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2004 Vol. 24, No. 10
Published: 2004-10-26

 
       光谱学与光谱分析
1153 Measurement and Analysis of Optical Constants of Bulk ZnSe in THz Region
XU Xin-long1, 2, WANG Xiu-min1, 2, LI Fu-li2,ZHANG Xi-cheng3, WANG Li1*
In the present paper the authors measured and analyzed the dispersion and absorption characteristics of the bulk ZnSe(110) in THz region using transmission THz time domain spectroscopy. After fitting the experiment data according to the Drude theory, the authors obtained the low-frequency dielectric constant and the high-frequency dielectric constant. The authors also observed the absorption by multi-phonon processes.
2004 Vol. 24 (10): 1153-1156 [Abstract] ( 550 ) PDF (990 KB)  ( 411 )
1157 Crystal Growth and Spectral Parameter Computation of Yb:YAG
ZHANG Qing-li, XIAO Jing-zhong, SUN Dun-lu, WANG Ai-hua, YIN Shao-tang
In this article, a good-quality crystal Yb:YAG was grown by pull method, and its absorption spectrum of 200-3 000 nm was measured at room temperature. Its absorption of 200-300 nm is from the host YAG, and there exists only the characteristic absorption of Yb3+ in the range of 390-3 000 nm. Judd-Ofelt theory computation indicates that the absorption and emission oscillator strengths of electric dipole of (24 at%)Yb:YAG are 3.58×10-6 and 4.77×10-6, respectively,and the absorption and emission transition probabilities are 879 and 1 171/s respectively. As for magnetic dipole, the absorption and emission oscillator strengths are 3.32×10-7 and 4.43×10-7 respectively, and the absorption and emission transition probabilities are 82 and 109/s respectively. The lifetime of the energy level 2F5/2 is 781 μs.
2004 Vol. 24 (10): 1157-1160 [Abstract] ( 1129 ) PDF (1230 KB)  ( 597 )
1161 Preparation of Ge/SiO2 Nanometer-Crystal Doped Glass and Study of Its Photoluminescence Property
GU Xiao-tian1,FENG Yu-ying1,JIN Tong-shun1,YU Zhong-qing2
Ge/SiO2 nanometer-crystal doped glass was prepared through sol-gel method. The gel was synthesized through the hydrolysis of a complex solution of Si(OC2H5)4 and Ge(OC2H5)4. The product gel was then heated at 700 ℃ in H2. Ge crystals appeared after the heating-reducing process. X ray diffraction analysis showed that there were Ge cubic crystals formed in the gel glass. The photoluminescence spectroscopic analysis showed that the Ge/SiO2 fluorescence peaked at 576 nm with excitation wavelength of 494 nm. By using the Brus quantum confinement model, the fluorescence peak energy suggested that the mean size of Ge crystal was about 3 nm.
2004 Vol. 24 (10): 1161-1163 [Abstract] ( 1028 ) PDF (845 KB)  ( 346 )
1164 Spectral Studies of Nanosized LnVO4:Eu(Ln= La, Gd, Y)
ZHANG Hong-wu1,FU Xiao-yan3,NIU Shu-yun3,HAN Yan3,SUN Gong-quan1,XIN Qin1,2*
Nanosized LnVO4:Eu (Ln=La, Gd, Y) with diameters ranging from 20 to 50 nm were synthesized by complex sol-gel technique. The structures and spectral properties of LnVO4:Eu were studied by X-ray powder diffraction (XRD), Fourier transform (FT-IR) spectroscopy, luminescence spectra and ultraviolet spectroscopy (UV). The experimental results show that YVO4:Eu and GdVO4:Eu have similar spectral properties because they both have the structure of xenotime, while the structure of LaVO4:Eu belongs to monazite, whose symmetry is inferior to the former vanadates. Consequently the spectral properties of LaVO4:Eu are obviously different from the other two luminescence materials, as the peaks of infrared spectrum and emission spectrum become wider and the number of peaks in UV-Vis spectrum increases.
