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2006 Vol. 26, No. 01
Published: 2006-01-26
 
       光谱学与光谱分析
1 Study on the Growth and Spectral Characteristics of LiNbO3:Cr:ZnO Crystal
YOU Zhen-yu1, TU Chao-yang1*, ZHU Zhao-jie1, LI Jian-fu1, WEI Min1, Alain Brenier2
The LiNbO3:Cr:ZnO crystals with the size up to 20 mm×50 mm were grown by the Czochralski technique. The absorption spectrum shows that there are two strong absorption wideband peaks and one weak absorption peak of to Cr3+ ion in the crystal. The peak values of the two strong absorption wideband peaks are 480 and 660 nm, which correspond to 4A2→4T1 and 4A2→4T2 transitions，respectively. The weak absorption peak at 727 nm corresponds to 4A2→2E(R line) transition; The fluorescence spectrum shows that one emission wideband peak ranging from 802 to 988 nm coexists with one weak emission peak at 754 nm corresponding to 4T2→2E transition. The peak value of emission wideband is at 871 nm, which corresponds to 4T2→4A2 transition. The crystal field and Racah parameters were calculated, and Dq/B=2.72 indicates that it has an stronger crystal field. The result shows that the wideband tunable laser can be obtained from this crystal because it not only has the necessary spectral characteristics required for tunable laser crystal but also has good physical chemical properties. Furthermore, the UV laser at about 420 nm can also be obtained from the crystal by its self-frequency doubling because it has a higher frequency-doubling coefficient.
2006 Vol. 26 (01): 1-5 [Abstract] ( 1632 ) PDF (690 KB)  ( 411 )
6 Spectroscopic Research on the Mechanism for 730 nm Component in Delayed Fluorescence of Chloroplast
WANG Cheng-long, XING Da*, ZENG Li-zhang
Charge recombination in reaction center of photosystem Ⅱ(PSⅡ) is regarded as the origination of delayed fluorescence (DF). The mechanism for 730 nm component appearing in the DF spectrum of chloroplast was studied with different spectral analysis methods. Experimental results of the delayed fluorescence spectrum at different chloroplast concentration showed that the apexes at 685 and 730 nm ascend when the concentration is relative low; the peak value at 685 nm reaches a maximum when the concentration is 7.8 μg·mL-1, however, the apex at 730 nm is still increasing. The peak value at 730 nm finally reaches a maximum at chloroplast concentration of 31.2 μg·mL-1, while the apex at 685 nm has apparently decreased. The results of absorption spectrum showed that the ratios of A685 to A730 are almost a constant during the process of increasing chloroplast concentration. Furthermore, the excitation spectrum for 730 nm fluorescence shows that the 685 nm light has a high excitation efficiency. Above experimental results indicated that the 730 nm component of DF spectrum is the fluorescence of chlorophyll a in PSⅠ reaction center excited by 685 nm DF. Meanwhile, this conclusion was further verified by the invariability of DF spectrum at different delay time (1-9 s).
2006 Vol. 26 (01): 6-10 [Abstract] ( 316 ) PDF (488 KB)  ( 349 )
11 Preparation and Characterization of Chitosan Membrane for Solid Phase Microextraction Technique
YANG Hong-li1, WANG Yi-ru1*, ZHUANG Zhi-xia1,WANG Xiao-ru1, 2
Chitosan is a kind of natural polymers containing plenty of amido and hydoxy.The chitosan membrane is tough, and since the partition coefficient of chlorophyll between chitosan membrance and water is as high as 9 090, the chitosan membrane may be easily manufactured as solid-phase microextraction membrane for the analysis of chlorophyll. The system may reach a complete equilibrium in 80 min. Then the membrane can be desorbed completely in 30 min in 5% NaOH with ultrasonic. Both IR and XRD indicated that hydrogen bonds between the molecules of chitosan were weakened and amido and hydoxy were considered as the keys during the process of extracting chlorophyll.
2006 Vol. 26 (01): 11-14 [Abstract] ( 1526 ) PDF (580 KB)  ( 395 )
15 Fluorescence Characterization of Oxygen Sensing Film for BOD Determination
LIN Ling1, XIAO Lai-long1,XIN Ling-ling1,ZHAO Li1,CHEN Xi1,２*
The film doped with tris-(4,7-diphenyl-1,10-phenanthroline) ruthenium (Ⅱ) ([Ru(dpp)3]2+) as an oxygen quenching indicator exhibited a good linear relationship, fast response time, long-term stability, and enhanced sensitivity to dissolved oxygen after optimizing the sol-gel processing parameters. Fiber-optical microbial sensors for the determination of biochemical oxygen demand (BOD) were described. The sensing films consist of two layers of an oxygen-sensitive fluorescent material, and three different kinds of seawater microorganisms immobilized in poly(vinyl alcohol) sol-gel matrix. The fluorescent properties and the response behaviors of the film were investigated. The effects of temperature, pH and sodium chloride concentration on the sensing films were studied as well. For low biochemical oxygen demand, the film of sieved bacteria from seawater was superior in respect of sensitivity and is expected for further development.
2006 Vol. 26 (01): 15-18 [Abstract] ( 1013 ) PDF (508 KB)  ( 395 )
19 Spectral Properties of Energy Transfer in Doubly Doped Polymer Electroluminescence
ZHANG Ting1, XU Zheng1，2, TENG Feng1, QIAN Lei1, WANG Yong-sheng1, XU Xu-rong1*
The authors report a cascade energy transfer based on the long-range dipole-dipole Frster energy transfer between polymer and two fluorescent dyes in solid thin films. The authors studied the fabrication and emission characteristics of a new doubly doped system for color purity and energy transfer efficiency, in which two fluorescent dyes, i.e. TPB and Rubrene were doped into PVK. In the blend film, PVK acted as the energy donor, Rubrene as the fluorescent dye, and the assistant dopant TPB was used to facilitate the energy transfer from PVK to the dye Rubrene. Orange emission comes from Rubrene via a cascade energy transfer from PVK to TPB and then from TPB to Rubrene.
