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2004 Vol. 24, No. 05
Published: 2004-05-26
 
       光谱学与光谱分析
513 Saltation Behavior in Excitation Spectra of Fluorescent Molecules
MIAO Di, XU Yi-zhuang, YANG Jun, XU Zhen-hua, WU Jin-guang*
Excitation spectra are commonly used to study relationship between molecular structure of fluorescent substances and energy transfer during the fluorescence process. It is generally taken for granted that the excitation spectrum of the sample is equivalent to its absorption spectrum, even a copy of the latter. However, exceptions have been found in many cases. Considering various factors that affect the excitation spectra of solution comprehensively, a model has been established to study the behavior of the excitation spectra. After analyzing the model mathematically, including introducing catastrophe theory, we came into the following conclusions: As far as the topological properties are concerned, the excitation spectra are the same as its absorption spectra, provided the concentration of the substance is below a threshold. However, when the concentration is beyond the threshold, the excitation spectra undergo a series of topological saltation, leading to significant a deviation from the absorption spectra. Comparative studies of both excitation and absorption spectra of naphthalene dissolved in n-hexane confirmed the above hypothesis.
2004 Vol. 24 (05): 513-518 [Abstract] ( 1625 ) PDF (1089 KB)  ( 415 )
519 Luminescence Properties of A New Kind of Rare Earth Complexes Tb(m-benzoicacid)3
LIU Jun-feng1，TENG Feng1*，XU Zheng1，HOU Yan-bing1，LI Yong2, XU Yi-zhuang2, WU Jin-guang2
The luminescence properties of a new kind of rare earth complex Tb (m-benzoicacid)3 were studied. With the new complex as the dopant and PVK as the host, the film of the mixed system was made, from whose spectra the authors learned that a highly efficient energy transfer process exists. The energy transfer is related to the mass proportion, and the more the mass proportion of Tb in the doped system, the more the emission proportion, and at the same time the emission of PVK is relatively weak. When the mass proportion of Tb(m-benzoicacid)3： PVK is higher than 20%, the emission of Tb is stronger than that of PVK, and plays the main role, while the emission of PVK disappears. The authors used the PVK:Tb(m-benzoicacid)3 system as the emission layer and Alq as the electron-transfer layer, thus the device，whose structure is ITO/PVK:Tb(m-benzoicacid)3/Alq/LiF/Al was formed. From the spectrum of this device, the characteristic emission of Tb can be observed. At the bias voltage of 21 V, a brightness 311 cd·m-2 was achieved.
2004 Vol. 24 (05): 519-523 [Abstract] ( 1493 ) PDF (889 KB)  ( 317 )
524 Optical Properties of Human Normal Small Intestine Tissue with Theoretical Model of Optics about Biological Tissues at Ar+ Laser and 532 nm Laser and Their Linearly Polarized Laser Irradiation in Vitro
WEI Hua-jiang1，XING Da1*，WU Guo-yong2，JIN Ying1，GU Huai-min1
A double-integrating-spheres system, basic principle of measuring technology of ray radiation, and optical model of biological tissues were used for the study. Optical properties of human normal small intestine tissue at 476.5, 488, 496.5, 514.5 and 532 nm laser and their linearly polarized laser irradiation were studied. The results of measurement showed that the total attenuation coefficient and scattering coefficient of the tissue at these wavelengths of laser and their linearly polarized laser irradiation increased with decreasing wavelengths. And obviously there was a distinction at 514.5 to 532 nm wavelength between lasers and their linearly polarized laser irradiation. Absorption coefficient of tissue at these wavelengths of laser and their linearly polarized laser irradiation increased with decreasing wavelengths. Absorption coefficient of tissue at 514.5 to 532 nm wavelength of laser was obviously decreasing，which was independent of these wavelengths of laser or their linearly polarized laser irradiation. Mean cosine of scattering of tissue at these wavelengths of laser and their linearly polarized laser irradiation also increased with decreasing wavelengths. But penetration depth of tissue at these wavelengths of laser and their linearly polarized laser irradiation also increased with increasing of wavelengths. Refractive index of tissue between these wavelengths of laser was within 1.38 to 1.48. Absorption coefficient, scattering coefficient, total attenuation coefficient, effective attenuation coefficients of tissue in Kubelka-Munk two-flux model at the same wavelength of laser and their linearly polarized laser irradiation showed no prominent distinction (P＞0.01). Absorption coefficient, scattering coefficient, total attenuation coefficient, effective attenuation coefficients of tissue in Kubelka-Munk two-flux model at different wavelength of laser and their linearly polarized laser irradiation showed obvious distinction. Optical properties of tissue at 514.5 to 532 nm wavelength of laser eｘhibited obvious distinction.
2004 Vol. 24 (05): 524-528 [Abstract] ( 1560 ) PDF (959 KB)  ( 348 )
529 The Experiment Study on the Resolution of Electro-Optical Imaging System at EUV Wave Band
XUE Ling-ling, CHEN Bo, LI Yu-min
An imaging system based on a Microchannel Plate(MCP) detector was designed to image the Eｘtreme Ultraviolet(EUV) light. The images of a 3 mm-width-slit were presented by this imaging system at the wavelengths of 13，17.1，19.5 and 30.4 nm respectively． Their corresponding spatial resolutions are 85，120，182 and 495 μm respectively． The best is 85 μm，corresponding to 13 nm． Moreover，the shorter the wavelength，the better the spatial resolution． So is the brightness of the image.
