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2004 Vol. 24, No. 02 Published: 2004-02-26

光谱学与光谱分析

	129	Spectroscopic Characterization of Tm³⁺ Ions in Zinc Tungstate Crystals
		ZANG Jing-cun¹，LIU Yu-long²，XU Dong-yong¹，GONG Feng¹，SHAN Bing-rui¹
		A series of high quality ZnWO₄:Tm³⁺ single crystals were grown with Czochralski method. The concentrations of thulium ions were 0.1, 0.3, 0.5, 0.7 and 1.0 mol%，respectively. When ZnWO₄: Tm³⁺ single crystals were excited by 807 nm laser, the up-conversion luminescence peaks at 486 and 695 nm which corresponded to transitions ¹G₄→³H₆ and ³F₃→³H₆， respectively，were detected. The intensity of 695 nm luminescence varied with the pump power in a double logarithmic relation whose indexes were 0.8 and 1.1 orders，respectively.
		2004 Vol. 24 (02): 129-131 [Abstract] ( 1501 ) PDF (996 KB) ( 466 )

	132	Electron Temperature of Al Plasma Estimated with Ar
		LI Zun-ying，LIU Fu-yi
		Protected with Ar, it would induce atom Ar breakdown to ablate aluminum target with a pulsed Nd:YAG laser beam. Further more, a lot of Ar⁺ ionic characteristic lines radiation appeared accompanying the aluminum plasma emission. In this work, based on the Ar⁺ ionic characteristic lines radiation, we analyzed time-resolved behavior of four Ar⁺ ionic characteristic lines Ar Ⅱ 385.057, Ar Ⅱ 386.853, Ar Ⅱ 404.291 and Ar Ⅱ 407.201 nm, respectively. Electron temperature of aluminum plasma in the stage of ionic lines emission was approximately calculated. As a result, in this stage, the electron temperature ranged from 15 000 to 22 000 Ｋ, and decreased successively with the delay time increasing. Compared with other similar works, we found that our results agreed with many similar estimations.
		2004 Vol. 24 (02): 132-134 [Abstract] ( 1598 ) PDF (906 KB) ( 370 )

	135	Analysis of Gas Absorption Coefficient at Various Pressures
		MA Wei-guang, YIN Wang-bao, HUANG Tao, ZHAO Yan-ting, LI Chang-yong, JIA Suo-tang
		The absorption coefficient α(ν) of gas plays an important role in quantitative analysis of pollution gases and theoretical investigation of molecular parameter. In this paper we first analyze α(ν) theoretically and present a calculation method. Then we analyze 2ν₃ band R3 manifold of pure CH₄ and draw a conclusion that α(ν₀) decreases and the peak absorption κ(ν₀) increases with increasing the pressure. When the pressure is ＜0.03 and ＞2 atm, we can calculate α(ν₀) using the Gaussian profile and Lorentzian profile respectively, and then analyze the relative error. Finally we analyze the peak absorption κ(ν₀) at various pressures, then define the high-resolution area and high-sensitive area respectively when the pressure is ＜0.01 and ＞1 atm.
		2004 Vol. 24 (02): 135-137 [Abstract] ( 565 ) PDF (884 KB) ( 984 )

	138	The Simultaneous Measurements of Time-Dependent Laser-Induced Fluorescence Intensity of Hematoporphyrin Monomethyl Ether in Animal Tissues with Rheumatoid Arthritis
		YU Chang-qing^1，3, HUANG Nai-yan², ZHAO Hai-ying¹, DOU Xiao-ming¹, LI Jia-ze³
		Since the selectivity of photodynamic therapy (PDT) depends on the distribution of a photosensitizer in a tissue during the treatment, an investigation of drug distribution is a key step for performing PDT effectively. The distribution of photosensitizer absorbed in tissues is adjusted by the animal body system, so an apparatus that can measure the fluorescence intensity of photosensitizer in different tissues of the same body simultaneously is in demand. To achieve precise estimate of tissue selectivity of the photosensitizer, a spatially separated three-channel laser-induced fluorescence (LIF) detection system was set up and employed in the present study to measure the fluorescence intensity of Hematoporphyrin Monomethyl Ether (HMME) in different tissues of the same body simultaneously. The time-dependent variations in the concentrations of HMME within the skin, cartilage, normal synovium and inflammatory synovium of rabbit were monitored in vivo. The results obtained showed that the synovium has higher absorptivity of HMME than the skin and cartilage. The difference is distinct from the very beginning of injection. Although the quantity of HMME absorbed in the inflammatory synovium is not very high in the first 20 min, it is still 6 times higher than that in the skin and cartilage. In addition, the absorptivity of HMME is much stronger for the inflammatory synovium than that for the normal synovium. If the laser beam irradiates outside the joint for the rheumatoid arthritis, tissues around the inflammatory synovium have less HMME, thereby causing weak PDT effect. This would help reduce the side effect of PDT. Thus we suggest that for PDT treated rheumatoid arthritis，taｋing the first 20 min after the injection for outside-the-joint eｘcitation employing HMME maybe a good choice.
		2004 Vol. 24 (02): 138-141 [Abstract] ( 544 ) PDF (903 KB) ( 378 )