2004 Vol. 24 (10): 1164-1167 [Abstract] ( 1587 ) PDF (903 KB)  ( 392 )
1168 The Luminescence Characteristic of a New Novel Coprecipitate Rare Earths Complexes
BAI Feng1, DENG Zhen-bo1*, XU Zheng1, GAO Xin1,LI Yong2, XU Yi-zhuang2, WU Jin-guang2
A new novel coprecipitate rare earths complexes La0.6Eu0.4(BSA)3phen has been synthesized and was chosen as the emitter material in the organic electroluminescent devices: ITO/PVK: La0.6Eu0.4(BSA)3phen/Alq/Al where PVK was used to improve the film-forming and hole-transporting property of the La0.6Eu0.4(BSA)3phen. It has been proved that it exists Frster energy transfer process from La3+ to Eu3+. This device has also been compared with the devices: ITO/PVK: Eu(BSA)3phen/Alq/Al and ITO/PVK: Tb0.6Eu0.4(BSA)3phen/Alq/Al. From the data, it indicated the device has the good purity of red color and good commutation property. The maximum EL brightness of 102 cd·m-2 had been got.
2004 Vol. 24 (10): 1168-1171 [Abstract] ( 277 ) PDF (880 KB)  ( 704 )
1172 Electroluminescence Property of MEH-PPV/ZnO Nano-Crystal Structure
LI Hai-ling,WANG Yong-sheng,TENG Feng,XU Zheng
A new structure with Ⅱ-Ⅵ nano-crystal ZnO film as the electron transport layer and MEH-PPV as the hole transport layer and emitting layer was fabricated. The new structure’s brightness and efficiency were improved markedly compared with that of the single MEH-PPV layer structure. And a new peak at 620 nm was found in the ITO/MEH-PPV/ZnO/Al structure’s electroluminescence spectrum, which should resulted from ZnO layer. In addition, the turning-on voltage of the two-layer structure decreased from 9 V of the single layer structure to 4 V. From the I-V curve, the authors concluded that the emitting area was around the interface of MEH-PPV/ZnO and the combination area could shift with changing the voltage.
2004 Vol. 24 (10): 1172-1175 [Abstract] ( 1588 ) PDF (888 KB)  ( 365 )
1176 Fluorescence Properties of Earth-Doped RE:YVO4 Crystals
LIN Shu-kun,XIONG Wei,HUANG Xiao-hui,CHEN Yu,WANG Bin
The (RE):YVO4 crystals with high quality optical properties and various dopant concentrations of Tm3+,Er3+ and Yb3+ were grown using the Czochralski method. The room temperature fluorescence spectra have been measured,with 326 and 658 nm used as a pumping source. The fluorescence spectral properties were analysed with various dopant concentrations of rare-earth ions. Upconversion luminescence for various dopant concentrations was discussed.
2004 Vol. 24 (10): 1176-1179 [Abstract] ( 1032 ) PDF (970 KB)  ( 350 )
1180 Research of Spectrum Characteristics for Light Conversion Agricultural Films
ZHANG Song-pei,LI Jian-yu,CHEN Juan,XIAO Yang,SUN Yu-e
The solar spectrum and the function spectrum in chrysanthemum and tomato were determined in this paper. The research for a relation plant growth to solar spectrum showed that the efficiency of plant making use of ultraviolet light of 280-380 nm and yellow-green light of 500-600 nm and near IR spectra over 720 nm are lower, that the blue-purple light of 430-480 nm and red light of 630-690 nm are beneficial to enhancing photosynthesis and promoting plant growth. According to plant photosynthesis and solar spectrum characteristic, the author developed CaS∶Cu+, Cl- blue light film, and red light film added with CaS∶Eu2+, Mn2+, Cl- to convert green light into red light, and discussed the spectrum characteristic of red-blue double peak in agricultural film and rare earth organic complex which could convert ultraviolet light into red light. Just now,the study on light conversion regents in farm films is going to face new breakthrough and the technology of anti-stocks displacement to study red film which can convert near infrared light are worth to attention.
2004 Vol. 24 (10): 1180-1184 [Abstract] ( 1665 ) PDF (908 KB)  ( 393 )
1185 Resonance-Enhanced Multiphoton Ionization Spectrum of NO by D2Σ State
ZHANG Gui-yin1, 2,ZHANG Lian-shui1,YANG Xiao-dong1,SUN Bo1,ZHAO Xiao-hui1
NO is an important pollutant molecule,and plays a key role in generating photochemical smog and destroying O3 in the atmosphere. So researchers have always been interested in it. In our experiment, the optical parameter generator and amplifier (EKSPLA) pumped by Nd:YAG (Quantel) laser were used as the radiation source. The REMPI spectrum of NO in the region of 460-570 nm was obtained. Based on theoretical calculation, most of the lines were attributed to the X2Π→D2Σ transition. The ionization pathway was discussed in detail, which can be shown as NO(X2Π)3hνNO(D2Σ)2hνNO+e. The vibration fundamental and force constant of NO(D2Σ) state were calculated. The results are ωe=2 339.2 cm-1 and k=2.41×105 dyn·cm-1. For future work, the resolution of the radiation source will be improved in order to obtain more information of the D2Σ state.