2004 Vol. 24 (05): 529-531 [Abstract] ( 1067 ) PDF (1079 KB)  ( 357 )
532 Structural Characteristics of Infrared Spectra for Polyaluminum Chloride in Enhanced Reactions of Modification
ZHOU Feng-shan1，WANG Shi-hu2，SU Jin-zhu3，SUN Hu3，DING Jie1，XU Yi-zhuang1，WU Jin-guang1
As an important preparation method of Inorganic Polymer Flocculants (IPFs) with all-round performance, the use of enhanced reactions of modification for Polyaluminum Chlorides (PAC) is a trend of application. In this paper, auctorial-made multicore oligomers as a complexing agent, polysilicate as a crosslinking agent and polyacrylamide as a compounding agent are respectively used to enhance PAC and prepared three kinds of IPFs, named CO-PAC, CR-PAC and PAM-PAC. The Fourier Transform Infrared spectra (FTIR) of the three flocculants show that there have been found new chemical bonds beyond Al—OH in their structures, and each characteristic band of primary group in PAC has a band shift to a lower frequency dure to its structural aberration． These evidences suggested that enhanced reactions of modification for PAC are not at all a simple process of physical mix, but a chemical reaction to form other structural characteristics of inorganic polymers. The excellent coagulation behavior of these new flocculants depends mainly on the chemical actions，but there are a little physical effects between the modifiers and PAC.
2004 Vol. 24 (05): 532-535 [Abstract] ( 1003 ) PDF (918 KB)  ( 352 )
536 The Interaction between La and Polyurethane System
LIU Zhi1, LIU Xin-hai2, CAO Chi-cheng3，SUN Xian-yu1, WENG Shi-fu1, XU Duan-fu2, WU Jin-guang1*
A series of polyether polyurethane (PU)-LaCl3 composites with different lanthanum contents were prepared. DSC results indicate that LaCl3 promotes phase transition behavior of the LaCl3/PU composites, which causes the endothermic peak at 11.58℃ to disappear. FTIR spectroscopy demonstrates that significant variation can be observed. The peak at 1 633 cm-1 attributed to carbonyl vibration and the peak at 3 311 cm-1 attributed to N—H stretching band moves to 1 647 cm-1 and 3 355 cm-1，respectively, when LaCl3 is introduced into the PU system. A new band (-200 cm-1) assigned to the La—O band was observed, and the far IR result provided a direct evidence of the coordination between La3+ ion and CO group of PU system.
2004 Vol. 24 (05): 536-538 [Abstract] ( 235 ) PDF (869 KB)  ( 371 )
539 Study of the Nucleation Sites in Collagen Mineralization
HUANG Zhao-long1，2，ZHANG Wei1, CUI Fu-zhai1*
By comparing IR spectra of collagen, collagen/CaCl2 and collagen/calcium phosphate, it was found that intensities of amide Ⅰ, Ⅱ and Ⅲ bands were significantly decreased after mineralization. Band amide Ⅰ shifted to wards lower wave number. This shift indicated chemical interaction between carboxyl groups and Ca ions formed in tie mineralization. The result indicated that there was another nucleation site, i.e. carbonyl (CO) on collagen, besides the previous reported nucleation site of carboxyl (—COOH) on collagen. The decrease of amide Ⅰ peak intensity was mainly due to blockage of CO stretch. Comparing the IR spectra of demineralized collagen and pure collagen, amide Ⅰ, Ⅱ and Ⅲ peaks intensity and position were almost the same. When the mineral dissolved, amide peaks rebounded，which indicated that the crystals nucleated on these sites enwrapped the groups and blocked the groups vibration. The decreases of peak intensity of amide Ⅰ, Ⅱ and Ⅲ were different due to their different vibration modes. The result confirmed that the carbonyl group was one kind of the nucleation site during collagen mineralization. The relationship between the process of collagen mineralization and variety of amide bonds was also studied.
2004 Vol. 24 (05): 539-542 [Abstract] ( 1033 ) PDF (1627 KB)  ( 568 )
543 Adsorption Studies of γ-Aminopropyltrimethoxysilane on Iron Surfaces by Surface-Enhanced Raman Spectroscopy
CHEN Hui1, SHEN Xiao-ying1, GU Wei1, GU Ren-ao1*, LIU Jin-xuan2, REN Bin2*, TIAN Zhong-qun2
The films of γ-aminopropyltrimethoxysilane (γ-APS) on iron electrode surfaces were studied. The silane films were characterized by in-situ Surface-Enhanced Raman Spectroscopy (SERS). It has been found that the potential-dependent Surface-enhanced Raman Spectroscopy are useful for diagnosing the formation and structure of γ-APS moieties bound onto the surface of metal substrates. Results of SERS indicated that the silanol and amino groups were adsorbed competitively on the metal surfaces. At the same time, the electrode potential, and illumination of laser all have great influence on the nature of these head groups. It was also found that the different states of amine transformed with the change in the potential.
