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2010 Vol. 30, No. 03
Published: 2010-03-01

 
       光谱学与光谱分析
577 The Error Analysis and Experimental Verification of Laser Radar Spectrum Detection and Terahertz Time Domain Spectroscopy
LIU Wen-tao1,LI Jing-wen1,SUN Zhi-hui2
DOI: 10.3964/j.issn.1000-0593(2010)03-0577-05
Terahertz waves (THz,T-ray) lie between far-infrared and microwave in electromagnetic spectrum with frequency from 0.1 to 10 THz. Many chemical agent explosives show characteristic spectral features in the terahertz. Compared with conventional methods of detecting a variety of threats, such as weapons and chemical agent, THz radiation is low frequency and non-ionizing, and does not give rise to safety concerns. The present paper summarizes the latest progress in the application of terahertz time domain spectroscopy (THz-TDS) to chemical agent explosives. A kind of device on laser radar detecting and real time spectrum measuring was designed which measures the laser spectrum on the bases of Fourier optics and optical signal processing. Wedge interferometer was used as the beam splitter to wipe off the background light and detect the laser and measure the spectrum. The result indicates that 10 ns laser radar pulse can be detected and many factors affecting experiments are also introduced. The combination of laser radar spectrum detecting, THz-TDS, modern pattern recognition and signal processing technology is the developing trend of remote detection for chemical agent explosives.
2010 Vol. 30 (03): 577-581 [Abstract] ( 2372 ) PDF (2586 KB)  ( 440 )
582 The Spectral Line Profile with Different Electric Microfield Distribution Functions
RAN Jun-xia1,ZHANG Shao-peng2,MA Dong3,WANG Xiao-fei1
DOI: 10.3964/j.issn.1000-0593(2010)03-0582-04
According to Stark broadening theory, Stark broadening spectral line profile is asymmetric in essence considering plasma ions impact. The electric microfield distribution function is very important for the spectral line profile. The Stark broadening spectral line profile is described with different electric microfield distribution functions. The results show that the Stark broadening spectral line profile is similar with the Holtsmark distribution and nearest-neighbor field distribution, and it is diversification with Mayer model. With the decrease in the electrons impact broadening parameter, the influence of different electric microfield distribution functions is diminished. With the decrease in the plasma ions impact parameter, the influence of different electric microfield distribution functions is trailing off. The results also show that the action of electric microfield distribution functions is similar when the plasma ions impact parameter is very small. It is illustrated that the intense impact of plasma ions has great influence on the spectral line profile. The results may have important reference for the plasma diagnosis.
2010 Vol. 30 (03): 582-585 [Abstract] ( 1629 ) PDF (1054 KB)  ( 447 )
586 Molecular Geometries and Theoretical Electronic Spectra of Four 1,8-Naphthyridine Derivatives
CHI Shao-ming1, 2, 3, LI Li1, 2, CHEN Yong1, FU Wen-fu1, 2*
DOI: 10.3964/j.issn.1000-0593(2010)03-0586-05
The molecular geometries of four 2,4-dimethyl-7-amino-1,8-naphthyridine derivatives were optimized with B3LYP/6-31G(d) method. The energies of their frontier molecular orbitals and the molecular structures were investigated theoretically. The theoretical electronic spectra were calculated with TD-DFT in gas phase, PCM-TD-B3LYP/6-31+G(d) and semiempirical ZINDO in CH2Cl2 solution. The influences of solvent model and calculation methods on the electronic absorption spectra were also probed. The calculated results show that delocalized π bonds exist in the four 1,8-naphthyridine derivatives, and their energy gaps (ΔE) between HOMO and LUMO are relatively small. The variation in their ΔE values gives a consistent trend with that of their electronic absorption with λmax. Theoretical spectra achieved prove that their absorptions are red-shifted when the delocalization of π electrons is enhanced or the capability to donate electron by a substituted group is increased. The maximum absorption peaks of the four derivatives originate from π(HOMO)→π*(LUMO) transition. The spectra calculated at the PCM-B3LYP/6-31+G(d) level have little difference from experimental results: the differences in wavelength are 2.6, 10.3, 5.3 and 6.9 nm, whereas those in energies are 0.03, 0.09, 0.04 and 0.08 eV, respectively. The obtained results suggest that electronic spectra calculated by TD-DFT on the bases of geometries optimized with B3LYP/6-31(d) are in agreement with experimental ones, and can account for the different spectroscopic properties of the four 1,8-naphthyridine derivatives.
2010 Vol. 30 (03): 586-590 [Abstract] ( 291 ) PDF (1003 KB)  ( 365 )
591 Effect of O2/Ar Ratio on Blue Photoluminescence Spectrum of Nanocrystalline ZnO Films
SONG Guo-li1,FANG Xiang-yun2,LIANG Hong1
DOI: 10.3964/j.issn.1000-0593(2010)03-0591-04
Nanocrystalline ZnO films were deposited on quartz substrates by radio-frequency magnetron sputtering (RFMS) method. The authors discussed the effect caused by the change in the ratio of oxygen to argon and quartz substrates temperature on the qualities of thin films and blue photoluminescence spectrum of ZnO films. Relationship between XRD intensity and FWHM of nanocrystalline ZnO films at different ratio of O2/Ar in processing was given. Photoluminescence spectrum (PL), absorption spectra (ABS), photoluminescence excitation spectrum (PLE) and X-ray diffraction pattern (XRD) of nanocrystalline ZnO film with excitation wavelength 300 nm were measured at room temperature. XRD pattern indicates that nanocrystalline ZnO film has a hexagonal wurtzite structure and is polycrystalline. Blue visible emission bands (430-460 nm) were observed, and its central wavelength is 445 nm. The relationship between PL area of integration and PL intensity of maximum of nanocrystalline ZnO films at different ratio of O2/Ar in processing was given. The luminescence emission peak located at 450 nm corresponds to the transition from the shallow level of oxygen vacancy to valence band or the interstitial.
2010 Vol. 30 (03): 591-594 [Abstract] ( 1249 ) PDF (815 KB)  ( 422 )
595 Measurement and Analysis of Blue-Violet Light Emitting Spectrum on Tiny Cubic Boron Nitride Crystal
LIU Hai-bo1,JIA Gang1*,XU Zhong-hui2,MENG Qing-ju1,SUN Xiao-bing3
DOI: 10.3964/j.issn.1000-0593(2010)03-0595-04
The electroluminescence effect can be observed by the micro N-type wide-gap CBN semiconductor crystal under the condition of static eletric field. The micro N-type CBN crystal was fixed on the focus of the parabolic reflector of grating monochromator, and the maximum value of transmission ratio and the ideal signal-noise ratio can be obtained. Under the condition of static ectric-field intensity (4.7×106 V·cm-1), the blue-violet light-emitting spectrum of the CBN crystal was measured in the range from 350 to 450 nm. The construction of the CBN energy band, which was calculated with the First-principles method, the nonlinear relationship between current density and the ectric-field intensity that was measured and the phenomenon of electrical break-down were considered together to enable us to discuss the luminescence mechanism. Finally, the authors came up with the luminescence mechanism concerning electron migration from Γ energy valley to X energy valley. The large number of excited electrons we talked about were generated by polarization and breakdown of defect dipole before avalanche breakdown occurred.
2010 Vol. 30 (03): 595-598 [Abstract] ( 1581 ) PDF (974 KB)  ( 405 )
599 Study on Luminescence Characteristics of Polymer Doped with Two Different Phosphorescent Materials
YUE Xin1, XU Zheng1*, ZHANG Fu-jun1, ZHAO Su-ling1, SONG Dan-dan1, YAN Guang1, HU Tao1,Wageh S2
DOI: 10.3964/j.issn.1000-0593(2010)03-0599-04
With the development of organic light-emitting diodes, interests in the mechanisms of charge carrier photo generation, separation, transport and recombination continue to grow. Phosphorescent organic light-emitting diodes have gained considerable interest in the last 10 years because of high luminance efficiency. In the present paper, the authors investigated the optical and electrical characteristics of the devices based on Ir(ppy)3 and Ir(piq)3 doped PVK matrix emission layer at room temperature. The PL spectra show that the energy transfer from PVK to Ir(piq)3 is harder than that of PVK to Ir(ppy)3. The Luminescence characteristics of devices with different doping ratio show that it is not the energy transfer from matrix, but the recombination of injected carriers on phosphorescent molecules that is the main origin of EL emissions. From the viewpoint of energy level, the characteristics of carrier-trap and transport in Ir(piq)3 are better than in Ir(ppy)3 due to the high HOMO and low LUMO in Ir(piq)3.
2010 Vol. 30 (03): 599-602 [Abstract] ( 1839 ) PDF (1081 KB)  ( 449 )
603 Preparation and Luminescence Properties of Transparent Gd2O3∶Eu Thick Film
GU Mu, ZHOU Feng, LIU Xiao-lin, NI Chen, HUANG Shi-ming, LIU Bo
DOI: 10.3964/j.issn.1000-0593(2010)03-0603-04
High-resolution X-ray imaging systems require materials with good scintillation performances, especially X-ray absorption performance. Compared with powder phosphors display devices, those with transparent crystalline phosphors are very interesting due to their higher contrast and resolution for having no optical scattering, superior thermal conductivity as well as high degree of uniformity and better adhesion. Europium-doped gadolinium oxide is a promising candidate due to its high density (7.62 g·cm-3), good light yield (18.5×103 photons/MeV), and the red emission of Eu3+ ion. The sol-gel method is one of the most important techniques for deposition of functional films, because it possesses a number of advantages over conventional film formation techniques, such as low processing temperature, easy coating of large surfaces, and homogenous multicomponent oxide films. In X-ray imaging application, the thickness of the film is the most important factor for commercial use, which can increase X-ray absorption of the film and then strengthen its luminescence yield. In the present work, transparent Gd2O3∶Eu3+ thick film was successfully prepared using sol-gel method and spin-coating technique by choosing Ln2O3 (Ln=Gd, Eu) as raw materials, 2-methoxyethanol as solvent,PVP as adhesive and PEG200 as surface modifier. The film was homogeneous and crack free. The thickness of the film could achieve 1.5 μm after 2 times of coating, and its transmittance was approximately 80% in visible region. It was shown that PVP played an important role in film preparation, which could suppress stress and increase viscidity of the sol. In addition, the excitation, emission and decay time of the Gd2O3∶Eu3+ scintillator film were studied. Their performances were quite good, which implied that the film would have promising applications in high-spatial-resolution X-ray imaging and flat panel display devices.
2010 Vol. 30 (03): 603-606 [Abstract] ( 1180 ) PDF (1000 KB)  ( 433 )
607 Synthesis and Photoluminescent Properties of Core/Shell Structure ZnS∶Mn/SiO2 Nanocrystals
JIANG Dai-xun, CAO Li-xin*, LIU Wei, SU Ge, QU Hua, SUN Yuan-guang, DONG Bo-hua
DOI: 10.3964/j.issn.1000-0593(2010)03-0607-05
Mn-doped ZnS nanopatricles synthesized by solvothermal method were successfully coated with SiO2 shells of various thicknesses by hydrolysis reaction of tetraethyl orthosilicate (TEOS). The samples were characterized by X-ray diffraction(XRD), transmission electron microscopy images (TEM), X-ray photoelectron spectroscopy (XPS) and the room temperature photoluminescence (PL) spectra. When the ZnS∶Mn nanoparticles were coated with SiO2 shells, an obvious increase in particle size and a clear shell of SiO2 can be observed. The XPS measurement also gave the evidence for the core/shell structure of ZnS∶Mn/SiO2 nanoparticles. Because the surface modification effect and the decrease in luminescent centers effect are concurrent in the SiO2 shells, the Mn emission intensity first increased and then decreased with the thickening of the SiO2 shell. The intensity, which attained its maxium at 5 shell thickness, was as 7 times as that for the bare ZnS∶Mn nanoparticles.