	142	Rheological Phase Synthesis and Characterization of Lanthanum Salicylate and Luminescence Properties of Tb³⁺-Doped Lanthanum Salicylate
		LI Liang-chao¹，LI Zi-cheng²，YUAN Liang-jie²，ZHANG Ke-li²，SUN Ju-tang²
		Lanthanum salicylate and Tb³⁺-doped lanthanum salicylate were synthesized with the rheological phase reaction method. Elemental analysis, IR, TG, DTA and powder X-ray diffraction were investigated to determine the composition, crystal structure and coordination manner between the COO^- and ion La³⁺ of lanthanum salicylate. The emission and excitation spectra of Tb³⁺-doped lanthanum salicylate were also discussed. Powder X-ray diffraction suggests that the compound has a layered monoclinic structure, and the lattice parameters are a=21.601 0 , b=13.801 5 (A), c=3.810 3 (A), β=97.11°, V=1 127.2 (A)³, Z=2, ρ_cal=1.621 g·cm^-3 and ρ_exp=1.653 g·cm^-3. The Tb³⁺-doped lanthanum salicylate exhibits very strong green luminescence of Tb³⁺ under the excitation of UV light. And the transition from ⁵D₄ to ⁷F₅ is the strongest one.
		2004 Vol. 24 (02): 142-144 [Abstract] ( 231 ) PDF (874 KB) ( 341 )

	145	Selective Quantitation of Analgin by Flow Injection Chemiluminescence Method
		YANG Feng-zhen^{1, 2}, ZHANG Chao², WANG Jian-ning², ZHANG Xin-rong²
		A new chemiluminescence-based method was proposed for selective quantitation of analgin in pharmaceutical preparation. The CL emission was generated by mixing analgin, polyethylene glycol-400 and rhodamine 6G in acidic medium. The analgin content could be determined by the CL intensity. No oxidants were used in the system, so it was difficult to explain why the CL emission was produced. The mechanism of CL emission remains under investigation. One of the advantages of this method is highly selective. No other pharmaceutical compounds and chemicals could produce CL emission whether they contain sulfuric group or not in the experiment. There was no disturbance in this method, which was different from others. Another advantage is high sensitivity. The quantitation range is from 0.01 to 10 μg·mL^-1 with a detection limit of 0.003 μg·mL^-1 for analgin. This is the lowest detection limit of any CL methods currently available for analgin determination. The proposed method was applied to the selective quantitation of analgin in pharmaceutical preparation.
		2004 Vol. 24 (02): 145-148 [Abstract] ( 1765 ) PDF (915 KB) ( 355 )

	149	Third Order Nonlinear Optical Properties of Three Kinds of Metal Phthalocyanines
		LI Lin，HUANG Yan-ping^*，LI Shan-shan，DAI Yu-wen
		Using YAG laser, the nonlinear optical refractive indexes of three kinds of metal phthalocyanines in DMF, ZnPCS(C₅₆H₃₂N₈S₄Zn)，AlPCS (C₅₆H₃₂AlClN₈S₄) and AlPCP (C₅₆H₃₂AlClN₈O₄) were studied with the method of Z-scan. Their third-order susceptibilities χ⁽³⁾ were also calculated. The result shows that different central ion and different substituents could affect their third-order susceptibilities. The mechanisms of third order optical nonlinearity and energy transfer in the photodynamic therapy were discussed.
		2004 Vol. 24 (02): 149-151 [Abstract] ( 1502 ) PDF (863 KB) ( 353 )

	152	A Comparative Study on the Resolution of Second Derivative and Fourier Self-Deconvolution
		WANG Dong-mei, WANG Hai-shui^*，ZENG Guang-fu, XI Shi-quan
		Infrared spectra of 2-alkyl-7,7,8,8-tetracyanoquinodimethane(C₁₂H₂₅TCNQ，C₁₅H₃₁TCNQ，C₁₈H₃₇TCNQ) were measured with the resolution of 1 and 4 cm^-1. In order to identify the peak number correctly in the CH₂ stretching region, second derivative and Fourier self-deconvolution were applied to the infrared spectra，respectively. The overlapping bands in the CH₂ stretching region could be identified when the infrared spectra，which were measured with the resolution of 4 cm^-1，were dealt with by Fourier self-deconvolution. However, the bands overlapped in the CH₂ symmetric stretching region could not be observed when these infrared spectra were dealt with by second derivative. The above results reveal that Fourier self-deconvolution method is more powerful than second derivative in identifying bands that are involved in an overlapping band feature.
		2004 Vol. 24 (02): 152-154 [Abstract] ( 1003 ) PDF (873 KB) ( 413 )

	155	Measurement of Borneol Based on Near Infrared Spectroscopy
		GU Xiao-yu¹，WANG Yan^1*，XU Ke-xin¹，LI Lin²，LING Ning-sheng²
		Infrared spectroscopy can provide integrated information of samples, and is easy to be applied to on-line control. So quality control specification of Chinese drugs can be improved by utilizing this method for the production of Chinese drugs. This method can accelerate the modernization process of Chinese drugs. Borneol is an effective constituent in lots of active Chinese drugs. The spectral characteristics of borneol in near infrared region were investigated in this paper. The characteristic absorption peaks of borneol were found by measuring its spectra in near infrared band. There are five absorption peaks of borneol close to 4 828，5 003，5 736，7 044 and 8 387 cm^-1，respectively. Establishing a partial least square (PLS) model can get optimal results in model building experiment. The predictive results show that the linear relationship between twenty-five samples’ predicted values and real values is good with regard to the content of borneol. In calibration model, the root mean square error of prediction (RMSEP) of the content of borneol is 0.28 mg·mL^-1 and the number of the principal components is equal to two. The experimental results show that infrared spectroscopy can be used as a means in the field of quality control of Chinese drugs and the measurement of effective constituents of Chinese drugs.
		2004 Vol. 24 (02): 155-157 [Abstract] ( 1617 ) PDF (885 KB) ( 435 )

