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2006 Vol. 26, No. 07
Published: 2006-06-26

 
       光谱学与光谱分析
1185 Study on In-Plane Optical Anisotropy of Semiconductor Materials by Reflectance Difference Spectroscopy
ZHAO Lei1, CHEN Yong-hai2, ZUO Yu-hua1, WANG Hai-ning3, SHI Wen-hua1
In the present review, the measuring principle of reflectance difference spectroscopy (RDS) is given. As a powerful tool in the surface and interface analysis technologies, the application of RDS to the research on semiconductor materials is summarized along with the origins of the in-plane optical anisotropy of semiconductors. And it is believed that RDS will play an important role in the electrooptic modification of Si-based semiconductor materials.
2006 Vol. 26 (07): 1185-1189 [Abstract] ( 220 ) PDF (989 KB)  ( 482 )
1190 Second-Harmonic Detection with Tunable Diode Laser Absorption Spectroscopy of CO and CO2 at 1.58 μm
TU Xing-hua, LIU Wen-qing, ZHANG Yu-jun, DONG Feng-zhong, WANG Min, WANG Tie-dong, WANG Xiao-mei, LIU Jian-guo
Tunable diode laser absorption spectroscopy has been applied in the fields of atmospheric chemistry and monitoring pollutant gases as a new method of measuring trace gases. The technique of remote sensing of CO and CO2 at 760 mm Hg pressure with tunable diode laser absorption spectroscopy in the near-infrared region is introduced. And the relationship between the second-harmonic spectrum of CO2 in Lorentzian line shape and the modulation amplitude is also presented.
2006 Vol. 26 (07): 1190-1194 [Abstract] ( 1645 ) PDF (922 KB)  ( 622 )
1195 VUV Excited Luminescence of LnZr(BO3)2∶Eu3+(Ln=Ba, Sr)
SHEN Fang1, HE Da-wei1*, LIU Hong-li1, XU Jian-hua2
Powder samples of Ba(1-x)SrxZr(BO3)2∶Eu3+(0≤x≤1) were prepared by the conventional solid state reaction method. The excitation spectrum shows a strong absorption in the VUV region with the broad absorption band edge at 130-170 nm due to the host and the f→d transition of Eu3+, and another absorption band of charge-transfer state (CTS) of Eu3+ in the region of 230 nm. The absorption of the charge-transfer band of Eu3+ can be increased by incorporating Al3+ ion into Zr4+ ion lattice. The luminescence of Ba(1-x)SrxZr(BO3)2∶Eu3+ is also increased by incorporating Al3+ into the lattices. In Ba(1-x)SrxZr(BO3)2∶Eu3+, the intensity of the absorption band (130-170 nm) decreases, and the band shifts about 30 nm toward lower energy with x increasing. The emission spectra revealed an intense and sharp (616 nm) red color emission from Eu 3+(5D07F2) transition under 147 nm VUV excitation.
2006 Vol. 26 (07): 1195-1198 [Abstract] ( 1507 ) PDF (925 KB)  ( 620 )
1199 The Electroluminescence of a Novel Complex Eu(o-BBA)3(phen)
LIU Ling1, XU Zheng1*, ZHANG Fu-jun1, LOU Zhi-dong1, SUN Bo2, PEI Juan
A novel rare earth complex of Eu ion with 2-benzoylbenzoic acid and 1,10-phenathrolinephen (Eu(o-BBA)3(phen)) was synthesized and used as a dopant to fabricate efficient electroluminescence(EL) devices. It was doped into poly(N-vinylcarbazole) (PVK) and spin coated into films. Devices using organic layer Alq3 (or inserted hole blocking layer BCP) and inorganic layer ZnS as electron transporting layer respectively were fabricated. The luminescence properties of the single-layer decvice A (ITO/PVK∶Eu/Al) and the organic-inorganic heterostructure device were analyzed. It was found that the device using ZnS as the electron transporting layer has higher brightness and lower threshold voltage while maintains pure emission.
2006 Vol. 26 (07): 1199-1202 [Abstract] ( 571 ) PDF (937 KB)  ( 485 )
1203 Synthesis and Photoluminescence of N-Benzoin Aniline, 1,10-Phenanthroline, and Europium Ternary Complex
XIAO Zun-hong
New N-benzoin aniline and Eu(BZA)3phen were synthesized, and they were characterized by EA, IR,1H NMR and UV. The Eu(Ⅲ) complex spectra were excited at the wavelength of 342 nm, which exhibited a red emissive color, and the Eu characteristic peaks appeared at 592 and 615 nm, respectively. The 615 nm transition showed the strongest emission. N-benzoin aniline sensitizes to Eu ions and it is a good ligand of Eu complex.
2006 Vol. 26 (07): 1203-1205 [Abstract] ( 1709 ) PDF (854 KB)  ( 614 )
1206 Study on Photo-Degradation Kinetics of Hemin in the Presence of Anion Surfactant
LIU Er-bao1,HAN Su-qin2
A novel photodecomposition behavior of hemin was described. With RhB-H2O2 system a flow injection chemiluminescence method has been applied to the study of the photolytic kinetics of hemin under ultraviolet light. And the sodium dodecyl sulfonate (SDS) was added as a photostability-stabilizer. The results showed that the decomposition reaction of hemin in the presence and absence of SDS corresponded to a first-order reaction. Furthermore, the presence of SDS in the system decreased the photolytic rate of hemin by 1.8 times compared to that in the absence of SDS.