2004 Vol. 24 (05): 543-546 [Abstract] ( 894 ) PDF (877 KB)  ( 313 )
547 The Applications of SERS to Labeled Immunoassay
QIU Li-qun, GU Ren-ao*
Combining the high sensitivity of a variety of readout technologies with the specific adsorption between antibody and antigen, labeled immunoassay possesses a remarkable effect in microanalysis. The discovery and confirmation of Surface enhanced Raman Spectroscopy (SERS) made Raman spectroscopy a powerful tool in many research fields, especially in biomedicine. In this report, the authors describe the applications of the high sensitivity of SERS to labeled immunoassay, and introduce some work in this field by our laboratory.
2004 Vol. 24 (05): 547-550 [Abstract] ( 539 ) PDF (916 KB)  ( 441 )
551 Surface-Enhanced Raman Scattering (SERS) of Amino Acids on Silver Colloid
KE Wei-zhong, WU Jian-zhong
The surface-enhanced Raman spectra of glycine, valine and lysine adsorbed on silver colloidal particles and the Raman spectrum of lysine in aqueous solution were obtained. The adsorption was accompanied by the appearance of the 238 cm-1 band corresponding to the oscillation of the molecule-metal chemical bond and indicating chemisorption of the amino acid. In the surface-enhanced Raman spectra of three amino acids, the peak bands at 900-930 cm-1, near 1 100 cm-1 and near 1 400 cm-1, corresponding to the carbon-carbon bond, carboxyl and amino group vibrations, respectively, were markedly increased on the silver colloidal particles. It means that the Raman spectra of polar groups such as COO-, NH2 and C—COO- were strongly enhanced via the carboxyl group. There was no influence under the low pH condition in the experimental system used.
2004 Vol. 24 (05): 551-553 [Abstract] ( 974 ) PDF (839 KB)  ( 727 )
554 Study on the Rapid and Nondestructive Identification of TCM Formula Particles by FTIR
TANG Jun-ming1, 2，SUN Su-qin1*，YUAN Zi-min1，QIN Zhu1
Formula particles made by Traditional Chinese Medicines (TCM) were studied systematically via Fourier Transform Infrared Spectroscopy (FTIR) in this paper. The products quality of different pharmaceutical factories (Guangdong Yifang, Jiangyin Tianjiang, Sanjiu Yiyao, Hongkong Purapharm) could be revealed directly in the FTIR spectra. Also the spectra of different batch numbers (same factory), particles before and after processing, and particles with different processing methods were studied. It is proved that FTIR is an effective, fast and advanced method to evaluate the production qualities.
2004 Vol. 24 (05): 554-556 [Abstract] ( 1701 ) PDF (818 KB)  ( 494 )
557 Spectroscopic Studies of Compounds with [(PO4)4MoⅤ6O15]12- Cluster
ZHANG Han-hui1, 2，LIN Zheng-zhong1, 2，HUANG Chang-cang1，SUN Rui-qing1，WU Xiao-yuan1，LIN Zhi-hua1
Five novel organic-molybdenum phosphates with [(PO4)4MoⅤ6O15]12- cluster, Na·(H4TETA)3·(H3O)5·{Zn[(HPO4)2(PO4)2Mo6O15]2} (2)，(H2en)7·(H3O)4·{Cu[(HPO4)2(PO4)2 Mo6O15]2}·H2O (3)，(H3DETA)2·(H3O)3·{Co0.5[(HPO4)2(PO4)2Mo6O15]}·H2O (4)，[Co(H3TETA)]2{Co0.5[(HPO4)(PO4)3Mo6O15]}·3.5H2O (5) and (H3DETA)·(H3O)4·{Co1.5[(HPO4)2(PO4)2Mo6O15]}·0.5H2O (6)，have been synthesized. The relationship between their properties and structures was studied by using FTIR，NIR FT-Raman，UV-Vis DRS and fluorescence etc. In these compounds, every two [(PO4)4Mo6 O15] clusters are coordinated by a metal atom to form a {M[(PO4)4Mo6 O15]2} dimer. In compound 2, 3 and 4, {M[(PO4)4Mo6 O15]2} dimers are hydrogenbonded by the organic molecules and water molecules to form a three-dimensional expended framework, respectively. In compound 5 and 6, {Co[(PO4)4Mo6 O15]2} dimers are coordinated by [Co(H3TETA)] groups and [CoO4] tetrahedra to form a network, respectively. These characteristic vibrational frequencies of the molybdenum phosphates are related to the structure of these compounds. Three characteristic bands in UV-Vis DRS spectra of these compounds have to be attributed to the absorptions of Od→Mo, Oμ→Mo and O→M charge transfer, respectively. These compounds exhibit strong fluorescence emission bands at about 410 nm when excited by 240 nm，which are caused by Oμ→Mo charge transfer.
2004 Vol. 24 (05): 557-560 [Abstract] ( 1550 ) PDF (916 KB)  ( 334 )
561 Study on Preparation and Optical Spectroscopy of Nickle Phthalocyanine-Doped Sol-Gel Materials
ZHAN Hong-bing1，2, CHEN Wen-zhe1, LI Guang-hui1, WANG Min-quan2
We report here the preparation of nickle tetrasulfo-phthalocyanine (NiTSPc)-doped silica xerogel matrix obtained by sol-gel technique. The evolution of silica matrix′s texture and the rate during the sol-gel process, as well as silica xerogel′s pore structure were studied. Dimerization behavior of NiTSPc molecules was characterized by electronic absorption spectra，and changes in the absorption spectra were correlated with various stages of the sol-gel process. The results show that in the composites NiTSPc concurs in the forms of monomer and dimer，and dimerization is stronger during the latter stages. The reason is given from the change in the micro-environment in which NiTSPc existed during the sol-gel process.