2010 Vol. 30 (03): 607-611 [Abstract] ( 1755 ) PDF (1189 KB)  ( 485 )
612 Synthesis and Luminiescence of Eu(Ⅲ) Complex Based on 4,4,4- Trifluoro-1-(4’-m-Terphenyl)-1,3-Butanedione and 1,10-Phenanthroline
LIU Sheng-gui1,2, LIN Cheng-you1, WANG Hui-hui1, HE Pei1, GONG Meng-lian1
A new europium (Ⅲ) complex, EuL3phen, was synthesized. Its structure was characterized by elemental analysis, IR and FAB-MS. The complex exhibits strongly red emission due to the 5D07FJ(J=0-4) transitions of Eu3+ ions under irradiation of UV or 395 nm emission light of InGaN chip. The strongest emission peak is located at 613 nm. The luminescence quantum yield is13%. The lifetime of the complex is 470 μs. The decay curve can be fit with a single exponential. The thermogravimetric analyses curve for the complex shows that the complex is stable up to 220 ℃, which meets the requirement of fabrication of LED device. A red luminescent LED was successfully fabricated by coating complex EuL3phen onto 395 nm emitting InGaN chip. The mass ratio of complex to the silicone is related to the chromaticity coordinates and efficiency of fabricated LED. When the mass ratio of complex to the silicone is 1∶25,the chromaticity coordinates of the fabricated LED with the europium complex are x=0.64 and y=0.35 and the efficiency achieves 0.89 lm·W-1. The results indicate that the complex may act as a potential red component in the fabrication of white LEDs.
2010 Vol. 30 (03): 612-615 [Abstract] ( 1905 ) PDF (909 KB)  ( 509 )
616 Study on Ultraviolet Upconversion Emissions of Gd3+ Induced by Tm3+ under 980 nm Excitation
CAO Chun-yan1,YU Xiao-guang1,QIN Wei-ping2,ZHANG Ji-sen3
DOI: 10.3964/j.issn.1000-0593(2010)03-0616-05
Series of Tm3+/Yb3+ co-doped GdF3 powders were synthesized through an easy and mild hydrothermal method. The phase and purity of powders were characterized by powder X-ray diffraction (XRD) (Rigaku RU-200b). The morphologies of the samples were characterized by field emission scanning electron microscopy (FE-SEM) (Hitachi S-4800). The ultraviolet (UV) up-conversion (UC)emission spectra were recorded by a fluorescence spectrophotometer (Hitachi F-4500) with a 980 nm semiconductor continuous wave laser diode as the excitation source. And the luminescent dynamics was measured by excitation with 980 nm using an optical parameter oscillator (OPO) laser pumped by a pulsed Nd∶YAG laser with a pulse duration of 10 ns,repetition frequency of 10 Hz,and the signal was recorded by using a monochromator and an oscillograph. Under 980 nm excitation, Gd3+, acting as a kind of host ion in the studied system, and its UV UC emissions were observed and studied. The luminescent dynamics of the characteristic emission of Gd3+ (311.6 nm, 6P7/28S7/2) was explored and studied. The luminescent dynamics analysis results indicated that, on UV UC emissions of Gd3+, Yb3+ ions served as primary sensitizer ions successively transferring energy to Tm3+ to populate the 3P2 level. Then, Tm3+ ions served as secondary sensitizer ions transferring energy to populate the multiple 6IJ states of Gd3+ 3P23H6 (Tm3+): 8S7/26IJ (Gd3+). Further, 6DJ levels were populated through other energy transfer processes between Gd3+ and Yb3+ or Tm3+. Finally, UV UC emissions from the excited 6D9/2, 6IJ, 6P5/2, and 6P7/2 states to the ground state 8S7/2 were observed. Meanwhile, Tm3+ acted as activator in its own UC emissions, and the article did not put emphasis on those except the 3P2 and 1I6 levels to the ground state 3H6 transitions. Especially, the dependences of UV UC emissions of Gd3+ on the Yb3+ concentrations, the Tm3+ concentrations,the annealing temperatures,and the excitation power densities of the 980 nm semiconductor continuous wave laser diode were studied, too.
2010 Vol. 30 (03): 616-620 [Abstract] ( 807 ) PDF (1203 KB)  ( 438 )
621 Blackbody Radiation of Cavitation Luminescence from Glycerin
HE Shou-jie1,HA Jing2,LIU Li-fang2,WANG Long3
DOI: 10.3964/j.issn.1000-0593(2010)03-0621-04
An improved conical bubble sonoluminescence U-tube was built. Using this setup, the spectra and light pulses of conical bubble luminescence in glycerin were detected. Results show that the spectra are continuum, which are well fitted by blackbody radiation. The cavitational temperature ranging from 2 600 to 3 050 K was calculated from the fitted spectra. The reasons for the existence of blackbody radiation in conical bubble luminescence were discussed both from special and temporal sides. The value of radius of cavitational bubble is about 1.7 cm theoretically, which is greater than that of the bubble acoustically excited. The width of light pulses of cavitational bubble reached 40-60 ms,and this provided enough time for the blackbody radiation. In addition, the light pulses at different wavelength were measured, and results show that the width of light pulses increased with the raise of wavelength of spectra, which proved the mechanism of blackbody radiation. Finally, based on the spectra and light pulses, the intensity of luminescence was calculated to be about 0.18 J.
2010 Vol. 30 (03): 621-624 [Abstract] ( 1861 ) PDF (863 KB)  ( 423 )
625 Spectral Characteristics of Novel Small Molecular Fluorene Derivative for Organic Light-Emitting Device
QIAN Jin-cheng1, JIA Kun-peng2, YU Jun-sheng1*, LOU Shuang-ling1, JIANG Ya-dong1, ZHANG Qing3
DOI: 10.3964/j.issn.1000-0593(2010)03-0625-05
Double-layer organic light-emitting devices (OLEDs) based on a blend system of novel small molecule fluorene material 6,6′-(9H-fluoren-9,9-diyl)bis(2,3-bis(9,9-dihexyl-9H-fluoren-2-yl) quinoxaline) (BFLBBFLYQ) and hole transporting material N,N′-biphenyl-N,N′-bis-(3-methylphenyl)-1,1′-biphenyl-4, 4′-diamine (TPD) were fabricated. The structure of the double-layer device was ITO/BFLBBFLYQ∶TPD/tris(8-hydroxyquinolinato)aluminum(Alq)/Mg∶Ag. The photoluminescence (PL) spectra of BFLBBFLYQ and TPD were located at 447 and 414 nm, respectively. The spectral characteristics of the blend system and the double-layer device were investigated, which indicated that a new long wavelength emission peaking at 530 nm was appeared both in PL spectra and electroluminescence (EL) spectra. The exciplex between BFLBBFLYQ and TPD may play the role in long wavelength emission in the blend device and the spin-coated film. Based on the absorption spectra of a red fluorescent dye 4-(dicyanomethylene)-2-tert-butyl-6(1,1,7,7-tetramethyljulolidyl-9-enyl)-4H-pyran (DCJTB) as probe and the PL spectra of the blend system showing good overlap, energy transfer from the blend system to DCJTB could be expected. Therefore, DCJTB could be selected as a molecular dopant to investigate the influence on EL spectra and the recombination of the devices. It was found that the excitons recombine at the interior Alq layer near to the BFLBBFLYQ∶TPD layer.
2010 Vol. 30 (03): 625-629 [Abstract] ( 2389 ) PDF (1186 KB)  ( 486 )
630 Study on Spectroscopic Characterization and Property of PES/ Micro-Nano Cellulose Composite Membrane Material
TANG Huan-wei1, ZHANG Li-ping1*, LI Shuai1, ZHAO Guang-jie1, QIN Zhu2,SUN Su-qin2
DOI: 10.3964/j.issn.1000-0593(2010)03-0630-05
In the present paper, the functional groups of PES/micro-nano cellulose composite membrane materials were characterized by Fourier transform infrared spectroscopy (FTIR). Also, changes in crystallinity in composite membrane materials were analyzed using X-ray diffraction (XRD). The effects of micro-nano cellulose content on hydrophilic property of composite membrane material were studied by measuring hydrophilic angle. The images of support layer structure of pure PES membrane material and composite membrane material were showed with scanning electron microscope (SEM). These results indicated that in the infrared spectrogram, the composite membrane material had characteristic peaks of both PES and micro-nano cellulose without appearance of other new characteristics peaks. It revealed that there were no new functional groups in the composite membrane material, and the level of molecular compatibility was achieved, which was based on the existence of inter-molecular hydrogen bond association between PES and micro-nano cellulose. Due to the existence of micro-nano cellulose, the crystallinity of composite membrane material was increased from 37.7% to 47.9%. The more the increase in micro-nano cellulose mass fraction, the better the van de waal force and hydrogen bond force between composite membrane material and water were enhanced. The hydrophilic angle of composite membrane material was decreased from 55.8°to 45.8°and the surface energy was raised from 113.7 to 123.5 mN·m-2. Consequently, the hydrophilic property of composite membrane material was improved. The number of pores in the support layer of composite membrane material was lager than that of pure PES membrane. Apparently, pores were more uniformly distributed.
2010 Vol. 30 (03): 630-634 [Abstract] ( 311 ) PDF (1111 KB)  ( 412 )
635 Determination of Protein and Gossypol Content in Cotton Kernel Powder with Near Infrared Reflectance Spectroscopy
QIN Li, SHEN Xiao-jia, CHEN Jin-hong, ZHU Shui-jin*
DOI: 10.3964/j.issn.1000-0593(2010)03-0635-05
Near-infrared reflectance spectroscopy (NIRS) was used as a rapid and nondestructive method to determine the protein content and gossypol content in cotton kernel powder samples, using 49 upland cotton (Gossypium hirsutum L.) germplasms and 188 recombinant inbred lines (RILs). The cottonseed samples harvested from the upland cotton germplasms and RILs grown in different cotton growing regions in different years were analyzed chemically for protein and gossypol contents, as well as scanned in the reflectance mode of a scanning monochromator. Using ISI software for scanning and data analysis, protein and gossypol calibration equations were obtained with a standard normal variate + detrending scatter correction and a 2, 4, 4, 1 math treatment and modified partial least square (MPLS) as the regression method. The protein content calibration results revealed that the multiple correlation coefficients (RSQ) and statistic 1-variance ratio (1-VR) for the determination of protein content in cottonseed kernels were 0.933 and 0.929, respectively, and its standard error of calibration (SEC) and standard error of cross validation (SECV) were 0.623 and 0.638, respectively. As the calibration equations were judged by the calibration RSQ (or 1-VR) and SEC (or SECV), the results indicated that NIRS is comparable to chemical methods in both accuracy and prediction and is reliable in the determination of protein content in cottonseed kernels. However, the RSQ, SEC, 1-VR and SECV for gossypol content determination of NIRS were 0.836, 0.811, 0.074 and 0.079, respectively. Although it was weaker than that of protein content, the NIRS method is still good enough for the determination and prediction of the gossypol content in cottonseed kernels. Therefore, NIRS models were successfully developed for protein content and gossypol content analysis of cotton kernel powder sample in the present study and they could be introduced into the cotton germplasm evaluation and breeding program for the cottonseed quality improvement.
2010 Vol. 30 (03): 635-639 [Abstract] ( 704 ) PDF (793 KB)  ( 461 )
640 Study on Different Proportion Formulas of Activating Blood Circulation by FTIR
XU Mao-ling1,LI Hui-fen3,ZHOU Qun2,YIN Quan1,SUN Su-qin2*,WU Xian-zhong4
DOI: 10.3964/j.issn.1000-0593(2010)03-0640-04
Fourier transform spectroscopy (FTIR) and two-dimensional correlation spectroscopy were used to analyze different compatibility forms of sargentgloryvine stem, radix paeoniae rubra and cortex moutan in order to study the FTIR spectra of different proportion formulas. The results indicate that different proportion formulas have distinct change regularity in FTIR spectra, second derivative spectra and synchronous 2D. Key components of sargentgloryvine stem’s characteristic absorption band are 1 610, 1 518 and 1 446 cm-1 which are characteristic absorption band of aromatic material, and in the original formula, that shows stronger peak than others, suggesting that original formula can make the best of composition of drug action. In the different proportion formulas, 1 614 cm-1 is nearer to 1 610 cm-1, which is sargentgloryvine stem’s characteristic absorption band, than to 1 706 cm-1, illustrating that sargentgloryvine stem is more influential formula than others. According to identification and ascription of characteristic absorption band, it was initially revealed that different proportion of drug dosage can affect pharmacodynamic action of integral formula.