	158	The Algorithm of Eliminating the Similar Samples in the Process of Calibration and Prediction
		LU Yong-jun, QU Yan-ling, PIAO Ren-guan, ZHANG Jun
		During the manufacture and debugging of the NIR instruments it is compulsory to make final calibration analysis to verify whether the instruments operate correctly. However, the conventional method of NIR calibration needs to make calibration analysis for the instruments with all the samples at hand. In fact in order to cover the samples that will be encountered in the future the amount of the samples set and the labor that the personnel need to offer are enormous. In this paper a new algorithm is presented which can be used to effectively eliminate the similar samples in the original sample set. By using this algorithm we have chosen 94 optimal samples in the original 178 sample set successfully. After performing calibration experiment we found that the sample set chosen by this algorithm are equally representative to the original sample set and obtained almost the same precision compared to the original sample set when the two sample sets were individually calibrated. This algorithm brings great relief to the labor of the workers, presents the possibility of performing more experiments and greatly improves the efficiency of performing calibration experiment. As a result, the amount of calibration sets and the labor of the personnel are reduced remarkably.
		2004 Vol. 24 (02): 158-161 [Abstract] ( 1044 ) PDF (895 KB) ( 419 )

	162	Study on the Synthesis and Spectra of 2-Thenoyl-2-Carbazolyl-N-Butyltrifluoroacetone
		YU Qian，LUO Zong-ming，YANG Chi，FANG Yan-xiong，ZHANG Kun，CAO Xian-yi
		In phene-50% NaOH medium, 1, 4-dibromobutane reacts with carbazole (CZ) to form N-bromobutylcarbazole (BCZ) at 70-80℃. The 2-thenoyl-2-carbazolyl-N-butyltrifluoroacetone(TCBTA) was synthesized by reaction of BCZ with 2-thenoyltrifluoroacetone(TTA) in acetone-K₂CO₃ medium at 50℃. The TCBTA is a light brown crystal with m. p. of 211-214℃. The structure of the synthesized TCBTA was characterized by UV, IR and GC/MS, and the UV and IR spectra of CZ , BCZ and TTA have been studied. In chloroform, TCBTA has three maximum absorptions at 241, 265 and 295 nm whose molar absorptivity is 1.88×10⁵, 1.25×10⁵ and 1.08×10⁵ L·mol^-1·cm^-1, respectively. Extraction rate of iron(Ⅲ) and neodymium(Ⅲ) by TCBTA in chloroform rises by 3 and 1.6 times compared with TTA. The fluorescence of TCBTA-Nd(Ⅲ) complex is 5 times higher than TTA-Nd(Ⅲ) complex. It was shown that TCBTA has excellent photosensitivity.
		2004 Vol. 24 (02): 162-165 [Abstract] ( 1172 ) PDF (940 KB) ( 681 )

	166	The Reaction Mechanism of Metolachlor and S-Isomer with Urease
		LIU Hui-jun, LIU Wei-ping, CHEN Ai-ping, YANG Wei-chun
		The binding of metolachlor and S-Isomer to urease in aqueous solution was studied using UV difference spectrum and fluorescence spectrum. According to the results of the UV difference spectrum curve, the UV difference adsorption ΔA changed rapidly when herbicide concentration increased from 0.0 to 1.6 μmol·L^-1. UV difference spectra were red-shifted and absorb-peaks became lower. It was shown that herbicide can quench the urease fluorescence mainly through a static quenching procedure. The binding constant K and the number of binding site n were calculated according to the fluorescence quenching results. For metolachlor, K＝1.49×10³ L·mol^-1 and n was 0.84; for S-isomer, K＝2.22×10³ L·mol^-1 and n was 0.89.
		2004 Vol. 24 (02): 166-168 [Abstract] ( 1340 ) PDF (879 KB) ( 368 )

	169	Studies and Application of the Interaction of Pentamethyl-p-Rosaniline Hydrochloride 6B and Nucleic Acids System
		LIN Xu-cong, XIE Zeng-hong, GUO Liang-qia, LIU Shao-feng, CHEN Guo-nan
		A cationic dye pentamethyl-p-rosaniline hydrochloride 6B was used as a chromic probe and its binding reaction with nucleic acids was studied. In the weak alkalescent medium, the cationic dye showed a decrease in absorption at its maximal absorption peak (584.5 nm) on binding to nucleic acids. Based on this fact, a new UV-Vis spectrophotometric method for the determination of nucleic acids has been developed. Effects of ion-intensity, surfactant and organic solvent were investigated to establish optimum reaction conditions, and then nucleic acids were detected with quantitative analysis. The calibration curves of nucleic acids such as hs-DNA, sm-DNA, ct-DNA and yeast-RNA were linear over the ranges 0.50-4.00 μg·mL^-1, 0.20-5.00 μg·mL^-1, 0.20-5.00 μg·mL^-1 and 0.20-4.50 μg·mL^-1, respectively. The detection limits (3σ/ K) were 0.082, 0.037, 0.038 and 0.041 μg·mL^-1. In applications to quantitative analysis of nucleic acids synthesis samples, the recoveries of DNA or RNA ranged from 93.5% to 105.0%. Furthermore, the mechanism of interaction of pentamethyl-p-rosaniline hydrochloride 6B and nucleic acids system was also discussed.
		2004 Vol. 24 (02): 169-172 [Abstract] ( 1563 ) PDF (891 KB) ( 324 )