2004 Vol. 24 (05): 561-564 [Abstract] ( 1558 ) PDF (879 KB)  ( 310 )
565 Synthesis and Spectroscopic Studies of Supermolecules of PWxV12-x-MV
WU Xiao-yuan1，ZHANG Han-hui1，2*，HUANG Chang-cang1，SUN Rui-qing1，YANG Qi-yu1，LIN Zhi-hua1，CHEN You-xing1
A series of supermolecules of PWxV12-x-MV( PWxV12-x: polyoxometalates x=2, 4, 6, 8, 10; MV: methyl violet ) with Keggin structure were prepared and their characters were studied by electronic spectra, infrared spectra and fluorescence spectra. As a result, the supermolecules were formed by the cooperating action between polyoxometalates and methyl violet. In the supermolecule, the structures of cation and anion are not destroyed. With the content of V increasing, the oxidation ability of polyoxometalates anion is enhanced, and the interaction of methyl violet cation and polyoxometalates anion is enhanced too. The FTIR absorption peaks of νas(MOt), νas(M—Ob—M) and νas(M—Oc—M) move from 966, 886, and 804 cm-1 to 955, 875 and 786 cm-1，respectively; the UV-Vis absorption peak moves from 519 to 506 nm; the emission peak excited at 530 nm moves from 692 to 644 nm too. These changes are according with the degree of the interaction of polyoxometalates and methyl violet.
2004 Vol. 24 (05): 565-568 [Abstract] ( 1567 ) PDF (932 KB)  ( 414 )
569 Raman Spectroscopic Study of Boron Carbonitride Nanotubes
ZHANG Hong-rui1，DING Pei1，GUO Xing-yong2，LIANG Er-jun1
Raman spectra of boron carbonitride(BCN) nanotubes made by thermal decomposition under different temperatures and with different catalysts were analysized. The intensity ratio of D to G band, ID/IG, increases and then decreases with the increase of the temperature. It was indicated that there exists an optimal temperature under which B and N incorporation is maximum. The catalysts influence also the Raman spectra of the BCN nanotubes. ID/IG is higher with cobalt/ferrocene and nickel/ferrocene than with cobalt, nickel and cobalt/nickel as catalysts. This means that better BCN nanotubes with B and N contents can be produced with the former. The results were confirmed by TEM observation.
2004 Vol. 24 (05): 569-572 [Abstract] ( 1543 ) PDF (3829 KB)  ( 472 )
573 Synthesis and Spectral Characterization of 4-Amino-4’-Chlorobenzophenone
WANG Xiao-yan, HUANG Xiang-hong
4-nitro-4’-chlorobenzophenone has been synthesized from p-nitrobenzol chloride and chlorobenzene in the presence of catalyst anhydrous AlCl3 and 4-amino-4’-chlorobenzophenone as an important organic intermediate was prepared by reduction of 4-nitro-4’-chlorobenzophenone with Na2S2. With the aid of orthogonal experiments the optimum reaction conditions were determined : reaction temperature 92℃, time 2.5 h, 4-nitro-4’-chlorobenzophenone: Na2S2=1∶1.7(mol), yield 85.80%, purity 98.08%, m.p. 177-179℃. The molecular structure of the title compound has been characterized by Elemental Analysis(EA), 1H and 13C Nuclear Magnetic Resonance Spectrometry(NMR), Infrared Spectroscopy(IR)，and Mass Spectroscopy (MS)，and the main infrared absorption peaks and nuclear magnetic spectral bands of this compound were assigned. The mass spectral fragmentations of the product’s important fragment ions were elucidated. The result provides useful information for developing substitutes of non-cancer-causing forbidden dye intermediate.
2004 Vol. 24 (05): 573-575 [Abstract] ( 1027 ) PDF (883 KB)  ( 373 )
576 Resonance Raman Spectra of Single Red-Cell from Human Blood
YAN Xun-ling1, DONG Rui-xin1，2 , WANG Qiu-guo1
Resonance Raman spectra of single redcell from human blood are presented by different laser sources. It is reported that there is 1 002 cm-1 line of insensitive conformation of phenylalanine aromatic ring stretching and 1 620 cm-1 line of C—N breathing stretching band of pyrrole ring，which cause strong and sharp resonance lines when eｘcited by 782 nm laser source. They are weaker and the intensity of other lines of high wave number is large and clear when excited by 514 nm laser source. But the intensity of lines of low wave number is strong and clear when eｘcited by 782 nm laser source. At the same time, the authors got Raman spectra lines at different times after taking blood under the same laser source. When using 782 nm laser source, there is no difference except for 1 601 cm-1. There are a lot of weakened lines and lines shifting about 4-10 cm-1 toward low wave number. The results indicate that Raman spectra may offer the experimental basis for studying structure, function and variability of single red-cell.