2010 Vol. 30 (03): 640-643 [Abstract] ( 1585 ) PDF (945 KB)  ( 406 )
644 Research on Spectrum Denoising Methods Based on the Combination of Wavelet Package Transformation and Mathematical Morphology
LI Hui1, 2, 3, LIN Qi-zhong1, 2, WANG Qin-jun1, 2, LIU Qing-jie1, 2, WU Yun-zhao4
DOI: 10.3964/j.issn.1000-0593(2010)03-0644-05
The present study introduced the generalized morphological filter into the denoising of visible and near infrared spectra for the first time, and provided a new method for denoising the reflectance spectra by combining mathematical morphology methods with the wavelet packet transformation. The authors used vegetable spectra from USGS spectral library as the reference spectra, and obtained the noised spectra by adding noises with different signal-to-noise ratios to the referenced spectra. The results were evaluated by signal-to-noise ratio (SNR), root mean squared error (RMSE), normalized correlation coefficient (NCC) and smoothness ratio (SR) of the denoised spectra. The authors’ results showed that both the thresholding on wavelet packet decomposition best bases method and the generalized morphological filter method could maintain the spectral shape and the spectral smoothness after denoising. The generalized morphological filter method can remove larger amplitude random noise whereas the continuous small amplitude random noise could not be removed well. Hence, the denoised spectra were not smooth. Nevertheless, the denoised spectra using the thresholding on the best base groups of wavelet packet decomposition method were smooth, but the larger amplitude noise could not be removed completely. The authors’ method by combining the two methods has the merits of the two methods but removing their defects. The results showed that both large and small amplitude noise could be removed completely, meanwhile the normalized correlation coefficient (NCC) and smoothness ratio (SR) were improved, which indicated that the authors’ method is superior to other methods in denoising visible and near infrared spectra.
2010 Vol. 30 (03): 644-648 [Abstract] ( 472 ) PDF (924 KB)  ( 461 )
649 Research on the Trash Content Measurement and Classification of Ginned Cotton by Using NIR Spectroscopy Technique
GUO Jun-xian1, 2, RAO Xiu-qin1*, CHENG Fang1, YING Yi-bin1, KANG Yu-guo3, LI Fu-tang3
DOI: 10.3964/j.issn.1000-0593(2010)03-0649-05
Near infrared (NIR) spectroscopy was investigated to predict trash content and classify types of ginned cotton by using a fiber-optic in diffuse reflectance mode. Different spectra preprocessing methods were compared, and partial least-squares (PLS) regression was established to predict the trash content of ginned cotton. Discriminant analysis (DA) was used to classify various types of lint and content level of trash. The correlation coefficient r was 0.906 for optimal PLS model using three factors based on first-order derivative spectra, and RMSEC and RMSEP was 0.440 and 0.823 respectively. To classify ginned cotton with and without plant trash, the accuracy rate reached 95.4% using 15 principal components (PCs) via DA, whereas the prediction accuracy rate was only 80.9% for the classification of sample types due to containing foreign fiber, and the classification result for the content level of trash in lint was not good for the samples without any preprocessing. The result indicated that the NIR spectra of sample can be used to predict trash content in ginned cotton, which is often disturbed by type, content and distribution of foreign matters, and the accuracy of some prediction model is unsatisfactory. In order to improve the prediction accuracy, some methods would be applied in future research, such as pretreatment according to acquisition request of solid sample, or using transmission mode.
2010 Vol. 30 (03): 649-653 [Abstract] ( 1796 ) PDF (788 KB)  ( 569 )
654 Total Analysis of Organic Rubber Additives
HE Wen-xuan1, Robert Shanks2, YOU Ye-ming1
DOI: 10.3964/j.issn.1000-0593(2010)03-0654-05
In the present paper, after middle pressure chromatograph separation using both positive phase and reversed-phase conditions, the organic additives in ethylene-propylene rubber were identified by infrared spectrometer. At the same time, by using solid phase extraction column to maintain the main component-fuel oil in organic additves to avoid its interfering with minor compounds, other organic additves were separated and analysed by GC/Ms. In addition, the remaining active compound such as benzoyl peroxide was identified by CC/Ms, through analyzing acetone extract directly. Using the above mentioned techniques, soften agents (fuel oil, plant oil and phthalte), curing agent (benzoylperoxide), vulcanizing accelerators (2-mercaptobenzothiazole, ethyl thiuram and butyl thiuram), and antiagers (2,6-Di-tert-butyl-4-methyl phenol and styrenated phenol) in ethylene-propylene rubber were identified. Although the technique was established in ethylene-propylene rubber system, it can be used in other rubber system.
2010 Vol. 30 (03): 654-658 [Abstract] ( 1158 ) PDF (1766 KB)  ( 399 )
659 Study on Infrared Characteristics of Bolt and Rock in Condition of Loading
JI Yuan-ming
DOI: 10.3964/j.issn.1000-0593(2010)03-0659-04
The infrared radiation experiments on bolt and rock in the process of loading were carried out. It was found that the infrared radiation temperatures rose wholly and uniformly before stress peak with increase in loading. The bolted rock presented local dissimilation in the thermal image after stress peak. The multi-layer round infrared radiation isothermal lines were formed around bolt. The temperature was gradually reduced from inside to outside. There were two kinds of infrared omens for bolted rock fracturing, i.e., the infrared thermal image anomaly and curve of infrared radiation temperature and time anomaly, which reflected the spatial and temporal features of infrared omens respectively. The curve of infrared radiation temperature and time anomaly was temperature drop. The infrared thermal image omen was classified as high-temperature strip and low-temperature strip.
2010 Vol. 30 (03): 659-662 [Abstract] ( 1070 ) PDF (1058 KB)  ( 360 )
663 Classification of Oils by Attenuated Total Reflectance-Fourier Transform Infrared Spectrometry Combined with Pattern Recognition Techniques
LIU Qian1, 2, SUN Pei-yan2, 3, GAO Zhen-hui2, 3, CAI Wen-sheng1, SHAO Xue-guang1*
DOI: 10.3964/j.issn.1000-0593(2010)03-0663-04
In the present work, the combination of attenuated total reflectance-Fourier transform infrared spectrometry (ATR-FTIR) and pattern recognition, including principal components analysis (PCA) and hierarchical cluster analysis (HCA), is used as a fast and convenient analytical tool to classify oil samples. Twenty five samples including crude oils and fuel oils with different total contents of n-alkanes were analyzed. It was found that multiplicative scatter correction (MSC) and continuous wavelet transform (CWT) as a pretreatment method could improve the classification results of pattern recognition. The classification results were proved to be in agreement with the origin of the oil samples. The oils with high content of n-alkanes and those with low content were classified clearly by this developed method, but it still had some constraint to differentiating oils with little difference. The present work provides a feasible method for quick classification of oils, which can be used for the initial identification of spill oils and afford useful information for the further identification of the oils.
2010 Vol. 30 (03): 663-666 [Abstract] ( 651 ) PDF (665 KB)  ( 466 )
667 Application of Near-Infrared Absorption Spectrum Scanning Techniques in Gas Quantitative Measurement
DING Hui1, LIANG Jian-qi2, CUI Jun-hong1, WU Xiang-nan1, LI Xian-li1
DOI: 10.3964/j.issn.1000-0593(2010)03-0667-05
A practical gas sensing system utilizing absorption spectrum scanning techniques was developed. Using the narrow-band transmission of a fiber tunable filter (TOF) and wavelength modulation technique, the so-called cross-sensing effects of the traditional spectrum absorption based gas sensor were reduced effectively and thus the target gas was detected sensitively and selectively. In order to reduce the effects of nonlinearity of TOF on the measurement results and improve the system stability in operation, the reflection spectrum of a reference FBG was monitored and employed to control the modulation region and center of TOF wavelength precisely. Moreover, a kind of weak signal detecting circuits was developed to detect the weak response signal of the system with high sensitivity. The properties of the proposed system were demonstrated experimentally by detection of acetylene. Approximate linear relationships between the system responses and the input acetylene concentrations were demonstrated by experiments. The minimum detectable acetylene of 5×10-6, with signal-noise ratio of 3, was also achieved by experiments.
2010 Vol. 30 (03): 667-671 [Abstract] ( 1224 ) PDF (1163 KB)  ( 423 )
672 Study on CuO-CeO2 Catalysts Doped with Alkali and Alkaline Earth Metal Oxides by In-Situ DRIFTS
ZOU Han-bo, CHEN Sheng-zhou, WANG Qi-ying, LIU Zi-li, LIN Wei-ming
DOI: 10.3964/j.issn.1000-0593(2010)03-0672-05
CuO-CeO2 series catalysts are the effective catalysts for the selective CO oxidation in hydrogen-rich gas. The adsorption species on the CuO-CeO2 catalysts doped with alkali and alkaline earth metal oxides were investigated with in situ diffuse reflectance FTIR spectroscopy (in-situ DRIFTS) technique. The results showed that a bane at 2 106 cm-1, due to the carbonyl species, appeared on the CuO-CeO2 catalysts. In the reaction atmosphere, the intensity of this band increased first and then decreased with increasing the temperatures. It was noted that the main active adsorption sites of the CuO-CeO2 catalysts were Cu+ species. At lower temperatures, the carbonyl species were desorbed from the surface of CuO-CeO2 catalysts in the reversible form, while they were desorbed mainly in the irreversible form at the higher temperatures. A sharp peak at 3 660 cm-1, attributed to the geminal Ce(OH)2 group, was also apparent on the surface of reduced CuO-CeO2 catalyst. The peaks at 1 568,2 838 and 2 948 cm-1 were attributed to formate species and the peaks centered at 1 257 and 1 633 cm-1 were assigned to carbonate species. CO could react with the active hydroxyl species and generate formate species. At higher temperatures, the C—H bond of formate species could break and form carbonate species. These two species would decrease the performance of CuO-CeO2 catalysts at higher temperatures. The stronger IR peaks attributed to CO2 and formate species were observed, moreover there was still a weak IR peak assigned to carbonyl species for Cu1Li1Ce9Oδ catalyst when the temperature was above 180 ℃. It was shown that as the electron donor, the doping of Li2O on CuO-CeO2 catalyst could contribute to the irreversible desorption of CO at lower temperatures and inhibit the adsorption of H2 on the catalytic surface, and benefit the formation of formate species as well. Although the amounts of CO adsorption on Cu1Mg1Ce9Oδ and Cu1Ba1Ce9Oδ catalysts were much more than other catalysts at lower temperatures, they were mainly desorbed in the reversible form, which had no contribution to the selective CO oxidation.
2010 Vol. 30 (03): 672-676 [Abstract] ( 498 ) PDF (1530 KB)  ( 400 )
677 Rapid Evaluation of Primary Nutrients during Plant-Field Chicken Manure Composting Using Near-Infrared Reflectance Spectroscopy
WANG Xiao-yan1,2, HUANG Guang-qun1, HAN Lu-jia1*
DOI: 10.3964/j.issn.1000-0593(2010)03-0677-04
The present study explored the efficiency of quantitative analysis for the contents of total nitrogen (TN), total phosphorus (TP) and total potassium (TK) during chicken manure composting with chrysanthemum residue in a plant field using a Thermo Nicolet Antaris near-infrared reflectance spectral apparatus equipped with InGaAs detectors (Thermo Nicolet Corporation, Chicago, USA). The samples used in this study were collected from different positions during composting and were scanned in polyethylene bags at 2 cm-1 interval from 10 000 to 4 000 cm-1 with 32 co-added scans. Regression models were developed using spectral data and reference data by partial least square (PLS). In order to enhance chemical information and reduce data systemic noise, different data preprocessing methods such as smoothing, 1st and 2nd derivative, standard normal variety (SNV) and multiplicative scatter correction (MSC) were tested. The optimum preprocessing method was selected with the lowest root mean square error of cross-validation (RMSECV). Outliers were removed on the basis of being labeled as compositional outliers by the criteria that the predicted-actual difference for the sample was three standard deviations from the mean difference. According to the concentration gradient of each parameter, all samples were divided into a calibration set (3/4 samples) and a validation set (1/4 samples). Leave-one-out cross validation was performed to avoid over-fitting on the calibration sets. Based on the values of determination coefficient (R2) and relative prediction deviation (RPD) in validation sets, the prediction results were evaluated as excellent for TP and TK, and approximate for TN. Hereinto, R2 and RPD values were greater than 0.82 and 2.0 for TN, and greater than 0.90 and 3.0 for TP and TK, respectively.