2004 Vol. 24 (10): 1185-1187 [Abstract] ( 989 ) PDF (853 KB)  ( 415 )
1188 Phase Separation and Transport Behaviors in La0.7-x DyxSr0.3MnO3 System
CAI Zhi-rang1,LIU Ning1, 2, TONG Wei2,XU Su-jun2,ZHANG Yu-heng2
The influence of Dy doping (0.00≤x≤0.30) on magnetic and electric properties of La0.7Sr0.3MnO3 was studied by measuring M-T curves, M-H curves, ESR curves, ρ-T curves and MR-T curves of the samples. The experimental results indicate that all samples undergo the transition from paramagnetism to ferromagnetism at TC. When TTC, the doped samples enter the cluster-spin glass state, and the antiferromagnetism is exhibited at lower temperature. For the samples x=0.2 , the phase separation occurs at thetemperature far above TC,the variation in magnetic structure caused by Dy doping leads to colossal magnetoresistance.
2004 Vol. 24 (10): 1188-1192 [Abstract] ( 1546 ) PDF (1001 KB)  ( 341 )
1193 Temperature Distribution Measurement of High Energetic Monopropellant by Spectroscopic Diagnostic Technology
ZHANG Jie1, ZOU Yan-wen1, HE Jun1, YANG Rong-jie2, ZHAO Wen-hua3, FANG Zhong-yan4
The combustion flame temperature distribution in the axes are measured by relative intensity method of the spectroscopic diagnostic technology for monopropellant hexanitrohexaazaisowurtzitane (HNIW) at 3 MPa and 5 MPa pressure, respectively. The investigation results show that the curves of combustion flame temperature distribution in all combustion course are accurately measured by relative intensity method for monopropellant HNIW. The measured highest combustion flame temperature in the axes are lower than theoretical combustion temperature at the same pressure, and are more close to theoretical combustion temperature along with the rising of the pressure. The experimental results indicate that the combustion flame temperature distribution can be measured by the relative intensity method for high energetic and high burning rate propellant at higher pressure.
2004 Vol. 24 (10): 1193-1196 [Abstract] ( 1462 ) PDF (858 KB)  ( 340 )
1197 Application of Molecular Absorption Spectrophotometric Method to the Determination of Biologic Macromolecular Structures
CAO Shu-xia1,ZHAO Yu-fen1, 2*
A review on recent applications of molecular absorption spectrophotometric method to the identification of the structures of biologic macromolecules, such as protein and nucleic acid, is presented. Molecular absorption spectrophotometric method is widely used in the structure determination of biologic macromolecules for its convenience and speed. Ultraviolet absorption spectrum (UV) can be used in the research on the mechanism of the interaction of anticancer drugs and DNA. UV can also be used to study the interaction of spectroscopic probe with biologic molecule and their binding mechanism. Protein secondary structure and conformation can be investigated by Fourier infrared spectroscopy (FTIR) deconvolution analysis. Molecular absorption spectrophotometric method is an important tool for structure study of biologic macromolecules.
2004 Vol. 24 (10): 1197-1201 [Abstract] ( 1077 ) PDF (854 KB)  ( 1020 )
1202 Investigation on the Detection of Pesticide Residue in Vegetable Based on Infrared Spectroscopy
LI Wen-xiu1,XU Ke-xin1,WANG Yan1*,LEI Zhen-lin2,ZHANG Zhen-hou2
In this paper, the mid-infrared Attenuated Total Reflection (ATR) spectra of two slathered pesticides dichlorvos and trichlorfon in vegetable juice solution have been investigated. It can be concluded that within characteristic absorption region of the two pesticides in the mid-infrared range, the pigments inside the vegetable have no effect on the pesticide’s absorbance; pesticides in standard solution and vegetable juice solution share almost the same absorbance characteristics. These results indicate that: the authors can use the model built by the absorbance data of pesticides in water solution to simulate their absorbance in vegetable solution, then based upon infrared spectroscopy, the direct detection of pesticide residue on the vegetable can be achieved; it also provides a possible way of rapid detection on vegetable in the future.