2006 Vol. 26 (01): 19-22 [Abstract] ( 1067 ) PDF (459 KB)  ( 392 )
23 Study of Color-Changing Device Controlled by Frequency and Its Mechanism
ZHANG Fu-jun1, XU Zheng1, 2, 3*,TENG Feng1, WANG Li-wei1, LIU Ling1, MENG Li-jian2
Absorption is the underlying reason for the change in luminescence traits. And the lifetime influences the absorption in turn. This is a common law not only suitable for photoluminescence but also for other types of luminescence. In field emission display, two kinds of luminescence center have dramatically dissimilar lifetimes, which are co-doped in the same material. The spectrum changes with excitation frequency. Tuning color comes into reality in the same materials. The experiment proves that this law has something to do with lifetime, but has nothing to do with the way of excitation and the reasons for abruptly quenching.
2006 Vol. 26 (01): 23-26 [Abstract] ( 1091 ) PDF (513 KB)  ( 374 )
27 Photoluminescence Properties of Nanocrystalline A3(VO4)2:Eu(A=Mg, Ca, Sr and Ba)
FU Xiao-yan1, NIU Shu-yun1*, ZHANG Hong-wu2, XIN Qin2
A series of europium doped alkali earth orthovanadates were prepared by Pechini-type sol-gel. The powders were characterized by transmission electron microscopy (TEM), infrared spectrum (IR) and photoluminescence (PL). The results of TEM show that high-quality nanopowders with controlled particle size about 50 nm were prepared. The relation between alkali earth ions and luminescence properties was observed from the results of luminescence spectra. Due to the similar ion radius of Ca2+ ions and Eu3+ ions, Ca3(VO4)2:Eu powders exhibit the strongest emission intensity among the four kind of phosphors.
2006 Vol. 26 (01): 27-29 [Abstract] ( 1070 ) PDF (461 KB)  ( 335 )
30 Synthesis and Characterization of Phenyl-Acetylmethylene Sulfoxide Complexes with Light Rare Earth and Fluorescence Spectrum of Eu(Ⅲ) Complex
LI Wen-xian, WANG Hong-sheng, QI Qi-ge, ZHANG Rui-ping
Five solid complexes of phenyl-acetylmethylene sulfoxide(L) with light rare earth(La, Pr, Nd, Sm, Eu) were synthesized and characterized. Elemental analysis and molar conductivities show that the complexes have a composition of RE(ClO4)3·L5·2H2O; two ClO-4 anions coordinated with rare earth ions and the other did not. IR spectra suggested that the ligand coordinated with RE3+ by oxygen atom in sulfinyl group, and the oxygen atom in carbonyl group did not bond. The phosphorescence and 1H NMR and TG-DTA of the ligand and complexes were determind. Fluorescence spectra of Eu(Ⅲ) complex with the sulfoxide indicated that the complex has no symmetrical center. All the complexes have good solubility.
2006 Vol. 26 (01): 30-32 [Abstract] ( 1011 ) PDF (370 KB)  ( 382 )
33 FTIR Spectroscopic Studies of Hydration Effect on the Molecular Structure of Polyether Urethane
LIU Zhi1, LIU Xin-hai2, ZHAO Ying2, SUN Xian-yu1, WENG Shi-fu1, XU Duan-fu2, WU Jin-guang1*
The interaction between water molecules and the polar groups in linear polyether urethane was studied by FTIR and subtraction spectroscopy technique. Direct proofs of the combining of water molecule and carbonyl group were obtained. The reorganizations of the ether linkage, carbamate, and carbon-hydrogen chain after hydration were also observed. These results suggest that the FTIR and subtraction spectroscopy technique could be a useful tool to investigate the hydration mechanism of polymer materials.
2006 Vol. 26 (01): 33-36 [Abstract] ( 1033 ) PDF (526 KB)  ( 399 )
37 The Measurement of the Ratio of Primary Hydroxyl Group to Second Hydroxyl Group in Polyether Polyol by Near Infrared Spectrum
ZHANG Jing1, 2, 3,XU Xiao-xuan1, 2,WU Zhong-chen1, 2, YANG Ren-jie1, 2, ZHANG Cun-zhou1, 2
The method of near infrared spectrum, combined with derivative spectrum and multiple linear regression was applied to measure the ratio of primary hydroxyl group to second hydroxyl group in polyether polyol. The authors obtained good predictive results by using the method in this experiment. The work is very helpful for the on-line measurement of polyether polyol.
2006 Vol. 26 (01): 37-39 [Abstract] ( 1463 ) PDF (321 KB)  ( 351 )
40 Structural Study on the Transparency of Cross-Linked Polyester Polyurethane
LIU Xin-hai1, LIU Zhi2, SUN Xian-yu2, LIN Yang2, ZHAO Ying1, WENG Shi-fu2, XU Duan-fu1, WU Jin-guang2*
The polyurethane material with cross-linked structure was synthesized using half pre-polymerization method. IR, UV-Vis, TEM and XRD methods, and physical properties measurements indicate that different moulding temperatures influence the apparent transparence of polyurethane and abrasive performance, and the nature of these changes is related to the conditions of process and chemical reaction which lead to gradual micro-phase separation of the polyurethane molecules with different compositions, resulting in the domain-forming with the size of sub-micro-, micro- and even more than ten micro-meters. Such domains aggregate one another to form particles with different shapes and complicated structures. The increase in the amount and size of these heterogeneous particles, distributed in the medium of transparent polyurethane, is the main cause that brings on an opaque appearance of polyurethane.
2006 Vol. 26 (01): 40-44 [Abstract] ( 1042 ) PDF (685 KB)  ( 361 )
45 The Calibration of Instrument Response Function during Passive FTIR Measurement
ZHANG Li-ming1, ZHANG Lin1, LI Yan1*, WANG Xiao-fei1，２, LIU Bing-ping1，３, REN Yi-bo1, WANG Jun-de1
In order to obtain infrared spectral radiance distribution of some infrared sources, such as spectral radiant flux density, spectral radiant intensity, spectral radiance and spectral irradiance, the instrument response function under different conditions must be known. In the present paper, the calibration of instrument response function during passive FTIR measurement has been discussed. The experimental results illustrate that under different experimental conditions, the instrument response function varies not only with the temperature of the blackbody but also with the signal amplitude received by the infrared instrument. So, during passive FTIR measurement, the temperature and the emission signal amplitude of the source must be observed carefully in order to get satisfactory instrument response function.