	173	Synthesis and Spectral Properties of L-Amino Acid Tailed Porphyrin and Their Zinc(Ⅱ) Complexes
		LUO Guo-tian, TENG Li-li, LAI Xiao-qi, LI Lei
		Three new L-amino acid tailed porphyrins and their zinc(Ⅱ) complexes were synthesized by L-amino acid and 5-[o-(bromoethoxyl)phenyl]-10,15,20-triphenyl prophyrin. FAB-MS, UV-Vis, IR, elemental analysis and chemical analysis were used to determine the structures of these porphyrins and their zinc complexes. The FTIR spectra (4 000-400 cm^-1) of L-amino acid tailed porphyrin and its zinc(Ⅱ) complexes were measured and investigated. The major bands have been empirically assigned in comparison with L- amino acid tailed porphyrin and its zinc(Ⅱ) complexes.
		2004 Vol. 24 (02): 173-176 [Abstract] ( 1333 ) PDF (911 KB) ( 364 )

	177	Chemical Modification on the Surface of Nano-Particles of ZnO and Its Characterization
		YU Hai-yin, DU Jun, GU Jia-shan, GUAN Ming-yun, WU Zheng-cui, LING Qing, SUN Yi-min
		After nano-particles (ZnO) had been encapsulated by a kind of water-soluble cellulose Hydoxyl-Propyl-Methyl Cellulose(HPMC), then methyl methacrylate was grafted onto the surface of them. Thus the surface of nano-ZnO had been successfully modified. FTIR, DTA and TEM were utilized to confirm the results. FTIR shows that HPMC was adsorbed onto the surface of ZnO, and PMMA was also grafted onto its surface, DTA says that the heat stability of HPMC，HPMC-g-PMMA and ZnO/HPMC-g-PMMA increased greatly, TEM photo demonstrates that polymer adhered onto the surface of nano-ZnO which was encapsulated by a layer of film-like polymer.
		2004 Vol. 24 (02): 177-179 [Abstract] ( 994 ) PDF (912 KB) ( 698 )

	180	The Negative Temperature Effect of UV Absorbance on C₆₀ in Different Solvents
		YANG Tao¹，ZENG Fan-qing^{1, 2*}，GE Qi¹，XIONG Qian¹，GUO Feng¹，ZHANG Xun-gao²
		Ultraviolet Absorption Spectrum of Difference in Temperature(UVSDT) of C₆₀ was studied in different solvents by UV-240 ultraviolet-visible spectrophotometer. Two samples were tested, one of which acted as reference sample and the other as ready test sample. During the period of the experiment, the temperature of the reference sample remained constant, while that of the ready test sample was changed to obtain difference in temperature. The two samples were scanned in succession by UV-240 ultraviolet-visible spectrophotometer using a certain range of wavelength. By changing the temperature of the ready test sample, we can get the ultraviolet absorption spectrum changing curve with temperature differential. In addition, the curve was studied by putting C₆₀ in different solvents(alcohol, cyclohexane, n-hexane and 2-propanol).The curve indicates that the intensity of the absorption peak wavelength of C₆₀ decreased with increasing the temperature of the sample, and a negative peak was observed in UVSDT. And the greater the difference in temperature, the higher the intensity of the negative peak. The result reflects that the structure of C₆₀ depends strongly on its temperature, and the dependent relationship is closely related to the type of π-π^* electron transition. So it’s valuable to test the absorption rate of C₆₀ and obtain the changing curve in real time. It’ll help us to separate, purify, analyze, and characterize C₆₀. And it’ll also help to do research on the mechanism of the chemical reactions, which take place in solvents, as well as to improve veracity.
		2004 Vol. 24 (02): 180-182 [Abstract] ( 2182 ) PDF (876 KB) ( 434 )

	183	UV-Vis Spectroscopic Characterization of Inclusion Compounds of β-Cyclodextrin with Lycopene
		WANG Luo-xin, Lü Jun, DU Zong-liang^*, LI Rui-xia, WU Da-cheng
		Water-soluble inclusion compounds of β-cyclodextrin with lycopene were prepared by two methods: (1) complexation in solution and (2) complexation by kneading. It was found that UV-Vis spectra of the inclusion complexes in water are different from those of lycopene in water-miscible organic solvents (tetrahydrofuran) and β-cyclodextrin in water, which confirms the formation of the inclusion complexes. Specific interactions of lycopene and β-cyclodextrin cause great changes in absorbance maximum (λ_max) of lycopene. It is considered that the inclusion complexes in water are formed as supermolecular aggregates with nanometer size, after card-pack type lycopene is included by β-cyclodextrin in molecular level.
		2004 Vol. 24 (02): 183-186 [Abstract] ( 2010 ) PDF (946 KB) ( 589 )

	187	Study on Solid-Phase-Extraction Spectrophotometric Determination of Silver with p-Sulfobenzylidene-Rhodanine
		WANG Lin¹，HU Qiu-fen²，YANG Guang-yu²，YIN Jia-yuan²
		The color reaction of silver with p-sulfobenzylidene-rhodanine (SBDR) was studied. Based on the color reaction of SBDR with silver (Ⅰ) and the solid phase extraction of its colored complex with Waters Porapak Sep-Park-C₁₈ cartridge, a new method for the determination of micro-amount of silver (Ⅰ) was studied. In the presence of pH=2.8 citric acid-sodium hydroxide buffer solution and Tween-80 medium，SBDR can react with silver (Ⅰ) to form a stable 2∶1 complex. The colored complex can be extracted by C₁₈ cartridge and eluted by ethanol (containing 5% acetic acid), and then can be determined by spectrophotometry. The molar absorptivity is 7.53×10⁴ L·mol^-1·cm^-1 at 520 nm. Beer′s law is obeyed in the range of 0-1.2 μg·(25 mL)^-1. This method can be applied to the determination of silver in water with satisfactory results.
		2004 Vol. 24 (02): 187-189 [Abstract] ( 1464 ) PDF (858 KB) ( 844 )

