary europium complexes were synthesized with the first ligand of 1, 10-phenanthroline and the reactive second ligands of maleic anhydride, acrylonitrile, undecenoic acid, oleic acid and linoleic acid, and also characterized by means of elemental analysis, EDTA titrimetric method, FTIR spectra and UV spectra. The fluorescence spectra show that the five new ternary complexes have much higher luminescence intensity than their corresponding binary complexes, and the synergy ability sequence of the five reactive ligands is as follows: linoleic acid＞oleic acid＞acrylonitrile＞maleic anhydride＞undecenoic acid. At the same time, the reactive ternary europium complexes coordinated with the reactive ligands, which can be copolymerized with other monomers, will provide a new way for the synthesis of bonding-type rare earth polymer functional materials with excellent luminescence properties.
		2004 Vol. 24 (09): 1028-1031 [Abstract] ( 501 ) PDF (878 KB) ( 595 )

	1032	Synthesis of Nanocrystalline ZnO and Its Luminescence Spectrum
		CHEN You-cun，ZHANG Yuan-guang
		ZnO nanocrystal was prepared with Zn(CH₃COO)₂·2H₂O and CO(NH₂)₂ as precursor by a solvothermal process. The products were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM)，and photoluminescence spectrum(PL). The results show that the ZnO nanocrystal has good characteristics, and the average particle size of the ZnO nanocrystal is about 17.2 nm. There is a broad PL peak for ZnO nanocrystal between 500-700 nm.
		2004 Vol. 24 (09): 1032-1034 [Abstract] ( 974 ) PDF (1334 KB) ( 435 )

	1035	Determination of Deoxyribonuceic Acids by Resonance Light Scattering Technique with Benzidine in the Presence of the Sensitizing Sodium Dodecyl Sulfate
		RAO Zhen-hong, XIONG Yan-mei, REN Li-ping^*, JIANG Shu-ren, ZHANG Chun-rong
		The resonance light scattering(RLS) spectra of benzidine with deoxyribonucleic acid(ctDNA) in the presence of Sodium Dodecyl Sulfate had been studied. RLS intensity of SDS- benzidine system was enhanced by trace ctDNA and was proportional to the concentration of ctDNA. Under optima conditions, the linear ranges of the calibration were 0.3-4 mg·L^-1, the linear regression equation was I=37.17c(ctDNA，mg·L^-1 ) +208.9, r=0.999 2. The limit of detection were 0.17 mg·L^-1(3δ), RSD%=3.5%. The method had been applied to the determination of DNA in synthetic samples and gene tobacco sample, and the results were satisfactory.
		2004 Vol. 24 (09): 1035-1038 [Abstract] ( 1501 ) PDF (914 KB) ( 389 )

	1039	Optical Properties of Human Normal Bladder Tissue at Five Different Wavelengths of Laser and Their Linearly Polarized Laser Irradiation in Vitro
		WEI Hua-jiang¹，XING Da^1*，WU Guo-yong²，JIN Ying¹，GU Huai-min¹
		A double-integrating-spheres system, the basic principle of measuring technology of radiation, and an optical model of biological tissues were used for the study. Optical properties of human normal bladder tissue at 476.5, 488, 496.5, 514.5 and 532 nm of laser and their linearly polarized laser irradiation were studied. The results of measurement showed that total attenuation coefficient and scattering coefficient of human normal bladder tissue at these wavelengths of laser and their linearly polarized laser irradiation increased with decreasing wavelengths. And these was an obvious distinction between the results at these wavelengths of laser and their linearly polarized laser irradiation. Absorption coefficient of human normal bladder tissue at these wavelengths of laser and their linearly polarized laser irradiation was tardily increased with decreasing wavelengths. But there were a number of gurgitations. And these were independent of the wavelengths of laser or their linearly polarized laser irradiation. Mean cosine of scattering of human normal bladder tissue at these wavelengths of laser and their linearly polarized laser irradiation also increased with decreasing wavelengths. And these was an obvious distinction with these wavelengths of laser and their linearly polarized laser irradiation. But penetration depth of human normal bladder tissue at these wavelengths of laser and their linearly polarized laser irradiation also increased with increasing wavelengths. But there were a number of gurgitations. Refractive index of human normal bladder tissue at these wavelengths of laser ranged from 1.37 to 1.44. Absorption coefficient, scattering coefficient, total attenuation coefficient, and effective attenuation coefficients of human normal bladder tissue in Kubelka-Munk two-flux model at the same wavelength of laser and the linearly polarized laser irradiation do not exhibit prominent distinction (P＞0.05). Some absorption coefficient, scattering coefficient, total attenuation coefficient, and effective attenuation coefficient of human normal bladder tissue in Kubelka-Munk two-flux model at different wavelengths of laser and their linearly polarized laser irradiation exhibit obvious distinction.
		2004 Vol. 24 (09): 1039-1041 [Abstract] ( 1605 ) PDF (843 KB) ( 410 )