2010 Vol. 30 (03): 677-680 [Abstract] ( 243 ) PDF (759 KB)  ( 426 )
681 Online Determination of pH in Fresh Pork by Visible/Near-Infrared Spectroscopy
LIAO Yi-tao, FAN Yu-xia,WU Xue-qian,CHENG Fang*
DOI: 10.3964/j.issn.1000-0593(2010)03-0681-04
The present research was focused on determination of the pH value online by visible and near-infrared spectroscopy. In the part of data gathering, fresh pork longissimus dorsi was moving at the constant velocity of 0.25 m·s-1 on the conveyor belt, and the visible and near-infrared diffuse reflectance spectrum (350-1 000 nm) was captured. In the part of data processing, band of 510-980 nm of the spectra was chosen to calibrate reflex distance, then to set up online detection model of pH value in fresh pork by partial least squares regression (PLSR). Kennard-stone algorithm was applied to divide the samples to the calibration set and validation set. The performances of several PLSR models employing various preprocessing methods including multiple scatter correction, derivative and both of them combined were compared. Further, the best performance model was optimized by interval PLSR to decrease the modeling variables of wavelength. The results indicated that the PLSR model based on preprocessing of multiple scatter correction (MSC) combined with first derivative gave the best performance with 0.905 of the correlation coefficient for validation set and 0.051 of the root of mean square errors for validation set. For the best PLSR model performance, the correlation coefficient of validation set increased to 0.926 and the root of mean square errors for validation set to 0.045 in the optimization interval PLSR model. However, only half of variables were used. The research demonstrates that using visible and near-infrared spectroscopy to determine fresh pork pH online is feasible.
2010 Vol. 30 (03): 681-684 [Abstract] ( 1344 ) PDF (725 KB)  ( 601 )
685 Rapid Evaluation of Beef Quality by NIRS Technology
YANG Jian-song,MENG Qing-xiang,REN Li-ping*,ZHOU Zhen-ming,XIE Xiang-xue
DOI: 10.3964/j.issn.1000-0593(2010)03-0685-03
The aim of the present study was to develop a near-infrared reflectance (NIR) spectroscopy rapid method for evaluation of beef quality. Partial least squares (PLS) prediction model for the physic-chemical characteristics such as moisture, fat, protein, pH, color and WBSF in beef was established with good veracity. One hundred fourteen samples from five different parts of beef carcass (tenderloin, ribeye, topside, shin, striploin) were collected from meat packer after 48 h aging. Spectra were obtained by scanning sample from 950 to 1 650 nm and pretreated the model by MSC, SNV and first derivative. Predictive correlation coefficients of physic-chemical parameters in beef were 0.947 2(moisture), 0.924 5(fat), 0.934 6(protein), 0.620 2(pH), 0.820 3(L), 0.864 6(a*), 0.753 0(b*) and 0.475 9(WBSF) respectively. Root mean square errors of calibration (RMSEC) were 0.313 3(moisture), 0.221 0(fat), 1.243 2(protein), 0.744 6(pH), 1.778 3(L*), 1.394 2(a*), 1.763 9(b*) and 1.0743(WBSF). They were externally validated with additional 30 beef samples. Statistics showed that there was no significant difference between predicted value and those obtained with conventional laboratory methods. The results showed that NIRS is a rapid, effective technique for evaluating beef quality. The predictions for chemical characteristics gave higher accuracy than prediction for physical characteristics.
2010 Vol. 30 (03): 685-687 [Abstract] ( 1852 ) PDF (483 KB)  ( 417 )
688 Effect of the Change in Fundamental Raman Scattering Coefficient with the Concentration on Fermi Resonance in Binary Solution
LI Dong-fei1,2,JIANG Xiu-lan2,SUN Cheng-lin2,JIANG Yong-heng2,ZHOU Mi2,LI Zuo-wei1, 2*,GAO Shu-qin2, LU Guo-hui2,YANG Jian-ge3
DOI: 10.3964/j.issn.1000-0593(2010)03-0688-04
The Raman scattering coefficients of the fundamental ν1(992 cm-1) of C6H6 and the fundamental ν1(656 cm-1) of CS2 changed dramatically with relative concentration of the binary solution of CS2 and C6H6. The Raman spectra of the binary solution with different relative concentrations were measured. The results show that both the ν1 fundamentals intensities changed dramatically with the relative concentration of the solution and the fundamental ν1 of C6H6 has little effect on the Fermi resonance ν16~ν8. On the contrary, the change in the ν1 fundamental intensity of the CS2 changed which has more effect not only on the Fermi resonance ν1~2ν2 but also on the ν2 fundamental. In this report, the experimental results were analyzed based on the J. F. Bertran theory and group theory.
2010 Vol. 30 (03): 688-691 [Abstract] ( 1723 ) PDF (739 KB)  ( 428 )
692 Micro-Raman Spectra for Lipids in Colorectal Tissue
GAO Ze-hong1, HU Bo2, DING Chao1, YU Jing-gong2
DOI: 10.3964/j.issn.1000-0593(2010)03-0692-05
Confocal Raman microscopy system was used to investigate the etiology of colorectal cancer at the molecular level. A total of two hundred and thirty four micro-Raman spectra were measured from thirty nine patients for surgically resected colorectal cancer specimens and adjacent normal tissues in the region 900-2 100 cm-1. Two bands at 1 064 and 1 134 cm-1 which are attributed to the all-trans bond stretching vibrations of the C—C lipid skeleton decreased in colorectal cancer tissue samples. The ratio of the Raman band intensity at 1 299 cm-1assigned to in-phase CH2 twisting vibrations of lipids to that at 1 264 cm-1 from CH in-plane deformation was different for colorectal cancerous and normal tissues. The mean values of the (I1 299/I1 264) were 3.17 for normal tissues and 1.33 for cancer tissues using the software function of “Compare Means”. Further, the scatter plots were used for grouping the ratio of Raman intensity at 1 299 to 1 264 cm-1 according to tissue pathologic types by graph of the SPSS16.00 software. The decision lines (I1 299/I1 264=1.96) separates between cancer and normal tissue with a coincidence rate of 94% (188/200) according to the histological results by graph. The results show that the differences between cancer and normal tissue spectra appear to arise from a decrease in the degree of the longitudinal order and an increase in the degree of unsaturation of lipid, which causes the fluidity of lipid to increases when normal cells are transformed into cancerous cells.
2010 Vol. 30 (03): 692-696 [Abstract] ( 509 ) PDF (1185 KB)  ( 420 )
697 Cryogenic Raman Spectroscopic Studies in the System of NaCl-MgCl2-H2O
YANG Dan1,2, XU Wen-yi2
DOI: 10.3964/j.issn.1000-0593(2010)03-0697-05
In the present paper, the best experimental conditions for producing hydrates in the NaCl-H2O and MgCl2-H2O systems were found through the cryogenic Raman spectroscopy. This experimental condition is rapidly cooling to -180 ℃ and slowly warming to observe hydrate formation process (that is manifested as a darkening of the vision in the microscope), and finally, rapidly cooling down to -180 ℃. Moreover, a qualitative or semiquantitative analytical method for NaCl-MgCl2-H2O system was established. This method is that 3 537 cm-1 may instruct the existence of NaCl hydrates, 3 514 cm-1 may instruct the existence of MgCl2 hydrates, and comparison of the intensity of 3 537 and 3 514 cm-1 peaks can be used to estimate the ratio of NaCl and MgCl2 in the system. All these are the foundations for quantifying the components of natural fluid inclusions. The author supports Samson’s idea through observing the phenomenon of experiments in the controversy of the meta-stable eutectics formation model, that is ice forms on initial cooling, leaving a residual, interstitial, hypersaline liquid. On warming, the salt hydrates crystallize from this liquid.
2010 Vol. 30 (03): 697-701 [Abstract] ( 1196 ) PDF (1328 KB)  ( 421 )
702 The Study of Nondestructive Defect Characterization of SiC by Cathodoluminescence
MIAO Rui-xia,ZHANG Yu-ming,TANG Xiao-yan,ZHANG Yi-men
DOI: 10.3964/j.issn.1000-0593(2010)03-0702-04
As the general method of defect characterization is destructive, during the current research on the effect of defect on device, nondestructive defect characterization is important especially. The defects of 4H-SiC homoepitaxial layer had been observed and studied, based on the principle of cathodoluminescence(CL). The results show that the intrinsic stacking faults(SFs), threading edge dislocations(TEDs), threading screw dislocations(TSDs) and basal plane dislocations(BPDs) can be observed by cathodoluminescence. The shape are rightangle triangle, dot and stick, repectively. So this method is available for nondestructive defect characterization. The correlation between 4H-SiC substrate defects and epilayer defects will be established if we characterize the defects of 4H-SiC wafers with and without an epilayer. In addition, if we characterize the defects of device before and after operation, the correlation between SiC defects of the devices before and after operation will be established, too.
2010 Vol. 30 (03): 702-705 [Abstract] ( 1187 ) PDF (1112 KB)  ( 449 )
706 Determination and Identification of Synthetic Food Colors Based on Fluorescence Spectroscopy and Radial Basis Function Neural Networks
CHEN Guo-qing, WU Ya-min, LIU Hui-juan, GAO Shu-mei, KONG Yan, WEI Bai-lin, ZHU Tuo*
DOI: 10.3964/j.issn.1000-0593(2010)03-0706-04
Taking ponceau 4R and amaranth as an example, concentration prediction and kind identification of synthetic food colors by fluorescence spectroscopy and radial basis function neural networks are introduced. By using SP-2558 multifunctional spectral measuring system, the fluorescence spectra were measured for solution of ponceau 4R and amaranth excited respectively by the light with the wavelength of 300 and 400 nm. For each sample solution of ponceau 4R, 15 emission wavelength values were selected. The fluorescence intensity corresponding to the selected wavelength was used as the network characteristic parameters, and a radial basis function neural network for concentration prediction was trained and constructed. It was employed to predict ponceau 4R solution concentration of the three kinds of samples, and the relative errors of prediction were 1.42%, 1.44% and 3.93% respectively. In addition, for solution of ponceau 4R and amaranth, the fluorescence intensity corresponding to the fluorescence wavelength was used as the network characteristic parameters, and a radial basis function neural network for kind identification was trained and constructed. It was employed to identify the kind of food colors, and the accuracy is 100%. These results show that the method is convenient, fast, and highly accurate, and can be used for the detection of synthetic food color in food safety supervision and management.