	190	Determination of Deoxyribonucleic Acids at Nanograms Levels with Toluidine Blue by a Resonance Light-Scattering Method
		XIAO Xi-lin，WANG Yong-sheng^*，LI Gui-rong，Lü Chang-yin
		Resonance light scattering(RLS) spectra of toluidine blue(TB) with DNA was studied. The RLS of TB was greatly enhanced by DNA in the range of pH 10-11. A RLS peak at 350 nm was found, and the enhanced intensity of RLS at this wavelength was proportional to the concentration of DNA. The linear range of the calibration curve was 0-900 ng·mL^-1 with the detection limit of 6.75 ng· mL^-1 for the ctDNA ,and for fsDNA the linear range was 0-900 ng·mL^-1 with the detection limit of 2.99 ng·mL^-1. Precision at 500 ng·mL^-1 for the two nucleic acids was 3.7% and 5.6%, respectively. Four synthetic samples were determined satisfactorily.
		2004 Vol. 24 (02): 190-193 [Abstract] ( 994 ) PDF (891 KB) ( 538 )

	194	Resonance Light Scattering Study on Interaction of Solochrome Cyanine R with Protein and Light Scattering Determination of Trace Protein
		FENG Ning-chuan，HE Su-ping，ZHANG Juan，LIU Jian-ping
		The resonance light scattering (RLS) of Solochrome Cyanine R(SCR) is greatly enhanced by proteins. Based on this phenomenon, a novel method for the determination of protein by using SCR as a labeling agent was developed. In the pH 4.0 solution the enhanced intensity of RLS at 400 nm is proportional to the concentration of protein. The linear range for bovine serum albumin (BSA) is 0-5.0 mg·L^-1 and the limit of detection is 44.4 μg·L^-1. The method is simple, rapid, sensitive, stable，and tolerant of many foreign substances. It has been used to determine proteins in human urine samples with satisfactory results.
		2004 Vol. 24 (02): 194-196 [Abstract] ( 989 ) PDF (887 KB) ( 359 )

	197	Analysis of Pb(Ⅱ), Cd(Ⅱ) and Cu(Ⅱ) in Chinese Medicine by the System of Porphyrin Complexes and Sulfhydryl Cotton Fiber
		LI Fang¹，ZHENG Huai-li²
		The reaction of α β γ δ-tetra(p-sulfophenyl)porphyrin(TPPS₄) with Pb(Ⅱ), Cd(Ⅱ) or Cu(Ⅱ) has been studied in this article, and the spectra of the Pb(Ⅱ)-TPPS₄, Cd(Ⅱ)-TPPS₄ and Cu(Ⅱ)-TPPS₄ show the spectral absorption of these complexes with high sensitivity. The molar absorptivities of Pb(Ⅱ)-TPPS₄, Cd(Ⅱ)-TPPS₄ and Cu(Ⅱ)-TPPS₄ are 2.5×10⁵ L·mol^-1·cm^-1, 5.2×10⁵ L·mol^-1·cm^-1 and 4.2×10⁵ L·mol^-1·cm^-1，respectively. With the sulfhydryl cotton fiber separation-enrichment method, this analytical system of porphyrin complexes has been successfully applied to determining the trace amounts of Pb(Ⅱ), Cd(Ⅱ) and Cu(Ⅱ) in Ginkgo bilobal leaves and tea leaves. The RSD of determining 10^-6-10^-7 g·g^-1 Pb(Ⅱ), Cd(Ⅱ) or Cu(Ⅱ) in samples lies between 3.3%-9.6%, and the recovery of added standard lies between 90%-103%.The proposed analytical method has the advantage of high sensitivity, simplicity and high efficiency of interfere-resisting.
		2004 Vol. 24 (02): 197-199 [Abstract] ( 271 ) PDF (903 KB) ( 806 )

	200	New Development of Modern Photometric Determination of Trace Aluminium in Environmental Samples
		GONG Ying-kun，ZHENG Huai-li
		In this paper, new development of modern photometric determination of aluminium in environmental samples in recent years was reviewed and discussed. The new development in modern photometric determination of aluminium in environmental samples was emphasized, including micelle photometric method, dual-wavelength photometric method, derivative photometric method, catalytic photometric method, solid phase photometric method and flow injection photometric method. Reaction systems of determination and it’s conditions, molar absorption coefficient(ε)or the limit of detection, the scope of determination and applications of the ordinary photometric method，and the micelle photometric method were summarized. Advantages and disadvantages of all kinds of photometric methods were discussed. The development trend of photometric method was prospected for the detection of trace aluminium in environmental samples.
		2004 Vol. 24 (02): 200-203 [Abstract] ( 1039 ) PDF (866 KB) ( 608 )

	204	Study on the Method for the Determination of Nitric Nitrogen, Ammoniacal Nitrogen and Total Nitrogen in Plant
		Lü Wei-xian¹，GE Ying¹，WU Jian-zhi²，CHANG Jie^1*
		This paper reports the determination of three nitrogen states in plants: nitric nitrogen, ammoniacal nitrogen and total nitrogen. The plant sample was digested by the Kjeldathl method with H₂SO₄+H₂O₂. The solution of the sample was determined by three methods: absorption photometric method, indigotic colorimetry，and UV absorption photometric method after K₂S₂O₈ oxidation. By comparing the results, the relationship among the three N states is that the total N= NH⁺₄+NO^-₃. Suitable methods were found for the determination of the elements, thus providing a scientific basis for the selection of suitable methods for chemical element analysis in plants.
		2004 Vol. 24 (02): 204-206 [Abstract] ( 635 ) PDF (856 KB) ( 831 )