	1042	Study of Net Analyte Signal with Near-Infrared Spectra for Quantitative Analysis
		LIU Rong，Lü Li-na, CHEN Wen-liang, XU Ke-xin^*
		Near-infrared spectroscopy is a rapid, high-efficiency, non-destructive and low-cost analytical technique, which has found widespread use for quantitative and qualitative analysis. Because of the complex nature of NIR spectra, multivariate calibration model plays a key role in the spectroscopic analysis. Further understandings of the model can be helpful for optimizing the model’s performance. This paper introduces a convenient definition of net analyte signal, which is one of the figures of merit charactering multivariate calibration model. The absorbance data of the glucose aqueous solution are used for the calculation of net signal and explanation of the qualitative relationships between net analyte signal of glucose and absorptivity coefficients of other components. Qualitative changes of net signal with the complexity of samples are also given. Finally a simple expression is proposed for estimating the prediction error of concentration, which is instructive for further study of the robustness and accuracy of the multivariate calibration model.
		2004 Vol. 24 (09): 1042-1046 [Abstract] ( 1003 ) PDF (885 KB) ( 407 )

	1047	The PLS Analysis with Short Wave Near-Infrared of Whole Wheat for Protein
		ZHENG Yong-mei¹, ZHANG Jun², CHEN Xing-dan², SHEN Xuan-guo¹, ZHANG Tie-qiang¹
		Short wave near-infrared spectrum of whole wheat was obtained by diffusion reflection. PLS method was used to analyze protein content of whole wheat. Different wavelength ranges were chosen for regression and information abstraction. The 3D-curves were shown for different factors，prediction residual sum of squares (PRESS)，and RMSECV. The best wavelength ranges and factors were determined. Analysis results for protein content of whole wheat were shown in three wavelength regions, and the predicted results were compared and discussed. The method of selecting advantageous wavelength ranges is feasible to obtain high prediction precision.
		2004 Vol. 24 (09): 1047-1049 [Abstract] ( 1051 ) PDF (875 KB) ( 494 )

	1050	Studies on the Changes in Rice Straw Composition in Relay Treatment of Chemical-Microbial Process by FTIR Spectroscopy
		XU Yong, SHEN Qi-rong^*, ZHONG Zeng-tao, CHEN Xiang-huai
		Direct burning of crop straw in the field has given or is giving rise to a serious pollution of atmosphere. The difficult decomposing of the crop straw by soil microorganisms is one of the reasons the crop straw is not popularly used in agriculture. Fourier transform infrared spectroscopy (FTIR) was used to study the changes in straw composition during the relay treatment of chemical-microbial process. The results showed that the method of FTIR spectra could indicate the changes in straw composition during the treatment processes. After the relay treatment of chemical-microbial process, the contents of cellulose, semi-cellulose, and silicon，and C／N ratio were decreased significantly，while the water soluble substances were increased, which was in accordance with the results of chemical analysis. The method to treat crop straw proposed in this paper could provide a practicable way in agricultural utilization of crop straw.
		2004 Vol. 24 (09): 1050-1054 [Abstract] ( 1502 ) PDF (956 KB) ( 412 )

	1055	Direct Identification of Ophiogon Japonicus (Thunb.)Ker-Gawl. from Its Confusable Varieties by Second Derivative FTIR Spectroscopy Combined with Statistics
		CHENG Cun-gui^1，2，SUN Cui-rong², PAN Yuan-jiang^2*
		In order to establish the theory and method for the identification of Ophiogon japonicus (Thunb.)Ker-Gawl. of traditional Chinese herbal medicines and its confusable varieties, second derivative FTIR spectroscopy was used combined with statistics. Samples were collected directly by Fourier Transform Infrared (FTIR) spectra with OMNI-Sampler. Then through converting FTIR spectra of the samples into second derivative spectra by derivative spectra software, Ophiogon japonicus (Thunb.)Ker-Gawl. could be identified from the confusable varieties with statistics. The result shows that the second derivative FTIR of Ophiogon japonicus (Thunb.)Ker-Gawl. and its confusable varieties are different, which differ greatly in 2 000-650 cm^-1 range in second derivative FTIR spectroscopy. The Ophiogon japonicus (Thunb.)Ker-Gawl. and its confusable varieties can be identified by identifying the inner layer parts of the cuticles of samples by second derivative FTIR spectroscopy with statistics directly, rapidly and accurately.
		2004 Vol. 24 (09): 1055-1059 [Abstract] ( 1650 ) PDF (902 KB) ( 468 )