2010 Vol. 30 (03): 706-709 [Abstract] ( 2070 ) PDF (865 KB)  ( 425 )
710 Discrimination and Spectral Response Characteristic of Stress Leaves Infected by Rice Aphelenchoides besseyi Christie
LIU Zhan-yu1, SHI Jing-jing1, WANG Da-cheng1,2, HUANG Jing-feng1*
DOI: 10.3964/j.issn.1000-0593(2010)03-0710-05
An ASD Field Spec Pro Full Range spectrometer was used to acquire the spectral reflectance of healthy and diseased leaves infected by rice Aphelenchoides besseyi Christie, which were cut from rice individuals in the paddy field. Firstly, foliar pigment content was investigated. As compared with healthy leaves, the total chlorophyll and carotene contents (mg·g-1) of diseased leaves decreased 18% and 22%, respectively. The diseased foliar content ratio of total chlorophyll to carotene was nearly 82% of the healthy ones. Secondly, the response characteristics of hyperspectral reflectance of diseased leaves were analyzed. The spectral reflectance in the blue (450-520 nm), green (520-590 nm) and red (630-690 nm) regions were 2.5, 2 and 3.3 times the healthy ones respectively due to the decrease in foliar pigment content, whereas in the near infrared (NIR, 770-890 nm) region was 71.7 of the healthy ones because of leaf twist, and 73.7% for shortwave infrared (SWIR, 1 500-2 400 nm) region, owing to water loss. Moreover, the hyperspectral feature parameters derived from the raw spectra and the first derivative spectra were analyzed. The red edge position (REP) and blue edge position (BEP) shifted about 8 and 10 nm toward the short wavelengths respectively. The green peak position (GPP) and red trough position (RTP) shifted about 8.5 and 6 nm respectively toward the longer wavelengths. Finally, the area of the red edge peak (the sum of derivative spectra from 680 to 740 nm) and red edge position (REP) as the input vectors entered into C-SVC, which was an soft nonlinear margin classification method of support vector machine, to recognize the healthy and diseased leaves. The kernel function was radial basis function (RBF) and the value of punishment coefficient (C) was obtained from the classification model of training data sets (n=138). The performance of C-SVC was examined with the testing sample (n=126), and healthy and diseased leaves could be successfully differentiated without errors. This research demonstrated that the response feature of spectral reflectance was obvious to disease stress in rice leaves, and it was feasible to discriminate diseased leaves from healthy ones based on C-SVC model and hyperspectral reflectance.
2010 Vol. 30 (03): 710-714 [Abstract] ( 1181 ) PDF (1082 KB)  ( 380 )
715 Spectral Characteristics of Corn under Different Nitrogen Treatments
SUN Hong, LI Min-zan*, ZHANG Yan-e, ZHAO Yong, WANG Hai-hua
DOI: 10.3964/j.issn.1000-0593(2010)03-0715-05
The canopy spectral reflectance and chlorophyll content of corn were measured and analyzed under different nitrogen treatments. The trends of chlorophyll content were discussed based on different growth stages and different nitrogen levels. It was observed that the chlorophyll content increased with the increase in nitrogen, and could be affected by the environment changes including the temperature, rain, fertilizer treatment and so on. The characteristics of canopy spectral reflectance indicated that the canopy spectral reflectance changed significantly at different stages. In the visible region (400-750 nm), the reflectance increased and reached the maximum until the shooting stage, and decreased subsequently with the growth progress. In near-infrared region (750-1 000 nm), the spectral reflectance climbed sharply. It increased from tillering stage to shooting stage first, and then began to decline at trumpet stage and was raised again at anthesis-silking stage. At milking stage, the reflectance was decreased again. There were clear distinctions of visible reflectance in different nitrogen regions. At shooting stage, with the increase in nitrogen the reflectance decreased at chlorophyll absorption band (430-450 nm, 640-660nm). Investigating the reflectance of the corn canopy under the different nitrogen treatment, it was found that the reflectance was higher in normal fertilizing region than others in 550 nm, with RNormal>RLow>RHigh. At trumpet stage, the canopy reflectance in low fertilizing region was higher than others in the visible region. It was clear that the corn canopy reflectance of normal fertilizing region was the same as high fertilizing region. The results indicated over fertilizing could not help increase the corn nitrogen uptake. The study provided the basic information of chlorophyll measurement based on spectral technology and could help to guide the precision fertilizer in the field.
2010 Vol. 30 (03): 715-719 [Abstract] ( 2048 ) PDF (960 KB)  ( 428 )
720 A Facile Colloid Aqueous Method for Synthesis of Water Soluble ZnSe Quantum Dots with High Fluorescence and Stability Characterization
SHI Bao-qin, CAI Zhao-xia, MA Mei-hu*
DOI: 10.3964/j.issn.1000-0593(2010)03-0720-05
Highly fluorescent and stable ZnSe quantum dots were synthesized by a facile colloid aqueous phase route. It overcame the defects such as instability and low quantum yields of the quantum dots synthesized by early aqueous phase route. Optimum conditions were found. L-glutathione was used as the stabilizer, the molar ratio of L-glutathione, Se2- and Zn2+ is 5∶1∶5, the reaction media is pH 10.5, and the proper temperature is between 90 and 100 ℃. Quantum yields (QYs) could reach to 50.1% without post irradiation in prime synthetical conditions. And the fluorescence intensity of ZnSe QDs almost didn’t change after 3 months. Its water-soluble property is also excellent. The properties of ZnSe QDs were characterized by means of ultraviolet visible spectra, fluorescence spectra, and transmission electron microscopy. The synthesized ZnSe QDs emit blue-purple fluorescence (370 nm) when excited at 300 nm. And the excellent photochemical characteristics of the ZnSe QDs will be advantageous in the application in optothermal device manufacture and chemistry biology domain.
2010 Vol. 30 (03): 720-724 [Abstract] ( 1539 ) PDF (1580 KB)  ( 426 )
725 Spectral Analysis of Cu(Ⅰ), Zn(Ⅱ) Complexes of Schiff Base and Their Dismutation to O-2 Free Radical
XIAN Jing-chun
DOI: 10.3964/j.issn.1000-0593(2010)03-0725-04
In the present paper a new 5-nitrosalicylaldehyde was prepared by the reaction of salicylaldehyde with mix acid, and this semicarbazide Schiff base ligand and its complex containing Cu(Ⅱ) and Ni(Ⅱ) were synthesized. Its compositions and structure were characterized by elemental analyses,thermal analyses,IR spectra and UV spectra,1H NMR and molar conductivity. The dismutation to O-2 free radical was also investigated. The result shows that the structure and thermodynamic properties were stable. The complexes showed a distinct -2 scavenging effect and some protective effects on hemoglobin of human erythrocyte in the system of -2 generating riboflavin with irradiation.
2010 Vol. 30 (03): 725-728 [Abstract] ( 1672 ) PDF (765 KB)  ( 372 )
729 Model and Analysis of Spectropolarimetric BRDF of Painted Target Based on GA-LM Method
CHEN Chao,ZHAO Yong-qiang,LUO Li,PAN Quan,CHENG Yong-mei,WANG Kai
DOI: 10.3964/j.issn.1000-0593(2010)03-0729-06
Models based on microfacet were used to describe spectropolarimetric BRDF (short for bidirectional reflectance distribution function) with experimental data. And the spectropolarimetric BRDF values of targets were measured with the comparison to the standard whiteboard, which was considered as Lambert and had a uniform reflectance rate up to 98% at arbitrary angle of view. And then the relationships between measured spectropolarimetric BRDF values and the angles of view, as well as wavelengths which were in a range of 400-720 nm were analyzed in details. The initial value needed to be input to the LM optimization method was difficult to get and greatly impacted the results. Therefore, optimization approach which combines genetic algorithm and Levenberg-Marquardt (LM) was utilized aiming to retrieve parameters of nonlinear models, and the initial values were obtained using GA approach. Simulated experiments were used to test the efficiency of the adopted optimization method. And the simulated experiment ensures the optimization method to have a good performance and be able to retrieve the parameters of nonlinear model efficiently. The correctness of the models was validated by real outdoor sampled data. The parameters of DoP model retrieved are the refraction index of measured targets. The refraction index of the same color painted target but with different materials was also obtained. Conclusion has been drawn that the refraction index from these two targets are very near and this slight difference could be understood by the difference in the conditions of paint targets’ surface, not the material of the targets.
2010 Vol. 30 (03): 729-734 [Abstract] ( 1732 ) PDF (1456 KB)  ( 413 )
735 Spectral Characteristics of Ce3+ in Alkali-Alkaline Earth Borate System
WANG Zhi-jun, LI Pan-lai*, GUO Qing-lin, YANG Zhi-ping, CHEN Jin-zhong
DOI: 10.3964/j.issn.1000-0593(2010)03-0735-03
Alkali-alkaline earth borate LiCaBO3∶Ce3+, LiSrBO3∶Ce3+ and LiBaBO3∶Ce3+ were investigated by solid-state method. CaCO3(99.9%), SrCO3(99.9%), BaCO3(99.9%), Li2CO3(99.9%), Na2CO3(99.9%), K2CO3(99.9%), H3BO3(99.9%) and CeO2(99.9%) were used as starting materials, After these individual materials were blended and ground thoroughly in an agate mortar, the homogeneous mixture was heated at 700 ℃ for 2 h in a reduced atmosphere (5∶95(H2/N2)), and these three phosphors were obtained. The excitation and emission spectra of these phosphors were measured by a SHIMADZU RF-540 fluorescence spectrophotometer. The spectral characteristics of Ce3+ in alkali-alkaline earth borate LiCaBO3, LiSrBO3 and LiBaBO3 were investigated. The emission spectra of Ce3+ in these three phosphors all exhibited a dissymmetrical band, and the emission peaks were located at 428, 436 and 440 nm, respectively. The excitation spectra for 428, 436 and 440 nm emission of these three phosphors showed a dissymmetrical band at 364, 369 and 370 nm, respectively. The effects of Li+, Na+ and K+ on the emission intensities of these three phosphors were studied. The results show that the emission intensities of these phosphors were enhanced, and the maximal emission intensity of doping Li+ is higher than that of Na+ and K+.
2010 Vol. 30 (03): 735-737 [Abstract] ( 602 ) PDF (1057 KB)  ( 454 )
738 Research on the Ultraviolet Reflectivity Characteristic of Simulative Targets of Oil Spill on the Ocean
FANG Si-an1,2, HUANG Xiao-xian1, YIN Da-yi1, XU Chong1,2, FENG Xin1, FENG Qi1
DOI: 10.3964/j.issn.1000-0593(2010)03-0738-05
The authors set up an experiment instrument to measure the ultraviolet (UV) characteristic of oil spill simulation targets for the marine oil spill. After selecting appropriate conditions for experiments, the authors tested UV reflective spectrum of four simulation targets for oil spill (gasoline, kerosene, diesel fuel, lubricating oil). The authors calculated the UV absolute spectrum reflectivity of all testing targets from the standard white board as reference, whose UV reflectivity was given. With processing and analyzing the data from experiments, the authors got the reflective characteristics of them in contrast to the reflectivity of water, which was measured in the same conditions. All targets were tested from 320 to 400 nm, and UV reflectivity wave-band between 360 and 380 nm was representative. Testing data were shown as follows: (1) The reflectivity of water was from 5.3% to 5.5%. (2) When the thickness of oil film was 400 μm, the reflectivity of gasoline was from 8.5% to 8.8%, 5.4%-5.8% for kerosene, 8.3%-8.4% for diesel fuel, and 9.4%-9.7% for lubricating oil in the same wave-band between 360 and 380 nm. Correspondingly, the indeterminacy of reflectivity was 0.32%, 0.45%, 0.25%, and 0.33% respectively. (3) Hence the thickness of oil film changed, the rule of the UV reflectivity varied depending on the sort of oil spill. The results show that there were some obvious reflectivity differences among oil films and water, which were mainly determined by the sort and thickness of oil film. This experiment method is also fit for the actual oil spill target, and it will fulfill some theory and experimental foundation for inspecting the marine oil spill by UV remote sensing in the future.
2010 Vol. 30 (03): 738-742 [Abstract] ( 1677 ) PDF (1591 KB)  ( 456 )
743 Endmember Selection Algorithm Based on Linear Least Square Support Vector Machines
WANG Li-guo,DENG Lu-qun,ZHANG Jing
DOI: 10.3964/j.issn.1000-0593(2010)03-0743-05
Endmember (EM) selection is an important prerequisite task for mixed spectral analysis of hyperspectral imagery. In all kinds of EM selection methods, N-FINDR has been a popular one for its full automation and efficient performance. Unfortunately, the implementation of the algorithm needs dimensional reduction in original data, and the algorithm includes innumerable volume calculation. This leads to a low speed of the algorithm and so becomes a limitation to its applications. In the present paper, an improved N-FINDR algorithm was proposed based on linear least square support vector machines (LLSSVM), which is free of dimensional reduction and makes use of distance measure instead of volume evaluation to speed up the algorithm. Additionally, it was also proposed to endow the algorithm with robustness by controlling outliers. Experiments show that the computational load for EM selection using the improved N-FINDR algorithm based on LLSSVM was decreased greatly, and the selection effectiveness and the speed of the proposed algorithm were further improved by outlier removal and the pixel pre-sorting method respectively.