2006 Vol. 26 (07): 1206-1208 [Abstract] ( 1669 ) PDF (830 KB)  ( 504 )
1209 FTIR Characterization of the Secondary Structure of a Staphylokinase Variant (K35R) Encapsulated within PLGA Microspheres
HE Jin-tian1,2, WANG Gai-zhen3, SONG Hou-yan1,2
The secondary structure of a staphylokinase variant (K35R, DGR) encapsulated in poly(lactic-co-glycolic acid) (PLGA) microspheres was quantitatively examined by Fourier transform infrared (FTIR) spectroscopy. Resolution enhancement technique and Fourier deconvolution were combined with band with curve-fitting procedures to quantitate the spectral information from the amide Ⅰ bands. Nine component bands were found under the broad, nearly featureless amide Ⅰ bands and assigned to α-helix, β-sheet, turn and irregular(random) structures. The changes of bands at 1 651 and 1 623 cm-1 after encapsulation were discussed.
2006 Vol. 26 (07): 1209-1212 [Abstract] ( 1642 ) PDF (878 KB)  ( 495 )
1213 Application of MALT-CLS Method to FTIR Quantitative Analysis of Atmospheric Trace Gas
GAO Min-guang,LIU Wen-qing,ZHANG Tian-shu,LIU Jian-guo,LU Yi-huai,XU Liang, ZHU Jun
The MALT-CLS method for quantitative analysis of atmosphere trace gas by FTIR spectrometry was studied. Some experiments are described, such as long-path White cell, and passive remote sensing of aircraft. The characteristic of this method is that the calibration spectra are calculated from a database of absorption line parameters HITRAN using MALT program, including environmental and instrumental effects in the calculation. It is particularly useful in long open-path and solar FTIR spectroscopy, or passive remote sensing by FTIR.
2006 Vol. 26 (07): 1213-1216 [Abstract] ( 1598 ) PDF (946 KB)  ( 567 )
1217 Study on N-Acetylated Chitosans by FTIR and XRD
REN Dong-wen1, BAO De-cai1, 2, WANG Wei1,MA Xiao-jun1*
The degree of N-deacetylation (DD) is an important property of chitosan. In the present article the reaction of N-acetylation was applied to prepare six chitosan samples with various DDs. The samples were studied by FTIR and XRD to investigate their IR absorbance characteristics and crystallinity, from which the DDs and crystallinity index (CrI) of chitosans were also determined respectively. The influence of N-acetylation on DD and CrI was also discussed,and it could be found from FTIR that the N-acetylation reaction became difficult for the remaining amino group in chitosan molecule as the reaction proceeded. XRD also indicated that the crystalline zone was broken by N-acetylation gradually,and another kind of crystal form appeared instead.
2006 Vol. 26 (07): 1217-1220 [Abstract] ( 1131 ) PDF (898 KB)  ( 907 )
1221 FTIR Research on the Modification of Plant Oil Pitch Binders by Polyester Waste
ZHENG Yu-ying,WANG Can-yao,WU Zhang-hong,DONG Mei-bin,ZHANG Xing
Various plant oil pitchs (cottonseed pitch, bean oil pitch, and mixed plant oil pitch) were used to prepare the plant oil pitch binders for casting. They were treated by polyester waste and processed by several technics such as esterifying. In the mean time, FTIR and TG were adopted to learn the structure, property, and sclerous mechanism of the binders. From the comparison with synthetic fat binder, the authors can see that the treated binders have similar components. They also have many excellent properties such as higher dry tensile strength and slower deflation velocity, which equal to or even exceed the properties of synthetic fat binder. Therefore, the treated binders, which were cheaper, can be used to make class Ⅰ mold and core binders.
2006 Vol. 26 (07): 1221-1225 [Abstract] ( 1051 ) PDF (910 KB)  ( 484 )
1226 FTIR Study of Nano-Iron Oxyhydroxides’ Decoloration on the Azo Dye
SUN Zhen-ya1,2, DU Jian-hua1, CHEN He-sheng2, GONG Wen-qi1
IR spectra were used to analyse the azo dye solution decoloration action by two kinds of iron oxyhydroxides. It was discovered that: (1)Acid Red G & methyl orange are apt to form complex on the surface of iron oxyhydroxides >FeOH, especially Acid Red G. which possesses two —SO3Na structures has a relatively high decoloration efficiency as a result of complexation reaction; (2) after 2 hours adsorption, the IR spectra of iron oxyhydroxides show characteristic wave numbers at 1 033 and 1 030 cm-1 which belong to —SO3Na,whereas the peaks at wave numbers between 1 450 and 1 400 cm-1, which belong to azo dye, disappear. These phenomena indicate that azo dye molecules are adsorbed on the surface of iron oxyhydroxides due to the negative —SO3Na structure, and at the moment azo dye molecules are adsorbed on the surface of iron oxyhydroxides, the electron transfer occurs between the azo dye molecules and the iron oxyhydroxides surface’s Fe3+ centre, which could lead to the rupture of azo bond. It can be infered that the decoloration of azo dye molecules is the co-effect of the selective chemical absorption and the oxidation-deoxidation effect on the surface of iron oxyhydroxides.
2006 Vol. 26 (07): 1226-1229 [Abstract] ( 549 ) PDF (930 KB)  ( 642 )
1230 The Analysis of Wood Microfibril Angle by Near Infrared Spectroscopy and X-Ray Diffractometry
JIANG Ze-hui, HUANG An-min,FEI Ben-hua, REN Hai-qing*
In the present paper, near infrared (NIR) spectroscopy and X-ray diffractometry were used to rapidly predict the microfibril angle (MFA). MFA is one of the most important factors affecting wood properties. Wood resource utilization and tree improvement programs require cost-effective methods for the rapid analysis of thousands of samples. In the experiment, the average MFA of each sample were rapidly measured by X-ray scanning diffractometry. Then, the PLS model was built between NIR data and MFA by the X-ray measured. As a result, a very strong linear relationship has been found between NIR spectra fitted and X-ray measured, and the coefficients (r2) of calibration and prediction models were 0.867 and 0.816 respectively.