2004 Vol. 24 (10): 1202-1204 [Abstract] ( 2031 ) PDF (898 KB)  ( 1102 )
1205 Outlier Diagnosis and Calibration Model Optimization for Near Infrared Spectroscopy Analysis
MIN Shun-geng, LI Ning, ZHANG Ming-xiang
Outlier diagnosis is a very important step in building near infrared calibration model. Data outlier includes spectral outlier and chemical value outlier. Mahalanobis’ distance, ratio of spectral residual and spectral variable leverage test were used to evaluate sample spectral outlier. Cook’s distance and the ratio of sample square error of chemical value and predict value to the mean square error of calibration set were used to test chemical value outlier. Three calibration models of protein content of 50 wheat samples, protein content of 90 corn samples and cyclohexane content of four compounds mixture were investigated. It is demonstrated that outlier test is very helpful for optimizing near infrared calibration model.
2004 Vol. 24 (10): 1205-1209 [Abstract] ( 1063 ) PDF (961 KB)  ( 1178 )
1210 The Analysis of Gynostemma Pentaphyllum(Thunb) Makino for Chinese Crude Drug by FTIR and FT-Raman
GUO Ping1, YUAN Ya-li2, XIONG Ping1
The Gynostemma Pentaphyllum is an important plant for Chinese crude drug. To qualitatively analyse the Gynostemma Pentaphyllum(Thunb) Makino, FTIR and FT-Raman were used to identify the contents of it. The results show, that the trough of each absorption in the picture of FTIR spectrum and the characteristic wave crest of each dispersion in the picture of FT-Raman spectrum had parallelism at their position, their relation pairs with each other. This is useful for the further on-line quantitative analysis and quality control of the Gynostemma Pentaphyllum(Thunb) Makino. This approach provide a quickly and accurately determination method of crude drug with out extraction and separation.
2004 Vol. 24 (10): 1210-1212 [Abstract] ( 993 ) PDF (834 KB)  ( 664 )
1213 Study on the Resonance Scattering Light Spectra of Atrazine-RNA and Its Analytical Application
REN Li-ping1, JIANG Shu-ren1, RAO Zhen-hong1*,XIONG Yan-mei1, ZHANG Chun-rong1, WANG Dong-dong2
The Resonance Light Scattering (RLS) spectra of atrazine with yeast ribonucleic acid (yRNA) had been studied. At pH 1.50, the enhanced RLS of atrazine-yRNA system is characterized by the maximum scattering peaks at 320 nm and the RLS intensity is proportional to the concentration of yRNA. Under optima conditions, the linear ranges of the calibration were 0.6-5.0 μg·mL-1, the linear regression equation was I=25.88+140.0 c(yRNA,μg·mL-1 ), r=0.997 5, with the limit of detection 20.7 ng·mL-1(3δ). The method was applied to the determination of yRNA in synthetic samples and RNA in salt cress (Thellungiella Halophila) sample satisfactorily. Mechanism studies show that there are two interaction modes between atrazine and RNA: electrostatic mode and intercalative mode.
2004 Vol. 24 (10): 1213-1216 [Abstract] ( 977 ) PDF (905 KB)  ( 358 )
1217 Catalytic Application of Synthesizing n-Butyl Acrylate by a New Type Nanometer Complex Heteropoly Acid Catalyst H3PW12O40/SiO2
ZHOU Li-qun1,2,LIU Shi-zhong2,SUN Ju-tang1
A new nanometer complex heteropoly acid with Keggin structure, H3PW12O40/SiO2, were prepared by sol-gel method,and were characterized with IR, UV, XRD and TEM techniques; By means of this nanometer catalytic materials, the optimum catalytic conditions of the n-butyl acrylate synthesis have been studied. The results show that the complex heteropoly acid H3PW12O40/SiO2 nanoparticles have the mean grain size of 40 nm and they are typical amorphous. A strong chemical interaction exists between H3PW12O40 and silica surface. The nanoparticles have high catalytic activity for synthesizing n-butyl acrylate. The optimum catalytic conditions are as follows: the mole ratio of acrylic acid and n-butyl alcohol is 1∶1.2,the reaction temperature is approximately 90-96 ℃,and the catalyst quantity in the reaction is 10% of the acid mass. The conversion proportion is 94.37% and product yield 91.2% in 5 h. Apparently, the unique structure of the Keggin anions and surface acid center and the high specific surface area and the pseudoliquid phase of H3PW12O40/SiO2 play an important role in the esterification reactions with the acid catalyst.