	207	Study on Spectral Identification of Methamidophos Artificial Antigen
		ZHAO Su-qing^1，2，3，CAI Yan-fei^1，2，LEI Hong-tao¹，SUN Yuan-ming^1*，HUANG Xiao-yu¹，ZHANG Hou-rui²，ZHU Zhen-yu³
		In this paper, spectral identification of methamidophos artificial antigen was reported. The results showed that UV absorbance spectrum of artificial antigens of BSAM changed compared with carrier BSA and hapten Met. The absorbance peaks which are similar to P—O—C and PO moiety in IR spectrum of Met molecule appeared in the IR spectrum of the artificial antigens of BSAM. The chemical shift of the artificial antigens of BSAM is the same as that of standard Met in ³¹P NMR spectrum. Phosphor concentration of the artificial antigens of BSAM was determined by phosphor molybdate blue spectrophotometry, and then conjugating ratio was calculated, to be 11. The results obtained with the above four spectrum methods showed that the artificial antigens of BSAM was synthesized successfully.
		2004 Vol. 24 (02): 207-209 [Abstract] ( 1056 ) PDF (875 KB) ( 315 )

	210	The Mistakes of E.Dinc′s Double Divisor-Ratio Spectra Derivative Method
		XU Jia-liang, TANG Xiao-dong, AN Dong, FENG Zheng-yu, YUAN Guo-lin, XIAO Wei, LIU Bing, LEI Zhi-yu
		Double divisor-ratio spectra derivative method has been developed and applied to determining two ternary mixtures simultaneously by E Dinc. In fact, E. Dinc’s double divisor-ratio spectra derivative method is completely wrong. It can not be applied to determining ternary mixtures simultaneously. This paper proves the Mistake of E. Dinc’s method in both theory and practice.
		2004 Vol. 24 (02): 210-213 [Abstract] ( 1726 ) PDF (898 KB) ( 347 )

	214	Experimental Study on Laser-Induced Plasma and Its Application to Spectral Analysis
		ZHAO Shu-rui, CHEN Jin-zhong, WEI Yan-hong, GUO Qing-lin
		The article summarizes the progress in the experimental study on laser-induced plasma and its application to spectral analysis domestically and abroad in recent years.It emphatically elaborates the experimental research on the formation,radiation,electron temperature,electron density, and expansion velocity of laser-induced plasma under different conditions (gas composition and pressure,laser energy,laser wavelength,power density and observation height). In addition,in the respect of material composition analysis using the laser-induced plasma,the article mainly interprets two aspects:one is the way to collect directly the plasma emission so as to analyze solid, liquid and gaseous samples，the other is the spectrochemical analysis when laser ablation and ICP are used together. And the article also discusses the factors that influence the precision and the limit of detection.
		2004 Vol. 24 (02): 214-219 [Abstract] ( 1574 ) PDF (931 KB) ( 812 )

	220	Application of Double Focusing Magnetic Sector High Resolution ICP-MS to the Study of Iron Stable Isotope Trace
		JIN Xin-di
		Iron absorption efficiency study is one of the key steps to overcome iron deficiency anemia. Determination of iron isotope ratios is the base of iron absorption study. For this purpose radioactive isotope trace method, neutron activation，and thermal ionization mass spectrometry etc. have been used as accessory means. A double focusing inductively coupled plasma mass spectrometry (DF-ICP-MS) was used to determine isotope ratios of Fe in food and human faeces in this paper. Interferences of ⁴⁰Ar¹⁶O to ⁵⁶Fe and ⁴⁰Ar¹⁴N to ⁵⁴Fe were avoided by using higher resolution (3 000). Longer times and fast electronic scanning were employed to decrease the influence of signal fluctuations from the plasma. Instrumental parameters of the mass spectrometer were optimized while keeping the total integral time under 27 s. RSD values obtained for isotope ratios of ⁵⁴Fe/⁵⁶Fe, ⁵⁷Fe/⁵⁶Fe and ⁵⁸Fe/⁵⁶Fe were 0.23％, 0.14％, 0.22%, respectively, for a natural standard solution of 5 μg·mL^-1. The method has been used to iron nutrition studies.
		2004 Vol. 24 (02): 220-222 [Abstract] ( 1571 ) PDF (845 KB) ( 336 )

	223	Determination of Trace Elements in Ancient Cheshi Human Costa by ICP-AES
		JIN Hai-yan¹，ZHANG Quan-chao², ZHU Hong²
		In recent years, the study on palaeodiet is an important research in the international archaeological field. Trace elements in human bones can supply a lot of valuable information to reconstruct ancient diet. In this study, The trace elements in Bronze age Cheshi human costa from Chubeixi cemetery in shanshan, Xinjiang were determined by ICP-AES. The sample was dissolved by HNO₃ and HCl. Under the optimum conditions, eight elements can be determined simultaneously. The recoveries of the method are in the rang of 87.4%-106.6%, and RSDs are in the range of 0.5%-3.3%. The method is simple, rapid, precise and convenient to operate. The results would be helpful for research in archaeology. This analysis established Xinjiang’s consult system of trace elements analysis for ancient human bones. The effects of various concentrations of acid solution on analysis results, the interference of coexistent elements, standard addition recovery, and precision of the method were investigated.
		2004 Vol. 24 (02): 223-225 [Abstract] ( 1007 ) PDF (877 KB) ( 319 )

	226	Determination of Trace Elements in Beans by ICP-AES
		WANG Ying，XIN Shi-gang
		In this paper,the contents of trace elements in beans such as Ca， Mg， Mn， Sr， Fe，Co，Ni，Se and Ba were determined by ICP-AES uing nitrifying method of high pressure nitrifying pot, and compared with the results of wet method. The two methods showed no obvious differences. The method proves to be simple， rapid， highly sensitive， accurate and can be used to determine many elements at the same time. In addition， there was little environment pollution.Its recovery is 96.8%-102%, and relative standard deviation is 3.35%.
		2004 Vol. 24 (02): 226-228 [Abstract] ( 1617 ) PDF (881 KB) ( 335 )