2006 Vol. 26 (07): 1230-1233 [Abstract] ( 773 ) PDF (984 KB)  ( 664 )
1234 Detection of Tofu Hardness by Near Infrared Spectroscopy
HAN Dong-hai, LU Chao, WEN Zhao-hui,GENG Zhao-xi
The possibility of determination of tofu hardness by near infrared spectroscopy (NIR, 833-2500 nm) was studied. The influences of water content and protein content on the spectra were discussed, in order to detect the hardness. The models of Tofu hardness were calibrated by partial least squares regression (PLS) after eliminating outline, spectra pretreatment, and wavelength optimization (r=0.994, RMSEC=0.391%, RMSEP=0.416%, RSD=2.27%). All of the results were better than those by sense assessing method.
2006 Vol. 26 (07): 1234-1237 [Abstract] ( 1541 ) PDF (937 KB)  ( 478 )
1238 Study on the Identification of Standard and False Gancao by Fourier Transform Infrared Spectroscopy
AYIGULI·Tashi1, 2, ZHOU Qun1, DONG Xiao-ou3, SUN Su-qin1*
Standard Gancao (Glycyrrhiza uralensis Fisch) and false Ciguogancao (Glycyrrhiza pallidiflata Batal) were identified fast, nondestructively by Fourier transform infrared spectroscopy(FTIR)combined with derivative spectra and two-dimensional correlation spectroscopy (2D) in the present article. The result shows that although the two kinds of Gancao belong to one genius, there are some certain differences in their chemical components that are reflected in the IR spectra, but with some similarity and dissimilarity in the IR spectra. The two kinds of Gancao are quite different from each other in second derivative spectra and 2D spectra. Based on the differences reflected in the IR and 2D IR, the standard gancao can be identified from the false easily and clearly. The result also proved that there is a relationship between the IR spectra and the chemical components of the herbs. This method is fast, accurate and nondestructive, and the wastage of sample is less. The fast, accurate property of 2D spectroscopy makes it a powerful and new approach to evaluating medicinal herbs impersonally.
2006 Vol. 26 (07): 1238-1241 [Abstract] ( 1162 ) PDF (1077 KB)  ( 636 )
1242 Analysis and Discrimination of Collocalia Esculenta L. via FTIR Spectroscopy
DENG Yue-e1, 2, SUN Su-qin1*, ZHOU Qun1, LI Ao3
Collocalia esculenta L. is called Yanwo in China. Thirty kinds of dry yanwo were identified by Fourier transform infrared spectroscopy (FTIR) . The results indicated that there were some obvious differences in FTIR between the dry yanwo and the natural yanwo, mainly represented in some absorption peaks of protein, amino acid (1 634, 1 535 cm-1) and amylase (1 034 cm-1). Meanwhile, the shape, position and intensity of the peaks from methylene (2 935 cm-1), protein and amino acid (1 647, 1 533, 1 447 cm-1) in dry yanwo were similar to those of the glutin. Therefore, different amounts of glutin were added in dry yanwo samples. The content of candy in some dry candy yanwo products was as high as 99%, but the content of yanwo was only 1%. The characteristic peaks of yanwo in these products even could not be found. So the quality of yanwo in the market could not be guaranteed from these results. FTIR is fast and direct to analyse and evaluate the quality of yanwo product.
2006 Vol. 26 (07): 1242-1245 [Abstract] ( 192 ) PDF (945 KB)  ( 644 )
1246 Analysis of Modifying Polymer in the Modified Asphaltum Waterproof Membrane
DU Zhen-xia, LIU Shan
The waterproof roller sheet of modified asphaltum is extensively used in many waterproof constructions. The modified asphaltum by polymer is of good performance, such as cold-resistant, high intension etc. In the present paper, the modifying polymer was seperated from the waterproof membrane of modified asphaltum. The structure of the modifying polymer was identified by IR, <sub>13C NMR, and Py-GC/MS. The results show that the polymers are SBS and polyisobutylene.
2006 Vol. 26 (07): 1246-1248 [Abstract] ( 1023 ) PDF (844 KB)  ( 569 )
1249 Method for Retrieving Pollution Gas Concentration from Raman Lidar Return
HONG Guang-lie1, ZHANG Yin-chao2, ZHOU Meng-ran1, CAO Kai-fa2, ZHOU Jun2
Raman lidar is an important tool for the detection of atmosphere pollution, and inversion for lidar returns is an important process. The key for inversion is to get transmission exponential function expR0[α(λ1,z)-α(λ2,z)]. Three methods with extinction coefficient as the center are presented. First, 532 nm atmospheric extinction coefficient was used to indirectly obtain α(λ1,z) and α(λ2,z), This method has been used generally by people. Two new methods were proposed: 1, reference gas with approximate Raman wavelength is used so that α(λ1,z)=α(λ2,z). 2, Mie-Rayleigh scattered return with wavelength λ1 or λ2 is used to compute expR0[α(λ1,z)-α(λ2,z)].
2006 Vol. 26 (07): 1249-1252 [Abstract] ( 1538 ) PDF (859 KB)  ( 515 )
1253 Application of Near-Field Raman Spectroscopy to Nano-Structure Characterization
WANG Yang1, WU Xiao-bin1, WANG Jia1*, YU Jian-yuan2
Near-field Raman spectroscopy is a novel technology in the near-field optics, and attracts much attention of scientists because of the realization of spectral characterization of nano-structure. The technical advantage of Raman spectroscopy is described in the present review. The principle and practical technical scheme of near-field Raman spectroscopy systems are introduced. Several applications of near-field Raman spectroscopy are mentioned in detail, including carbon nanotube characterization, biological specimen imaging, thermoelectric crystal characterization, dye single molecule detection etc., revealing a broad prospect of the development of near-field Raman spectroscopy in various scientific research fields.