2010 Vol. 30 (03): 743-747 [Abstract] ( 1190 ) PDF (1072 KB)  ( 408 )
748 Study on the Mechanism of Ca2+-Buffering by Sodium Glycodeoxycholate Micelles
CHEN Hu-he,YU Fang-ting,YANG Zhan-lan*,XU Yi-zhuang,WENG Shi-fu,WU Jin-guang
DOI: 10.3964/j.issn.1000-0593(2010)03-0748-05
In the present article, NaGDC was used to study the Ca2+-buffering capability of bile salt micelles. NaGDC is a naturally occurring bile salt which constitutes approximately 10 molar percent of bile salt composition in gallbladder. The authors selected glycine conjugated bile salts NaGDC because it precipitates with Ca2+ ions fast. The Ca2+-buffering property of sodium glycodeoxycholate (NaGDC) micelles was studied by utilizing turbidity titration, quasi-elastic light scattering (QELS), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). When the concentration of NaGDC was above the CMC, the precipitation of Ca2+ ions with NaGDC was buffered. The Ca2+-buffering capability was enhanced when the concentration of NaGDC increased. The possible mechanism of Ca2+-buffering by NaGDC micelles was discussed. When the concentration of NaGDC was below the CMC, the Ca2+ ions reacted with GDC-anions to form the Ca(GDC)2 precipitation. However, at the concentration above the CMC, NaGDC simple micelles were connected by Ca2+-bridge to form larger fibriform micelles via the interaction of carboxyl groups of NaGDC simple micelles with Ca2+ ions. When the ratio of Ca2+ to Na+ was enhanced to the fixed value, NanCam(GDC)n+2m complexes were precipitated by the further addition of Ca2+ ions.
2010 Vol. 30 (03): 748-752 [Abstract] ( 1791 ) PDF (1125 KB)  ( 361 )
753 Spectral Analysis of the Effect of Annealing on CdTe Polycrystalline Film
WANG Wen-wu, ZHENG Jia-gui*, FENG Liang-huan, CAI Ya-ping, LEI Zhi, ZHANG Jing-quan, LI Bing, LI Wei, WU Li-li
DOI: 10.3964/j.issn.1000-0593(2010)03-0753-04
Polycrystalline CdTe thin films were prepared by close-spaced sublimation (CCS) and were annealed in different condition. The thin films were characterized by scanning electron microscopy (SEM),X-ray diffraction (XRD) and X-ray photoelectron spectroscopy(XPS). The content distribution and valence state of all elements after annealing were studied. All results show that the as-deposited CdTe thin films are in a cubic phase and have the preferred orientation in (111) direction. After annealing, the peak intensity of (111), (220), (311) grows and the crystal grains grow up, while the crystal boundary decreases. So the compound probabilities of current carrier decrease, therefore shunt resistance and drain current are improved. From detailed analysis of X-ray photoelectron data, it is proposed that tellurium oxides present and its content reduces with depth increasing and that there are TeCl2O building blocks.
2010 Vol. 30 (03): 753-756 [Abstract] ( 1146 ) PDF (962 KB)  ( 396 )
757 Spectral Characteristics Analysis and Remote Sensing Inversion of Water Quality Parameters in Han Shiqiao Wetland
DU Wei-jing1, 2, LI Shu-min1, LI Hong1*, SUN Dan-feng2, ZHOU Lian-di1
DOI: 10.3964/j.issn.1000-0593(2010)03-0757-05
The research object of the present paper is the water quality of Han Shiqiao wetland water. Water spectrum and quality parameters were measured on the site and in the lab. The authors simulated the relationships between water quality parameters and the best bands or combination, and built the multiple linear regression equation to obtain characteristic spectrum of the key water quality parameters. Besides, several key issues involved in applying ASTER satellite imagery to water quality include atmospheric correction, discussing methods for ASTER data bands analysis, and choosing the best bands and band combination. Results indicated that although the simulation model is not universal, the analysis of spectral characteristics based on ground spectrometer could provide foundations for the choice of remote sensing characteristics bands. The band ratio of water quality parameters simulated from ASTER spectral characteristics moves to relatively long-wave band. Finally, based on the analysis of ASTER remote sensing characteristics bands, the authors built water quality parameters regression model. The models for water quality parameters were recommended, and the accuracies of these models were analyzed. Making use of regression model, we executed spatial distribution map of water quality parameters to achieve wetland water monitoring with remote sensing in terms of variation in space and with time.
2010 Vol. 30 (03): 757-761 [Abstract] ( 1268 ) PDF (1557 KB)  ( 431 )
762 On-Line Coupling of Microcolumn Electrophoresis and UV-Vis Spectrophotometry
LI Lian, HE You-zhao*, GAN Wu-er, WANG Xiao-kui, XIE Hai-yang, GAO Yong
DOI: 10.3964/j.issn.1000-0593(2010)03-0762-05
In the present paper, a laboratory-made high-performance electrophoresis microcolumn unit was prepared for UV-Vis spectrophotometer. X-ray diffraction was used in the preparation of electrophoretic microcolumns. And an analytical technique of microcolumn electrophoresis coupled with UV-Vis spectrophotometry was introduced. Uniform quartz microncrystals were prepared by hydrothermal synthesis. Their crystalline phase and morphology were identified by X-ray diffraction and scanning electron microscope, respectively. The quartz microncrystals were packed into a 2-mm i.d. fused-silica tube to prepare the electrophoretic microcolumn. With 1.5 mmol·L-1 disodium phosphate buffer solution (pH 11.5) containing 25% (φ) methanol and 10% (φ) acetonitrile, tryptophan, phenylalanine and tyrosine were on-line separated on line and detected by microcolumn electrophoresis coupled with UV-Vis spectrophotometry without derivatization. The limits of detection were 0.037, 0.20 and 0.20 μmol·L-1, respectively. The separation efficiency of tryptophan was 4.5×104 plates/m. The sample capacity of the electrophoretic microcolumn achieved 35 μL. It was found that the electrophoretic microcolumn packed with quartz microncrystals was able to limit Joule heat, increase sample capacity and enhance detection sensitivity. The laboratory-made electrophoretic microcolumn could be a high-performance separation unit for conventional UV-Vis spectrophotometer. The on-line coupling of microcolumn electrophoresis and UV-Vis spectrophotometry could separate and determine samples with complicated matrices, reduce zone broadening and enhance separation efficiency, so expand the analytical function of spectrophotometer in the trace analysis of mixed components with overlapped spectra.
2010 Vol. 30 (03): 762-766 [Abstract] ( 2346 ) PDF (1302 KB)  ( 452 )
767 Preparation of Anatase-Type TiO2 Nanoparticals from Ti(SO4)2 Solution under Hydrothermal Conditions and Its Photocatalytic Performance
LI Hai-long1,ZHU Di1, LIU Ran-ran1,CHEN Tao1, TIAN Wen-yu1, SUN Mao1, LI Chun1, ZHAO Yu-liang2, LIU Chun-li1*
DOI: 10.3964/j.issn.1000-0593(2010)03-0767-03
Anatase-type TiO2 fine powders were synthesized under hydrothermal condition. The precursor was obtained via precipitation route using Ti(SO4)2. The characterization of the as-prepared sample was confirmed by TEM, XRD, UV-Vis and low temperature N2 adsorption measurements(BET). The photocatalytic activity was also investigated by the degradation of methyl orange solutions. The particles of the as-synthesized sample with narrow size distribution had an average diameter of about 24 nm. The specific BET surface area of the as-synthesized sample was about 56 m2·g-1,which is similar to the commercial TiO2(P25). The prepared materials showed the similar photocatalytic activity when compared with the performance of commercial TiO2(P25).
2010 Vol. 30 (03): 767-769 [Abstract] ( 292 ) PDF (734 KB)  ( 529 )
770 Spectral Navigation Technology and Its Application in Positioning the Fruits of Fruit Trees
YU Xiao-lei1, 2, ZHAO Zhi-min3*
DOI: 10.3964/j.issn.1000-0593(2010)03-0770-04
An innovative technology of spectral navigation is presented in the present paper. This new method adopts reflectance spectra of fruits, leaves and branches as one of the key navigation parameters and positions the fruits of fruit trees relying on the diversity of spectral characteristics. The research results show that the distinct smoothness as effect is available in the spectrum of leaves of fruit trees. On the other hand, gradual increasing as the trend is an important feature in the spectrum of branches of fruit trees while the spectrum of fruit fluctuates. In addition, the peak diversity of reflectance rate between fruits and leaves of fruit trees is reached at 850 nm of wavelength. So the limit value can be designed at this wavelength in order to distinguish fruits and leaves. The method introduced here can not only quickly distinguish fruits, leaves and branches, but also avoid the effects of surroundings. Compared with the traditional navigation systems based on machine vision, there are still some special and unique features in the field of positioning the fruits of fruit trees using spectral navigation technology.
2010 Vol. 30 (03): 770-773 [Abstract] ( 2128 ) PDF (896 KB)  ( 370 )
774 Application of Least Square Support Vector Machine Based on Particle Swarm Optimization in Quantitative Analysis of Gas Mixture
LI Yu-jun1,2, TANG Xiao-jun1*, LIU Jun-hua1
DOI: 10.3964/j.issn.1000-0593(2010)03-0774-05
According to the difficulty in selecting parameter of least square support vector machine (LS-SVM) when modeling on the gas mixture, and the high computational complexity of the infrared spectrum data, LS-SVM optimized by particle swarm optimization (PSO) algorithm was proposed to build an infrared spectrum quantitative analysis model with feature extracted by principal component analysis (PCA). Firstly, seven feature variables were extracted by PCA as the input of the model from 550 infrared spectrum data of the main absorption apex field, so the computational complexity was reduced. This model aimed at three components of gas mixture, in which methane, ethane and propane gases are included. The concentration of each component ranged from 0.1% to 1%,0.1% to 1% and 0.1% to 1.5% respectively. Each component quantitative analysis model was built by LS-SVM and the parameters were optimized by PSO algorithm, then the regression model would be reconstructed according to the optimal parameters. This method replaced the traditional ergodic optimization. The experiment results show that the time of offline modeling by PSOwas reduced to one fortieth of that of ergodic optimizing. The precision of the model was corresponsive. It can meet the requirement of the measure. PSO algorithm has more superior performance on global optimization and convergence speed. So it is feasible to combine PSO algorithm with LS-SVM to create the infrared spectrum quantitative analysis model. It has definite practice significance and application value.
2010 Vol. 30 (03): 774-778 [Abstract] ( 1753 ) PDF (764 KB)  ( 451 )
779 Application of PCA to Diesel Engine Oil Spectrometric Analysis
LIU Tao, TIAN Hong-xiang*, GUO Wen-yong
DOI: 10.3964/j.issn.1000-0593(2010)03-0779-04
In order to study wear characteristics of a 6-cylinder diesel engine, six different working statuses were arranged by altering the clearance between cylinder and piston. Sixty-nine oil samples were taken from engine at different loads under 6 working statuses and analyzed by Spectroil M Instrument made in US. Principal component analysis (PCA) was applied to analyzing spectrometric data of sixty-nine oil samples and clustering those data according to elements and oil samples separately based on the weighted coefficient and principal component scores. All 21 elements were used in element clustering and only 6 wear-related elements, namely iron, chromium, aluminum, copper, plumbum and silicon, were used in sample clustering. It is shown that PCA effectively clustered oil spectrometric data into three different principal components according to elements. The projection of two different principal components exhibited five types of elements combinations, namely wear elements (Fe, Cr, Cu, Al and Pb), high concentration additives elements (Na,Zn,P,Ca and Mg), low concentration additives elements (Ba and B), base constituent of lubricating oils (C and H) and interferential elements (Ni,Ti,Mo,V,Ag and Sn). Furthermore, PCA clearly clustered oil samples according to different clearance between cylinder and piston in the diesel engine. The study suggests that analyzing oil spectrographic data by PCA could find the sources of different elements,monitor engine conditions and diagnose wear faults.