	1060	Fractionation and Spectroscopic Property of Dissolved Organic Matters in Soils
		ZHOU Jiang-min^{1, 2}, DAI Jing-yu^1*, PAN Gen-xing¹
		Based on a modified Leenheer DOM fractionation scheme, fractionation of DOM from paddy soils was conducted by using XAD-8 resin into hydrophobic bases (HOB), hydrophobic acids (HOA), acid-insoluble matter (AIM), hydrophobic neutrals (HON) and hydrophillic matter (HIM), and their structural characteristics were studied by means of elemental composition, FTIR and ¹H-NMR spectroscopy. The fractionation scheme used here provided a preferable separation of the fractions in terms of hydrophobicity and a high recovery. Of the DOC extracted from the soils, the HOB was the least fraction, accounting for 0.73%-3.83%, and the HIM fraction was the largest, accounting for 36%-42%. The HON fraction represented 7%-15%. The relative content of the HOA plus AIM was about 50%. Separated by this technique, the large-chain alkylate and the major portion of the N components mainly characterized HON, while the HOA fraction contained a large amount of carboxyl groups but less amount of aromatic groups with a higher quantity of carbohydrates compared to that of FA. AIM fraction was dominated by high branched(n value) polyphenols and humus bound carbohydrates. HIM was characterized by considerable amount of carboxyl and carbohydrates.
		2004 Vol. 24 (09): 1060-1065 [Abstract] ( 251 ) PDF (1002 KB) ( 564 )

	1066	Study on Effect of Thermal Process on the Morphology and Mechanical Properties of RIM PUU by In-situ FTIR
		LI Zai-feng¹，ZHANG Tian-lin²，XU Chun-ming³
		The samples of PUU polymers were characterized by In-situ FTIR in a temperature-controlled cell. The spectra of FTIR showed that the absorbance of ordered hydrogen-bonded urea carbonyl group(1 643 cm^-1) became stronger with increasing thermal process time (at 100 ℃), then changed little after a certain time. The rate of change for absorbance of ordered hydrogen-bonded urea link, attributed to microphase separation kinetics, was enhanced with increasing thermal process temperature. In carbonyl region of FTIR spectra, absorbance for various carbonyls available in PUU polymers, associated with micro-hard domain, was observed before thermal process. However, after the process, only the absorbance of free urethane, hydrogen-bonded urethane and ordered urea became obvious. At 100 ℃, the longer the process time (beyond 8 h), the worse the mechanical properties obtained. The PUU polymers processed at 100 ℃ with the identical process time exhibited the best mechanical properties.
		2004 Vol. 24 (09): 1066-1068 [Abstract] ( 989 ) PDF (883 KB) ( 345 )

	1069	*Study on Spectroscopy of α, α’-Dioxoketene Cyclic s, s-Acetals*
		AN Yue¹, ZHU Zai-ming¹, HU Jie-han², GE Jun-jie¹
		The rule of infrared spectroscopic characteristics of the five α, α’-dioxoketene cyclic s, s-acetals was studied, and the influence of the molecular structure on the IR was indicated. All ¹H and ¹³C NMR chemical shifts of the five compounds were assigned, and the effects of structures on the chemical shifts of ¹H and ¹³C NMR were discussed. The rule of change is the same as that of IR. The study offers a method of elicitation for studies on the structure and the spectroscopy of this kind of compounds.
		2004 Vol. 24 (09): 1069-1071 [Abstract] ( 1033 ) PDF (832 KB) ( 369 )

	1072	Raman Spectroscopic Study on the Iron Oxide Film Prepared by Iron Oxidation Method
		HU Tao, LU Xin, YAN Yan, FU Yun-yi, ZHANG Han, ZHANG Shu-lin
		Micro-Raman spectroscopy was used to investigate the chemical composition, microstructure and crystalline phase of an iron oxide sample with three-layer macro-structure prepared by iron oxidation. Two laser lines of 514 and 633 nm with a power of 0.5 mW on the sample were employed to excite the Raman spectra. Comparing the sample spectra to that of bulk α-Fe₂O₃, the sample Raman peaks were assigned. And it was found for the top-layer that the Raman frequencies were down shifted and the peak widths broadened. Therefore we verified that the top-layer of the verified sample is a nano-structure α-Fe₂O₃, the main component of the middle-layer is Fe₃O₄ and the bottom-layer is most like bulk α-Fe₂O₃.
		2004 Vol. 24 (09): 1072-1074 [Abstract] ( 1223 ) PDF (858 KB) ( 469 )