2006 Vol. 26 (07): 1253-1259 [Abstract] ( 1064 ) PDF (1346 KB)  ( 601 )
1260 Application of p-Aminothiophenol as a SERS Reporter in Immunoassay
JIANG Yun,CUI Yan, GU Ren-ao*
The adsorption of p-aminothiophenol (PATP) molecule on the gold electrode was investigated. The result suggests that PATP was adsorbed perpendicularly onto the substrate. By immobilizing goat anti-mouse IgG on a glass slide modified by special organic molecules, the antibody/antigen/reporter-labeled immunogold nanoparticle sandwich assay was build for surface-enhanced Raman spectroscopy(SERS) measurements. The p-aminothiophenol(PATP) was used as SERS-reporter molecule. Thus the authors can identify the single type biospecific species by SERS signal of the reporter molecules which are coimmobilized with antibody molecules in gold colloids.
2006 Vol. 26 (07): 1260-1263 [Abstract] ( 1059 ) PDF (872 KB)  ( 902 )
1264 Studies of Laser Raman Spectra of Sodium Glutamic Acid Solution Effected with Environmental Light
LIU Wen-han, ZHANG Dan, WU Xiao-qiong, ZHENG Jian-zhen, MA Chun-an
The laser Raman spectra influenced by environmental light have been studied in the determination of sodium glutamic acid solution. The environmental light included natural light from outdoors and the light from indoor fluorescents. The results show that different influences on laser Raman spectra of sodium glutamic acid solution can be produced in different environmental light. There were some characteristic spectral lines, minus peaks or sharpened peaks. These influences cannot be ignored. The determinations of laser Raman spectra must be performed in darkroom or in the sheathing or mantle etc.
2006 Vol. 26 (07): 1264-1266 [Abstract] ( 1571 ) PDF (882 KB)  ( 598 )
1267 Study the Raman Spectroscopy of Breast Tumor Limbic Tissue
ZHAO Yuan-li1, Lü Jing2, GE Xiang-hong1, YAO Shu-xia1, LIANG Er-jun1
The confocal Raman micro-spectra of breast tumor limbic fat tissues of forty cases after surgery were collected. Substantial differences were found among breast infiltrative ductal carcinoma, hyperplasia and fibroadenoma, which is possibly to be used as a character of breast cancer and other breast tumor and offers the evidence for the breast tumor diagnosis. So, the Raman spectroscopy of the breast limbic fat tissue is of great value.
2006 Vol. 26 (07): 1267-1271 [Abstract] ( 1413 ) PDF (1120 KB)  ( 798 )
1272 Studies of Relationships between Cu Pollution and Spectral Characteristics of TritiZnm Aestivum L.
CHI Guang-yu1, LIU Xin-hui1*, LIU Su-hong2, YANG Zhi-feng1
The effect of Cu pollution on the Cu uptake by wheat, the characteristics of chlorophyll concentration, and the visible-near infrared spectra were studied under the condition of solution culture, and the relationships among the three indices were discussed. The results indicate that the content of Cu in TritiZnm aestivum L. increases and the concentration of chlorophyll reduces with the increase of Cu in solution. The spectral characteristics also take on the disciplinary diversification (the spectral reflectivity ascended in the visible light band and decreased in the near infrared band; the range of red edge shift decreased) with the increase of Cu in solution.
2006 Vol. 26 (07): 1272-1276 [Abstract] ( 1679 ) PDF (886 KB)  ( 611 )
1277 Syntheses and Spectral Characterization of Low-Molecular-Weightchitosan-Ce(Ⅲ) Complexes
WANG Ke-jun1, 2, WEN He-rui1, LIU Fang2, JIA De-min2
The low-molecular-weightchitosan-Ce(Ⅲ) complexes were synthesized at pH value 1-2 and characterized by UV spectrum, fluorescence spectrum, FTIR spectrum and 1H NMR spectrum. Its coordination mechanism was also investigated. The results showed that Ce(Ⅲ) was coordinated with —OH group instead of —NH2 group of low-molecular-weight chitosan.
2006 Vol. 26 (07): 1277-1280 [Abstract] ( 1102 ) PDF (861 KB)  ( 525 )
1281 Research of Hg2+ Sol-Gel Membrane Made of Organically Modified
GUO Liang-qia, ZHANG Wei, YAN Jian-feng, LIN Xu-cong, XIE Zeng-hong*, CHEN Guo-nan
A photochemical sensor for the determination of Hg2+ consisting of organically modified silicates (ormosils) was developed. Hg2+-sensitive fluorescent sol-gel films were prepared by co-condensation of tetramethoxysilane (TMOS) and dimethyldimethoxysilane (DMOS), and the fluorescent indicator 5,10,15,20-tetra (p-sulfonatophenyl)porphyrin sodium was embedded in sol-gel in the form of ion pairs with cetyltrimethyl ammonium bromide. The optimization condition of preparation and response performance of sol-gel membrane were investigated. The experimental results showed a linear range of Hg2+ concentrations from 1.0×10-5 to 1.0×10-4 mol·L-1 in a Tris-HCl buffer at pH 8.0 with fast response and good repetition. The indicators in the sol-gel membrane did not leak out and the sensor showed good selectivity over other metal ions.