2004 Vol. 24 (05): 576-578 [Abstract] ( 1525 ) PDF (844 KB)  ( 336 )
579 Micro-Raman and Fluorescence Spectra of Several Agrochemicals
XIAO Yi-lin1, ZHANG Peng-xiang2*, QIAN Xiao-fan3
Raman and fluorescence spectra from several agrochemicals were measured, which are sold for the use in vegetables, frutis and grains. Characteristic vibration Raman peaks from some of the agrochemicals were recorded, hence the spectra can be used for their identification. Other marketed agrochemicals demonstrated strong fluorescence under 514.5 nm excitation. It was found that the fluorescence spectra of the agrochemicals are very different. According to these results one can detect the trace amount of agrochemicals left on the surface of fruits, vegetables and grains in situ and conveniently.
2004 Vol. 24 (05): 579-581 [Abstract] ( 1005 ) PDF (839 KB)  ( 469 )
582 Near-Infrared Luminescence of Yb3+-Chrome Blue-Black R Complex
MENG Jian-xin, DENG Zhao-xia, CHEN Da-zhi, FENG De-xiong
In the present work, sensitized near-infrared fluorescence from Yb3+-chrome blue-black R (CBR) complex was studied. It was found that Yb3+ forms 1∶2 complex with CBR in natural ethanol solution. The visible fluorescence from CBR was quenched when the complex forms, while the near-infrared fluorescence from Yb3+ was greatly enhanced. A mechanism in which CBR absorbs excitation light and transfers its energy to Yb3+ ions was suggested. Near-infrared fluorescence intensity of Yb3+ is proportional to its concentration under the experimental condition, and was not disturbed by the addition of a small amount of other lanthanide ions, which indicate that near-infrared fluorometric analysis should be promising in the determination of single langthanide ions.
2004 Vol. 24 (05): 582-584 [Abstract] ( 927 ) PDF (886 KB)  ( 413 )
585 Identification of Different Lac with Infrared Spectrum
DONG Qin1，QIU Jian2，HE Run-xi2，ZHANG Jian-yun2
Fourier infrared spectrum was used to differentiate raw lac, bleached las and lac mixed with resin. The results indicate that the infrared spectra of raw lac and lac mixed with resin are similar, so the authors can differentiate them by the following items: (1) the position and the shape of absorbing peak between 3 500 and 2 500 cm-1, (2) the difference of the vibration peak at 1 700 cm-1 for CO，(3) characteristic peak between 1 200 and 1 400 cm-1, (4) the number of peaks and the change in the position of peak. But with bleached and graft copolymerization lacs the properties have been changed by chemical processing． Graft copolymerization of lac is made from methyl-acrylic acid-methy fat by using potassium permanganate as stimulant. Their main differences are： the change of vibration peak of 1 700 cm-1 for CO, a sharp small peak at 1 558 cm-1, a peak with middle strength at 681 cm-1, and spliting to two small peaks at 1 151 cm-1. The experiment shows that the method of infrared spectrum is more scientific and effective than traditional method.
2004 Vol. 24 (05): 585-587 [Abstract] ( 985 ) PDF (922 KB)  ( 490 )
588 Synthesis of 2-(4-Dimethylaminophenyl)-5-Fluoro-6-(Morpholin-4-yl)-1H-Benzimidazole and Its Spectroscopic Research
TANG Ling-tian, WANG Xiang-yun, LIU Xin-qi, WANG Yi*
A new potential pharmaceutical compound, 2-(4-dimethylaminophenyl)-5-fluoro-6-(morpholin-4-yl)-1H-benzimidazole (4) was synthesized. The effect of the pH value of aqueous solution on the absorption spectrum of compound 4 and its interaction with β-cyclodextrin (β-CD) were investigated by UV-Vis spectrum, steady-state fluorescence and time-resolved spectroscopic measurements. The results indicate that compound 4 mainly exists in neutral molecular state when pH value of the aqueous phase is above 7.0. In the pH range from 7.0 to 3.8 the neutral molecular state and protonated univalent cationic form coexist. As the pH value decreases, the content of univalent cationic form increases. When 2.76＜pH＜3.8, the protonated univalent cationic form is the predominant species. With further decrease of the pH value, the univalent cation is protonated by another H+ to form a bivalent cation，and both univalent and bivalent cations coexist in the solution. The steady-state fluorescence and time-resolved spectroscopic measurements revealed that compound 4 is a sensitive molecular probe. The interaction of compound 4 and β-CD is very strong. The guest: host ratio of inclusion complex between compound 4 and β-CD formed in the aqueous solution (pH=9.50) is 1∶1，and the association constant was determined to be (1.02±0.04)×103 mol·L-1.
2004 Vol. 24 (05): 588-591 [Abstract] ( 1110 ) PDF (886 KB)  ( 389 )
592 Spectral Study of the Compound Zn(Pht)∶ 0.05 Sm
SUN Rui-qing，ZHANG Han-hui，YANG Qi-yu
Zn(Pht) ∶0.05 Sm compounds have been synthesized by microwave. The compound was characterized by XRD，FTIR，NIR FT-Raman，DRS UV/Vis，fluorescence spectra，and TG analysis. FTIR and FT-Raman indicated that each of the carbonyl group in the phthalate of the compound combined with metal zinc as mono-dentate terminal chelating. Compared with Pht, the title compound’s π→π* from phthalate shifted from 255 and 289 nm to 235 and 270 nm，respectively. In the fluorescence spectra, there are emission peaks at 560, 596, 642 and 670 nm when excited by 240 nm，which correspond to the transitions from Sm3+’s emission states of 4G5/2，6H7/2，6H9/2 and 6H11/2 to the ground state. As a result, Zn(Pht) improves the emission efficiency of Sm3+ notably. At the emission peak of 596 and 642 nm when excited by 240 nm, the fluorescence lifetime of the compound is τ1=1.57 ns and τ2=76.94 ns, and τ1=1.19 ns and τ2=55.64 ns，respectively. TGA showed that the title compound begins to decompose at 380℃, while it is stable below 380℃.