2004 Vol. 24 (10): 1217-1220 [Abstract] ( 1544 ) PDF (1057 KB)  ( 353 )
1221 Study of Photocatalytic Activity, Characterization and Preparation of Supersuspended Nano-TiO2 Ⅱ.Study of Photocatalytic Activity
ZHAO Jin-wei1,2,YUAN Min2,LIU Xiao-heng1,CHEN Guang1
From the change in the absorption of methyl-orange solution at 470 nm, the photocatalytic activity of nano-TiO2 prepared by pyrolysis method, and then by cooling treatment in silicon oil and in air respectively, was studied with methyl-orange solution as model waste water under irradiation by UV-lamp. Their photocatalytic mechanisms, the percentage of degradation in 35 min and the kinetic reactive process were also analyzed. The results show that the photocatalytic activity of both products is obvious with little difference. However, the nano-TiO2 powder modified with silicone oil can degrade harmful components more effectively on the surface of waste water with sunlight and other extra light.
2004 Vol. 24 (10): 1221-1223 [Abstract] ( 1009 ) PDF (842 KB)  ( 344 )
1224 Effect of CHAPS on the Stability of Spirulina Platensis Phycobilisomes
ZHANG Xi-ying, LIU Lu-ning, CHEN Xiu-lan, ZHANG Yu-zhong*,ZHOU Bai-cheng
The Spirulina Platensis phycobilisomes were isolated by sucrose density gradients ultracentrifugation,and the fluorescence emission maximum of the phycobilisomes at room temperature was at 671 nm. The effects of ionic strength and the zwitterionic detergent CHAPS on the stability of the Spirulina Platensis phycobilisomes were studied by room temperature fluorescence spectrum. The phycobilisomes were stable in 1.0 mol·L-1 phosphate buffer solution, and their fluorescence emission maximum could remain unchanged for 7 days. The fluorescence emission maximum of phycobilisomes was blue-shifted to 648 nm when the concentration of the phosphate buffer solution was diluted to 0.1 mol·L-1 with deionized water, which suggested that the phycobilisomes had been dissociated. The phycobilisomes were readily dissociated in phosphate buffer solutions of low concentrations (<0.6 mol·L-1 ) and the speed of the dissociation increased with decreasing the concentration of the phosphate buffer solution. The fluorescence emission maximum of the phycobilisomes in 1.0 mol·L-1 phosphate buffer solution was blue-shifted to 648 nm when 10 mmol·L-1 CHAPS was added into the phycobilisomes solution, suggesting that CHAPS could dissociate phycobilisomes under high ionic strength conditions. The results might be useful for isolating intact substructures of phycobilisomes.
2004 Vol. 24 (10): 1224-1226 [Abstract] ( 1946 ) PDF (884 KB)  ( 356 )
1227 Research on Discrimination of 3D Fluorescence Spectra of Phytoplanktons
ZHANG Qian-qian1, LEI Shu-he2, WANG Xiu-lin1*, WANG Lei1, YU Ping1
Six phytoplankton species belonging to four divisions,which may cause red tide,were selected and cultivated under different temperature(20 ℃ and 15 ℃) and illumination(7 000,4 100 and 1 100 Lux)in lab. 3D fluorescence spectra were measured in each growth period. Discrimination of these phytoplanktons’ 3D fluorescence spectra was explored using discriminant analyses. The result showed that discriminant analyses based on the principal component analysis of spectra data was an efficient method. Isochrysis galbana, Platymonas helgolanidica and Skeletonema costatuma can be discriminated effectively. Skeletonema costatuma, which is an diatom, can be distinguished from Alexandrium tamarense and Prorocentrum micans which belong to Dinophyta.
2004 Vol. 24 (10): 1227-1229 [Abstract] ( 504 ) PDF (851 KB)  ( 745 )
1230 Studies on a New Fluorescence-Enhanced System of Nucleic Acids-Morin-Al(Ⅲ)
LIN Xu-cong, XIE Zeng-hong*, GUO Liang-qia, CHEN Guo-nan
A fluorescence-enhanced system was developed for the determination of nucleic acids by using morin-aluminum(Ⅲ) complex as a new fluorescent probe. In aqueous solution, morin-aluminum(Ⅲ) complex showed maximum excitation and emission wavelengths at 420.0 nm and 532.8 nm, respectively, and its fluorescence could be greatly enhanced in the presence of nucleic acids. Under optimal conditions, the calibration graph was linear over the range 0.25-1.50 μg·mL-1 for fish sperm DNA, 0.10-1.60 μg·mL-1 for salmon sperm DNA, 0.25-2.00 μg·mL-1 for calf thymus DNA and 0.25-2.00 μg·mL-1 for yeast RNA. The corresponding detection limits are 3 ng·mL-1, 2 ng·mL-1, 2 ng·mL-1 and 3 ng·mL-1, respectively. Applied for the determination of nucleic acids in synthetic samples, the relative standard deviation for five replicates is less than 3.6%, and the recovery ranges from 93.3% to 107.9%. Additionally, the interaction mechanism of morin-aluminum(Ⅲ) with nucleic acids is also discussed.