2006 Vol. 26 (07): 1281-1284 [Abstract] ( 365 ) PDF (928 KB)  ( 427 )
1285 Study on the Characterization of β-Cyclodextrin-Diferrocenylenone Inclusion Complex and Micro-Environmental Effects
CHEN Xiao-yan, LIU Wan-yi*, ZHANG Jing
The structure of the inclusion complex of diferrocenylenone and β-cyclodextrin prepared by a novel method of solid-grinding was studied by UV, FTIR and powder X-ray diffractometry. Continuous variation plot proved that 2∶3(DFE∶β-CD) inclusion complex has been formed. The binding constant of the inclusion compound was found to be 1.48×1015 (L4·mol-4) with the data of UV spectroscopy. Furthermore, the influence of different solvents and pH on the UV spectrum of DFE and β-CD-DFE was discussed respectively. The results show that different micro-environment has apparently different effects on the electric spectra of guest and inclusion complex.
2006 Vol. 26 (07): 1285-1289 [Abstract] ( 1040 ) PDF (975 KB)  ( 415 )
1290 VUV Spectral Properties of MO-Y2O3-B2O3:Re(M=Mg, Sr; Re=Eu, Tb)
LIANG Zhong-yi, HE Da-wei*, SHI Yan-ning
DOI: 2006-07-1290
Eu and Tb doped 17MO-7.88Y2O3-75B2O3 samples were prepared by the solid state reaction. VUV excitation properties and luminescence properties under VUV excitation were studied. Excitation spectra exhibited high absorption in VUV region(120-220 nm). There existed strong emission peaking at 591 and 613 nm corresponding to the 5D07FJ(J=1, 2, 3, 4) emission transition of Eu3+ when MgO-Y2O3-B2O3:Eu was energized by the VUV radiation(147 nm). By the introduction of Sr into MgO-Y2O3-B2O3:Eu absorption peaking at 147 nm and red emission peaking at 613 nm are enhanced strongly. Besides the host absorption band of MgO-Y2O3-B2O3:Tb,there existed strong absorption band peaking at 170,178,195,204,225 nm corresponding to the 4f8→4f75d transition of Tb3+; emission spectra showed strong emission peaks at 491,547,590,621 nm corresponding to the 5D47FJ(J=6,5,4 and 3) emission transition of Tb3+.
2006 Vol. 26 (07): 1290-1293 [Abstract] ( 1554 ) PDF (943 KB)  ( 432 )
1294 Highly Sensitive Fluorescent Reaction of Acridine Red with Chromium(Ⅵ) and Its Application
YE Cun-ling1, 2, WANG Xin-ming1*, FAN Jing2, FENG Su-ling2
A simple and highly sensitive fluorimetric method for the determination of Cr(Ⅵ) was developed in the present paper. The method is based on the fluorescence enhancement of acridine red with Cr(Ⅵ) in the sulfuric acid medium. The effects of some experimental conditions on the determination of Cr(Ⅵ) were investigated in detail. The detection limit for Cr(Ⅵ) is 0.6 μg·L-1, and the linear range of the determination is 2.0-32 μg·L-1. The relative standard deviation of 11 replicate measurements is less than 2.0%. The proposed method has been successfully used to determine Cr(Ⅵ) in electroplating solution, waste chromic acid mixture,and alloy steel samples. The results obtained were compared with the certified values of Cr(Ⅵ) in standard samples and those provided by 1,5-diphenylcarbazide method with satisfaction.
2006 Vol. 26 (07): 1294-1297 [Abstract] ( 1607 ) PDF (932 KB)  ( 444 )
1298 Studies on the Mechanism of the Interaction between Hydrazide-Podophyllic Ni(Ⅱ), Co(Ⅱ), Zn(Ⅱ) Metal Complexes and DNA
WANG Ping-hong1, ZHANG Qi1*, YUAN Wen-bing1, WANG Liu-fang2, SONG Yu-min3, LIU Hui-hong1
The mechanism of the interaction between hydrazide-podophyllic (HDPP) metal (Me) complexes and calf thymus (ct) DNA in Tris buffer (pH 7.08) was studied by viscosity measurements, electronic absorption, gel electrophoresis, and ethidium bromide (EB) fluorescence spectroscopy. The results from varied experiments show that the intensity of the maximal absorption peaks from absorption spectra is weakened in the presence of DNA compared with that in the absence of DNA. Meanwhile, DNA can remarkably quench the emission intensity of the complex Me-HDPP system. The Me-HDPP complexes can increase the viscosity of ct DNA slightly and catalyze the cleavage of super coiled pBR322 DNA to the nicked form. The complexes of Ni-HDPP and Co-HDPP can be bound to ct DNA mainly by interaction, while the partial interaction of Zn-HDPP and ct DNA is the major modes. The binding constant of Me-HDPP complexes with ct DNA was determined.
2006 Vol. 26 (07): 1298-1302 [Abstract] ( 1031 ) PDF (904 KB)  ( 512 )
1303 Decoloring and Spectral Properties Analysis of Innoxious Ultraviolet
FANG Yi-wen1, NI Wen-xiu1, HUANG Chong2, XUE Liang1, YU Lin1
The ultraviolet absorbent extracted from mango leaves, was discolored by some decoloring agent. Then the spectral properties of the discolored ultraviolet absorbents were analyzed. The discolored method of ultraviolet absorbent was studied by comparing one with the others. The results showed that the discoloring effect was satisfactory by using active carbon, H2O2, citric acid, and oxalic acid as decoloring agent. Specially, when oxalic acid was used as decoloring agent, the color of the production was slight, the rate of production was high, and the absorption effect of ultraviolet ray was well. When the concentration of the ultraviolet absorbent solution is 0.5%(w/w), the ultraviolet ray transmission was smaller than 0.3% in 200-370 nm, and it increased slightly from 370 nm. There was a maximum value at 400 nm, approaching 12%.