	1075	Temperature Dependence Study of Calf Thymus DNA by Raman Spectra
		DONG Rui-xin^1，2, YAN Xun-ling¹, WU Jing², ZHANG An-ying²
		In this paper, the authors obtained Raman spectra of DNA in fiber and aqueous solution at different temperatures. These spectra revealed that the vibration of bases and phosphate group were influenced by varying temperature. Adenine was the most sensitive to varying temperature in all of the vibrational modes. The wave numbers of most of the vibrational modes decreased as the temperature increased except for the band at 1 101 cm^-1，and the shift of wave numbers mainly concentrated upon the beginning point of denaturation at 70 ℃. The temperature dependence of Raman intensity was discussed, and two peaks were obtained at 38 and 82 ℃，respectivelｙ. The results obtained by Raman spectra were in agreement with experimental data by DSC at 82 ℃. The peak at 38 ℃ was related to the biological activity region of DNA function.
		2004 Vol. 24 (09): 1075-1078 [Abstract] ( 1331 ) PDF (882 KB) ( 381 )

	1079	Study on Fluorescence Spectra of the Four Heterocyclic Compounds in Solution
		QIAN Yi-ming, WANG Ying, WU Xue-mei, ZHAO Ying,LIAO Xian-wei^*
		The fluorescence spectra of the four compounds have been studied. Geometric configurations of the four compounds have been optimized by semi-empirical mothod RHF/AM1 of quantum chemistry. There is no imaginary frequency in vibrational analysis. Their fluorescence spectra have also been calculated by RHF/CIS. The results of calculation in solution are better agreement with experimental values than in gas phase.
		2004 Vol. 24 (09): 1079-1081 [Abstract] ( 1092 ) PDF (832 KB) ( 531 )

	1082	Study on the Reaction of Lys-ZCN-CTMAB Complex
		BAI Jin-wei¹, CHI Yan-hua^1*, ZHUANG Jia¹, LI Ke-an²
		The interaction of lysozyme(Lys)，O-｛2-〔α-(2-Hydroxy-5-Sulphophenlylazo)-benzylidene〕hydrazino｝benzoic acid(ZCN) and cetyltrimethy ammonicumbromide(CTMAB) was investigated by UV spectrophotometric method. The effect of temperatｕre，time，and ion intensitｙ in the bｕffer solｕtion (pH 4.46) on reaction system was determined． Linear range of the reaction was 0～10 μg·mL^-1． The molar absorptivity was ε=4.616 4×10⁵ L·cm^-1·mol^-1． The reaction mechanism and interference of inorganic substance，biological substance and surface active agent to the reaction was investiｇated. Study system was established.
		2004 Vol. 24 (09): 1082-1085 [Abstract] ( 1068 ) PDF (946 KB) ( 395 )

	1086	Study on Fluorescence Characteristics of Pefloxacin-La(Ⅲ) Complex and Its Application
		LI Gui-zhi¹，LIU Yong-ming¹，LI Gai-zhi²
		The complex of pefloxacin-La³⁺ was formed in the pH 5.6 HAc-NaAc buffer. Its fluorimetric intensity was 1.5 times that of the pefloxacin，and the excitation and emission peaks of the complex were at 276 and 440 nm, respectively. The new fluorescence method was developed for determining pefloxacin in serum based on the characteristics. The content of pefloxacin in serum was 4.79 mg·L^-1，the RSD and recovery were 6.3% and 95% respectively. The determination range was 0.04-2.0 mg·L^-1 with the detection limit of 2.8 μg·L^-1. The proposed method and UV-Vis photometric method were both applied to determining the pefloxacin in the same capsules with satisfactory results.
		2004 Vol. 24 (09): 1086-1088 [Abstract] ( 170 ) PDF (859 KB) ( 746 )

	1089	Study on Spectral Properties of the Associated Particle of Berberine-PHLO and Its Analytical Application
		KANG Cai-yan¹, JIANG Zhi-liang^1*, MO Wei-ming²
		In neutral medium, berberine forms a red-violet association microparticle with PHLO which has an maxmimum absorption at 560 nm, Beer’s law is obeyed for berberine in the concentration range of 6.65×10^-7-7.71×10^-5mol·L^-1. Spectral properties of the berberine-PHLO system were studied. In neutral medium, there are a maximum absorption peak at 520 nm and a fluorescence peak at 560 nm for PHLO. Berberine and PHLO combine into a hydrophobic berberine-PHLO association molecule by static gravitation. With stronger Van der Waals and hydrophobic forces among berberine-PHLO molecules, it forms association particle in red-violet which exhibits three resonance scattering peaks at 385, 470 and 586 nm，respectively. The fluorescence quenching at 560 nm is because the PHLO molecule in the body of the particle may not be excited by incident photons, so it does not emit fluorescence.
		2004 Vol. 24 (09): 1089-1092 [Abstract] ( 1111 ) PDF (930 KB) ( 396 )