2004 Vol. 24 (10): 1230-1234 [Abstract] ( 1584 ) PDF (961 KB)  ( 407 )
1235 Determination of Free Chlorine with Spectrophotometric Method Using N,N-diethyl-1,4-Phenylenediamine
XU Xiao-jie, LIN bin, CHEN Yu-qing
In this paper, the absorption spectra of free chlorine in the visible region has been measured after free chlorine in the solution had reacted with N,N-diethyl-1,4-phenylenediamine(DPD). The relation between the absorption spectra and peak wavelength has been discussed. From the experiment of liquor with different concentration, the error of spectral measurement is less than 0.04%. By nonlinear data fitting, the relation between the concentration of free chlorine and the transmittivity has been given.
2004 Vol. 24 (10): 1235-1237 [Abstract] ( 982 ) PDF (834 KB)  ( 555 )
1238 Study on the Simultaneous Spectrophotometric Determination of Three Components Including Deoxyschizandrin by Ridge Regression Method
ZHANG Li-qing,LI Ping,MU Jie,ZHU Xian-liang,LI Ju-qing
Ridge Regression (RR) spectrophotometry was used in the present paper to analyse three components: deoxyschizandin, schisandrin, and γ-schisandrin. The basic principle and the analytical steps of the approach are described in detail. The computer program of RR is based on VB language. The experimental results show that the RR method has no systematical error as compared to classical method, and the average recovery of each component is all in the range of 92.35% to 108.69%. High accuracy of RR method was obtained. Each component was determined with satisfactory results without any pre-separation. As compared with conventional methods, this method is simple, rapid and suitable for the computer-aided analysis. It was developed in statistical literature to treat these ill-conditioned systems and is an useful analytical method.
2004 Vol. 24 (10): 1238-1240 [Abstract] ( 1351 ) PDF (890 KB)  ( 381 )
1241 Molecular Recognitions of Purines by Hematoporphyrin and Metalloporphyrin Receptors
ZHANG Yong, LEI Ya-chun, PAN Jing-hao, LIU Dian-sheng
The present paper studies the interactions of purines and porphyrin by fluorescence, UV,and NMR spectra. The optimal conditions (acidity and ion intensity) of the interaction of purines and hematoporphyrin and metalloporphyrin were investigated in detail. The result shows that hematoporphyrin and metalloporphyrin exhibit significant recognition of purines. The binding constants of metalloporphyrin: KNi(Ⅱ)-HPKCo(Ⅱ)-HPKZn(Ⅱ)-HPKCu(Ⅱ)-HP in pH 11.2 Kolthoff buffer solution. The mechanism of recognition was further discussed. Recognition is achieved by cooperative functions of three recognition groups (metalloporphyrin) and two recognition groups (hematoporphyrin).
2004 Vol. 24 (10): 1241-1243 [Abstract] ( 1445 ) PDF (863 KB)  ( 456 )
1244 Measurement of Uranium Isotope Ratio in Solid Sample by Laser Ablation and Double-Beam Diode Laser Atomic Absorption
LIU Hong-tao1,ZHANG Zhan-xia1,Quentmeier A2,Niemax K2
The 235U/238U isotope ratio was determined by diode laser atomic absorption spectrometry in a plasma induced by a Nd:YAG laser. Two diode lasers, which probed almost the same plasma volume, were used as light sources. 235U and 238U absorption signals were simultaneously measured by tuning the diode lasers to the absorption lines 682.673 6 nm and 682.076 8 nm, respectively. The optimal focus position for the Nd:YAG laser was found to be 0.4 cm below the sample surface. The precision and accuracy of 235U/238U isotope ratio determination were obtained to be 5% and 2%, respectively. The detection limit of the 235U isotope, evaluated on the basis of 3σ criteria, was estimated to be 18 μg·g-1. All these results show an improvement compared with the method in which only one diode laser was used as a light source.