2006 Vol. 26 (07): 1303-1305 [Abstract] ( 1553 ) PDF (894 KB)  ( 487 )
1306 Study on the Spectral Properties of Nickel Tetrasulfo-Phthalocyanine Doped Vinyl Modified Silicate Glass
LIN Ai-mei, ZHAN Hong-bing*, CHEN Wen-zhe
Nickel tetrasulfo-phthalocyanine(NiTSPc) was successfully doped into vinyltriethoxysilane(VTES)modified silicate gel glass by sol-gel technique, IR and UV-Vis spectral examination was carried out. The results show that vinyl has been introduced into SiO2 network, and the structure of gel glass is therefore changed. The encapsulation of NiTSPc does not make any noteworthy changes in the composition and structure of gel glass matrix. NiTSPc molecules are well dispersed in the organic modified matrix, and the phenomenon of aggregation is greatly suppressed.
2006 Vol. 26 (07): 1306-1309 [Abstract] ( 501 ) PDF (871 KB)  ( 456 )
1310 Fluorescence Spectral Characteristics of Human Blood and Its Endogenous Fluorophores
LI Bu-hong1,2,ZHANG Zhen-xi1,XIE Shu-sen2,CHEN Rong2
The three-dimensional fluorescence spectra and excitation-emission matrix of human blood were measured, and an attempt was made to exploit the endogenous fluorophores of major peaks in the UV and visible. The result indicates that the absorption peaks of human blood appear at 274, 345, 415, 541 and 576 nm. Based on the analysis of fluorescence excitation-emission matrix, the major emission peaks of human blood occur at excitation-emission wavelength pairs of 260-630, 280-340, 340-460 and 450-520 nm, which are attributed to endogenous porphyrins, tryptophan, reduced nicotinamide adenine dinucleotide (NADH) or reduced nicotinamide adenine dinucleotide phosphate (NADPH), and flavin adenine dinucleotide (FAD), respectively. These results can be used to analyze and explain the effect of blood on the distortion of fluorescence signal of human tissues for optical diagnosis.
2006 Vol. 26 (07): 1310-1313 [Abstract] ( 1419 ) PDF (969 KB)  ( 739 )
1314 Spectrometry Study on the Interaction of Magdala Red and Bovine Serum Albumin
SHI Yan, YE Fan-di, ZHENG Wei-wan
In the present paper,the interaction of Magdala red and bovine serum albumin(BSA) was studied by UV-absorption and fluorescence spectrometry. The results of UV-absorption spectrometry show that the way of the interaction of Magdala red and BSA should obey the Scatchard Model. In other words, Magdala should be combined to some certain regions of BSA. Meanwhile, taking advantage of fluorescence quenching, the reaction mechanism of Magdala with BSA was explored. Protein molecule conformation change is discussed by synchronous fluorescence spectrometry.
2006 Vol. 26 (07): 1314-1317 [Abstract] ( 1081 ) PDF (962 KB)  ( 575 )
1318 Application of L-Cysteine-Capped Nano-ZnS as a Fluorescence Probe to the Determination of Proteins in Human Serum
ZHAO Dan-hua1, LI Yong-xin2,ZHU Chang-qing2
Nanometer-sized L-cysteine-capped ZnS particles as a fluorescence probe were synthesized, and the effect of proteins on the fluorescence intensity has been investigated. With Δλ=190 nm, the maximum and constant synchronous fluorescence enhancement was produced at 268.0 nm and pH 5.12 in the presence of proteins. A highly sensitive synchronous fluorescence method for the rapid determination of proteins was developed. Under optimum conditions, the calibration curve was linear over the range 0.05-6.0 μg·mL-1 for human serum albumin (HSA), and 0.05-8.0 μg·mL-1 for γ-globulin(γ-G), respectively. The relative standard deviations of seven measurements were 1.90% for 1.0 μg·mL-1 HSA, and 1.65% for 1.0 μg mL-1 γ-G.
2006 Vol. 26 (07): 1318-1321 [Abstract] ( 1028 ) PDF (969 KB)  ( 491 )
1322 Spectrophotometric Determination of Heparin with Neutral Red
SUN Wei, DING Ya-qin, RAO Jun, JIAO Kui
The interaction of neutral red and heparin was studied by UV-Vis spectrophotometry in pH 3.0 Britton-Robinson (B-R) buffer solution. Neutral red has a strong absorbance at 523 nm and the addition of heparin into neutral red solution resulted in the decrease in the absorbance value at 523 nm without the appearance of new absorbance peak. The decrease in absorbance value was linear with the concentration of heparin. The conditions for the interaction were optimized and the interferences of coexistent substances were investigated. Under the optimal conditions a linear regression equation was obtained as ΔA=0.044+0.076c(mg·L-1) (n=12, r=0.997) in the range of 0.10-15.0 mg·L-1 with the detection limit of 0.073 mg·L-1. The molar absorptivity of the method was calculated to be 2.037×106 L·mol-1·cm-1. The method was applied to determine the heparin sodium injection solution with satisfactory results. The stoichiometry of heparin with neutral red was calculated as 1∶3.
2006 Vol. 26 (07): 1322-1325 [Abstract] ( 382 ) PDF (916 KB)  ( 654 )
1326 Principal Component Analysis and Cluster Analysis of Inorganic Elements in Panax Quinquefolium. L
CHEN Jun-hui1, XIE Ming-yong1*, FU Bo-qiang2, YANG Miao-feng2, WANG Xiao-ru2
The contents of elements such as Mg, Al, P, Ca, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd and Pb in twelve Panax quinquefolium. L samples were determined by means of ICP/MS. The results were used for the development of element fingerprint chromatogram. The principal component analysis of SPSS was applied for the study of characteristic elements in Panax quinquefolium.L. Five principal components which accounted for over 90% of the total variance were extracted from the original data. The analysis results show that Fe, Al, V, Mn, Mg, Sr, Mo, Ca and Cu may be the characteristic elements in Panax quinquefolium.L. The results of Q-type cluster analysis show that the samples could be clustered reasonably into five groups, and the elemental distribution characteristics are related to the breeds of Panax quinquefolium.L.
