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2005 Vol. 25, No. 10
Published: 2005-10-26

 
       光谱学与光谱分析
1537 Simultaneous Determination of Rate Ratio of Recombination to Capture and Trap Depth from Thermo-Luminescence of ZnS:Cu, Co
WANG Li-wei1, XU Zheng1,2, 3*, TENG Feng1,ZHANG Fu-jun1, MENG Li-jian2,XU Xu-rong1
The recombination luminescence is in nature a bimolecular process, but the decay rule may be changing from that of mono-molecular to bimolecular rule, i.e., from exponential to hyperbolic rule, depending on the behavior of conduction electrons. This behavior is represented by relative rate of recombination with ionized centers to that of capture by traps. This relative rate depends partly on the intrinsic parameters of the specified materials, and partly on the concentration of conduction electrons supplied by traps. Each point of the TL curve is related to the material parameters and the release of electrons from traps. The ratio of relative rate of recombination to that of capture γ(ε)=σ0n0/σ(ν-n) involves the parameter ε. They are inseparable and must be determined at the same time. In the present report, starting from the same sample ZnS:Cu, Co which has only one peak in its TL(i.e., only one kind of luminescent center and only one kind of traps), and the experimental value of σ/σ0=0.005,the authors use thermo-luminescence kinetics models and some mathematic tools to exactly estimate the ratio σn0/σν and the trap depth ε simultaneously from the glow curve. The authors found that σ0n0/σν=2.6 and ε=0.86 eV.
2005 Vol. 25 (10): 1537-1541 [Abstract] ( 1780 ) PDF (592 KB)  ( 389 )
1542 Spectrum of Dielectric Barrier Discharge at Atmospheric Pressure Intensified by Mixing a Little Argon
DONG Li-fang, MAO Zhi-guo, ZHANG Lian-shui, RAN Jun-xia
In this paper, the spectrum of dielectric barrier discharge at atmospheric pressure was measured by using the special setup with two water electrodes. The variation of spectrum was studied when a little argon was mixed. Nitrogen molecular spectrum(C3Πu(v′=0)→B3Πg(v″=0-4)) and nitrogen atomic spectrum(4d4D7/2→3p4P01/2) were found in the range of 300-800nm. After a little argon was mixed, the breakdown voltage of discharge obviously decreased. The spectral line intensities of nitrogen molecules and nitrogen atoms increased. The full width at half maximum (FWHM) of spectral line was obviously broadened. Because Stark broadening is a linear function of electron density, it can be seen that electron density increased after a little argon was mixed with the air, which caused the probability of excitation collision of N2 and N with electrons to increase, and the number of N2 and N excited to higher excitation state to increase. So the intensity of spectrum was intensified.
2005 Vol. 25 (10): 1542-1544 [Abstract] ( 1111 ) PDF (302 KB)  ( 395 )
1545 Hα Line and the Optimum Experimental Condition for Diamond Deposition in EACVD
DONG Li-fang, WANG Zhi-jun, SHANG Yong
The process of atomic hydrogen emission in the CH4/H2 gas mixture in EACVD was simulated by Monte Carlo method. In the simulation the collision between electron and H2 molecule has two basic types: elastic collision and inelastic collision. Four types of inelastic processes have been considered, namely vibrational excitation, dissociation, electron excitations and ionization. For e-CH4 collision, elastic momentum transfer, vibrational excitation, dissociation, ionization, and dissociation ionization were considered. The relationship between the numbers of H, and CH3, and the atomic hydrogen emission line intensity under different experimental conditions was investigated. A method of extrapolating the optimum experimental condition for diamond deposition by the atomic hydrogen emission line is given. The result is of great importance to depositing high quality diamond films by controlling the conditions of technology efficiently.
2005 Vol. 25 (10): 1545-1547 [Abstract] ( 1031 ) PDF (274 KB)  ( 331 )
1548 Optimization Analysis Based on Wavelength Bandwidth for Multi-Band Pyrometry
FU Tai-ran, CHENG Xiao-fang, FAN Xue-liang, DING Jin-lei
The present paper establishes the optimization criteria for achieving the optimum measurements in three-band pyrometry under the assumption of linear emissivity model and the sensor design with Gaussian distribution. By varying the FWHM of Gaussian distribution, the optimization analysis is investigated with the choice of the wavelength bandwidth in three-band pyrometry. For specific cases, the simulation results present the optimum bandwidth distribution. Therefore, the discussions in this paper will provide significant theoretical instructions for the design of radiation pyrometer.
2005 Vol. 25 (10): 1548-1551 [Abstract] ( 1203 ) PDF (433 KB)  ( 543 )
1552 Electroluminescent Device Based on Terbium Complex
XIAO Jing1, DENG Zhen-bo1*, XU Deng-hui1, XU Ying1, WANG Rui-fen2
Rare earth complex Tb(BA)3phen has been synthesized, which is used as an emitting material in electroluminescence. The properties of monolayer device with the rate of 1 000 r·min-1 and the impure concentration of 1∶5 are the best. And the highest brightness of this device reached 26.8 cd·cm-2 at a fixed bias of 21 V. Bright green emission can be obtained from the optimized double-layer device and the highest EL brightness of the device reaches 322cd·m-2 at the voltage of 22V.
2005 Vol. 25 (10): 1552-1555 [Abstract] ( 1073 ) PDF (416 KB)  ( 360 )
1552 Electroluminescent Device Based on Terbium Complex
XIAO Jing1, DENG Zhen-bo1*, XU Deng-hui1, XU Ying1, WANG Rui-fen2
Rare earth complex Tb(BA)3phen has been synthesized, which is used as an emitting material in electroluminescence. The properties of monolayer device with the rate of 1 000 r·min-1 and the impure concentration of 1∶5 are the best. And the highest brightness of this device reached 26.8 cd·cm-2 at a fixed bias of 21 V. Bright green emission can be obtained from the optimized double-layer device and the highest EL brightness of the device reaches 322cd·m-2 at the voltage of 22 V.
2005 Vol. 25 (10): 1552-1555 [Abstract] ( 1559 ) PDF (416 KB)  ( 346 )
1556 Proof of Solid State Cathodoluminescence by Using Brightness Waveform
LIU Ming1, 2,CHEN Xiao-hong3,XU Zheng1,TENG Feng1,YI Li-xin1,GAO De-wen2,GUO Li-qun2
DOI: 1000-0593(2005)10-1556-04
Three different inorganic-organic hetero-junctions (A: ITO/SiO2/Alq3/Al, B: ITO/Alq3/SiO2/Al and C: ITO/SiO2/Alq3/SiO2/Al ) were fabricated. The emission can be observed only under positive bias in devices A and B, but under both biases in device C according to their brightness waveforms. With increasing voltage, the increase in blue emission in devices B and C is faster than that in green emission. This is because that the recombination of hot electrons and holes, i.e., electron-hole pairs, produced blue emission in devices B and C, and the recombination of electrons injected from Al with the accumulated holes, which are excited by hot electrons, produced green emission in device A. Hence, the emissions of the devices are attributed to not only the recombination of electrons and accumulated holes, but also the cathodoluminescence-like (CL-like) emission.