2004 Vol. 24 (10): 1244-1247 [Abstract] ( 1053 ) PDF (1057 KB)  ( 401 )
1248 Uncertainty in-Statistical-Monitor for ICP-AES Measurement System by Using Moving Range Pooled
WANG Dou-wen1,ZHAO Xue-rong1,ZENG Ze1,ZHAO Si-qi2
This paper describes how to estimate the uncertainty when Fe in metallic silicon is determined by ICP-AES (Inductively Coupled Plasma Atomic Emission Spectrometry). The technique of the averaged moving range(MR) pooled in-statistical-dynamic-monitor is proposed. The study suggests that the uncertainty contribution of ICP-AES measurement system is, by using this technique, a combination of quality control (QC) and linear fit. This conclusion maximized the combination of the effects on various variances, refrained from the complicated relativity, and favored the uncertainty evaluation for ICP-AES measurement system.
2004 Vol. 24 (10): 1248-1252 [Abstract] ( 1460 ) PDF (891 KB)  ( 348 )
1253 Application of Orthogonal Test in Determination of Trace Elements in Wild Vegetables by ICP-AES
WANG Ying, XIN Shi-gang
In this paper, orthogonal test was applied to determination of trace elements in wild vegetables just as Mn, Se, Cu, Fe, Mg and Zn by ICP-AES. It could provide many informations for us by less experimental times, and could choice the best experimental conditions by square-error analysis. It would be helpful for improving experimental accuracy. The method was simple, rapid, and possessed of highly sensitivity, good accuracy and determination of many elements at the same time, in addition little environment pollution. The recoveries of the method were in the range of 97.2%-103.3%, and relative standard deviations were less than 2.15%. The experimental results proved wild vegetables were valuable and nutritious food, they had rich trace elements.
2004 Vol. 24 (10): 1253-1256 [Abstract] ( 1482 ) PDF (840 KB)  ( 382 )
1257 Determination of Main Components in Nd-Fe-B Magnetic Materials by ICP-AES
LIU Yong-ming
The method for direct determination of neodymium,iron and boron in Nd-Fe-B permanent magnetic materials by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) was studied and suitable analytical lines were selected. The interference from matrix elements in samples was diminished by matrix matching method. The memory effect of the determination of boron by ICP-AES was discussed and was eliminated by way of detecting and subtracting blank value from testing result of samples frequently. The method was applied to the determination of Nd,Fe and B in Nd-Fe-B permanent magnetic materials samples with a precision of RSD 0.62%,0.56% and 0.90%,respectively.
2004 Vol. 24 (10): 1257-1259 [Abstract] ( 1535 ) PDF (869 KB)  ( 355 )
1260 Study on the Determination of Calcium in Chinese Medicine by ICP-AES
ZHANG Sheng-bang,ZHANG Xue-jun,GUO Yu-sheng
Calcium is the necessity element in human body and its content has effect on exciting muscle or nerve. Calcium is important in the physiologic process of muscle or nervous reaction, nervous impulse transmission,heartbeat rhythm maintenance, blood solidification, cell coherence and so on. Determination of calcium element in Chinese medicine wild jujube seed decoction and radix puerariae was studied by ICP-AES after they were digested with HNO3-HClO4. The precision (RSD) is 1.7%. The average recovery of calcium in wild jujube seed decoction is 97.7% and in radix puerariae is 104.4%. Calcium was abundant in Chinese medicine and could play certain pharmacologic role in Chinese medicine. It is of important significance to assess the value of Chinese medicine by determination of calcium element in Chinese medicine with ICP-AES.
2004 Vol. 24 (10): 1260-1261 [Abstract] ( 1006 ) PDF (862 KB)  ( 383 )
1262 Study on the Determination Cu, Cr, Al, Ni and Ti in Corrosion Solution of Oxidation Equipment in Supercritical Water by ICP
ZHU Xiao-mei, GE Hong-guang
The Cu,Cr,Al,Ni and Ti in corrosion solution of oxidation equipment in supercritical water by inductively coupled plasma-atomic emission spectrometry has been investigated, the authors used catalysts(CuO/Al2O3) to oxidize unsymmetrical dimetyl-hydrazine in supercritical water in a stainless steel(1Cr18Ni9Ti)reactor. The test was operated under condition of 400-500 ℃ and 24-26 MPa. The results indicate that the dissolution of Cr in stainless steel were occurred in supercritical water and dissolution became severe with higher temperature and pressure.