2006 Vol. 26 (01): 45-46 [Abstract] ( 178 ) PDF (249 KB)  ( 422 )
47 Passive FTIR Remote Sensing of Gaseous Pollutant in Heated Plume
GAO Min-guang1,LIU Wen-qing1,ZHANG Tian-shu1,LIU Cheng2,LIU Jian-guo1,WEI Qing-nong1,LU Yi-huai1,WANG Ya-ping1,ZHU Jun1,XU Liang1
The principle and techniques of passive remote sensing of gaseous pollutant in heated plume was illustrated and discussed in this paper. The algorithm of radiance spectra and transmittance spectra in measured region was proposed，and the method of retrieving gas concentrations with NLLS fitting algorithm was also proposed. The remote senseing of actual gaseous pollutant of smokestack was done, and the quantitative analysis of SO2 and CO2 was completed.
2006 Vol. 26 (01): 47-50 [Abstract] ( 1571 ) PDF (435 KB)  ( 396 )
51 Automated Recognition of VOCs Using Artificial Neural Networks
LIU Bing-ping1，2, LI Yan1*, ZHANG Lin1, ZHANG Li-ming1, WANG Xiao-fei1，3, WANG Jun-de1
Quantitative analysis of FTIR spectra, which are seriously overlapped in the spectral bands, was studied by artificial neural networks. The optimum network was chosen by a new criterion, i.e. the degree of approximation. After the network was established, two kinds of spectra were resolved. It was demonstrated that accurate results could be obtained when two components were both included. In addition, the unknown spectrum could be identified and quantified. It was showed that the artificial neural network has excellent non-linear ability of solution. Meanwhile, the method provides an efficient approach to the identification and quantification of the unknown samples.
2006 Vol. 26 (01): 51-53 [Abstract] ( 1460 ) PDF (377 KB)  ( 393 )
54 Synthesis and Infrared Spectroscopic Study of 1-D Magnetic Chain Compound Based on [BrBzPy][Ni(dmit)2]
CHEN You-cun, SHU Qing-hai
The synthesis and functional study of one-dimensional free radical-metal chain compound has been a hotspot task in molecule material, especially in composing high TC molecule ferromagnet. A new compound [BrBzPy][Ni(dmit)2] has been prepared and characterized. The crystal structure at room temperature was determined. The crystal is triclinic with space group P21/c，a=0.627 5(1) nm，b=1.743 8(3) nm，c=2.283 9(3) nm，α=90°，β=91.87(1)°，γ=90°，V=2.497(7) nm3，Z=4，Mr=700.57，and Dc=1.863 g·cm-3. The planar [Ni(dmit)2]- is nearly perfect, which shows that it has good conjugate characteristic and is a 1-D magnetic chain compound.
2006 Vol. 26 (01): 54-56 [Abstract] ( 1109 ) PDF (429 KB)  ( 367 )
57 Building Artificial Neural Networks Model on Portable NIR Integrity Wheat Component Measuring Apparatus
JI Hai-yan,WEN Ming, HAO Bin
The quantitative analysis model of protein in integrity wheat was built by three layers back propagation artificial neural networks for portable near infrared (NIR) integrity wheat component measuring apparatus. The structure diagram of integrity wheat component measuring apparatus, light route structure of apparatus and the spectrum of integrity wheat were given in the present paper. The theory of artificial neural network was briefly introduced and the results of quantitative analysis model of protein were given. For calibration set and prediction set, the correlation coefficient was 0.90 and 0.96 respectively; the relative standard deviation is 3.77% and 4.46% respectively. Because of the influence of light route structure, electrical circuit, and integrity sample forms on the measuring apparatus, some nonlinearity exists between the spectral parameters and chemical values. The results of artificial neural networks nonlinear model were superior to linear model.
2006 Vol. 26 (01): 57-59 [Abstract] ( 1665 ) PDF (362 KB)  ( 369 )
60 Fast and Nondestructive Discrimination of Donkeyhide Glue by Near-Infrared Spectroscopy
QU Hai-bin, YANG Hai-lei, CHENG Yi-yu*
Near-infrared (NIR) diffuse reflectance spectroscopy and pattern recognition techniques were applied to develop a fast identification method of a Chinese patent medicine-donkeyhide glue. Samples from different manufactures (eight genuine samples and six counterfeits) were collected, and their NIR spectra were obtained. NIR spectra were pretreated with multiplicative signal correction (MSC) and wavelet transformation to diminish baseline offset. Similarity and Mahalanobis distance methods were separatemy used to qualify donkeyhide glue. For the similarity calculation, spectra of the two real ones were selected as standards, and then others were compared with the standards to obtain the match value. All the samples were rescanned once for the Mahalanobis distance methods, and totally twenty eight spectra were separated into three sets for cross-validation. The two methods can both distinguish the counterfeits of donkeyhide glue successfully. The proposed method is accurate and robust, and could be used in the discrimination of other traditional Chinese medicines.
2006 Vol. 26 (01): 60-62 [Abstract] ( 1383 ) PDF (413 KB)  ( 377 )
63 Sugar Content Prediction of Apple Using Near-Infrared Spectroscopy Treated by Wavelet Transform
YING Yi-bin, LIU Yan-de，FU Xia-ping
Based on wavelet transform (WT) by using the difference in wavelet modulus maxima evolution behaviors between singular signals and random noises in multi-scale space, the near infrared spectroscopic signals of 90 fruit samples were denoised by wavelet transform. The sugar content in intact apple was calculated by stepwise regression method. The result of calibration model after noise filtering was satisfactory. The relative standard error of prediction is reduced to 6.0% from 6.1% of original spectra. It is concluded that wavelet transform is an useful method to eliminate noise of NIR signals, as it makes the final calibration model more representative and stable and robust.
2006 Vol. 26 (01): 63-66 [Abstract] ( 1088 ) PDF (430 KB)  ( 429 )
67 Near Infrared Spectrometry (NIRS) Method for the Determination of Borneol in Sustained-Release Drugs
NI Li-jun, ZHU Jing, ZHANG Li-guo
In order to detect the release profile of borneol in sustained-release preparations, a series of NIRS calibration models were established on the basis of chemometrics and internal relationships between NIRS and analytical concentrations of samples, which contained the same substances as the preparations. Partial least square (PLS) algorithm was used to establish the model for predicting the content of borneol. The effect of spectra types，concentration range of samples, and calibration range on the models and predicting results were investigated. It was found that uhe best calibration models and prediction results can be obtained by using original spectra in the 5 314-7 032 cm-1 region. The models established according to standards’ concentration levels are better than those established without considering concentration levels. Using the model 2 in which calibration standards had medium or high concentration levels, rapid and accurate measurement of borneol released from sustained-release preparation was realized. The results indicated that the method and models provide valuable criteria for developing sustained-release borneol preparations.