2005 Vol. 25 (10): 1556-1559 [Abstract] ( 1665 ) PDF (443 KB)  ( 405 )
1560 Preparation and Characterization of CaAl2O4:Eu2+, Nd3+ Nanoparticles
ZHANG Xi-yan, JIANG Wei-wei, LIU Xue, LU Li-ping, WANG Xiao-chun, BAI Zhao-hui, LIU Quan-sheng, CAO Zhi-feng
Long persistent phosphoresceoce CaAl2O4:Eu2+, Nd3+ nanoparticles were synthesized through sol-gel method. The structures and properties of the samples were analyzed by DTA, TGA, XRD, TEM and spectrometer. Results indicated that the CaAl2O4 crystalline phase was formed at 800 ℃. The particles are spherical in shape and about 20-40 nm in size. The peaks of the excitation, emission and thermoluminescence spectra shift compared with the CaAl2O4:Eu2+, Nd3+ coarse crystals. The luminescence decay includes a initial rapid part and a following slow part. The decay time lasts for about 5 h.
2005 Vol. 25 (10): 1560-1563 [Abstract] ( 245 ) PDF (566 KB)  ( 396 )
1564 The Study on Electrochemiluminescence of Luminol on ITO Glass
WANG Zhi-yong, GUO Wen-ying, DI Jun-wei, TU Yi-feng*
The indium tin oxide(ITO) glass was applied as the electrode to study the electrochemiluminescent behavior of luminol on its surface. The experimental results indicated that it was an excellent electrode material for ECL of luminol with very high sensitivity. The detection limit of the luminol is as low as 10-15 mol·L-1 order of magnitude. Compared with the voltammetric behavior of luminol, it was revealed that both the two oxidation processes of luminol led to the emission of ECL on the surface of ITO glass, which was different from the ECL behavior of luminol on platinum electrode. Although the ECL intensity of first step oxidation of luminol was relative weak than that of the second step oxidation, it was profitable because it was a reversible process and more stable. It might be useful to fabricate the flow-cell of ECL based on its ECL activity and transparence for light. The influences of the electric parameters and the dissolved oxygen on luminol’s ECL on the ITO glass, and the mechanism were also studied in the present paper.
2005 Vol. 25 (10): 1564-1567 [Abstract] ( 1160 ) PDF (500 KB)  ( 415 )
1568 Study of the Characterization of β-Cyclodextrin-Acetylferrocene- Thiosemicarbazone Inclusion Complex and Micro-Environmental Effects
ZHANG Jing, LIU Wan-yi*, ZHANG Xia
Inclusion complex of acetylferrocene-thiosemicarbazone(TAF) with β-cyclodextrin(β-CD) has been prepared by using kneading method. Elemental analysis and the solubility determination proved that 1∶1 inclusion complex has been formed. Characterization of the inclusion complex was studied by UV, FTIR, and X-ray diffractometry. The association constant was calculated to be 227 L·mol-1 from the straight portion of the phase-solubility diagram. Furthermore, the influence of different solvents and pH on UV spectrum of acetylferrocene-thiosemicarbazone and β-CD -TAF was discussed respectively. The results show that different micro-environment has apparently different effects on electric spectra of guest and inclusion complexes.
2005 Vol. 25 (10): 1568-1572 [Abstract] ( 1035 ) PDF (586 KB)  ( 383 )
1573 Application of FTIR Spectra Fitting Method in Retrieving Gas Concentrations
ZHU Jun1,2, LIU Wen-qing1, LIU Jian-guo1, GAO Min-guang1, ZHAO Xue-song1, ZHANG Tian-shu1, XU Liang1
The method of retrieving gas concentrations by FTIR spectra measurement system is studied. NLLS fitting algorithm is used to complete the quantitative analysis of CO gas under WINDOWS operating system. The spectra of HITRAN database is employed as calibrating and training sets during the procedure of fitting FTIR spectrum. The measured IR transmittance spectra of CO are best fitted with the calculated spectra in HITRAN. The CO concentrations are acquired after the best fitting. The absolute accuracy of the results of retrieve achieves 1%-5%.
2005 Vol. 25 (10): 1573-1576 [Abstract] ( 1169 ) PDF (497 KB)  ( 360 )
1577 Ester Derivatives of Tetracyanoquinodimethane and Their CT Complexes: Synthesis and Studies by Infrared Spectroscopy
HUANG Wu-qiao1,WU Yi-qun1,2,GU Dong-hong1,GAN Fu-xi1
Three ester derivatives of tetracyanoquinodimethane and their CT complexes were synthesized and characterized by elementary analysis and infrared spectra. The principal infrared absorption peaks were assigned and discussed for the region of 4 000-400 cm-1. Principal factors affecting principal infrared absorption were analyzed.
2005 Vol. 25 (10): 1577-1580 [Abstract] ( 1742 ) PDF (340 KB)  ( 379 )
1581 Application of Near-Infrared Diffuse Reflectance Spectroscopy to the Detection and Identification of Transgenic Corn
RUI Yu-kui1, LUO Yun-bo1, HUANG Kun-lun1, WANG Wei-min2, ZHANG Lu-da3*
With the rapid development of the GMO, more and more GMO food has been pouring into the market. Much attention has been paid to GMO labeling under the controversy of GMO safety. Transgenic corns and their parents were scanned by continuous wave of near infrared diffuse reflectance spectroscopy range of 12 000-4 000 cm-1; the resolution was 4 cm-1; scanning was carried out for 64 times; BP algorithm was applied for data processing. The GMO food was easily resolved. Near-infrared diffuse reflectance spectroscopy is unpolluted and inexpensive compared with PCR and ELISA, so it is a very promising detection method for GMO food.
2005 Vol. 25 (10): 1581-1583 [Abstract] ( 247 ) PDF (369 KB)  ( 448 )
1584 Charge Control and IR Analysis of Amine on Diarylide Yellow Pigment PY14
LI Lu-hai1,2,ZHANG Shu-fen1,YANG Jin-zong1,ZOU Jing1,2,ZHAO Qiang2
To study the reaction of amine with dairylide yellow pigment (PY14) used in electrophoretic display, especially the reaction mechanism between polyisobutylene imide (PIBI) and PY14, some amines were selected to react with PY14. At the same time, tetraethylene pentamine was treated with HCl. The zeta potential and IR of the above products were tested. Based on the zeta potential and IR frequency, the charge control intensities of different amines on PY14 were compared, and it is confirmed that the reaction of PY14 with amines is Lewis reaction, the charge control of secondary and primary amines with less steric obstacle is stronger. The PY14 zeta potential value reverse is due to the adsorption of bigger reverse ion.
2005 Vol. 25 (10): 1584-1587 [Abstract] ( 1487 ) PDF (441 KB)  ( 353 )
1588 Characteristics of FTIR Spectra of Biogenic Aragonite in Mollusk Shells
ZHANG Gang-sheng, LI Xuan-hai
The FTIR spectra of aragonites in outer and inner layers of thirteen species of mollusk shells were systematically measured, and the frequency variations of ν1ν2 and ν4 bands of the aragonites with the positions of shell layers were analyzed. The results showed that the frequency of ν2 band differed in different species of shells and the positions of shell layers, but the frequencies of the other two bands were not altered, and had the same values with synthetic aragonites. In the same species of shells, the frequency of ν2 band in inner layers was greater than that in outer layers, and the frequency shift of ν2 band between inner and outer layers was in the range of 0.5-4.5 cm-1 in all studied samples. The detection of frequency shift of ν2 band in different layers of aragonitic mollusk shell was first reported in this paper.