2006 Vol. 26 (07): 1326-1329 [Abstract] ( 472 ) PDF (902 KB)  ( 718 )
1330 Determination of Rare Earth and Microelements in Chinese Herbal Medicine by Inductively Coupled Plasma Mass Spectrometry
WANG Song-jun1,2, CAO Lin3, CHANG Ping4, HOU Tian-ping5, HOU Yue6
In this article, through the condition experiment of simultaneous determination of rare earth and trace elements in wolfsbane by inductively coupled plasma mass spectrometry(ICP-MS),the methods of low temperature ashing and nitric acid-overoxidation hydrogen(HNO3-H2O2) were compared. It was proved that the sample disposed with low temperature ashing for microelements and the sample disposed with acid digestion for rare earth satisfied the request for the method of determination. The accuracy is between 1.21% and 15.15%, and the precision is between 0.38% and 8.54%. The data of the experiment proved that the method completely satisfied the request for the determination of rare earth and microelements in the sample of Chinese herbal medicine.
2006 Vol. 26 (07): 1330-1333 [Abstract] ( 1587 ) PDF (825 KB)  ( 837 )
1334 Study on the Method for the Determination of Soil Available B by ICP-MS
WANG Yan-ze1,SHI Yan-zhi1*,ZHANG Hua1,WANG Ying-feng1, CHEN Yu-hong2
A method was established for the determination of soil available B by inductively coupled plasma mass spectrometry(ICP-MS). Compared to the traditional method for B analysis, the recommended method does not need filtration, so it escapes the contamination. The method not only proved simple and rapid, but also showed satisfying precision and accuracy. The detection limit of this method is 0.009 ng·g-1. The relative standard deviation is 2.66%, and the recovery is 93.0%-102.0%.
2006 Vol. 26 (07): 1334-1335 [Abstract] ( 1564 ) PDF (871 KB)  ( 734 )
1336 Study of Determination Method of Trace Elements in White Jade Snail
XIN Shi-gang, WANG Ying, ZHOU Wan-qiu
The contents of six trace elements, Ca, Mg, Fe, Zn, Cu and Co, in white jade snail were determined by ICP-AES and AAS using nitrifying method of high pressure nitrifying pot. The results of two analysis methods were compared, showing no obvious differences. The recoveries were 92.4%-103.0%, and the relative standard deviations were less than 2.98%. The experiment proved that white jade snail contains rich useful trace elements, and is a kind of green food with high nutrition.
2006 Vol. 26 (07): 1336-1338 [Abstract] ( 1034 ) PDF (823 KB)  ( 500 )
1339 Study on Determination of Metal Elements in Buds of Syzygium Aromaticum(L.)Merr. et Perry by ICP-AES
ZHANG Sheng-bang,GUO Yu-sheng
Determination of metal elements in buds of Syzygium aromaticum(L.)Merr. et Perry was studied by ICP-AES after HNO3-H2O2 digestion. The average recovery of the method for K,Mg, and trace elements such as Cu,Fe,Cr,Zn,Mn and Pb in the buds of Syzygium aromaticum(L.)Merr. et Perry was found to be 91.8%-112.2%,while RSD (n=5) is 0.4%-4.9% for the metal elements. The method was applied to the analysis of some practical samples, and the results obtained were satisfactory. There is rich Mn in the samples. It is of important significance to assess the value of the Chinese medicine by the determination of trace elements in Chinese medicine with ICP-AES.
2006 Vol. 26 (07): 1339-1341 [Abstract] ( 978 ) PDF (882 KB)  ( 444 )
1342 Determination of Copper and Chromium in the Cartridges of Permanent Marker Pen and Ink by ICP-AES
DUAN Xu-chuan
The method for the determination of copper and chromium in the cartridges of permanent pen oil base and ink by ICP-AES was reported. This mainly concerned the different methods for pretreatment of samples. The study indicated that the better method for the pretreatment of the cartridges of permanent pen and the ink containing resin is dry ashing at 550 ℃ followed by wet-decomposition with mixed acid (VHNO3VHClO4=3∶1); the better method for the pretreatment of water soluble ink is hydrodigestion with mixed acid (VHNO3VHClO4=3∶1 ). After suitable dilution with acid, copper and chromium were determinated by ICP-AES. It was shown that the method is reliable for the test of precision and accuracy. RSD and recovery were in the range of 5.9%-7.9% and 90%-104%, respectively.
2006 Vol. 26 (07): 1342-1344 [Abstract] ( 1024 ) PDF (889 KB)  ( 543 )
1345 Determination of Pb and Cd in Environmental Water Sample by On-Line Mini-Column Preconcentration and Flow Injection-Flame Atomic Absorption Spectrometry
WANG Ai-xia, GUO Li-ping, WU Dong-mei
Trace Pb and Cd in environmental water samples were preconcentrted and determined by on-line mini-column field sampling and flow injection-flame atomic absorption spectrometry(FI-FAAS), and the adsorption materials of the column were activated carbon loaded 8-HQ,DDTC and APDC. Satisfactory results of the determination of Pb and Cd in the certified reference materials(trace elements in water GBW 08608) and the South lake water were obtained by using the above method. The detection limit of 10 mL enrichment of Pb and Cd was 1.58 and 0.062 μg·L-1, respectively, and the relative standard deviation of Pb and Cd was 1.62% and 1.96% respectively.