2006 Vol. 26 (01): 67-69 [Abstract] ( 1060 ) PDF (385 KB)  ( 359 )
70 Quantitative Analysis of Two-Component Polymer Blends (PEG/PE) by Infrared Spectroscopy
WU Hong, LIN Zhi-yong, QIAN Hao*
The concentration of the component of PEG/PE blends was analyzed quantitatively by infrared spectroscopy. The absorption peak area ratio of the selected mixture peaks used as the calibrating basis for the quantitative analysis was more reasonable than the peak area ratio of the pure peaks. The theoretical equation deducted by Beer-Lamber law was used to establish the working curve to calculate the composition of the responding functional groups in the film of the PEG/PE blends. The characteristic peaks of the crystal can not be selected as the calibrating basis for the quantitative measurement, because the crystallization has a great effect on the intensity of the absorption peaks.
2006 Vol. 26 (01): 70-74 [Abstract] ( 1115 ) PDF (538 KB)  ( 386 )
75 The Catalysis-Oxidation Studies of Formic Acid on Platinum Electrode by Surface-Enhanced Raman Spectroscopy
GU Ren-ao, JIANG Yun, SUN Yu-hua
In the non-aqueous solution and recurring to the confocal Raman system, the authors studied the catalysis and oxidation of formic acid on the surface of platinum electrode utilizing surface-enhanced Raman spectroscopy (SERS). Results showed that the intermediate CO, the oxidized product of HCOOH, was produced first. As the potential moves to positive, the first oxidation wave for CO is observed over 0.1 V. As a result the product of CO counteracts its consumeption, so the Raman intensity and coupling under the certain overlay was not decreased. As the oxidation of CO was expedited, the finally oxidized product CO2 was detected at 0.6 V.
2006 Vol. 26 (01): 75-77 [Abstract] ( 1131 ) PDF (397 KB)  ( 383 )
78 In situ Resonance Raman Spectra of Organic Pigments in Freshwater Cultured Pearls
HAO Yu-lan,ZHANG Gang-sheng*
In situ resonance Raman spectra of Chinese freshwater pearls were collected and analysed systematically with three different excitation wavelengths at λ＝514，633 and 785 nm. At the same time, the Raman spectra of eggshells of Pomacea canaliculata were also collected under the same experimental conditions in order to compare with pearls’ Raman spectra. The conclusions were as follows: (1) Frequency dispersions of Raman spectra of organic pigments were obviously observed in Raman spectra of pearls. In contrast, Raman spectra of organic pigments in eggshells of Pomacea canaliculata showed no frequency dispersion phenomena; (2) It was considered that the organic pigments in pearls were polyacetylenic materials but not carotenoids which was proposed by previous researchers, and the organic pigments in eggshells of Pomacea canaliculata were carotenoids; (3) The conjugated CC number of polyacetylenic material in pearls was calculated to be about 10 and 16, and the conjugated CC number of carotenoid in eggshells of Pomacea canaliculata was about 13 based on the Raman shifts caused by conjugated CC double bonds.
2006 Vol. 26 (01): 78-80 [Abstract] ( 1692 ) PDF (379 KB)  ( 390 )
81 Synchronous Fluorescence and Raman Spectroscopy Study on the Interaction of Pulsed Electric Field (PEF) and Bovine Serum Albumin (BSA)
LI Le-jun, CHEN Shu-de*, QIAO Deng-jiang
The interaction of pulsed electric field (PEF) and bovine serum albumin (BSA) was studied by synchronous fluorescence and Raman spectroscopy. The results of synchronous fluorescence showed that pulsed electric field exerted its effects on the emission fluorescence spectrum and reduced the fluorescence intensities of the tyrosine and tryptophan side chains. The results of Raman spectroscopy verified this. These two experiments indicated that PEF exposure changed the microenvironments of the two aromatic amino acids, which were located in the active parts of BSA, and further indicated the conformational changes of the proteins, and the change in its biological functions.
2006 Vol. 26 (01): 81-85 [Abstract] ( 1666 ) PDF (518 KB)  ( 385 )
86 Calculation of Optical Parameters and Investigation of Luminescence Spectra in Sm3+ Doped Borate Glasses
YANG Dian-lai1, LIN Hai1*, HOU Yan-yan1, XU Long-quan1, ZHAI Bin1, BAN Li-xia1, LIU Gui-shan1, TANG Nai-ling1, WANG Shu-chuan1, MA Tie-cheng1, WANG Xiao-jun２, LIU Xing-ren２
In the present paper, Sm3+ doped borate glasses (LBLB) with high effective visible fluorescence emission have been synthesized. The absorption and fluorescence spectra of this glass were measured and analyzed. The absorption spectra were fitted by J-O theory, and the intensity parameters Ωt=(2, 4, 6) were found to be 6.81×10-20, 4.43×10-20, and 2.58×10-20 cm2, respectively, then the relative intensity of spectral lines of every energy level transition, radiative transition probabilities, radiative lifetimes, and fluorescence branching ratio were calculated. Under the excitation of UV light, Sm3+ doped borate glasses (LBLB) emit bright salmon pink light. The excitation spectra indicate that argon laser is an effective excitation source in Sm3+ doped LBLB glasses.
2006 Vol. 26 (01): 86-89 [Abstract] ( 1464 ) PDF (369 KB)  ( 383 )
90 Raman Scattering Study of DL-Alanine
GONG Yan,WANG Wen-qing
Studies of Raman vibration spectra are useful to obtaining information on biomolecular crystals. The cell dimensions of the L- and DL-alanine crystals are nearly identical, and both structures belong to the orthorhombic system, but the space group is P212121 for the L-isomer, and Pna21 for the racemate crystal. The Raman spectrum of L-alanine has been measured by many authors. The present work is focusing on the Raman scattering study of DL-alanine powder. Based on the analysis of the differences between DL-alanine and L-alanine Raman spectra, the authors obtained indispensable information on hydrogen bond and the motion of the molecular conformation in alanine crystals.