2005 Vol. 25 (10): 1588-1590 [Abstract] ( 469 ) PDF (353 KB)  ( 351 )
1591 Spectra Studies on the Interaction of Mn2+ and Poly N-Isopropylacrylamide
GUO Shao-fen1, CHEN Ming-qing1, LU Tian-hong2,3, HUANG Xiao-hua1,2*, Mitsuru Akashi4
The interaction of Mn2+ and poly (N-isopropylacrylamide) (PNIPAAm) was studied by using UV-Vis, FTIR and fluorescence spectroscopic methods. The results indicated that Mn2+ could be bonded to oxygen atoms of carbonyl in PNIPAAm and form the complex of Mn2+-PNIPAAm. It was found that there existed efficient Förster energy transfer from Mn2+ to PNIPAAm due to the emission spectra of Mn2+ overlapping the excitation spectra of PNIPAAm and that the emission peak of Mn2+ at 561 nm disappeared in Mn2+-PNIPAAm complex. Therefore the fluorescence intensity at 307 nm was increased by 314%.
2005 Vol. 25 (10): 1591-1594 [Abstract] ( 1539 ) PDF (447 KB)  ( 365 )
1595 Hydrothermo-Assisted Functionalization, FTIR, Raman and XPS Spectra Characterization of Carbon Nanotubes
WU Xiao-li1,2, YUE Tao1*, LU Rong-rong1, ZHU De-zhang1, ZHU Zhi-yuan1
The chemical functionalization process of carbon nanotubes(CNTs) by hydrothermal treatments was investigated systematically under various reaction conditions, including different reagents, treatment time, and temperature. The treated samples were characterized by the FTIR, XPS and Raman spectroscopy. The results revealed that the hydrothermal technology is an effective method for the functionalization of CNTs and the control of the resulting chemical groups.
2005 Vol. 25 (10): 1595-1598 [Abstract] ( 350 ) PDF (410 KB)  ( 468 )
1599 Analysis of Essential Oil Components by GC/FTIR and GC/MS
CAI Ji-bao1, LIN Ping2, SANG Wen-qiang2, LI Jun2, SU Qing-de1*
The volatile components of clary sage (Salvia sclarea L.) oil were identified by gas chromatography-Fourier transform infrared spectroscopy (GC/FTIR) and gas chromatography-mass spectrometry (GC/MS). The application of GC/FTIR in analysis of essential oil was mainly discussed. The accuracy of qualitative analysis for essential oil was improved by such technique as the reconstruction of different spectra regions Gram-Schmidt Fourier transforms infrared spectroscopy, and the application of subtracting of Fourier transforms infrared spectroscopy, and the mass spectrometry.
2005 Vol. 25 (10): 1599-1602 [Abstract] ( 1794 ) PDF (540 KB)  ( 407 )
1603 Study on the Modification of Short Chain Phoshate Ammonium Salt of Bentonites
ZHENG Yu-ying1,PENG Cao2, SUN Rui-qing1, FU Ming-lian1, WANG Can-yao1
The Organobentonites were synthesized by means of the ionexchange reaction of Na+ between tetramethylammonium chloride and tetrabutylammonium chloride quaternary ammonium salts, and sodium base bentonites. The authors used FTIR, X-ray diffraction diagram and DSC thermograms to characterize the structure of the modified bentonites, and discussed the effect of different quaternary ammonium salt on the properties of organobentonites. The results showed that ions of the surfactants had entered into the chip layer of the bentonites, changed the hydrophilic environment of the chip layer into a hydrophobic enviro nment, increased the distance among the chip layers, and improved the compatibility between montmorillonite and the organic phases. All of these have laid a base for the preparation of nanometer composite material of high polymer/bentonite.
2005 Vol. 25 (10): 1603-1605 [Abstract] ( 1961 ) PDF (385 KB)  ( 364 )
1606 Implication of Structure for Nano Clays Used in Thermalsetting PU/PLS Composite
LI Zai-feng1, MA Tong1, MA Xi-liu1, Luba Kotlyar2, XU Chun-ming3
Clays such as kaolinite and montmorillonite, are commonly used as an additive to modify the thermal properties of polymer. In the present work, the morphology, composition, shape and structure of montmorillonite and kaolinite were characterized and compared by various advanced techniques. The TEM/ EDX data showed that the kaolinite has a larger particle size and a lower Si/Al ratio than montmorillonite. These clays were stacked by platelets. The TGA results revealed that montmorillonite loses significant weight (around 7%) from 60 to 90 ℃ due to the dehydration of absorbed water, however, kaolinite almost doesn’t lose weight in this temperature range. Kaolinites loses its weight because of the loss of its structural OH groups at a lower temperature (around 510 ℃) than montmorillonite (670 ℃). The PAS-FTIR spectra showed that montmorillonite has a strong absorbance of hydroxyl group in hydrogen bond region at room temperature, which presents a strong ability to adsorb water on its surface. The results of varied infrared temperature and TGA showed that their structural OH group is very stable from 100 to 500 ℃, and it is possible to form thermosetting PU/PLS composite by reaction with the isocynate group of polyurethane prepolymer.
2005 Vol. 25 (10): 1606-1609 [Abstract] ( 612 ) PDF (685 KB)  ( 362 )
1610 Application and Improvement of Partial-Least-Squares in Fourier Transform Infrared Spectroscopy
ZHANG Lin, ZHANG Li-ming, LI Yan*, LIU Bing-ping, WANG Xiao-fei, WANG Jun-de
Partial least squares(PLS) algorithm is an effective chemometric tool. It takes the advantages of multipal linear regression (MLR) and principal component regression (PCR), which makes Fourier transform infrared spectrometry (FTIR) more powerful and useful. Accompanied with increasing use of FTIR, the algorithm is modified and corrected under different circumstances. The applications of PLS to FTIR were mentioned. Improved algorithms were presented, such as moving windows PLS(MWPLS), robust PLS (RPLS), weighted PLS(WPLS), and non-linear PLS. Data pre-processing, selection of variable, noise elimination and non-linear model of PLS were introduced.
2005 Vol. 25 (10): 1610-1613 [Abstract] ( 1565 ) PDF (477 KB)  ( 403 )
1614 Advances in Passive OP-FTIR
ZHANG Li-ming, ZHANG Lin, LI Yan*, WANG Xiao-fei, LIU Bing-ping, WANG Jun-de
As an OP-FTIR(Open Path FTIR) technology, passive OP-FTIR not only has the advantages of OP-FTIR, but also has the ability to collect data from any direction without prior background information. This technology allows mobile, fast, man-held and stand-off detection of hazardous chemical cloud. The present paper presents some developments of passive OP-FTIR, including high altitude atmospheric pollution detection, auto-detection of toxic cloud, hot gases detection (such as the determination of major combustion products in aircraft exhausts, remote sensing of smoke plumes, and remote sensing of volcano emissions), temperature and combustion products determination (including cloud temperature determination). The present paper also gives the application of passive OP-FTIR in the military. With the development of FTIR and computer science, more and more applications of OP-FTIR to environment supervision, aviation and space flight, engine exhausts, combustion and military will be fulfilled.