2006 Vol. 26 (07): 1345-1348 [Abstract] ( 2118 ) PDF (841 KB)  ( 596 )
1349 Determination of Trace Lead in Water Samples and Salt Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction
ZHANG Yuan, LUO Wen-hong*, LI Hui
A method was developed for the determination of trace lead in water samples and salt samples by GFAAS after cloud point extraction. The parameters of extraction system such as pH, the concentrations of the extractant and the surfactant, and the time for cloud point extraction were optimized. Under the optimized conditions, the detection limits of lead were 0.000 5 μg·g-1 for salt, and 0.01 μg·L-1 for water, respectively. The proposed method was applied to the determination of lead in water samples and salt samples, and satisfactory results were obtained.
2006 Vol. 26 (07): 1349-1351 [Abstract] ( 1815 ) PDF (834 KB)  ( 492 )
1352 Simultaneous Determination of Trace Arsenic and Antimony in Textile by Intermittent Flow-Hydride Generation-Atomic Fluorescence Spectrometry with L-Cysteine as a Prereducer
Lü Shui-yuan, DAI Jin-lan, ZHONG Mao-sheng
A method for the simultaneous determination of trace arsenic and antimony in textile by intermittent flow-hydride generation-atomic fluorescence spectrometry with L-cysteine as a prereducer was developed. The optimal instrument condition was established. The influence factors such as the acidity of sample solution and carrier liquid, the concentrations of KBH4 and L- cysteine, the flow rate of carrier, and the interference of coexistent elements were investigated. The method was convenient and rapid. Under the optimal condition, the detection limits were 0.35 and 0.22 μg·L-1, the relative standard deviations were 1.3% and 2.8%, and the recoveries were in the ranges of 93.6%-98.4% and 92.2%-103.6% for As and Sb respectively.
2006 Vol. 26 (07): 1352-1355 [Abstract] ( 530 ) PDF (906 KB)  ( 574 )
1356 Measurement of NO2 Concentration in Atmosphere in Chengdu by Solar Spectra
ZUO Hao-yi1, GAO Jie1, CHENG Juan1, Andrew Yuk Sun Cheng2, YANG Jing-guo1*
In the present paper, a new improved method for measuring NO2 concentration of atmosphere by using differential optical absorption spectroscopy of solar spectrum was reported. The sample solar spectra were collected in Chengdu city and Xiling Mountain respectively by a CCD optical multi-channel analyzer. With the upper atmosphere solar spectrum as the reference spectrum, by fitting the sample spectrum and the reference spectrum using least-square method in five spectrum ranges, the various NO2 concentrations(vertical column density) of 3.1×1016 to 5.8×1016(molecule·cm-2)in Chengdu city and 0.7×1016 to 1.0×1016(molecule·cm-2)in Xiling Mountain were obtained respectively. The NO2 concentrations of atmosphere showed an increasing tendency with the rising temperature.
2006 Vol. 26 (07): 1356-1359 [Abstract] ( 416 ) PDF (872 KB)  ( 804 )
1360 Studies on the Synthesis of Zeolite 4A in Mirowave Field by Means of X-Ray Diffraction
ZHONG Sheng-liang, ZHANG Mai-sheng*, SU Qiang
Good quality zeolite 4A with homogenous particle size, high whiteness and high calcium exchangeability was successfully synthesized in microwave field. The effects of the ratio of silica to aluminium, the ratio of water to sodium, the power of microwave, and the time of microwave heating on the synthesis of zeolite 4A were studied by means of X-ray diffraction. And the products were also characterized by IR, SEM and DSC. The optimal condition for the synthesis of zeolite 4A in microwave was found.
2006 Vol. 26 (07): 1360-1363 [Abstract] ( 1029 ) PDF (976 KB)  ( 513 )
1364 Differential Kinetic Spectrophotometric Determination of Chlorpromazine Hydrochloride and Promethazine Hydrochloride by Chemometric Method
NI Yong-nian,QI Zheng-bao
Chlorpromazine hydrochloride and promethazine hydrochloride were oxidized fastly resulting in red intermediate product, which was then gradually changed into a colorless product by ammonium cerous sulfate in appropriate acidic medium. The chemometric multivariate calibration methods, such as partial least squares (PLS) and principal components regression (PCR) were applied to the resolution of the kinetic curves to determine these two compounds. The linear ranges are 8.3-66.7 mg·L-1 and 3.3-26.7 mg·L-1 for chlorpromazine and promethazine, respectively. The limits of detections are 2.32 and 0.95 mg·L-1 for these two compounds, respectively. This method was successfully applied to the analysis of pharmaceutical samples with satisfied results.
2006 Vol. 26 (07): 1364-1367 [Abstract] ( 1660 ) PDF (854 KB)  ( 478 )
1368 Stellar Spectral Recognition Based on Wavelet De-Noising and SVM
XING Fei,GUO Ping*
present paper describes a new technique for stellar spectral recognition. Considering the characteristics of stellar spectral data, support vector machine (SVM) was adopted to build a recognition system as kernel. Because stellar spectral data sets are usually extremely noisy, the correct classification rate of direct applying SVM is low. Consequently, wavelet de-noising method was proposed to reduce noise first and extract the main characteristics of stellar spectra. Then SVM was used for the recognition. Based on the real-world stellar spectra contributed by Jacoby et al. (1984), it has proven that there will be a better performance using this composite classifier which combines wavelet and SVM than using SVM with principle component analysis data dimension reduction technique. From the experiment of comparison of discriminant analysis and SVM based on stellar spectra for evolutionary synthesis, we can see that the correct classification rate of SVM is higher than that of discriminant analysis methods, and a well generalization ability is achieved.
2006 Vol. 26 (07): 1368-1372 [Abstract] ( 1090 ) PDF (889 KB)  ( 567 )