2006 Vol. 26 (01): 90-93 [Abstract] ( 442 ) PDF (536 KB)  ( 516 )
94 The Three-Dimension Spectral Subtraction Fluorescence to Check Adulteration of Diesel Oil by 120# Solvent Naphtha
YANG Ren-jie1，3, XU Xiao-xuan1, SHANG Li-ping2, XU Jia-lin1, ZHANG Cun-zhou1
The characteristics of a adulterated sample of diesel oil by 120# solvent naphtha were studied with three-dimension spectral subtraction fluorescence technique, and it is shown that the technique could determine quickly whether there is a adulterated sample of 120# solvent naphtha in diesel. At the same time, by measuring the volume of three-dimension spectral subtraction fluorescence graph, the authors found that this total volume is directly related to the concentration of the adulterant present in the sample. The study is important for us to analyse whether there is a adulterated sample of 120# solvent naphtha in diesel, and is of significance for us to maintain the stability of market.
2006 Vol. 26 (01): 94-96 [Abstract] ( 1090 ) PDF (631 KB)  ( 407 )
97 Study on the Chemical Reaction of DNA with Congo Red
CHI Yan-hua1, ZHUANG Jia1, XUE Qi-bin1, LI Ke-an2
The interaction of deoxyribonucleic acid(DNA) and Congo red (GGH) was investigated by UV-Vis spectrophotometry in Tris-HCl solution (pH 4.56). When DNA was added into GGH solution, the color of the system changed from red to purple, which indicated the formation of the DNA-GGH complex. The maximum absorption of the complex is at 600 nm. The molar absorptivity measured at this wavelength ε=1.41×105 L·cm-1·mol-1, the maximum binding number is n=32，and the detection limit is c＝8.04×10-8mol·L-1. The basic reaction condition of best pH value, time, and temperature, and the interference of different materials on the system were also studied. The ionic strength could affect the absorption of the system. The interaction of small molecule and DNA, the molecule structure, and the relationship between the molecule conformation and the distribution of electron cloud were studied.
2006 Vol. 26 (01): 97-101 [Abstract] ( 404 ) PDF (625 KB)  ( 357 )
102 Ultraviolet Transmission Spectra of BCxN Thin Films
WANG Yu-xin1, 2, FENG Ke-cheng1, LI Ying-ai2, LI Wei-qing2, LIU Li-hua2, ZHAO Chun-hong2, ZHAO Yong-nian2
BCN, BC2N and BC3N thin films with transmission increasing properties in the ultraviolet region were deposited by RF magnetron sputtering with different sputtering power (80-130 W). Fourier transform infrared absorption and X-ray photoelectron spectroscopy results suggested that the films were atomic-level hybrids composed of B, C and N atoms. The compositions and transmission increasing properties of samples in the ultraviolet region were strongly influenced by sputtering power, which determined the transmission increasing properties in the ultraviolet region by changing compositions. And the lower the atomic number of C in the thin films, the better the transmission increasing properties in the ultraviolet region. The BCN thin films deposited at the sputtering power of 110 W possessed the lowest atomic number of C and the best transmission increasing properties in the ultraviolet region. And the increase in average transmissivity from 200 to 350 nm was about 40% compared with glass.
2006 Vol. 26 (01): 102-105 [Abstract] ( 1037 ) PDF (523 KB)  ( 374 )
106 Synthesis of 4-(Benzeneazo) Salicyladelhyde Hydrazones and Study on Their Spectral Properties
WU Bo-wan,ZHANG Bing,YU Xin-qiao,LIU Jian-ning
4-(benzeneazo) salicyladelhyde was synthesized with aniline and salicylaldehyde. Benzoylhydrazine and p-hydroxybenzoylhydrazine were synthesized using the reaction of ethyl benzoate and methyl p-hydraxy benzoate with hydrazine hydrate. Four novel 4-(benzeneazo) salicyladelhyde hydrazones were synthesized using the reaction of 4-(benzeneazo) salicyladelhyde with benzoylhydrazine, p-hydroxybenzoylhydrazine, phenylhydrazine, and isonicotinyl hydrazine respectively. IR, UV and the fluorescence spectrum of 4-(benzeneazo) salicyladelhyde hydrazones were studied.
2006 Vol. 26 (01): 106-108 [Abstract] ( 234 ) PDF (342 KB)  ( 415 )
109 Microemulsion Sensitized Fluorophotometric Determination of Protein with Probe of Phenylfluorone-Molybdenum(Ⅵ) Complex
WEI Qin, LI Yan, DUAN Cai-hong, GUO Gui-xiang, DU Bin
The fluorescence spectral behavior of interaction of phenylfluorone(PF)-Mo(Ⅵ) and protein was investigated in Triton X-100 microemulsion medium at pH 2.0. A novel method for the determination of protein using phenylfluorone (PF)-Mo(Ⅵ) as a fluorescence spectrum probe was developed. Excitation and emission wavelengths are 465 and 525 nm, respectively. The effective factors and the optimum conditions have been studied, and the reducing value of fluorescence intensity is in proportion to the concentration of proteins in the range 0-6.00 μg·L-1 for bovine serum albumin, 0-4.00 μg·L-1 for human serum albumin, 0-5.00 μg·L-1 for ovalbumin, and 0-4.00 μg·L-1 for lysozyme. The Triton X-100 microemulsion was efficiently used to enhance the sensibility and stability of the system, and the limits of detection are 5.4, 5.2, 1.5 and 8.2 ng·L-1, respectively. Most of foreign substances do not interfere with the determination, and this method has good selectivity and high sensitivity. It has been applied to the determination of proteins in the urine samples with satisfactory results.