2005 Vol. 25 (10): 1614-1617 [Abstract] ( 580 ) PDF (399 KB)  ( 427 )
1618 Spectroscopic Research on the Interaction of 2-(4-Dimethylaminophenyl)-5-Fluoro-6-(Morpholin-4-yl)-1H-Benzimidazole and Calf Thymus DNA
TANG Ling-tian, WANG Yi, LIU Xin-qi,HU Shao-wen, CHU Tai-wei, WANG Xiang-yun*
UV-Vis spectra of the aqueous solutions of 2-(4-dimethylaminophenyl)-5-fluoro-6-(morpholin-4-yl)-1H-benzimidazole (1) at different pH values revealed that compound 1 is a tertiary base, which can combine three protons. Through the non-linear least square method, the logarithm of the three accumulative protonation constants of compound 1, namely, lgβ1, lgβ2 and lgβ3, were determined to be 4.96±0.03, 5.72±0.07 and 7.95±0.10, respectively. UV-Vis and the steady-state fluorescence spectra indicated that a special interaction occurs between compound 1 and calf thymus DNA at the pH value of 3.40, of which the binding constant, Kb, is (2.30±0.10)×104 mol-1·L. Compound 1 in the concentration range of 10-8 to 1.2×10-6 mol·L-1 has a potential application to the quantitative determination of DNA.
2005 Vol. 25 (10): 1618-1621 [Abstract] ( 1141 ) PDF (422 KB)  ( 401 )
1622 A Silicon Phthalocyanine Axially Substituted by Nipagin: Synthesis, Molecular Spectroscopic Properties, and in vitro Photodynamic Activities
ZHANG Guo-cai1, HUANG Jian-dong1*, CHEN Yan-mei1, SUN Jian-cheng2, LIU Hong1, CHEN Nai-sheng1, HUANG Jin-ling1
A new silicon phthalocyanine axially substituted by Nipagin, i.e. bis(4-methoxycarboxyl phenoxy)phthalocyaninatosilicon, has been synthesized and characterized by IR, NMR, HPLC and elemental analysis. Its electronic absorption spectra and fluorescence spectra in different solvents were investigated. It was found that the compound existed in the form of monomer in a saline solution containing 2%(φ) Cremophor EL and 20%(φ) propanediol. The electronic absorption spectra of the compound in the above saline solution were typical for non-aggregated phthalocyanines, showing an intense and sharp Q band at 683 nm with a molar absorption coefficient of 7.47×104 mol-1·L·cm-1. The compound exhibited a relatively strong fluorescence emission at 690 nm with a quantum yield of 0.34 and with a fluorescence lifetime of 4.7 ns. The primary in vitro assay showed the compound had photodynamic killing activities against B16 melanoma cells with a LD50(half lethal dose) of 1.2×10-4 mol·L-1.
2005 Vol. 25 (10): 1622-1626 [Abstract] ( 2016 ) PDF (731 KB)  ( 404 )
1627 Determination of Benzo(a)pyrene in Cigarette Mainstream Smoke by Second-Order-Derivative Synchronous Fluorescence
FAN Hu1, 2,SHENG Liang-quan1, TONG Hong-wu1, JIN Zhong-xiu1, 2,LIU Shao-min1*
The synchronous fluorescence, first-order and second-order-derivative synchronous fluorescence spectra of BaP in cigarette mainstream smoke were studied. It was indicated that the second-order-derivative synchronous fluorescence spectrum could decrease the disturbances of BaP homologous compounds and background of sample. Hereby the present paper introduces a new method to determine BaP in cigarette mainstream smoke by solid-phase-extraction second-order-derivative synchronous fluorescence. The detection limit is 0.2 ng·mL-1, the average recoveries of BaP are 80.2%-86.2%, and the RSD is 2.64%-3.02%.
2005 Vol. 25 (10): 1627-1629 [Abstract] ( 556 ) PDF (404 KB)  ( 408 )
1630 Spectral Properties of Hematoporphyrin Derivative after Interacted with Human Serum Albumin
WU Yun-xia,XING Da*
The spectral properties of photosensitizer HpD, human serum albumin (HSA) and their complex have been studied. The results show that HpD can form HpD-HSA complex with HSA in physiological condition. Compared with pure HpD, the maximum absorption and the fluorescence peaks for HpD-HSA complex had 8-10 nm red-shift. When HpD-HSA complex was excited by the light of corresponding to excitation peaks of HSA (228 and 279 nm) and HpD (394 nm), it was found that the absorption of HSA and HpD both contributed to the emission of HpD-HSA complex at 622 nm. The complex of HpD-HSA was individually excited by wavelengths corresponding to HpD absorption peaks of 402, 502, 537 and 570 nm, and the excitation efficiency of HpD-HSA at pumping wavelength of 537 and 570 nm was higher than that of HpD. The results demonstrate that the red-shift caused by the interaction of HpD and the special proteins in blood should be considered in selecting the excitation and emission wavelength in photodynamic diagnosis and therapy. The results also indicate that the excitation efficiency of porphyrin-protein complex in vivo is higher than that of HpD in vitro when a longer wavelength light corresponding to the week absorption peaks of porphyrin-protein complex is used in photodynamic therapy.
2005 Vol. 25 (10): 1630-1633 [Abstract] ( 578 ) PDF (445 KB)  ( 376 )
1634 Determination of Enoxacin in Urine by Synchronous Fluorimetry
DAI Gang, AODENG Gao-wa*
The effect of metal ions on uhe fluorescence spectra of enoxacin was studied in detail. It has been found that aluminum can enhance the fluorescence intensity of enoxacin remarkably in the buffer solution of NaH2PO4-Na2B4O7 with pH 6.3. A new method using synchronous fluorimetry has been developed for the determination of enoxacin in human urine. The synchronous fluorescence intensity of Al/ENX system is linearly proportional to the concentration of ENX in the concentration range of 0.04-1.0 μg·mL-1. The detection limit, calculated according to IUPAC recommendations, was 0.018 μg·mL-1. The precision of the method was established by repeated assays (n=12) using 0.4 μg·mL-1 solution of ENX, and the relative standard deviation was 3.1%. The method was satisfactorily applied to the determination of enoxacin in human urine samples. The recovery was within the range of 95%-105%.
2005 Vol. 25 (10): 1634-1636 [Abstract] ( 1603 ) PDF (409 KB)  ( 372 )
1637 Theoretical Studies on Fluorescence Spectra of Polyamic Acid and It’s Grafted Derivatives
ZHANG Zhen-jiang1, ZHOU Wei-qun1, LU Jian-mei1,2*, QI Xiu-xiu1
A theoretical study on the polyamic acid (PAA) and its derivatives with different side chain (GPAA1-4) by semi-empirical PM3 is presented in this paper. After optimization, the authors get their balanceable geometric configurations. For all optimal geometric configurations, there is no imaginary frequency in vibrational analysis, which proves that the geometric configurations are stable. On this basis, the electronic spectra have been calculated by a single-excitation configuration interaction (CIS) method. Tie calculated results are consistent with experimental values on the whole. The authors found that the fluorescence intensity of polyamic acid (PAA) with p-π conjugation side chain is enhanced obviously, and the longer the alkyl side chain the more intense the fluorescence will be. This will help us to design and synthesize the polymer fluorescence material.
2005 Vol. 25 (10): 1637-1640 [Abstract] ( 1652 ) PDF (479 KB)  ( 360 )
1641 Simultaneous Synchronous Spectrofluorimetric Determination of Vitamin B1, B2 and B6 by PARAFAC
NI Yong-nian, CAI Ying-jun
In the present study, a synchronous spectrofluorimetric method has been applied to the simultaneous determination of vitamin B1, B2 and B6. However, their spectra are overlapped so it is difficult to determine them individually. The parallel factor analysis (PARAFAC) was applied to the resolution of the overlapped spectra of mixtures of vitamin B1, B2 and B6. The Δλ range used was from 20 to 120 nm, and the excitation wavelength range was selected from 200 to 500 nm. From the measured fluorescence data a four-factor PARAFAC model was established, and was applied to the determination of a set of synthetic validation samples and some commercial samples with satisfactory results. This work shows that PARAFAC method is a powerful chemometric tool to the determination of mixtures of vitamin B1, B2 and B6.