	1093	Study on the Synthesis of a New Reagent 3-(4′-Fluorophenyl)-5-(2′- Arsenoxylphenylazo)-Rhodanine and the Fluoresence Determination of Bismuth(Ⅲ)
		YU Jing-hua^{1, 2}，OU Qing-yu²，LU Yan¹，WANG Lai-guo¹，LI Tao¹
		A new fluorescence reagent, 3-(4′-fluorophenyl)-5-(2′-arsenoxylphenylazo)-rhodanine，was synthesized. The structure of the reagent was clarified by elemental analysis and IR. At pH 5.4，the reagent can react with trace bismuth (Ⅲ) to form a chelate which reduces the fluorescence intensity greatly. And when λ_ex／λ_em=305／407 nm, the fluorescence is intensive. There is a linear relationship between the decrease of fluorescence intensity and the concentration of bismuth (Ⅲ) in the range of 0-0.025 μg·mL^-1. The detection limit is 1.2×10^-10 g·mL^-1. A new method of fluorescence spectrophotometric determination of bismuth (Ⅲ) was developed.
		2004 Vol. 24 (09): 1093-1095 [Abstract] ( 1598 ) PDF (909 KB) ( 401 )

	1096	Study on the Ultraviolet-Visible Spectra of Au／Al₂O₃ Catalysts
		CHEN Wei, XIAO Yi-hong, ZHAN Ying-uing, CAI Guo-hui, WEI Ke-mei, ZHENG Qi^*
		A variety of synthesis parameters for the preparation of gold nanoparticles by NaBH₄ solution reduction in the W／O microemulsion media consisting of Cetyl Trimethyl Ammonium Bromide(CTAB)／n-hexanol／water system was investigated. The results showed that the molar ratio of water to surfactant (r_w) had nothing to do with the gold particle size, but the concentration of the aqueous gold salt solution had a significant effect on the size of gold particle. Through optimizing the preparation parameters, Au／Al₂O₃ catalysts were prepared with two different methods, then the catalysts were characterized by ultraviolet-visible spectra, XRD and TEM, and the effect of two different preparation methods on active component gold particle size in the catalysts was studied.
		2004 Vol. 24 (09): 1096-1098 [Abstract] ( 1016 ) PDF (1003 KB) ( 396 )

	1099	Study on the Inclusion Complexation Interaction of β-Cyclodextrin and β-Carotene by UV-Vis Spectra
		FENG Guang-zhu，LU Kui，LI He-ping
		β-cyclodextrin(β-CD), a kind of cyclic oligosaccharides, was found to possess a strong inclusion ability with β-carotene. The inclusion compounds of β-CD with β-carotene were prepared by the coprecipitation method, and studied by UV-Vis spectra of different mole ratio β-CD/β-carotene in the H₂O+ethanol solution (H₂O for β-CD, and ethanol for β-carotene). Equilibrium constant of inclusion compound was determined by UV-Vis spectra. The results indicate that 3.25 moles of β-CD can include one mole β-carotene to form inclusion compound by Van der Waals force and hydrophobic interaction etc. The optimum synthesis conditions of inclusion compound of β-CD with β-carotene is that the mole ratio of β-CD/β-carotene is 3.25∶1(mol/mol), the concentration ratio of β-CD H₂O solution/ β-carotene solution is 12∶1(mol·L^-1/mol·L^-1), and the time and temperature of inclusion reaction are 2 h and 30 ℃, respectively. Equilibrium constant of inclusion compound(K_a) is 9.46×10¹¹ L·mol^-1. The selective binding ability of β-CD with β-carotene has been discussed from the viewpoint of size/shape-fitting and geometry fitting between the host cavity and the guest molecule. The resistance to oxidation and photooxidation, and the solubility in H₂O of β-carotene were increased by inclusion with β-CD.
		2004 Vol. 24 (09): 1099-1102 [Abstract] ( 245 ) PDF (927 KB) ( 842 )