2004 Vol. 24 (10): 1262-1263 [Abstract] ( 1012 ) PDF (853 KB)  ( 460 )
1264 Determination of Mercury and Selenium in Bone by Atomic Absorption Spectrometry after Microwave Digestion
LI Hui1, HU Xiao-rong1, CHENG Guang-lei2
Mercury and selenium in the rats’ thighbone were determinated by cold atom absorbance and flow injection hydride atom absorbance after digesting by microwave. The method of sample’s making and digesting was discussed. The factors of determination of selenium were studied. The detection limits of mercury and selenium are 1.65 and 1.78 ng·mL-1 respectively. The RSD% of mercury and selenium are 4.1% and 3.6% respectively. The linearity of calibration curve of mercury and selenium are in the concentrations of 0-120 ng·mL-1 and 0-50 ng·mL-1 respectively. The recovery of mercury and selenium are 93.72%-101.8% and 95.53%-102.2% respectively.
2004 Vol. 24 (10): 1264-1266 [Abstract] ( 1623 ) PDF (842 KB)  ( 404 )
1267 Direct Determination of Trace Arsenic in Coal by Slurry-Sampling Graphite-Furnace Atomic Absorption Spectrometry
CHEN Shi-zhong
A method for direct determination of trace arsenic in coal by slurry-sampling Graphite-Furnace Atomic Absorption Spectrometry (GFAAS) was developed, using Pd as a matrix modifier. The effects of slurry stability, particle size of sample, matrix modifiers, ashing temperature, atomization temperature,and common coexisting components on the signal intensity of arsenic were investigated. Under optimized operating conditions, the detection limits and relative standard deviation of this method were 0.054 μg·g-1 and 8.9%, respectively.
2004 Vol. 24 (10): 1267-1269 [Abstract] ( 1019 ) PDF (842 KB)  ( 623 )
1270 Determination of Trace Gold by Flow Injection On-Line Preconcentration Flame Atomic Absorption Spectrometry with Trioctylamine Levextrel Resin
YE Ming-de,LIN Mei-jin
A new method for the determination of trace amount of gold by flow injection on-line preconcentration and flame atomic absorption spectrometry with trioctylamine levextrel resin was developed. The experimental condition of Au(Ⅲ) on the resin, such as the time of preconcentration, the flow rate, the elutropic time, the elutropic rate, the acidity of medium, the concentration and acidity of eluting agent was studied in this paper. The detection limit is 1.3 μg·L-1, The enhancement factor of 24 was achieved for a loading period of 90 seconds. The recoveries of Au were 98.0%-102.0%. The developed method has been applied to the determination of trace amount of gold in water samples with satisfactory results.
2004 Vol. 24 (10): 1270-1272 [Abstract] ( 1491 ) PDF (900 KB)  ( 401 )
1273 Determination of LF-VD Refining Furnace Slag by X ray Fluorescence Spectrometry
KAN Bin,CHENG Jian-ping,SONG Zu-feng
Eight components, i.e. TFe, CaO, MgO, Al2O3, SiO2, TiO2, MnO and P2O5 in refining furnace slag were determined by X ray fluorescence spectrometer. Because the content of CaO was high, the authors selected 12 national and departmental grade slag standard samples and prepared a series of synthetic standard samples by adding spectrally pure reagents to them. The calibration curve is suitable to the sample analysis of CaO, MgO and SiO2 with widely varying range. Meanwhile, the points on the curve are even. The samples were prepared at high temperature by adding Li2B4O7 as flux. The experiments for the selection of the sample preparation conditions about strip reagents, melting temperature and dulition ratio were carried out. The matrix effects on absorption and enhancement were corrected by means of PH model and theoretical alpha coefficient. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.
2004 Vol. 24 (10): 1273-1275 [Abstract] ( 1570 ) PDF (835 KB)  ( 366 )
1276 Development of Portable LED-Based NIR Integrity Wheat Component Measuring Apparatus
WEN Ming, JI Hai-yan*
A integrity wheat component quickly measuring apparatus which based on NIR LED was developed, by using new chip and designing software. While providing a lower cost apparatus, it also provides quick answer speed and smaller size for fieldwork of wheat’s components measuring. The apparatus is made up of NIR LED, interference filter, lens, Si photronic detector, microprocessor system and calibration model. Compared with other instrument, the apparatus has many advantages, such as compact space, simple structure, low power waste, and anti-shake. This paper introduces the design of the apparatus, and predicts the concentration of wheat protein. The apparatus can realize non-damage measurement of wheat components’ concentration on fieldwork.
2004 Vol. 24 (10): 1276-1279 [Abstract] ( 1600 ) PDF (883 KB)  ( 410 )