	229	ICP-AES Method for the Determination of Active Components Mo and Bi in Catalyst for Acrylonitrile Production
		SHI Hui-fang
		An ICP-AES method for the determination of active components Mo and Bi in catalyst for acrylonitrile production was established and reported in this paper. 0.2 g of the sample was dissolved with 5 mL of aqua regia and 8 mL of HF at 75 ℃ on a water bath and evaporated till dry to expel SiF₄. The residue was dissolved and made volume with 3% HCL up to 100 mL. The soution was prepared for Bi determination. Successively diluted with 3% HCL for 10 times the solution was used for Mo determination. Spectral interferences were investigated in detail by means of profiling the analytical lines with wavelength scanning of the blank and coexisting elements in the vicinity of the lines. Three Mo lines, MoⅡ202.030, MoⅡ203.844 and MoⅡ204.598，and two Bi lines, BiⅡ190.241 and BiⅠ223.061 were selected as the analytical lines considered free of spectral interferences. Utilizing multiple lines in a full spectrum for simultaneous determination of one element is of benefit to the improvement of accuracy and precision of the analysis. The method has been successfully used for monitoring the activity of the catalyst in acrylonitrile production.
		2004 Vol. 24 (02): 229-232 [Abstract] ( 1055 ) PDF (902 KB) ( 326 )

	233	Determination of Trace Platinum, Palladium and Gold in Samples by ICP-AES and Fire Assay Preconcentration
		SUN Zhong-hua, ZHU Kun, MAO Ying, WANG Wei-guo
		A method of elemental determination is put forward in this paper. Namely, Pt, Pd, Au in 10-20 g samples were preconcentrated in milligram microgranular silver alloy by using fire assay. When compounded in solution，trace platinum, palladium, and gold in the solution were determined by ICP-AES. The detection limits of this method were 0.01, 0.005, and 0.01 μg·mL^-1 for Pt, Pd and Au，respectively. Recoveries of standard were more than 97% with precision of 0.1%, 0.12%, and 0.09% of RSD(n=10)，respectively. It has proven that this analysis method is quick, simple and accurate. The method has been applied to the determination of contents of Pt, Pd and Au in samples.
		2004 Vol. 24 (02): 233-235 [Abstract] ( 654 ) PDF (842 KB) ( 381 )

	236	Determination of Trace Mercury in Rice by Microwave Digestion-Hydride Generation-Atomic Fluorescence Spectrometry
		MOU Ren-xiang，CHEN Ming-xue，ZHU Zhi-wei，CHEN Neng
		It was reported in this paper that trace mercury in rice was determined by microwave digestion-hydride generation-atomic fluorescence spectrometry. The microwave digestion of samples was used, and the optimum conditions for the digestion were developed. The relative factors of hydride generation atomic fluorescence spectrometry for the determination were tested and discussed. The temperature and the relative humidity were discussed too. The detection limit was 0.005 ng·mL^-1. Mercury in reference materials (rice flour，GBW 08508) was determined also by the described method. The result obtained was in good agreement with standard value. The relative standard deviation(RSD) was 2.1%, and the recovery of mercury in rice samples was 95.2%-106.4%.
		2004 Vol. 24 (02): 236-237 [Abstract] ( 1172 ) PDF (843 KB) ( 544 )

	238	Study on the Determination of Trace Gallium in Molybdenum-coated Pyrolytic Graphite Tube by Electrothermal Absorption Spectrometry
		HUANG Yu-an, ZHOU Fang-qin^*, LONG Si-hua, YANG Liu
		The effects on gallium atomization in the pyrolytic graphite tube imposed by different matrix modifiers and different coatings were discussed detailedly in this paper. In the presence of matrix modifier of Ni(NO₃)₂ the matrix interference was eliminated efficiently. The pyrolytic graphite tubes were coated differently with lanthanum, zirconium, and molybdenum to avoid producing gallium carbide. Results showed that the tube with molybdenum coating was the best. On this basis, the mechanism of gallium atomization in the molybdenum-coated pyrolytic graphite tube using Ni(NO₃)₂ as a matrix modifier was studied furthermore; in addition, the parameters of the operation were optimized. As a result, a new method improved in many aspects was developed to detect trace gallium in complicated sample of gangue. The outcomes of practical applications indicated that the method could satisfy the requests of analysis and that the manipulations were simple to achieve. The characteristic content, the detection limit, and the adding recoveries were 2.12×10^-11 g, 1.4×10^-10 g and 97.4%-102.7% respectively, and the relative standard deviation was less than or equal to 3.6%(n=11).
		2004 Vol. 24 (02): 238-241 [Abstract] ( 1426 ) PDF (909 KB) ( 490 )

	242	Rapid Determination of Trace Sb in Plastic Pipes for Dringing Water by GFAAS
		LU Dan，QIAN Yan-er
		A new method for the determination of trace Sb in plastic pipes for drinｋing water was found. Cu is used as a matrix modifier in the transverse-orientation Zeeman background dedution GFAAS to determine trace Sb in plastic pipes for drinｋing water rapidly. The ashing temperature and atomization temperature were obtained by optimization process. The influences of medium acidity were studied. The best measurement conditions were selected. The sensitivity and precision of the method were improved. Sb was detected directly with a linear range of 0.27-20.0 μg·L^-1. The equation of working curve is Y= 0.006 8 X-0.000 2, r=0.999 6. The characteristic mass of the method is 6.7 pg. The detection limit is 5.4 pg. The recovery is 92.2%-102.5%. The RSDs were obtained from the data of 6 determinations at the concentration level of 5.0，10.0 and 20.0 μg·L^-1 is 6.47%，4.97% and 2.45% respectively. The method is simple，rapid，accurate and of highly sensitive and precise. Satisfactory results are obtained.
		2004 Vol. 24 (02): 242-244 [Abstract] ( 1825 ) PDF (913 KB) ( 412 )