2010 Vol. 30 (03): 779-782 [Abstract] ( 2296 ) PDF (552 KB)  ( 416 )
783 Experimental Study on High Alloy Steel Sample by Laser-Induced Breakdown Spectroscopy
GUO Qian-jin1, YU Hai-bin1, XIN Yong1, LI Xiao-li2, LI Xian-hong1
DOI: 10.3964/j.issn.1000-0593(2010)03-0783-05
The laser-induced breakdown spectroscopy (LIBS) technique is a fast, non-contact method with no need for any sample preparation, and can be carried out under various atmospheric conditions. These properties make LIBS applicable to process control in metallurgy. In the present paper, a series of high alloy steel GBW01605—01609 samples were determined by laser induced plasma spectroscopy, based on a Nd∶YAG Q-switched solid laser with wavelength 1 064 nm as an excitation source and CCD as detector. Experimental study on the interaction between laser and high alloy steel samples was completed. The effects on LIBS in high alloy steel such as observation distance and laser power density were systematically studied. The time-resolved spectrum of LIBS was also investigated. The optimum experiment conditions for the application of LIBS to the trace analysis in high alloy steel were obtained firstly.
2010 Vol. 30 (03): 783-787 [Abstract] ( 1207 ) PDF (1730 KB)  ( 478 )
788 Nonradioactive Iodine-Labeled Antibodies-Inductively Coupled Plasma Mass Spectrometry for Immunoassay
LI Jing-xi1, WANG Xiao-ru1, 2*, ZHUANG Zhi-xia2, CUI Wei-gang1
DOI: 10.3964/j.issn.1000-0593(2010)03-0788-04
In the present study, the system of nonradioactive iodine-labeled-antibodies linking inductively coupled plasma mass spectrometry for immunoassay was reported. The goat-anti-Escherichia coli and goat anti rabbit were considered as simulant antigen and antibody respectively in order to establish a new method of immunoassay by inductively coupled plasma mass spectrometry which has the advantage of high sensitivity, low detection limit and preferable linearity range. During the experiment, the N-bromosuccinimide, a mild oxidant, was used to oxidize the non-radioactive iodine (127I) that labeled the protein. The method of nonradioactive iodine labeled protein was established and the best labeling condition was explored. The compound of I was purified by Sephadex G50 column chromatography, then the stability and activity were examined. The results showed that the labeling program was simple, reaction time was within two minutes, the labeling yield achieved 63.12% and none of I shed from the compound after 96 hours. The simulant antigen and antibody reacted on polystyrene microtiter plate and the I was detected by ICP-MS, the detection limit of the method was 0.12 mg·L-1, relative standard deviation (n=9) was less than 3% and the linearly dependent coefficient was 0.998 7. This system can also be used in analysis of other protein, nucleic acid and so on.
2010 Vol. 30 (03): 788-791 [Abstract] ( 2119 ) PDF (1050 KB)  ( 480 )
792 Analysis of Properties of Cadmium Adsorption onto Whisker Surface Ion-Imprinted Polymer by Inductively Coupled Plasma Atomic Emission Spectrometry
ZHANG Zu-lei, LI Chun-xiang, YAN Yong-sheng*, GAO Jie, PAN Jian-ming, ZHANG Xiao-jie
DOI: 10.3964/j.issn.1000-0593(2010)03-0792-05
A new type of surface ion-imprinted polymer was synthesized in aqueous media with sodium trititanate whisker in the presence of Cd(Ⅱ), chitosan and γ-glycidoxypropyl trimethoxysilane (KH-560). A batch of adsorption experiments were performed to evaluate its adsorption of Cd(Ⅱ) using inductively coupled plasma atomic emission spectrometry (ICP-AES). The factors affecting adsorption capacity, including pH and sorbent amount, were discussed. The adsorption kinetics and adsorption isothermals were also obtained. The Langmuir isotherm can fit in the experimental equilibrium data. Under the optimum conditions, the value of the adsorption was above 99 %, and the maximum adsorption capacity was 52.34 mg·g-1. In accordance with the parameters distribution coefficient (Kd) and selectivity coefficient (K), the selectivity for Cd(Ⅱ) of the prepared imprinted polymer was estimated. Finally, the adsorption mechanism was discussed and the detection limit of 0.024 μg·mL-1 with the relative standard deviation (RSD) of 1.74% (=1.0 μg·mL-1, n=13) for Cd(Ⅱ) was obtained. Results showed that the surface Cd(Ⅱ)-imprinted polymer was a solid sorbent with high efficiency, low-cost, convenient separation/enrichment for environmental trace Cd(Ⅱ).
2010 Vol. 30 (03): 792-796 [Abstract] ( 2097 ) PDF (917 KB)  ( 422 )
797 Spectral Analysis of Elements in Different Samples of Processed Foeniculum vulgare
ZHANG Fan1, 2, LI Zhen2, HAMULATI Wufuer1, TIAN Shu-ge2
DOI: 10.3964/j.issn.1000-0593(2010)03-0797-04
The compositions and contents of chemical compounds in traditional Chinese medicines would be changed after being processed using different methods, and their pharmacological activity may be influenced. ICP-AES, AAS and AFS were the first methods to be used to scan and analyze macro elements, trace elements and heavy metals in Foeniculum vulgare and its nine different processed samples in the present paper, which were correlated with people’s health and lives. The experiment results showed that the three kinds of analyzing methods could be used to judge the contents and the changing trend of all elements in traditional Chinese medicine quickly and truly. Thirty two elements were found in F. vulgare, and there were noticeable changes in the contents of some elements in processed samples compared with F. vulgare without processing. These results indicated that there is great relevance between changes in the contends of elements with different processing methods, and auxiliary materials can not only change the contents of elements but also play a role in treating ills with effective constituents. Also, it was firstly found that the content of Hg rose greatly in the experiment, and these showed there was notable potential safety hazard when processed Foeniculum vulgare was used. These experiments widen the application of spectrum analyzing methods in safety evaluation of traditional Chinese medicine.
2010 Vol. 30 (03): 797-800 [Abstract] ( 624 ) PDF (447 KB)  ( 397 )
801 Comparison of the Contents of Trace Elements in the Roots of Four Original Danshen (Salvia Miltiorrhiza Bunge)
HE Chun-e, WEI Jian-he*, CHEN Shi-lin,JIN Yue
DOI: 10.3964/j.issn.1000-0593(2010)03-0801-03
The root and rhizome of danshen (salvia miltiorrhiza bunge), one of the earliest and also the most commonly used herbal drugs in practice of traditional Chinese medicines, has been confirmed effective for coronary heart disease, including angina pectoris, coronary artery spasm, myocardial infarction, etc., based on modern investigations. And some trace elements were found related to these diseases. Therefore it was important to research trace elements and their contents in the root for studying pharmic mechanism of danshen. The contents of 22 trace elements, including Ca, Mg, Fe, Zn, V, Mn, Cr, Cu, Rb, Sr, Ba, Pb, B, As, Se, Li, Co, Ni, Mo, Cd, Sn and Hg, in the roots of danshen germplasm, originating from four planting regions and grew in the same place, were analyzed by ICP-MS/ICP-AES. The results showed that the contents of trace elements in the root of Shandong white flower danshen were higher as a whole. And the contents of Ca, Fe, Zn, Mn, Cu, Ba, Li, Co, Ni and Hg in the root of Shandong white flower danshen were the highest among the four kinds of original danshen,in which the contents of Zn, Mn, Cu, Ni and Hg were significantly higher than those in the three kinds of original violet flower danshen. The contents of Rb and Mo in the root of Shanxishangluo violet flower danshen were the smallest and that of Ni was the highest among the three kinds of original violet flower danshen. Compared with the difference between white flower danshen and violet flower danshen, the difference of rest nineteen kinds of trace elements contents among the three kinds of original violet flower danshen was smaller. The difference in the contents of trace elements has an important effect on the research into the contents of officinal ingredients and their curative effect of the roots of four kinds of original danshen germplasm.
2010 Vol. 30 (03): 801-803 [Abstract] ( 1144 ) PDF (414 KB)  ( 394 )
804 Determination of Trace Elements in Lophatherum Gracile Brongn from Different Habitat by Microwave Digestion-Atomic Absorption Spectroscopy
YUAN Ke1, XUE Yue-qin1, GUI Ren-yi1, SUN Su-qin2, YIN Ming-wen3
DOI: 10.3964/j.issn.1000-0593(2010)03-0804-05
A method of microwave digestion technique was proposed to determine the content of Zn,Fe,Cu,Mn,K,Ca,Mg,Ni,Cd,Pb,Cr,Co,Al,Se and As in lophatherum gracile brongn of different habitat by atomic absorption spectroscopy. The RSD of the method was between 1.23% and 3.32%, and the recovery rates obtained by standard addition method were between 95.8 %and 104.2%. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of metal elements in lophatherum gracile brongn. The experimental results also indicated that different areas’ lophantherum gracile brongn had different trace elements content. The content of trace elements K, Mg, Ca, Fe and Mn beneficial to the human body was rich. The content of the heavy metal trace element Pb in lophantherum gracile brongn of Hunan province was slightly high. The content of the heavy metal trace element Cu in lophantherum gracile brongn of Guangdong province and Anhui province is also slightly higher. Beside, the contents of harmful trace heavy metal elements Cd,Cu,Cr,Pb and As in lophatherum gracile brongn of different habitat are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation and National Food Sanitation Standard. These determination results provided the scientific data for further discussing the relationship between the content of trace elements in lophantherum gracile brongn and the medicine efficacy.
2010 Vol. 30 (03): 804-808 [Abstract] ( 2306 ) PDF (683 KB)  ( 427 )
809 Determination of Selenium in Poultry Eggs by Flow Injection-Hydride Generation-Atomic Absorption Spectrometry
DENG Shi-lin,LI Xin-feng,GUO Xiao-lin
DOI: 10.3964/j.issn.1000-0593(2010)03-0809-03
A flow injection- hydride generation-atomic absorption spectrometric method for the determination of selenium in poultry eggs was developed. Various testing conditions and effect factors for the determination of selenium were studied. The authors also discussed the content of selenium in poultry eggs and the application of scientific feed method in improving selenium content in poultry eggs. The detection limit for selenium was 0.25 μg·L-1 under optimum conditions. The linear range for selenium was 0.25-60 μg·L-1. The relative standard deviation was less than 2.5% and the recovery was 95%-108%. This method overcame the problem of severe matrix interferences of graphite furnace atomic absorption spectrometry, in which matrix modifier must be added to eliminate matrix interference by raising ashing temperature. Additionally this method overcame the shortcoming of slow analysis procedure, complex operation and error caused by manual injection in traditional interval hydride generation-atomic absorption spectrometry. It is a simple, rapid, highly sensitive and automatic method and has been applied to the determination of selenium in poultry eggs with satisfactory results.