2004 Vol. 24 (05): 592-595 [Abstract] ( 1383 ) PDF (934 KB)  ( 420 )
596 Spectroscopic Evaluation of Time-Resolved Fluoroimmunoassay
GUO Zhou-yi，TIAN Zhen，JIA Ya-li
The lanthanide trivalence ion and its chelates are used for marking substance in Time-Resolved Fluorescence Immunoassay(TRFIA), marking protein, hormone，antibody，nucleic acid probe or biologic alive cell，to measure the concentration of the analysis substance inside the reaction system with time-resolved fluorometry after the reaction system occurred，and attain the quantitative analysis’s purpose. TRFIA has therefore become a kind of new and more sensitive measurement method after radioisotope marking, enzymatic marking, chemiluminescence, electrochemiluminescence, primarily depending on the special physics and chemistry characteristics of lanthanide trivalence ion and its chelates. In this paper, the result of spectroscopic evaluation of europium trivalence ion and its chelate, and the principle of time-resolved technology and fluorescence-enhanced technology are reported. At the same time, the experiment shows that the excitation wavelength chosen between 336 and 337 nm benefits the excitation and the energy transfer of chelate diketone of europium trivalence ion.
2004 Vol. 24 (05): 596-599 [Abstract] ( 954 ) PDF (1039 KB)  ( 302 )
600 Study on Fluorescence Characteristics of Pefloxacin Based on Charge Transfer Reaction
LI Gui-zhi，LIU Yong-ming
The charge transfer complex formed between pefloxacin mesylate (PM) as the donor and tetrachlorobenzoquinone (TCQ) as the acceptor has been studied by fluorimetry. Experiment shows that PM reacted with TCQ in methanol with light and the complex was formed. Its fluorimetric intensity was stronger than that of PM and the excitation and emission peaks of the complex were red shifted to 80 nm and 60 nm, respectively. A linear calibration graph was obtained over the PM concentration from 0.05 μmol·L-1 to 10 μmol·L-1 with the detection limit of 0.004 μmol·L-1 of PM. The proposed method and UV-Vis photometric method were both applied to determining the pefloxacin in the same capsules with satisfactory results.
2004 Vol. 24 (05): 600-602 [Abstract] ( 1336 ) PDF (849 KB)  ( 311 )
603 Effect of Oxygen Partial Pressure on the Band-Gap of the TiO2 Films Prepared by DC Reactive Sputtering
ZHAO Qing-nan1, 2，LI Chun-ling1, 2，LIU Bao-shun1，ZHAO Xiu-jian1
TiO2 films have been deposited on glass substrates using DC reactive magnetron sputtering at different oxygen partial pressures from 0.10 to 0.65 Pa. The photoluminescence (PL) spectra of the films were recorded. The results of the PL spectra showed that there were three emission peaks at 370，472 and 514 nm for the films sputtered at 0.35 and 0.65 Pa, and there were two peaks at 370 and 490 nm for the films sputtered at 0.10 and 0.15 Pa. The band-gap for the films was 3.35 eV. For the films sputtered at 0.35 and 0.65 Pa there were two defect energy levels at 2.63 and 2.41 eV, corresponding to 0.72 and 0.94 eV below conduction band for the band-gap, respectively. For the films sputtered at 0.10 and 0.15 Pa, there was an energy band formed between 3.12 and 2.06 eV, corresponding to 0.23 and 1.29 eV below the conduction band. With increasing the oxygen partial pressure, the defect energy band changed to two energy levels, and the energy levels nearly disappeared for the film sputtered at 0.65 Pa of oxygen partial pressure.
2004 Vol. 24 (05): 603-605 [Abstract] ( 1648 ) PDF (848 KB)  ( 346 )
606 Determination of Deoxyribonucleic Acids Based on the Enhanced Effect of Resonance Light Scattering of Malachite Green Sensitized by Cetyltrimethylammonium Bromide
FENG Su-ling, LIU Xue-ping，FAN Jing
A resonance light scattering(RLS) enhancement method was reported for the determination of deoxyribonucleic acids. The proposed method was based on the enhanced effect of deoxyribonucleic acid on the resonance light scattering of malachite green(MG) sensitized by cetyltrimethylammonium bromide(CTMAB). Alkaline medium was necessary for the experiment. Under optimal conditions, the linear ranges for both calf thymus DNA(ctDNA) and fish sperm DNA(fsDNA) were 0-1.5 μg·mL-1, the detection limits were 0.05 μg·mL-1 for ctDNA and 0.03 μg·mL-1for fsDNA. The measurement can be made on normal spectrofluorimeter. Mechanic studies show that MG probably aggregates on the molecular surface of single-chained DNA, and then interacts on CTMAB to form large particles, which produce strong RLS. This method was successfully applied to the determination of DNA in synthetic samples.