	245	Study on the Determination of Trace Cadmium in Serum by GFAAS
		FENG Shang-cai
		Based on the self-absorption background correction method, HNO₃-K₂HPO₄ was used as matrix modifier in the direct GFAAS determination of trace amounts of cadmium inserum. Optimum conditions for the determination were studied thoroughly. The linear range and the recovery were 0-5 μg·L^-1 and 97.8%-102.5%，respectivly，with the characteristic mass of 4.38×10^-11g.
		2004 Vol. 24 (02): 245-247 [Abstract] ( 1439 ) PDF (900 KB) ( 559 )

	248	X-ray Diffraction Quantitative Analysis with Polynomial-fit Method for Polycrystalline Materials
		YU Quan-zhi¹, SONG Lian-ke¹, CHI Yan-ling², FAN Shu-hai¹，LI Guo-hua¹
		The polynomial-fit method for XRD quantitative analysis of polycrystalline materials is presented in this paper, which combines a mathematic function model with computer technology. Based on the construction of diffraction peak mathematic function model, the XRD atlases from experiments were analyzed by means of polynomial whole pattern fitting to the spectral lines using computer software, then the integral intensities of every peak and weight percentages of each phase could be obtained accurately. This paper mainly includes three parts: 1. According to the fact that the diffraction atlases of mixture are weighted superposition of the powder diffraction atlases of each component and the weight factor of each component is relevant to its volume fraction or weight percentage, the theory of polynomial whole pattern fitting is constructed and the weight factor and weight percentage can be worked out. 2. Describe the method and procedure of data acquisition and analysis. 3. Discuss the result of quantitative analysis. The polynomial-fit method not only simplifies the process of data handling, but also increases the accuracy of analytical result.
		2004 Vol. 24 (02): 248-250 [Abstract] ( 1405 ) PDF (874 KB) ( 500 )

	251	Study on Crystal Structure of Modified Mordenite
		CAO Jian-jin
		The crystal structure of the mordenite modified by supplementing Al³⁺ on Si⁴⁺ was studied with IR, DTA, and XRD. The results indicated that the crystal structure of nature mordenite remains unchanged. But, more Na⁺, K⁺, and other positive ions have gone into lattices due to negative charges produced by supplementing Al³⁺ on Si⁴⁺. This increased crystal water is combined with positive ions. Supplementing Al³⁺ on Si⁴⁺ also results in that the dimension of unit cells of mordenite was extended，the volume of vacancies in the mordenite was expanded and the adsorption capacity of the modified mordenite was increased.
		2004 Vol. 24 (02): 251-254 [Abstract] ( 993 ) PDF (910 KB) ( 369 )

	255	Quantitative Elemental Speciation: Challenges and Strategies Based on Multi-Labelled Multi-Species Isotope Dilution ICP-MS
		Alfredo SANZ-MEDEL, Pablo RODR(I)GUEZ-GONZ(A)LEZ, Jorge RUIZ ENCINAR，J.Ignacio GARC(I)A ALONSO
		According to IUPAC, a chemical species is defined as “the specific form of an element defined as to isotope composition, electronic oxidation state and/or complex or molecular structure^[1]. To carry out chemical speciation, new speciation analysis techniques and strategies are needed. Probably the most popular and useful techniques for speciation analysis are hybrid techniques where a powerful separation is coupled (preferable “on-line”) to an element-specific detector. In fact, the whole strategy for speciation analysis involves a considerable number of discrete steps. These include usually: solid-liquid extraction (if the sample is solid), preconcentration, derivatization, separation of derivatized analytes (e.g. chromatography) and final specific detection (e.g. “on-line” ICP-MS). It is well known that important errors can occur at any of those individual speciation steps. First, solid-liquid extractions should preserve the molecular form (species) of the analytes. Second, preconcentration, derivatization, separation and detection speciation methods should be fully investigated and understood in order to obtain accurate (reliable) determinations of the sought species.From all the above, it is clear that validation of quantitative speciation results is urgently needed. A powerful approach for analytical validation is the use of isotope dilution analysis (IDA). Therefore the application of “speciated” IDA (SIDA) techniques for validation of results for mono-, di-, and tributyltin (MBT, DBT and TBT, respectively) in sediments^[2] and seawater samples^[3] will be discussed using a multi-species spike enriched with ¹¹⁹Sn and final measurement by a hybrid GC-ICP-MS technique. Similarly, the synthesis of multi-labelled multi-species spikes will be described. The application of “doubly- and triply-labelled spikes” has allowed the evaluation of the extent of possible decomposition reactions (the corresponding decomposition factors can be quantified) during several solid-liquid extraction procedures under different conditions. Results on application of a double spike approach (which can correct for the stepwise degradation of TBT) to validate common extraction procedures (e.g. mechanical shaking, ultrasonic leaching, microwave assisted and accelerated solvent extraction) for the determination of butyltin species in sediments^{[4, 5]} will be discussed in detail. Finally, a new triple spike methodology (which can correct not only for the stepwise degradation of TBT but also for other alternative degradation routes) as well as the application of this innovative tool to the analysis of biota (such as mussel tissue) or human samples (urine and blood) will be presented. References
		2004 Vol. 24 (02): 255-255 [Abstract] ( 1495 ) PDF (626 KB) ( 358 )

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