	1103	Spectrophotomatric Determination of Antioxidative Activity of Extractives of Chinese Traditional Medicine by Supercritical Fluid CO₂ Extraction Technology
		ZHANG Li-wei，WANG Jin-shan，JIANG Chong-qiu^*
		Applying supercritical CO₂ fluid extraction technology, flavonoids were extracted from Chinese traditional medicine asarum heterotropoides, atractylodes macrocephala, and rheum palmatun. Using the method of autoxidation pyrogallol (known as 325 nm method), the superoxide radical scavenginｇ effect of the extraction was carried out in the buffer solution of HCl-tris(pH 8.2). With spectrophotometry, hydroxyl radical created by the system Co²⁺+H₂O₂ in the reaction like Fenton reaction was eliminated by alizarin violet as the color developing agent in the buffer solution HCl-tris (pH 9.0) and the reaction condition was investigated. Result showed that these extractions are elimination agent for these radicals. Asarum heterotropoides is the best of the three.
		2004 Vol. 24 (09): 1103-1105 [Abstract] ( 216 ) PDF (899 KB) ( 417 )

	1106	Determination of Germanium in A. Arborescens by Spectrophotometric Method
		HUI Rui-hua，HOU Dong-yan，GUAN Chong-xin
		A new spectrophotometric method for the determination of germanium in A. arborescens was developed. The method was based on the fact that germanium forms a stable complex with phenylfluorone in the acidified solution with CTMAB as solubilization agent. The maximum absorption of association complex is at 530 nm, the linear range is 0.1-0.7 μg·mL^-1，the regression equation is A=0.081 7+0.867 7c₅₃₀,(μg·mL^-1) the correlation coefficient r=0.917 7, and the limit of detection is 0.65 μg·mL^-1. The leaves and stems of A. arborescens were determined by the proposed method. The total amount of germanium is 697.0-1 219.5 ng·g^-1, and the content of organic Ge is 95.45%-98.99%. The method is suitable for the analysis of samples which contain both organic Ge and inorganic Ge.
		2004 Vol. 24 (09): 1106-1109 [Abstract] ( 1090 ) PDF (920 KB) ( 421 )

	1110	Study on the Solid Phase Extraction Spectrophotometric Determination of Mercury in Water with 5-(2-Hydroxy-4-Sulfo-5-Chlorophenol-1-Azo)-Thiorhodanine
		YANG Bo¹, ZHOU Li-qiong¹, YIN Jia-yuan²
		Based on the color reaction of mercury with 5-(2-hydroxy-4-sulfo-5-chlorophenol-1-azo)-thiorhodanine (HSTC) and the solid phase extraction of the colored complex with C₁₈ cartridge, a new method for the determinations μg·L^-1 level of mercury was studied. In the presence of pH 3.6 HAc-NaAc buffer solution. HSTC reacted with mercury (Ⅱ) to form a stable 2∶1 complex. This complex was enriched by solid phase extraction with C₁₈ cartridge and the retained complex from cartridge was elｕted with DMF. An enrichment factor of 80 was achieved. In the measured solution, the molar absorptivity was 6.24×10⁴ L·moL^-1·cm^-1 at 545 nm. Beer’s law was obeyed in the range of 0-1.5 μg·mL^-1. This method was applied to the determination of mercury in water. The relative standard devitions were 1.8%-2.2% and the recoveries were 93％-106％. The results are satisfactory.
		2004 Vol. 24 (09): 1110-1112 [Abstract] ( 1656 ) PDF (841 KB) ( 391 )

	1113	Determination of Rare-Earth and Trace Elements in Teeth Enamel by Inductively Coupled Plasma Mass Spectroscopy
		WANG Song-jun¹，CHANG Ping¹，SU Wei-na¹，SUN Chun-hua¹，WANG Li-juan¹，ZHANG Gui-ying²，HOU Tian-ping³
		Determination of rare earth and trace elements in teeth enamel was studied by inductively coupled plasma mass spectroscopy. The sample was completely dissolved by HNO₃-H₂O₂. The range of precision is 0.50%-6.79% given by the relative standard deviation and the range of accuracy is 94.45％-104.78% obtained by measuring standard recovery rate. The above data satisfied completely the requirements of biological sample. While this study provides experimental data of rareearth and trace elements of teeth enamel for carious teeth and none carious teeth of human for prevention and cure of decayed tooth. A reasonable method is provided for mouth medicine research.
		2004 Vol. 24 (09): 1113-1116 [Abstract] ( 1064 ) PDF (889 KB) ( 376 )