2004 Vol. 24 (05): 606-609 [Abstract] ( 1869 ) PDF (921 KB)  ( 318 )
610 Determination of Deoxyribonucleic Acid with Nitro-Tetrazolium Chloride Blue by Resonance Light-Scattering Technique
LONG Yun-fei1，2，CHEN Xiao-ming1*，CAI Tie-jun2
Characteristics of the interaction of nitro-tetrazolium chloride blue and Deoxyribonucleic Acid(DNA) were studied in the of pH 1.8 buffer solution by Resonance Light-Scattering (RLS) technique. The effects of interference substances and the optimization of the procedure were investigated，and a new method for the determination of the DNA was established based on RLS. The linear range of the DNA is 0-7 mg·L-1 with a correlation coefficient of 0.995 8. The detection limit is 30.04 μg·L-1. The method has been applied to the determination of DNA in mixed samples with satisfactory result.
2004 Vol. 24 (05): 610-612 [Abstract] ( 1477 ) PDF (841 KB)  ( 416 )
613 Synthesis and Spectroscopic Analysis of Complex α-Na7H[GaW9Fe3(H2O)3O37]·16H2O
WANG Li，WANG Xiu-li，HOU Yu，WANG En-bo*
α-Na7H[GaW9Fe3(H2O)3O37]·16H2O has been synthesized and it′s IR, UV, ICP and XPS, have been studied. The IR spectrum exhibits νas(W—Oa—W)，νas(W—Ob—W)，νas(W—Oc—W) and νas(W—Od—W) four peaks, which indicates that it has Keggin structure. The UV spectrum has two peaks, at 210 and 268 nm, corresponding to Od—W→pπ-dπ and Ob/Oc→pπ-dπ. Ob/Oc→pπ-dπ is character peak. Both GaW9 and GaW9Fe3 have a 4 electrons reductive peaks，with E1/2 of GaW9 minus even more，the GaW9Fe3 is α. Mssbauer spectrum has been studied. Effective magnetic moment is 6.00×10-23A·m2. The Mssbauer spectrum at 75 K shows an isomer shift δ=0.43 mm·s-1, within the range of 0.3 to 0.6 mm·s-1 observed for high-spin iron(Ⅲ) complexes. The authors found that title complex has antiferromagnetic properties. These kinds of heteropoly compounds have attracted our attention for the study of new materials.
2004 Vol. 24 (05): 613-615 [Abstract] ( 1559 ) PDF (905 KB)  ( 349 )
616 Nonlinear Partial Least Squares Method for Simultaneous Derivative Spectrophotometric Determination of Two Components in Compound Sulfamethoxazole
ZHOU Tong, ZHONG Jia-yue, FENG Jiang
A nonlinear model of consistency with derivative absorption in multiple components systems has been given. Model data were estimated by partial least squares method. A method for the simultaneous derivative spectrophotometric determination of two components with nonlinear partial least squares method was established. The method has been applied to the simultaneous determination of two components in compound sulfamethoxazole tablets. The average recoveries of sulfamethoxazole and trimethoprim in synthetic samples were 99.8% and 100.1%，and relative standard deviations were 1.3% and 1.6%，respectively. The results by nonlinear PLS method are significantly better than those by linear PLS method. The results for actual compound formulation agreed with those obtained by standard method.
2004 Vol. 24 (05): 616-618 [Abstract] ( 1411 ) PDF (828 KB)  ( 354 )
619 Unequal Interval Jump Grey Modeling and Its Application to the Spectral Analysis of Lubricating Oil
ZHANG Hong, LI Zhu-guo, CHEN Zhao-neng
Unequal interval jump grey model was built for raw data series with unequal interval and jump trend in this paper. Levenberg-Marquardt arithmetic that belongs to non-linear least-square estimation was used to recognize the parameters. The model built was used to fit spectrometric analysis values of diesel engine and the fitting precision is good. It is helpful to improve the accuracy and reliability of spectrometric analysis by revising test data after oil change with model parameter.
2004 Vol. 24 (05): 619-621 [Abstract] ( 415 ) PDF (844 KB)  ( 350 )
622 Determination of Mercury in Battery by Microwave Digestion Cold Atomic Absorption Spectrometry
TANG Bao-ying1, LI Yu-jie1, XIE Xiao-dan1, LI Gong-ke1*, LIU Zhi-hong2, LIU Li2, LI Ying2
In this paper, a method of microwave digestion followed by cold atomic absorption spectrometry (CAAS) for the determination of mercury in battery was developed. Microwave digestion conditions and operational conditions of CAAS were optimized. The digestive solution was a mixture of hydrochloric acid-sulfuric acid (4∶1, volume ratio) and the digestive time was 3 min at a microwave power of 1.0 MPa. The reaction medium was 0.5 mol·L-1 sulfuric acid at room temperature. The characteristic concentration was 0.25 μg·L-1. Five battery samples were determined, the recoveries were from 99.9% to 113%, and the relative standard deviations were from 4.85% to 11.9% (n=6). The analytical results were satisfactory. The method is fast, simple, accurate and solvent-saving.