2006 Vol. 26 (01): 109-112 [Abstract] ( 1549 ) PDF (500 KB)  ( 384 )
113 Synchronous Fluorimetric Determination of the Residues of Three Quinolones in Eel by Partial Least Squares
ZHANG Guo-wen1, NI Yong-nian2*
In the present paper, the synchronous fluorimetric spectra of norfloxacin, lomefloxacin chlorhydric acid, and levofloxacin lactate with Δλ=190 nm in a B-R buffer medium of pH 2.87 were measured, and the partial least squares (PLS) method was applied to the quantitative resolution of the seriously overlapped fluorimetric spectra of these compounds. The linear ranges for norfloxacin, lomefloxacin chlorhydric acid, and levofloxacin lactate are 0.016-0.40 μg·mL-1, 0.01-0.336 μg·mL-1 and 0.01-0.336 μg·mL-1, respectively. The limits of detection are 0.012 6 μg·mL-1 for norfloxacin, 0.006 μg· mL-1 for lomefloxacin chlorhydric acid, and 0.007 2 μg·mL-1 for levofloxacin lactate. The analytical results by PLS were compared with principal components regression (PCR) and classical least squares (CLS), and this method was applied to the determination of these three compounds in eel samples with satisfactory results.
2006 Vol. 26 (01): 113-116 [Abstract] ( 1689 ) PDF (486 KB)  ( 374 )
117 Simultaneous Quantitative Analysis of Three Kinds of Phenols by Elman Recurrent Neural Network
GAO Ling, SHI Jun-xian, REN Shou-xin*
Elman recurrent neural network ( ERNN) was applied to study the simultaneous quantitative analysis of seriously overlapped spectra of a p-nitrophenol, o-nitrophenol and 2,4-dinitrophenol system. The multivariate linear regression (MLR) method was also applied in this study for comparison. Two programs (PERNN and PMLR) were designed to perform the calculations. By optimization, the structure and parameters of Elman recurrent neural network were defined. The relative standard errors of prediction (RSEP) for all components with ERNN and MLR were 3.1% and 2 027.3%, respectively. Experimental results showed the method to be successful even where there was a severe overlap of spectra. The ERNN method is a valuable tool in solving the minimum problem and improving the convergence rate, and can be used to analyze the whole spectra rather than just picking out a few characteristic values. The method provides a new way of simultaneous determination of severely overlapped molecular spectra without prior separation.
2006 Vol. 26 (01): 117-120 [Abstract] ( 754 ) PDF (436 KB)  ( 365 )
121 Determination of Nucleic Acids Using Toluidine Blue as a Fluorescence Probe
GUO Liang-qia,YE Fang-gui,LIN Xu-cong,XIE Zeng-hong*
A new fluorimetric method has been developed for the determination of deoxyribonucleic acid (DNA) with toluidine blue(TB) as a fluorescence probe. It is based on the fluorescence quenching of toluidine blue in the presence of DNA. In Tris-HCl buffer solution (pH 8.5), the calibration graph was linear over the range 0.10-6.00 μg·mL-1 for ctDNA, and the detection limit was 27 ng·mL-1. The result of the determination of DNA of camphor tree’s leaf by this method was satisfactory.
2006 Vol. 26 (01): 121-124 [Abstract] ( 1631 ) PDF (542 KB)  ( 361 )
125 Study on the Interaction of Tetrabromofluorescein and DNA
BIAN Wei1, WEI Yu-xia2, WEI Yan-li2, DONG Chuan2
The interaction of tetrabromofluorescein (TBF) and DNA was studied by the fluorescence and SS-RTP. The effect of the ion strength and ethanol on the fluorescence spectra of TBF in the presence of DNA and absence of DNA was investigated. In addition, the effect of pH on the SS-RTP spectra of TBF was also examined. The quenched constant was 719.74 and 880.22 in the absence and presence of DNA respectively. Finally, the interaction mode between TBF and DNA was discussed from the fluorescence quenched and phosphorescence polarized experiments.
2006 Vol. 26 (01): 125-129 [Abstract] ( 1467 ) PDF (540 KB)  ( 396 )
130 Spectral Analysis and Study of the Microsome Cytochrome P450 Aromatase of Thais clavigera
HAN Ya-li1,DENG Rui-peng2,ZHOU Xiao-peng2
The microsomes were prepared from the viscera masses of Thais clavigeras. It is well known that there are some main components in microsome cytochrome P450 aromatase, including cytochrome P450, cytochrome b5 and NADPH-cytochrome P450 reductase. So the contents of cytochrome P450 and cytochrome b5, and the activity of NADPH-cytochrome P450 reductase were determined by Shimadzu UV Visible spectrophotometer. And the microsomal proteins were analysed by SDS-PAGE. All the results indicated that there exists P450 arom in the T. clavigeras.
2006 Vol. 26 (01): 130-133 [Abstract] ( 1002 ) PDF (645 KB)  ( 326 )
134 Study on the CD and ORD of the Crystal NaClO3
TAO Wei-dong1，3, ZHANG Hui2, FANG Xue-ming2, WANG Fang2, ZHANG Zi-fang2, BAI Gui-ru1
Chiral isotropy material should be obtained in order to manufacture chiral optical waveguide. In the present paper, a chiral crystal of NaClO3 was grown from water solution by standard rocking techniques. Crystal incising and optical polishing were done and a transparent 10.9 mm× 8.2 mm× 4.7 mm crystal NaClO3 was obtained. Along the six directions perpendicular to the surface of the crystal NaClO3, its circular dichroism and UV spectra were collected, and at the same time its optical rotatory dispersion was measured by a self-fabricated ORD apparatus. It was approved by our experiment that the CD, UV spectrum and the optical rotatory dispersion of the crystal NaClO3 were isotropic, which is not the same as those of quartz.
2006 Vol. 26 (01): 134-136 [Abstract] ( 995 ) PDF (429 KB)  ( 363 )
137 Study on Determination of Trace Nitrite and Reaction Mechanism by Two-Wavelength Negative Absorption-Catalytic Spectrophotometry
ZI Yan-qin, LU Hao-miao
A new method was proposed for the determination of trace nitrite by two wavelength negative absorption catalytic spectrophotometry based on the catalysis of nitrite on the oxidation fading reaction of acridine orange by potassium bromate in phosphoric acid medium. The additive value of negative absorbances at two wavelengths was linear to the nitrite concentration in the range of 1.0×10-5-5.0×10-7 mol·L-1. The method has been used to the determination of nitrite in environment water sample with satisfactory result.