	1117	Determination of Trace Cs, Th and U in Ten Kinds of Human Autopsy Tissues by ICP-MS
		WANG Jing-yu¹, ZHU Hong-da², OUYANG Li¹, LIU Ya-qiong¹, WANG Xiao-yan¹, HUANG Zhuo¹, WANG Nai-fen¹， LIU Hu-sheng¹
		This paper studied the trace elements Cs, Th and U in ten kinds of human autopsy tissues by ICP-MS. The instrumental operating conditions were optimized for the measurement of Cs, Th and U. Rhodium (Rh) was used as an internal standard element to compensate matrix effect. Detection limits for Th, U and Cs were 5.7-17.8 pg·mL^-1. The recoveries for spiking liver samples were 96%-107%, and their RSDs were 4.8%-8.9%. Reference materials of NIST SRM 8414 Bovine and NIST SRM 1 486 Bone Meal were analyzed by the described method, and the analytical results agreed well with the reference values. Human autopsy tissues samples were digested by mixed acid (HNO₃+HClO₄). The determination of Cs, Th and U in lung, liver, bone, heart, stomach, spleen, muscle, kidney, thyroid gland and intestinum tenue was performed by ICP-MS without separation and enrichment procedures. The obtained results indicated that this method is rapid, sensitive and accurate; the distribution of the three elements is different from one to another human organ sample; the main organ targets for Th and U are lungs and kidneys; and a coordinated variation of Cs, Th and U concentration in lungs was found in the samples collected from Hebei and Sichuan provinces.
		2004 Vol. 24 (09): 1117-1120 [Abstract] ( 1591 ) PDF (911 KB) ( 365 )

	1121	Rapid Analysis of Mercury in Sediments by Laser Ablation Inductively Coupled Plasma Mass Spectrometry
		TAO Guan-hong¹, FUJIKAWA Yoko²
		Laser ablation inductively coupled plasma mass spectrometry was used for the rapid analysis of mercury in sediment samples. The ground samples were simply briquetted prior to laser ablation. The effects of internal standardization, particle size and elemental speciation on the analytical performance were investigated. Direct analysis of sediment samples without internal standardization could yield satisfactory results. Elemental speciation and particle size within the studied range did not significantly affect the measurements. The calibration curve was obtained simply by analyzing one soil and two sediment reference materials. With the proposed LA-ICP-MS system, a detection limit of 0.02 mg·kg^-1 was achieved with a sample through put of 10 h^-1. Analytical results of sediment samples using the current system were in good agreement with those by isotope dilution hydride-generation ICP-MS.
		2004 Vol. 24 (09): 1121-1123 [Abstract] ( 1067 ) PDF (853 KB) ( 365 )

	1124	Simultaneous Determination of Pb, Cd，Cr and Co Released from Ceramic Ware by ICP-AES
		Lü Shui-yuan, LI Xiao-jing, LIU Wei, LIN Hua
		The method for the determination of Pb, Cd, Cr and Co released from ceramic ware by ICP-AES has been presented. The factors such as the influence of power in 4% acetic acid，the selection of analytical wavelength，and the interference of coexistent element have been investigated. The detection limits were 6.8 μg·L^-1 for Pb, 0.18 μg·L^-1 for Cd, 0.61 μg·L^-1 for Cr, 1.0 μg·L^-1 for Co. The recovery rates of the procedure were between 98% and 104%. The RSDs were between 0.27% and 1.24%. The method was simple, rapid, precise，convenient and suitable for daily inspection of import and export ceramic ware.
		2004 Vol. 24 (09): 1124-1126 [Abstract] ( 985 ) PDF (822 KB) ( 404 )

	1127	Determination of Soluble Heavy Metal Pb，Cd and Cr in Water Based Architectural Coatings for Indoor Decorating and Refurbishing Materials by ICP-AES
		JIN Xian-zhong, ZHENG Shu-zhao, LI Rong-zhuan, QIU Yin, CAI Yan-ping
		In this paper the authors have studied coexisting element interference and acidity effect in sample, corrected spectral overlapping interference and non-spectral interference by interference coefficient method and standard addition method respectively, and established a method for the determination of soluble heavy metal Pb，Cd and Cr in water based architectural coatings by ICP-AES. The method is accurate and of low detection limit, and can be applied to the inspection work of water based architectural coatings.
		2004 Vol. 24 (09): 1127-1129 [Abstract] ( 337 ) PDF (895 KB) ( 383 )

	1130	Determination of Platinum in Membrane Electrode Assembly(MEA) by Graphite Furnace Atomic Absorption Spectrometry
		FU Chuan
		The contents of platinum in Membrane Electrode Assembly(MEA) is very important to the cost of proton exchange membrane fuel cell. In this paper, the contents of platinum in MEA were determinated by graphite furnace atomic absorption spectrometry. The influences of the program for graphite furnace and the optimum conditum of experiment were systematically studied. The method is simple, rapid, accurate and practical. The result indicates that the relative standard deviation of Pt determination is less than 2.67%. The rate of recovery is 97.3%-101.2%.
		2004 Vol. 24 (09): 1130-1132 [Abstract] ( 980 ) PDF (835 KB) ( 379 )