2004 Vol. 24 (05): 622-624 [Abstract] ( 405 ) PDF (869 KB)  ( 347 )
625 Analysis of the Contents of Zn, Cu, Fe, Mn, Co and Ni in Thymopeptide and Transfer Factor Biological Injections
LENG Hong-xia, LIU Wei-ming, ZHU Zhi-guo，HAN Li-qin
Thymopeptide and transfer factor are two common clinic biological preparations, which are used to cure immunodeficiency, low immunofunction or infectious disease caused by virus or fungi owing to their functions of increasing body immunity. In order to discuss the relationship between trace elements and those related diseases, to coordinate sound clinic use of the preparations and to provide productive data on them, atomic absorption spectrophotometry was used to detect the contents of Zn, Cu, Fe, Mn, Co and Ni in thymopeptide and transfer factor biological preparations. Respective contents of detected elements were compared in a statistical way. Results show that Zn and Co contents in thymopeptide were lower than in transfer factor; the contents of Cu，Fe，Mn and Ni, in thymopeptide were higher than in transfer factor. For Zn，Cu，Mn and Co，there was a significant difference between the two biologicam preparations (P＜0.01). For Fe and Ni there was a great difference (Q＜0.05). The results can provide useful data for sound clinic biological injection to promote immune function, and for increasing or decreasing certain trace elements in preparation.
2004 Vol. 24 (05): 625-627 [Abstract] ( 566 ) PDF (830 KB)  ( 330 )
628 The Design and Application of Domestic Mid-IR Fiber Optics
WENG Shi-fu1, GAO Jian-ping2, XU Yi-zhuang1, YANG Li-min1, BIAN Bei-ya2, XIANG Hai-bo2, WU Jin-guang1*
The combination of mid-IR fiber optics and FTIR has made the non-invasive determination of samples in situ, with long distances， and in vivo possible. In this paper domestic mid-IR fiber optics was improved to investigate the transmission ability of fiber optics and its application to the sample determination. New design was applied to obtaining one bare fiber optics, which has a minor energy loss and higher signal-to-noise ratio. The spectra of H2O/EtOH and tissue samples were measured using the new designed fiber optics and the results show that home-made mid-IR fiber optics can be applied to the field of determination of general and biological samples.
2004 Vol. 24 (05): 628-630 [Abstract] ( 1066 ) PDF (855 KB)  ( 359 )
631 Small-Invasive Photoelectric Detection of Blood Glucose
FANG Yun-jie, HUANG Lan, DING Hai-shu*
A new type of photoelectric small-invasive blood glucose monitor was developed. This instrument is based on a 16 bit microprocessor MSP430F413 which belongs to a low-power microprocessor of the component family of Texas Instruments promotion recently. There are three advantages of this instrument: (1) using the method of two optical beams to decrease the influence of the LED’s power fluctuation, (2) using the multiple comparative method to determine the terminative time of enzymatic reaction and the start time of computing and processing, (3) to store a lot of measured data up to 50 samples. The data measured by this instrument were compared with Prestige blood glucose monitor, and the result shows that the accuracy and the reliability of this instrument is better. The specialties of this instrument are easy operation, getting results quickly, low-power and low cost. It is an ideal instrument for diabetic test and control of blood glucose concentration at home.
2004 Vol. 24 (05): 631-633 [Abstract] ( 934 ) PDF (840 KB)  ( 355 )
634 Simultaneous and Real-Time Collection by Multi-Fiber Coupling and Optical Multi-Channel Analyzer
HE Ying-hong1, CHENG Juan1, RAN Rui-jiang1, XUE Kang1, YANG Jing-guo1*，TAN Hua2, HU Shao-lou2, WANG Xiao-song2
A new kind of instrument and method for simultaneous and real-time collection of multi-object spectra by using multi-fiber coupling and Optical Multi-channel Analysis(OMA) was reported. The spectral signals of one object, three objects and five objects were collected successfully in experiments. The spacial resolution of 0.5 mm and detected spectral range of 200-1 100 nm were reached, and at most twenty objects could be collected on the image plane of 1 cm2 area with OMA 4 system. The design of the coupling lens’s light path was discussed to guarantee enough light energy to enter the instrument and little effect on the resolution of spectral instrument. The instrument can be applied widely to the areas of supervising and controlling the quality of light beam in transmission and in the time-resolved and spatial-resolved spectral measurement.
2004 Vol. 24 (05): 634-636 [Abstract] ( 1570 ) PDF (1310 KB)  ( 414 )
637 Analysis of Anti-Ultraviolet Characteristic of Liquid-Crystal Display
HUANG Chong1, OUYANG Yan-dong1, WU Yong-jun2, ZHAN Qian-xian2
As liquid-crystal display is developing to be used outside and becomes colorful and larger, the influence of ultraviolet on liquid-crystal display is becoming more and more apparent． And the anti-ultraviolet character of liquid-crystal display becomes more important． In this paper, the spectroscopic characteristics of ITO glass and polaroid were measured with ultraviolet of various wavelengths. By comparing the ultraviolet transmission spectrum of normal polaroid (LN-1205T) with that of anti-ultraviolet polaroid (F-1225DU), the anti-ultraviolet characteristic of a new style liquid-crystal display (LCD) was discussed. And the results show，the anti-ultraviolet polaroid (F-1225DU) is better in the absorption of ultraviolet． The anti-ultraviolet polaroid (F-1225DU) can enhance the performance of liquid-crystal display used outside．
2004 Vol. 24 (05): 637-639 [Abstract] ( 201 ) PDF (842 KB)  ( 347 )

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