2005 Vol. 25 (10): 1641-1644 [Abstract] ( 2028 ) PDF (482 KB)  ( 408 )
1645 Study on Fluorescence Analysis for Carbamate Pesticides
WANG Zhong-dong1,2,WANG Yu-tian1
In the present paper the basic theory that an organic substance can emit fluorescence as it is excited by ultraviolet rays is described and the relationships between the molecular structures of organic substances and fluorescence generation are studied. According to this theory, the molecular structures of a few common carbamate pesticides such as carbaryl, carbofuran and propoxur etc. are analyzed, their fluorescence characteristics are shown, and the mechanism of fluorescence generation of carbamate pesticides is ascertained. It provides a theoretic basis for further detecting carbamate pesticides by means of a fluorescence analytical method. Moreover a steady-state fluorescence spectrograph is applied to conduct fluorescence spectrum experiments with standard carbaryl solution and carbofuran solution. The results indicate that carbamate pesticides may emit fluorescence as excited by UV under the condition of a certain solvent, and that their fluorescence spectra are distinct and have fine resolution and less interference. It is feasible to detect carbamate pesticides by fluorescence spectral analysis.
2005 Vol. 25 (10): 1645-1647 [Abstract] ( 1056 ) PDF (366 KB)  ( 374 )
1648 Stability of Patient Bile and Study on Its Influential Factors
SHEN Yu-hua1, 3, HUANG Fang-zhi1, XIE An-jian1, 3, XIONG Qi-ru2, CHEN Kai-bo1
The patient bile and its centrifugate were studied by FTIR spectra, UV-Vis spectra, particle size analysis, and zeta potential determination. The result showed that the patient bile was in a heterogenetic and unstable state, and some of the ultramicrons in the patient bile assembled to form precipitate after centrifugalized at different speeds. According to FTIR and UV-Vis spectra, the authors found that the composition of the precipitates was mainly cholesterol, bilirubin, calcium bilirubinate, protein, phospholipid and so on, which was much close to that of the core of patient gallstone. The change in the properties of cholesterol/phospholipid vesicles, and the production of the undissolvable calcium salt in the patient bile had crucial influence on the stability of the patient bile, which played important roles in the core-formation and initial growth of gallstone that were induced by the matrixes such as proteins, phospholipids etc.
2005 Vol. 25 (10): 1648-1651 [Abstract] ( 1089 ) PDF (544 KB)  ( 361 )
1652 Spectroscopic Studies on the Interaction of Nicotine and BSA
CHEN Yun,KONG Xiang-rong,SHEN Xing-can,LIANG Hong*
The interaction of nicotine and bovine serum albumin(BSA) was investigated by fluorescence spectra and UV-vis spectra. The fluorescence spectrum showed that BSA fluorescence quench regularly with the addition of nicotine. The fluorescence quenching mechanisms were also studied in pH 5.0, pH 7.4 and pH 11.0 by Stern-Volmer equation, indicating dynamic quenching(pH 5.0) and static quenching(pH 7.4 and pH 11.0) respectively. Association constants (k) of nicotine and BSA at pH 7.4 and pH 11.0 at the temperatures of 20 and 37 ℃ were given by the Lineweaver-Buck equation, which are: k20 ℃=140.15 L·mol-1 and k37 ℃=131.83 mol·L-1(pH 7.4), and k20 ℃=141.76 mol·L-1, k37 ℃=27.79 mol·L-1 (pH 11.0), suggesting that the association constant is effected by the temperature much more remarkably at pH 7.4 than that at pH 11.0 because of the different states of nicotine at different pHs. The UV-Vis spectra exhibit that the absorbance of BSA(210 nm) shifts to red and decreases gradually with the addition of nicotine, reflecting the transition of secondary structure of BSA, namely, the helix of BSA becomes looser. The UV-Vis second derivative spectra and synchronous spectra (Δλ=λemex=15 nm and Δλ=λemex=60 nm) imply the change of the microcircumstance of aromatic amino residues of BSA(Trp, Tyr and Phe) from hydrophobicity to hydrophilicity at high concentration of nicotine.
2005 Vol. 25 (10): 1652-1657 [Abstract] ( 1808 ) PDF (637 KB)  ( 358 )
1658 Application of Wavelet Packets Analysis-Interpolation-RBF to the Simultaneous Determination of Fe, Mn, Cu and Zn in Aluminous-Alloy
CHENG Zheng-jun, ZHANG Yun-tao*
A new approach was proposed so that noises in visible spectra are eliminated by wavelet packets, and the specimen numbers of calibration samples are increased by linear interpolation. It can used to solve problems of few specimen numbers and many variables in simultaneous spectrophotometric determination. Thus forecasting resultant veracity is improved. The contents of Fe, Mn, Cu and Zn in aluminous-alloy was determined simultaneously by using wavelet packets analysis-linear interpolation-RBF (radial basis function) neural networks (WPA-Interp-RBF). Wavelet packets analysis can eliminate noises to a desired level. Linear interpolation makes specimen of training samples cover recognizable room better. So RBF can abstract more characteristic information and improve its performance. Relative error(RE) of sample is reduced remarkably with desired results.
2005 Vol. 25 (10): 1658-1661 [Abstract] ( 2089 ) PDF (475 KB)  ( 376 )
1662 Study on β-Cyclodexdrin Sensitizing Catalytic Kinetic Spectrophotometric Determination of Mn(Ⅱ)
GUO Liang-qia, LIN Xu-cong, XIE Zeng-hong*, FU Yan-bin
A new catalytic spectrophotometric method for the determination of trace amount of Mn(Ⅱ) has been developed. The method is based on the oxidation of alizarin green(AG) by potassium periodate in the presence of β-cyclodexdrin(β-CD) as a sensitizer and nitrilotriacetic acid as an activator. The linear range of the method was 0-2.4 ng·mL-1 for Mn(Ⅱ), the determination limit was 0.097 ng·mL-1, the relative standard deviation was 0.45%(n=12) for 1.6 ng· mL-1 of Mn(Ⅱ), and the sensitivity was increased by a factor of 2.5 compared to that in the absence of the β-CD. The method was used for the determination of Mn(Ⅱ) in cereal samples and wine samples with satisfactory results. The mechanism of this reaction system was also presented.
2005 Vol. 25 (10): 1662-1666 [Abstract] ( 1996 ) PDF (557 KB)  ( 339 )
1667 Study on Solid Phase Extraction Spectrophotometric Determination of Zinc with 2-(2-Quinolylazo)-5-Dimthylaminophenol
ZHOU Shi-ping1, 2,DUAN Chang-qun1*,LIU Hong-cheng3,HU Qiu-fen1
A highly sensitive, selective and rapid method for the determination of zinc based on the rapid reaction of zinc(Ⅱ) with 2-(2-quinolylazo)-5-dimthylaminophenol (QADMAP) and the solid phase extraction of zinc ion with anion exchange resin cartridge was developed. In the presence of pH 8.5 buffer solution and Triton X-100 medium, QADMAP can react with zinc(Ⅱ) to form a stable 2∶1 complex (QADMAP∶Zn(Ⅱ)). The molar absorptivity is 1.22×105 L·moL-1·cm-1 at 590 nm. Beer’s law is obeyed in the range of 0-1.0 μg·mL-1. The zinc ions in the samples can be enriched and separated by solid phase extraction with anion exchange resin cartridge. Testing results show that recovery for zinc(Ⅱ) was from 95% to 104%, and RSD was below 3%. This method was applied to the determination of zinc in water and food with good results.