2006 Vol. 26 (01): 137-139 [Abstract] ( 2792 ) PDF (332 KB)  ( 397 )
140 Determination of Trace Elements Hg and Rh in Gelatin by Inductively Coupled Plasma Emission Spectrometry ——Applying MSF Model to Improve the Precision and Detection Limit
DU Bao-an1, YANG Yu-hua2, LI Zheng-ping1
Using ICP-AES, the method was developed to quantitatively determine the trace elements Hg and Rh in gelatin for the first time. The unknown samplers were processed with the wet digestion method. Multiple trace elements in gelatin could be quantitatively determined by ICP-AES at the same time. Applying the MSF model, the method to correct the spectral interference and the background was discussed. The result’s precision and detection limit could be greatly improved by MSF model. The results of the experiment showed that the method features high accuracy, rapidity, high performance and a wide linear dynamic range, and the results were very satisfactory.
2006 Vol. 26 (01): 140-143 [Abstract] ( 138 ) PDF (490 KB)  ( 429 )
144 AAS Method for Determination of Manganese in Fluorspar
CHEN Zong-hong,WEN Wei-jiang,JIANG Hai-ning
An AAS method for the determination of manganese in fluorspar was established for the inspection of export product. The fluorspar sample was treated with HF, then fumed with HClO4. After cooling, the residue was dissolved by adding HCl and boric acid with gentle heating. The series of standards for calibration were prepared by adding the same amount of Ca for matrix matching. The linear range of the determination of manganese is 0.09-2.5μg·mL-1. The determination limit of the method for Mn in fluorspar was 0.001 0%. Analytical results of real samples with various levels of content by the proposed method were in good agreement with those by the ISO method of spectrophotometry. The method features good precision, easy operation, and convenience for application.
2006 Vol. 26 (01): 144-146 [Abstract] ( 1027 ) PDF (375 KB)  ( 337 )
147 Studies of Complexing Action Mechanism in the Indirect Determination of Arginine by FAAS with ZnS
LIU Wen-han, ZHANG Dan, ZHENG Jian-zhen, LI Dan, MA Chun-an
Each state of arginine and zinc ion in aqueous solution under different pH conditions was calculated by computer, giving out the scattergram. After the investigation, the mechanism of complexing action in indirectly determining arginine by flame atomic absorption spectrometry with ZnS was studied in terms of the influence of solution pH. It is with different state of arginine and zinc ion in aqueous solution in differential pH that the response peak with pH in given conditions is obtained. The reason for forming the left peak is different from the reason for forming the right peak. The soluble complexing ion is composed of +1 valence arginine Arg++- and Zn(OH)2. The theoretical analysis from computing and scattergram dovetails very well the data determined from the experiments. The structure of complexing ion is[HNCH(NH+3)NH(CH2)3CH(NH+3)COO]2Zn(OH)2.
2006 Vol. 26 (01): 147-150 [Abstract] ( 1871 ) PDF (433 KB)  ( 372 )
151 Determination of Trace Selenium in Edible Fungi with Graphite Furnace Atomic Absorption Spectroscopy
TIE Mei1，2,ZHANG Wei2 ,LI Jing２, JING Kui２,ZANG Shu-liang2*,LI Hua-wei3
In the present article, samples were digested by a quartz high-pressure digestion pot, reducing the loss of selenium in digestion. The content of selenium in edible fungi was determined by using graphite furnace atomic absorption spectroscopy, and the results showed that when the content of selenium in edible fungi was determined by using 1% Ni(NO3)2 as a matrix modifier, ashing temperature of 500 ℃, and atomization temperature of 2 500 ℃, and rectifying background by deuterium light, the recovery was in the range of 92.1%-115.5%, the relative standard deviation of the method was 1.28%, and the limit of detection was 15.8 μg·L-1. The method was suitable for the determination of trace selenium in edible fungi with the advantages of being simple, rapid, sensitive, stable and accurate etc., and the results were satisfactory.
2006 Vol. 26 (01): 151-153 [Abstract] ( 1462 ) PDF (412 KB)  ( 400 )
154 Determination of 8 Elements in Elaeagnus Mollis by AAS
XIE Su-jing
Eight kinds of trace elements of Elaeagnus mollis were determinated with flame atomic absorption spectrophotometry method. The result shows that there is evident difference of the trace elements in different organs and growing stages. The trace element is plentiful in this kind of plant, specially in root, leaf and seed.
2006 Vol. 26 (01): 154-155 [Abstract] ( 1039 ) PDF (261 KB)  ( 369 )
156 Comparative Study on Trace Elements in Flos Chrysanthemi and Flos Chrysanthemi Indici
CHENG Cun-gui1,LI Dan-ting1,LIU Xing-hai2, HONG Qing-hong1，3
The contents of elements Ni，Zn，Mn，Cu，Mg，Fe，Ca and Pb in flos chrysanthemi and flos chrysanthemi indici were determined by flame atomic absorption spectrometry. The recovery rates obtained by standard addition method were between 94.20% and 110.50%, and the RSDs were lower than 4.12%. The results of the determination show that flos chrysanthemi is rich in the inorganic elements such as Ni，Zn，Fe and Pb, and flos chrysanthemi indici is rich in the inorganic elements such as Mn and Ca. The results will provide scientific data for the study on the elements in flos chrysanthemi and flos chrysanthemi indici and on their relativity of efficacy of medicine.
2006 Vol. 26 (01): 156-158 [Abstract] ( 1591 ) PDF (370 KB)  ( 404 )
159 Analysis of Films by X-Ray Fluorescence Spectrometry
HAN Xiao-yuan, ZHUO Shang-jun*, WANG Pei-ling
As a quantitative method of film sample, the X-ray fluorescence (XRF) technique has been used extensively because it is non-destructive, fast and accurate. Moreover it could determine the concentration and thickness of film sample simultaneously. A review was given of the study on the quantitative method of films by X-ray fluorescence spectrometry, in which the theoretical calculation of fluorescence intensity, the matrix effects and the methods for their correction, the sources of errors, the software for quantitative analysis, and the application of the method were summarized and discussed. New development and application of films characterization by X-ray fluorescence spectrometry were also expected. Because the similar calibration specimen for film sample is difficult to prepare and the fundamental parameter method could quantitatively analyze film samples even if only the pure element specimen is employed, the fundamental parameter method is studied extensively. The fundamental parameter method was introduced mainly in the present article, including the fundamental parameter equations to calculate the theoretical intensity of fluorescence, the source of error in calculation, and the software for analysis.