	1133	Determination of Trace Mercury in Coal by Microwave Digestion and Cold Vapor Atomic Fluorescence Spectrometry
		LIU Jing，ZHENG Chu-guang，XU Jie-ying
		A method of determining trace Hg in coal by microwave digestion and cold vapor atomic fluorescence spectrometry is reported. The digestion system of HNO₃-HCl-HF was evaluated. The experimental conditions of microwave digestion, including pressure, temperature, power and time of digestion were evaluated. The operating conditions such as flow rate of carrier gas, flow rate of shield gas and negative high voltage, and interference were also investigated. Testing results show that the detection limit is 0.03 ng·mL^-1 and RSD (n=7) is below 5%. This method is simple and rapid. The treatment method was applicable to determining trace Hg in coal and gave results that were in good agreement with the certified values of the standard reference material.
		2004 Vol. 24 (09): 1133-1135 [Abstract] ( 1078 ) PDF (903 KB) ( 453 )

	1136	X-Ray Microanalysis of the Activity of Immobilized L-Asparaginase
		DING Liang^{1, 2}, YAO Zi-hua¹
		The localization of activity of immobilzed L-asparaginase by covalent binding was studied by X-ray microanalysis. Asparagine and MgCl₂ served as substrate and capture aｇent respectively. Substrate was catalysed by immobilized L-asparaginase to produce NH₃，and NH₃ was captured by MgCl₂ to form precipitate MgNH₄PO₄. Precipitae was deposited on active site of immobilized L-asparaginase. The results show that the macroporous resins of immobilized L-asparaginase has greater enzyme activity, while distribution of activated enzyme was uniform. Most of activated enzyme was immobilized on the macroporous resins. The optimum condition of localization of activity of immobilized L-asparaginase was studied.
		2004 Vol. 24 (09): 1136-1139 [Abstract] ( 1526 ) PDF (3047 KB) ( 506 )

	1140	Biosynthesis and Characterization of Jarosite
		ZHOU Shun-gui¹, ZHOU Li-xiang^1*, WONG Jonathan W. C.²
		A yellow ochre-colored jarosite was synthesized by bacterial oxidation of ferrous ion by Thiobacillus ferrooxidans at 28 ℃ and 1 atm. The identification of the bacterially oxidized ion precipitate was carried by SEM, XRD, FTIR and chemical analysis. Results showed that resting T. ferrooxidans cells could completely oxidize ferrous ions to ferric ions in FeSO₄-K₂SO₄-H₂O system at pH 2.5. In the presence of suitable monovalent K⁺ and excess sulfate, the yellow precipitate was produced from bacterially oxidized iron solutions. The subsequent characterization showed that it was high-quality jarosite without by-product such as amorphous ferric hydroxysulfates.
		2004 Vol. 24 (09): 1140-1143 [Abstract] ( 1661 ) PDF (1487 KB) ( 750 )

	1144	Flame Temperature Distribution Measurement of Solid Propellants
		ZHAO Wen-hua¹, ZHU Shu-guang¹, LI Yan², FANG Zhong-yan²,YANG Rong-jie³, LI Yu-ping³, ZHANG Jie³, LIU Yun-fei³
		Many high temperature bodies such as flame, in which chemical reactions are very complex, emit their own spectra. These emission spectra usually consist of the spectral lines, spectral bands and the continuous spectra. In some cases, the spectral lines gather together. It is very difficult to find the right single spectral line when the spectral line intensity method is used. To deal with this problem, the idea that the single spectral line intensity is replaced by the total intensity of many spectral lines to measure the temperature is mentioned. And the relative intensity method is also changed to deal with this idea. The measurement of the temperature distribution based on this improved method is successful, and the measurement results are compared with the results of the thermocouple method.
		2004 Vol. 24 (09): 1144-1147 [Abstract] ( 992 ) PDF (879 KB) ( 394 )

	1148	Effect of High Performance Liquid Chromatographic Instrument System on the Analysis of Erythromycin A Oxime
		SUN Jing-guo^{1, 2}，YAO Guo-wei¹，OU Yu-xiang³
		A HPLC chromatography for the determination of erythromycin A oxime and relative compounds was studied, amd the effect of chromatography systems including a HITACHI L-7100, a Shimadzu LC-6A, a Waters^TM 474 and relative columns was analyzed. It was revealed that different HPLC apparatus and columns have obvious impact on the peak separation and retention time under the general chromatographic condition. The suitable chromatographic conditions for several different chromatography systems were summarized with good linear relationship，which is very significant to the quality control of erythromycin A oxime and relative compounds.
		2004 Vol. 24 (09): 1148-1150 [Abstract] ( 1008 ) PDF (863 KB) ( 491 )

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