2005 Vol. 25 (10): 1667-1670 [Abstract] ( 1116 ) PDF (529 KB)  ( 356 )
1671 Multi-Wavelength Negative Absorption Fading Spectrophotometry to Determine Trace Nitrite and It’s Mechanism
SI Wen-hui1, ZI Yan-qin2
Using negative absorption rectifyingtechniquie, the authors investigated spectra of the reaction of nitrite with acridine yellow in 1.0 mol·dm-3(1 dm=10 cm=0.1 m) hydrochloric medium. The authors established the new dynamics method of mensuratiog trace nitrous acid radical by the negative absorption undertint spectrophotometry at multi-wavelengths, based on the linear relation between the negative absorbance value or the AT value of absorbance sum and the nitrous acid radical concetration in a certain range. The linear range was 7.2×10-6-3.6×10-4 mol·dm-3, RSD was 1.06%-3.12%,and CV (recovery) was 98.00%-100.20%. In application to the determination of nitrite in environmental water sample, satisfoctory result was abtained with high accuracy, better selectivity and common ions ceasing to effect measuring. According to the change in the absorption peak value in the reactive system, the liquor acidity, the different order for added reagent, liquor temperature, reactive time, acid kind etc., the authors believe that the reaction of acridine yellow with mitrite is diazotization-coupling, under the condition of feasible pH value, temperature, and additive order of midium.
2005 Vol. 25 (10): 1671-1673 [Abstract] ( 1036 ) PDF (381 KB)  ( 340 )
1674 Kinetic Spectrophotometric Determination of Trace Chromium(Ⅵ) with Sensitized Function of Microemulsion
YU Ping, GAO Jun-jie, SONG En-jun
A sensitive catalytic spectrophotometric method for determining μg·L-1 of chromium(Ⅵ) has been developed. The method, based on the catalytic effect of Cr(Ⅵ)on the oxidation of aligarin red with hydrogen peroxide, was monitored spctrophotometrically in the medium of microemulsion which consists of CTMAB , n-pentanol, n-heptane and water. The variables affecting the rate of the reaction were investigated. The linearity range of the calibration graph is dependent on the reaction temperature. The sensitivity of this method is 72.5% higher in the microemulsion medium than in CTMAB medium. The apparent active energy of the catalytic reaction is 55.7 kJ·mol-1. The calibration graph is linear for 2.4-75 μg·L-1 Cr(Ⅵ)at 80 ℃, the detection limit is 4.27×10-10 g·mL-1, and the relative standard deviation of eleven determinations of 60 μg·L-1 Cr(Ⅵ)was 1.84%. The method has been successfully applied to the determination of chromium(Ⅵ)in the electroplating waste water.
2005 Vol. 25 (10): 1674-1676 [Abstract] ( 1088 ) PDF (355 KB)  ( 360 )
1677 Study of Photocatalytic Activity, Characterization and Preparation of Supersuspended Nano-TiO2 (Ⅱ) Photocatalytic Activity
ZHAO Jin-wei1,2,YUAN Min1,2,LIU Xiao-heng1
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. The results show that the photocatalytic activity of both products is obvious with no great 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.
2005 Vol. 25 (10): 1677-1679 [Abstract] ( 1656 ) PDF (334 KB)  ( 381 )
1680 Study on BS-12 as a New Probe for the Determination of DNA by Resonance Light Scattering
CHEN Zhan-guang1, 2, LIAO Xu-hong1, HAN Ya-li1, YANG Ying-yi1, LU-Feng1, DING Wei-feng1
A new method has been developed for the determination of DNA by resonance light scattering with dodecyl dimethyl betaine (BS-12) in aqueous solution as a new probe. At pH 9.3, the interactions of BS-12 and DNA gave strong RLS signals at 388.0 nm. Linear relationships were found between the enhanced intensity of RLS and the concentration of DNAs in the range 0.25-12.0 μg·mL-1for fsDNA and 0.25-11.0 μg·mL-1 for ctDNA. The limits of detection were 0.15 ng·mL-1 and 0.16 ng·mL-1 for fsDNA and ctDNA, respectively. The method was applied to the determination of synthetic samples with satisfactory results.
2005 Vol. 25 (10): 1680-1683 [Abstract] ( 1057 ) PDF (461 KB)  ( 358 )
1684 Determination of Rare Earth Elements in Trialkyl Phoshine Oxide (TRPO)-Kerosene by ICP-AES
ZHANG Lin,WANG Jian-chen*,XIN Ren-xuan
The present paper describes the determination of rare earth elements (REEs) in 30% TRPO-kerosene by inductively coupled plasma atomic emission spectrometry (ICP-AES) with ethanol as diluent. The relative intensities of REEs vary slowly when the content of 30% TRPO-kerosene varies from 4% to 20%. The relative intensity of Ce increased with the contents of H2O increasing from 1% to 7% , but the other REEs did not vary. No effects on the relative intensities of REEs are seen when the concentration of HNO3 varies from 0.065 to 0.315 mol·L-1 . The effects of Fe and Zr on the relative intensities of REEs are also investigated. The effects of Fe on the relative intensities of REEs are not obvious, but when the concentration of Zr is ten times larger than REEs, the effects are obvious. The method is applicable when the content of 30% TRPO-kerosene ranges from 4% to 20%, the limits of detection of La, Ce, Pr, Nd, Sm are 0.012, 0.040, 0.029, 0.040 and 0.021 μg·mL-1 respectively, the RSD% is lower than 2%, and the relative error is lower than 3% when compared with the determination result of digestion. In contrast with digestion, this method is simple and rapid, and can accord with the requests of analysis.
2005 Vol. 25 (10): 1684-1687 [Abstract] ( 1459 ) PDF (499 KB)  ( 357 )
1688 Study on Hg2+ Distribution and Speciation in Different Tissues of Rats
SHEN Jin-can1, HUANG Zhi-yong3, ZHUANG Zhi-xia1, 2, WANG Xiao-ru1, 2*, Lee Frank S C2
Mercury is one of the important pollutants that threaten people health greatly in environment. The purpose of this paper was to determine mercury distribution and mercury binding proteins in different tissues of rat fed orally with mercuric chloride by ICP-MS and SEC-UV-ICP-MS. The result showed that liver and kidney induced large amount of metallothioneins that was found to bind to mercury, copper and zinc after mercury intake in stomach and intestines. The metallothioneins induced may be prior to combine the mercury so that it would decrease mercury binding with the other proteins that would disable their normal function.
2005 Vol. 25 (10): 1688-1692 [Abstract] ( 1105 ) PDF (625 KB)  ( 376 )
1693 Effect of Lens-to-Sample Distance on Laser-Plasma Radiative Properties
CHEN Jin-zhong1, ZHAO Shu-rui2, WEI Yan-hong1, GUO Qing-lin1, HUAI Su-fang1
In the present paper, the effect of lens-to-sample distance (LTSD) on the radiative properties from the plasma induced by a high-energy neodymium glass laser (~25J) in the argon ambient gas at a pressure of 0.43×105 Pa was studied. The experimental results showed that when the focus point of the focusing lens (f=130 mm) shifts above and below the sample surface, the radiation intensities of the plasma, the excitation temperature, and the mass of ablated material are all changed, and their maxia appear at a focusing location of the laser beam, which is about 0.4 mm under the sample surface for alloyed-steel samples. If soil samples are used as the targets, the emission intensities of the laser plasma and the mass of ablated material have the maxima at a focus position about 0.2 mm below the sample surface. To investigate the influence of LTSD on the shape of the laser plasma, the images of the plasma formed have been shot in argon and air for the alloyed-steel samples. From these results, it was found that the properties of the laser plasma depend strongly on the LTSD.