2006 Vol. 26 (01): 159-165 [Abstract] ( 1588 ) PDF (679 KB)  ( 411 )
166 Study on the Compositions in the Interface of Corrosion Inhibition Membrane／Copper Plating Layer／Iron Substrate by Depth Etching and Photoelectron Spectroscopy
FENG Shao-bin1, SHANG Shi-bo2, FENG Li-ting1, LIU Qing1，ZHANG Jing-wei3, LI Zong-hui3
In order to explore the reason for the weak bond intensity between pyro-phosphate copper plating layer and iron substrate, spectrum technology was adopted. The compositions of various elements in the perpendicular interface were analyzed. The effect of surface roughness in the metal substrate on various elements distribution was discussed. According to etching time, the membrane layer was divided into three portions: surface layer with nitrogen and oxygen content decreasing quickly, mesosphere of basic fixed composition, and mix disturbing layer with substrate element appearing and occupying a half thickness. Through analyzing oxygen content in the mix layer, it was concluded that the oxygen layer in the interface of copper layer／iron substrate was the main cause of influencing the bond intensity between the plating layer and substrate.
2006 Vol. 26 (01): 166-169 [Abstract] ( 1695 ) PDF (477 KB)  ( 407 )
170 The Application of X-Ray Diffraction in the Study of Urinary Stones
OUYANG Jian-ming
Urolithiasis is a common disease throughout the world. The accurate analysis of chemical composition and phases of urinary stones is the base of understanding the mechanism of formation of urolithiasis. X-ray diffraction (XRD) is one of the most important methods used for the study of urinary stones. It is reliable when used for qualitative analyses and is accurate when used for quantitative analyses. In addition, XRD has the advantages such as speediness, briefness and high sensitivity, as well as simultaneous detection of many compositions. In the present paper, the research progress was reviewed in the qualitative and quantitative analyses of urinary stones by XRD and by the combined methods of XRD with other techniques such as X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), and proton induced X-ray emission (PIXE) etc.
2006 Vol. 26 (01): 170-174 [Abstract] ( 1035 ) PDF (667 KB)  ( 382 )
175 Influence of Sun Radiation on Optical Properties of Liquid Crystal Display Device
HUANG Chong, ZHOU Xue-ping, LIN Xu-sheng, OUYANG Yan-dong
Sunlight affects mainly the light stability and life of liquid crystal display device, which will lead to rapid aging of the device. By measuring the optical properties of liquid crystal display devices radiated with different time by spectrophotometer, the influences of long time sunlight radiation on the optical properties of the device were studied, and the changes of its optical properties were analyzed. The results indicate that structural and optical properties of liquid crystal slices of calculator LCD (B group) and telephone LCD (C group) are similar and the qualities are relatively good, while the aging problem of personal computer LCD (A group) liquid crystal slice is more serious than those of B and C groups, moreover, the qualities of liquid crystal slices in A group are worse. The structural and optical properties of liquid crystal display device will change accordingly after long time sunlight radiation. The surface of liquid crystal display device will become yellow and nigrescent, and the spectrum transmission properties will decline markedly, which is related to liquid crystal materials and manufacturing techniques.
2006 Vol. 26 (01): 175-177 [Abstract] ( 1935 ) PDF (396 KB)  ( 375 )
178 Analysis of Spectral Properties of Car Solar Films
HUANG Chong, ZHOU Xue-ping, LIN Xu-sheng, OUYANG Yan-dong
A dual-beam ultraviolet/visible spectrometer (UV-Vis 8500) automatically controlled by computer was used to measure qualitatively and to analyze the spectral properties of car solar films of a certain brand in the market. The experimental results indicate that transparency characteristics of the ordinary series of solar films are well, but their violet insulation and heat insulation properties are moderate, and moreover, their thermal-proof property is not ideal. The heat insulation, violet-proof and transparency properties of the anti-crack series are all in normal level. The heat insulation and transparency properties of anti-crack and anti-wear series are moderate, however, their violet insulation characteristics are better than those of other series mentioned above. For the super front film, its transparency property is excellent, moreover, its violet insulation and heat insulation properties are quite well. In general, it can be concluded that the super front series are the best car solar films.
2006 Vol. 26 (01): 178-181 [Abstract] ( 367 ) PDF (379 KB)  ( 466 )
182 A Novel Method for the Determination of Redshifts of Normal Galaxies by Non-Linear Dimensionality Reduction
XU Xin1,2, WU Fu-chao1, HU Zhan-yi1, LUO A-li2
It is difficult to determine the redshifts of normal galaxies (NG) from their spectra because of their common weak absorption property. In the present work, a novel method is proposed to effectively deal with this issue. The proposed method is composed of the following three parts: At first, the wavelet transform coefficients at the fourth scaling are experimentally found to be appropriate and used as our features to represent the absorption information from NG absorption lines, break points, and absorption bands. Then, the features are mapped by a non-linear method, LLE(locally linear embedding)，onto an one-dimensional manifold in the 3D space; Finally, the NG redshifts are obtained by the nearest neighborhood technique from the redshift distribution on the manifold. Besides, the proposed method is compared with widely used PCA method in the literature with SDSS database, and is shown to be more accurate for the redshifts determination.
2006 Vol. 26 (01): 182-186 [Abstract] ( 1077 ) PDF (587 KB)  ( 474 )
187 Determination of Metallic Elements in Different Parts of Salvia Miltiorrhiza by FAAS
SHEN Xiao-fang,ZHANG Yong*,QIN Xue-mei
The root, stem and leaf of Salvia miltiorrhiza were digested with HNO3-HClO4(4∶1), and the contents of five metallic elements such as K, Cu, Zn, Fe and Mg were detected by flame atomic absorption spectrophotometry. The recovery ratio by standard addition is 99.7%-104.4% and RSD is less than 2%. It was found that the content sequence of metallic elements is as follows: K＞Mg＞Fe＞Zn＞Cu. K, Cu, Zn, Fe and Mg in the leaf are clearly richer than those in the root and stem. The content ratio of Zn to Cu is relatively lower than that in the terrestrial angiosperms. The results provide a useful data for discussing the relationship between the contents of these elements in Chinese medicinal herb Salvia miltiorrhiza and the medical effects. Furthermore they also provide a data for the distribution of these elements in different parts of Salvia miltiorrhiza.
2006 Vol. 26 (01): 187-188 [Abstract] ( 1700 ) PDF (317 KB)  ( 416 )

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