2005 Vol. 25 (10): 1693-1696 [Abstract] ( 1633 ) PDF (522 KB)  ( 378 )
1697 Determination of Fe, Al and Ni in ZrO2 by Electrothermal Vaporization ICP-AES
CHEN Shi-zhong
A novel method for the analysis of ZrO2 powder via in-situ separation of the matrix from the analytes is described, based on the use of a polytetrafluorethylene (PTFE) emulsion as a chemical modifier. The main affecting factors, including the flow rate of carrier gas and auxiliary carrier gas, ashing temperature and time, matrix concentration, signal record time, and vaporization temperature and time, were investigated systematically. Under the optimum operating conditions, the detection limits (DL) of analytes vary from 4.2 ng·mL-1 (Al) to 11 ng·mL-1 (Fe). The relative standard deviations (RSDs) are 3.1%-4.9%.
2005 Vol. 25 (10): 1697-1699 [Abstract] ( 1622 ) PDF (419 KB)  ( 393 )
1700 The Application of Trace Element Analysis to the Study of Provenance of Copper Minerals in Ancient Bronzes
LI Qing-lin1,2,ZHU Jun-xiao3,QIN Ying4,MAO Zhen-wei4, WANG Chang-sui4*,CHEN Jian-li5
The simulated smelting and founding experiment of bronze showed that the copper minerals from different regions could be distinguished clearly by using the multi-statistical analysis based on choosing the chalcophile elements determined by ICP-AES. In the present paper, the data of trace elements in bronzes from Panlongcheng Site and Ezhou, which were determined by NAA, were tried to be processed. The analytical result showed that the bronzes from Panlongcheng and Ezhou could be divided clearly, just like the results of the former simulated smelting and founding experiment of bronze. So, the feasibility of trace element analysis for the study of provenance of copper minerals in ancient bronzes was proved again.
2005 Vol. 25 (10): 1700-1702 [Abstract] ( 2222 ) PDF (373 KB)  ( 404 )
1703 Analysis of 23 Mineral Elements in Tea Samples Collected from China and Japan by Using ICP-AES and ICP-MS Combined with a Closed Decomposition
WANG Xiao-ping1, MA Yi-jin1,Mitso itoh2
After a closed decomposition, the concentrations of Al, Ba, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, La, Mg, Mn, Na, Ni, Pb, Rb, Sb, Sr, Th, U, Y and Zn in thirteen Chinese tea samples and six Japanese tea samples were analysed by using ICP-AES and ICP-MS, a tea standard reference material (GBW07605) was used to verify the accuracy and the precision of analytical method. It was demonstrated that a closed decomposition can help to get good results for the concentrations of mineral elements in tea samples. Compared with those in Japanese tea samples, the concentrations of Cd, Co, Cr, Cs, Fe, Pb, Rb, Sb, Th, U and Zn in Chinese tea samples are significantly high, which means the atmosphere in China is contaminated by heavy metal particles more severely than that in Japan. Moreover, it was found that the concentrations of many mineral elements in tea samples correlate each other.
2005 Vol. 25 (10): 1703-1707 [Abstract] ( 397 ) PDF (544 KB)  ( 440 )
1708 Determination of Mercury in Chinese Medicinal Material and Biological Samples Using Pyrolysis Atomic Absorption Spectrometry
HUANG Ru-jin1, ZHUANG Zhi-xia1,2*,WEI Jin-feng3, ZHANG Shu-qiong1, SHEN Jin-can1, WANG Xiao-ru1, 2
In this paper a rapid and simple method using pyrolysis coupled with atomic absorption spectrometry for the analysis of total mercury in Chinese medicinal material and biological samples is presented. No sample digestion was needed and this greatly simplifies the analytical procedure and minimizes potential sources of contamination. Under optimum conditions, the reproducibility of the method was 2.1% for peak area and 9.1% for peak height. The detection limit (3σ) was 6.3 ng·g-1, and the recovery was within the range of 95%-105%. Several standard reference materials were analyzed and the results were obtained with satisfaction. The performance of the method was compared with inductively coupled plasma-mass spectrometry (ICP-MS), and excellent agreements were observed between these two methods.
2005 Vol. 25 (10): 1708-1710 [Abstract] ( 1681 ) PDF (429 KB)  ( 383 )
1711 Study of Determination Method for Lead and Cadmium in the Semen and Liquor Follicle of Genetic Fluid
YU Jian-qiao1,SHI Xiao-yong1,YANG Ming-ming2,PAN Li2, CHEN bo1
Lead and Cadium as the key elements influencing human genetic health were selectively determined in the present paper. In the area of metal elements determination in body fluid,most samples used in the study are blood,plasma and saliva. No literature about genetic fluid determination has been found so far. In the present paper the preparation of samples,volume of samples, and determination parameters were investigated. An easy reliable method of determining lead and cadium in semen and liquor follicle is established. The recoveries of lead are 99.0%-118% and the recoveries of cadium are 96.3%-109%. The determination limit of lead is 0.8 μg·L-1 and the determination limit of cadium is 0.05 μg·L-1. The relative standard deviations (RSD)(n=5)are 3.74%-8.54%.
2005 Vol. 25 (10): 1711-1713 [Abstract] ( 376 ) PDF (330 KB)  ( 355 )
1714 Spectrometric Determination of Trace Elements in Pagoda Flower
FAN Wen-xiu1,LI Xin-zheng2
The twelve trace elements in the pagoda flower, including K, Na, Ca, Mg, Pb, Cd, Cu, Mn, Co, Zn, Cr and Fe were determined simultaneously by FAAS. The relative standard deviation of the method is 0.07%-2.31%, and the recovery is 97.0%-107.0%. The analytical results were satisfactory. The results showed that there were comparatively rich metal elements in the pagoda flower. Proportions of the twelve elements are in the order that K>Ca>Mg>Na>Fe>Zn>Cu>Mn>Co>Pb>Cr>Cd. It implied that the nutritive value of the pagoda flower is high.
2005 Vol. 25 (10): 1714-1716 [Abstract] ( 1068 ) PDF (358 KB)  ( 386 )
1717 Studies of Complexing Action Mechanism in Indirect Determination of Cysteine by FAAS with ZnS
LIU Wen-han, SHAN Shen-yan, ZHANG Dan, WU Xiao-qiong
Each state of cysteine and zinc ion in aqueous solution at different pH conditions was calculated by computer, giving out the distribution curve. The mechanism of complexing action in indirectly determining cysteine by flame atomic absorption spectrometry with ZnS, and the influence of solution pH were studied. The state of cysteine and zinc ion in aqueous solution at different pH is different. The reason for forming the peak is the change of concentration of cysteine and zinc ion at different pH. The soluble complexing ion is composed of -1 valence cysteine Cys- and Zn(OH)2. The theoretical analysis is well conformable with the data determined from the experiments. The structure of complexing ion is Zn(OH).
2005 Vol. 25 (10): 1717-1719 [Abstract] ( 1169 ) PDF (378 KB)  ( 410 )
1720 Non-Nascent Hydrogen Mechanism of Plumbane Generation
ZOU Yan, JIN Fu-xia, CHEN Zhi-jiang, QIU De-ren, YANG Peng-yuan*
The mechanism of plumbane generation in dichromate system was studied via investigation of the relationship between the plumbane yield and the molar number of the reactants. A flow injection hydride generator was used in the study. Reactant moler number was calculated by the injected volume and the reactant concentration, and the plumbane yield was measured via an AAS spectrometer equipped with an electrothermal quartz tube atomizer. Experimental results show that the acid was first used for the neutralization of NaOH and successively participated in the redox reaction of borohydride with dichromate with a constant molar ratio of 9.95±0.42(expressed in terms of mean±standard deviation). At the same time,plumbane generation was displayed as synchronously taking place with the redox reaction, and the yield increased with the increase of acid. The mechanism of plumbane generation was thus deduced as an induced reaction or a catalytic reaction by the redox reaction. Up to this end, the non-nascent hydrogen mechanism of hydride generation has been verified for all the IVA elements.
2005 Vol. 25 (10): 1720-1723 [Abstract] ( 1608 ) PDF (408 KB)  ( 379 )
1724 CCD-Array Detection-Flow Injection Analysis of Oligomeric Proanthocyanidins in Health Food
LI Yuan-qian1, Lü Xing1, ZOU Xiao-li1, MI Jian-ping1, YANG Jing-guo2
A flow-injection-CCD array detection spectrophotometry for the determination of oligomeric proanthocyanidin (OPC) in health foods was developed in the present paper, based on the reaction that OPC can form red anthocyanidin in hydrochloric acid medium with ferric ion as a catalytic agent. The absorption spectrum of OPC was scanned and the absorbance at 545 nm was determined by flow injection with CCD-array detector. The influencing factors of the chromogenic reaction and parameters of the flow injection analysis were optimized. There is a good linear relationship between the absorbances and the concentrations of OPC in the range of 0.010-0.20 mg·mL-1. The detection limit of the method was 5 μg·mL-1. The recoveries were 82.47%-98.18% with the relative standard deviation (RSD) of 1.5%-4.9%. The proposed method is sensitive, accurate and rapid with the sampling frequency of 10 samples·h-1 and suitable for the determination of OPC in the health food.
2005 Vol. 25 (10): 1724-1726 [Abstract] ( 1052 ) PDF (424 KB)  ( 385 )
1727 Determination of Net Electric Field in Dielectric Barrier Discharge in N2 by Relative Spectrum Line Intensity
DONG Li-fang1,YIN Yan1,DONG Jian-ming2
The process of N2 discharge in direct current electric field is simulated by Monte Carlo method. The electron drift velocity as a function of E/N is given, which is in good agreement with experimental result. The variations of the number density of electronic excitation states of N2 (A3Σ+u and a1Πg) with the reduced field E/N are simulated. A method is proposed to determine the net reduced electric field in dielectric barrier discharge by monitoring the relative intensity of spectrum line 145 nm and spectrum line 201 nm.
2005 Vol. 25 (10): 1727-1729 [Abstract] ( 1053 ) PDF (394 KB)  ( 383 )
1730 Effect of the Cu+ Concentration on the Curve of Thermoluminescence of ZnS:Cu Electroluminescent Material
LI Zhi-qiang, TIAN Shao-hua, SONG Wei-peng, WEI Zhi-ren, DOU Jun-hong, LI Juan
In the paper, five ZnS∶Cu electroluminescent material specimens were prepared by adding 0.05%, 0.10%, 0.15%, 0.20% and 0.25% Cu+ to ZnS. From the sample’s thermoluminescence curve and luminance, the authors can see that with the variation of Cu+ concentration, the peak of thermoluminescence curve changed correspondingly. At first with the increase of Cu+ concentration, the peak of thermoluminescence curve rised gradually. When the Cu+ concentration was 0.05%, the peak of thermoluminescence curve was 124.15 which attainded max, when the Cu+ concentration was 0.25%, the peak of the curve of thermoluminesence forther decreased to 51. But the temperature corresponding to the peak of the curves of thermoluminesence didn’t change, which means that the depth of electron trap did not vary. The authors therefore conclude that excessive Cu+ results in a decline of luminance because the energy of trapped electrons turns into the transition without radiation, though the probability of trapping electrons increases and the life of photoelectrons shortens as the luminescence center increases. In this way, there is an optimal value for Cu+ concentration, which leads to the peak of the curves of thermoluminesence and the maximum of luminance.
2005 Vol. 25 (10): 1730-1732 [Abstract] ( 1127 ) PDF (313 KB)  ( 356 )
1733 Photostimulated Luminescence Properties of KCl:Cu+ after UV Excitation
SUN Li1, WANG Yong-sheng1, ZHAO Su-ling1, XU Zheng1,2, XUE Wei-wei1
KCl:Cu+ powder sample was prepared with high temperature solid reaction process. After being excited by UV, the sample shows near ultraviolet blue luminescence by stimulation with 560 nm light. The research result indicates that Cu+ acts as a luminous center, and Cu+ does not change into Cu2+ by UV irradiation. So, Cu+ ions do not act as hole traps, while anion vacancies act as electron traps. Once UV excited sample is stimulated, electrons from F center combine with hole trapping center or VK center, and cause subsequent energy transfer to Cu+ ion. Then, a character emission attributed to d-s transition of Cu+ in lattice occurs.
2005 Vol. 25 (10): 1733-1735 [Abstract] ( 1576 ) PDF (326 KB)  ( 385 )
1736 Study on Preparation and Spectroscopy of Silica-Alumina Hydrogel and Silica from Kaolin
LI Yan-feng1, PAN Xiao-bing1, LIU Gang2 , MEN Xue-hu1 , ZHANG Shu-jiang1 , WANG Xiao-long1
In our research, silica-alumina hydrogel was prepared by activation with NaOH and reaction with HCl from kaolin, and silica was obtained from the hydrogel by drying and acidifying with HCl. IR, XRD and XRF were used for testing the results, and better result was obtained. The optimal conditions of processing for kaolin 40 g were 15-20 g of sodium hydroxide and 4-5 mol·L-1 of hydrochloric acid. Finally, preparation processing to get silica, as well as the structure and purity of the resulting silica were characterized by means of IR, XRD and XRF.
2005 Vol. 25 (10): 1736-1738 [Abstract] ( 1489 ) PDF (387 KB)  ( 393 )
1739 Luminescence Spectra of Sm3+ Doped Sr2CeO4 Synthesized through Co-Precipitation Process
SHI Shi-kao1, 2, LI Jun-min1,ZHOU Ji2*
The precursor powders of Sm3+ doped Sr2CeO4 were obtained by the application of (NH4)2C2O4 as a precipitant. After calcinations, the precursor powders became a white emitting fluorescent material. The XRD and emission spectra manifest that the optimum temperature and Sm3+ concentration for synthesizing Sr2CeO4:Sm are 1 050 ℃ and 1 mol%, respectively. The better the phosphor powders crystallize, the higher their emission intensities are. The excitation spectrum implies that the transition emissions of Sm3+ at 608 and 654 nm originate from the Ce4+-O2- charge transfer (MLCT) resulting from the interaction of Ce4+ and the neighboring O2-. Therefore, it can be concluded that the host Sr2CeO4 acts as a sensitizer, which transfers the energy to Sm3+. The emission intensity of the phosphor synthesized through co-precipitation is much higher than that of phosphor prepared using conventional solid state reactions.
2005 Vol. 25 (10): 1739-1741 [Abstract] ( 1030 ) PDF (393 KB)  ( 346 )