2010 Vol. 30 (03): 809-811 [Abstract] ( 524 ) PDF (432 KB)  ( 435 )
812 Determination of Metals in Ginkgo Biloba Leaves by Atomic Absorption Spectrometry with Microwave Digestion
JIANG Bo, JIANG Guo-bin, LIU Chang-jian, MA Kun, JIN Li-ming, GAO Jiang-mei
DOI: 10.3964/j.issn.1000-0593(2010)03-0812-04
Microwave digestion technique was used in the decomposition of Ginkgo biloba leaves from six different trees at the same age in the same area. HNO3-H2O2 (5∶1 v/v) was used as microwave digestion agent at a suitable temperature and time. The contents of Ca, Mg, K, Na, Cu, Zn and Zn/Cu were determined by flame atomic absorption spectrometry to study the distribution rule of metallic elements in the trees at the same age and in the same area. The recovery ratio ranged from 95.2% to 104.6%. The results showed that there were certain differences between different trees in the distribution of metallic elements. The contents of calcium were from 39 586 to 48 320 μg·g-1, and those of magnesium from 10 076 to 12 918 μg·g-1, of potassium from 2 004 to 5 240 μg·g-1, of sodium from 9.05 to 35.30 μg·g-1, and of copper from 1.50 to 3.05 μg·g-1, while Zn/Cu values were from 2.68 to 5.93 in the leaves of 6 different trees in the same growing area. Therefore there were abounding calcium, magnesium and potassium, while the content of sodium and Zn/Cu values were lower, and the metal contents were different in the leaves. The experimental results provided useful bases for studying the distribution rule of metallic elements in Ginkgo biloba leaves, the relationship between the contents of calcium, magnesium, potassium and sodium and the Zn/Cu value in ginkgo biloba leaves and the treatment for cardio-cerebral vascular disease.
2010 Vol. 30 (03): 812-815 [Abstract] ( 432 ) PDF (502 KB)  ( 427 )
816 Determination of Serum Copper and Zinc in Different Chemical Forms by Graphite Furnace Atomic Absorption Spectrometry with Ethanol-EDTA Precipitation Method
ZHANG Yuan, LIN Zhe-xuan,LI Hui,PENG Lin, LUO Hong-jun,LI Wei-qiu,LUO Wen-hong*
DOI: 10.3964/j.issn.1000-0593(2010)03-0816-04
A simple and reliable method was developed for the determination of serum copper and zinc in different chemical forms by graphite furnace atomic absorption spectrometry (GFAAS) with ethanol-EDTA precipitation. The serum and ethanol were mixed with volume ratio 1∶2. The mixture was incubated at 70 ℃ and ultra-centrifuged to precipitate proteins. Zinc and copper can be released from albumin after EDTA treating. Thus, macroglobulin-zinc, ceruloplasmin-copper, and albumin-bound zinc or copper could be determined by two proposed precipitation steps. The determination limit of copper (3σ) was 1.2 μg·L-1 and the recovery was 92.3%-104%, while the determination limit of zinc (3σ) was 0.098 μg·L-1, and the recovery was 90%-107%. This two-step precipitation method can be used to determine serum zinc and copper in various chemical forms in tumor, Wilson patients and heathy human.
2010 Vol. 30 (03): 816-819 [Abstract] ( 1258 ) PDF (706 KB)  ( 430 )
820 Comparative Analysis of Endogenous Hormones between Two Species of Ammopiptanthus Seedlings around Germination and under Pb2+ Stress
ZHENG Chun-xia, CHEN Bo-lang, JIA Hong-tao, SHENG Jian-dong*, PAN Xin-yan
DOI: 10.3964/j.issn.1000-0593(2010)03-0820-05
The changes in three endogenous hormones, phytohormones gibberrelic acid (GA3), indoles-3-acid (IAA) and abscisic acid (ABA), were studied around germination and under tress of different density of Pb2+ between two species of Ammopiptanathus. It was found that (1) around germination, in Xinjiang Ammopiptanthus the rate IAA decreased 77.80%, and the rate of ABA decreased 98.90%; and in Mongolia Ammopiptanthus the rate of IAA decreased 75.80%, the rate of ABA decreased 66.20%, and the GA3 contents in both had no big change. (2) With the increase in Pb2+ concentration (20-1 500 mg·L-1), the IAA decreased significantly; and only under the high density (more than 1 000 mg·L-1) of Pb2+, the GA3 was affected by it; the ABA did not change regularly. So the three endogenous hormone levels of Mongolia Ammopiptanthus were higher than those of Xinjiang Ammopiptanthus.(3)the distributions of Pb2+ in Ammopiptanthus seedlings are the root>stems>leaves. (4) the stress of high concentration of Pb2+ damages irreversibly the leaf cells of Ammopiptanthus. This study can provide the basis of reference data for further research on the growth characteristics, resilience and the mechanism of specific broad-leaved evergreen shrubs-Ammopiptanthus in desertification area.
2010 Vol. 30 (03): 820-824 [Abstract] ( 1744 ) PDF (1311 KB)  ( 368 )
825 EDXRF Analysis of Soil Heavy Metals on Lead-Zinc Orefield
CHU Bin-bin1,2, LUO Li-qiang1*
DOI: 10.3964/j.issn.1000-0593(2010)03-0825-04
Due to the impact of lead-zinc mining and smelting, the soil of lead-zinc orefield and nearby areas has been widely polluted. Moreover, the concentration of lead and zinc was high, and their concentration range was wide. Furthermore, the impact of overlapping interference between low concentration As and high Pb was serious, and the lack of soil standards of lead and zinc was also a problem. According to these problems, the present work studied an effective solution to setting up the EDXRF analysis of Pb, As, Cd, Cu and Zn of soil on lead-zinc orefield. The measurable concentration of Pb was 4.4-23 600 μg·g-1, and that of Zn was 7.0-39 400 μg·g-1. The detection limit was 1.1 μg·g-1 for Pb and 0.9 μg·g-1 for Zn. The average relative error was 7.6% for Pb and 6.2% for Zn.
2010 Vol. 30 (03): 825-828 [Abstract] ( 1220 ) PDF (480 KB)  ( 447 )
829 Rapid Determination of Major and Trace Elements in the Salt Lake Clay Minerals by X-Ray Fluorescence Spectrometry
WANG Xiao-huan1, 2, MENG Qing-fen1, DONG Ya-ping1*, CHEN Mei-da1, 2,LI Wu1
DOI: 10.3964/j.issn.1000-0593(2010)03-0829-05
A rapid multi-element analysis method for clay mineral samples was described. This method utilized a polarized wavelength dispersive X-ray fluorescence spectrometer—Axios PW4400,which had a maximum tube power of 4 000 watts. The method was developed for the determination of As, Mn, Co, Cu, Cr, Dy, Ga, Mo, P, Pb, Rb, S, Sr, Ni, ,Cs, Ta, Th, Ti, U, V, Y, Zn, Zr, MgO, K2O, Na2O, CaO, Fe2O3, Al2O3, SiO2 and so on. Thirty elements in clay mineral species were measured by X-ray fluorescence spectrometry with pressed powder pellets. Spectral interferences, in particular the indirect interferences of each element, were studied. A method to distinguish the interference between each other periodic elements in element periodic table was put forward. The measuring conditions and existence were mainly investigated,and the selected background position as well as corrected spectral overlap for the trace elements were also discussed. It was found that the indirect spectral overlap line was the same important as direct spectral overlap line. Due to inducing the effect of indirect spectral overlap,some elements jlike Bi,Sn,W which do not need analysis were also added to the elements channel. The relative standard deviation (RSD) was in the range of 0.01% to 5.45% except three elements Mo, Cs and Ta. The detection limits, precisions and accuracies for most elements using this method can meet the requirements of sample analysis in clay mineral species.
2010 Vol. 30 (03): 829-833 [Abstract] ( 1197 ) PDF (415 KB)  ( 417 )
834 Effects of Dynamic High-Pressure Microfluidization on the Structure of Waxy Rice Starch
TU Zong-cai, ZHU Xiu-mei, CHEN Gang, WANG Hui, ZHANG Bo, HUANG Xiao-qin, LI Zhi
DOI: 10.3964/j.issn.1000-0593(2010)03-0834-04
The effects of dynamic ultra high-pressure microfluidization on the structure of waxy rice starch solutions (6%) were analyzed using SEM, UV-Vis spectra, polarized light microscopy, and X-ray diffraction spectra. The results showed that: SEM graphs demonstrated that the crystal structure of waxy rice starch under different pressure treatment was destroyed with different degrees and impacted into flake up to 160 MPa; from the ultraviolet-visible spectrum we know the reduction in the blue iodine value and the decrease in the amylopectin content, which illustrated that the structure of waxy rice starch was fractured; polarized microscopic images showed that the polarization crosses of starch molecules became misty with the pressure increasing, and most of starch molecules lost polarization cross when the pressure reached 160 MPa; X-ray diffraction spectra indicated that relative crystallinity began to decline at 120 MPa with pressure treatment, and the decreased amplitude was slightly lower.
2010 Vol. 30 (03): 834-837 [Abstract] ( 1180 ) PDF (1145 KB)  ( 462 )
838 Spectral Classification Based on Bayes Decision
LIU Rong1, JIN Hong-mei2, DUAN Fu-qing3*
DOI: 10.3964/j.issn.1000-0593(2010)03-0838-04
The rapid development of astronomical observation has led to many large sky surveys such as SDSS (Sloan digital sky survey) and LAMOST (large sky area multi-object spectroscopic telescope). Since these surveys have produced very large numbers of spectra, automated spectral analysis becomes desirable and necessary. The present paper studies the spectral classification method based on Bayes decision theory, which divides spectra into three types: star, galaxy and quasar. Firstly, principal component analysis (PCA) is used in feature extraction, and spectra are projected into the 3D PCA feature space; secondly, the class conditional probability density functions are estimated using the non-parametric density estimation technique, Parzen window approach; finally, the minimum error Bayes decision rule is used for classification. In Parzen window approach, the kernel width affects the density estimation, and then affects the classification effect. Extensive experiments have been performed to analyze the relationship between the kernel widths and the correct classification rates. The authors found that the correct rate increases with the kernel width being close to some threshold, while it decreases with the kernel width being less than this threshold.
2010 Vol. 30 (03): 838-841 [Abstract] ( 2158 ) PDF (594 KB)  ( 408 )
842 Study of LED Chip Spectrum Acquisition System Based on CPLD
SHI Wei1, 5, ZHOU Da-bing2, DONG Zhan-min3, SUN Hong-san4, XI An-min5
DOI: 10.3964/j.issn.1000-0593(2010)03-0842-04
The light emitting diode (LED) chip spectrum inspection is a key technology in LED chip scaled manufacturing. According to the principle of spectrum inspection and aiming at the demand of applications of LED chip spectrum inspection, the present paper studies the spectrum acquisition system based on complex programmable logic device (CPLD). The CPLD, the main chip, provides the working timing signal to the linear charge coupled device (CCD) and controls the signal modulating, conversion and storage, and transmission of sampling rate and data in transfer module. The system adopts raster monochromator as prismatic parts of apparatus and linear CCD as photoelectricity conversion parts to inspect the opposite spectrum energy distributing curve, and meanwhile calculate the spectrum parameter of LED chip photics characteristic. Based on the CPLD , the LED chip spectrum acquisition system with the virtues of simplicity and celerity satisfies the precision request of LED chip spectrum inspection.
2010 Vol. 30 (03): 842-845 [Abstract] ( 1535 ) PDF (963 KB)  ( 358 )
846 A Novel Near-Infrared Spectra Detection System Based on MEMS Grating Light Modulators
WEI Wei,HUANG Shang-lian,CHEN Wei-min,WANG Ning,ZHANG Jie,ZHU Yong
DOI: 10.3964/j.issn.1000-0593(2010)03-0846-05
A novel near-infrared spectrum detection system based on grating light modulators is proposed in the present paper. A new spectrum detection method that combines MEMS grating light modulators with a single near infrared detector is applied in the system, which can avoid using costly near infrared detector array. Firstly, the optical structure of the spectra detection system was designed. Secondly, the spectra detection principle of this system was addressed in detail that with a series of voltages actuated on the grating light modulators array, the optical energy of each wavelength is reflected onto the single near-infrared detector by corresponding grating light modulator pixel orderly and the transmission spectra can be acquired after a scanning period. Finally, the grating light modulators array device was fabricated by surface micromachining processing and a near-infrared spectra detection system was set up to test the key parameters such as resolving power, wavelength accuracy, system stability and response characteristics of grating light modulators. The experimental results illuminated that the spectrum range of this spectra detection system is from 1 320 to 1 400 nm, the resolving power is below 10nm, the wavelength accuracy is within 1nm,the stability of the system is below 0.5% and the response frequency is 5 kHz. The results of theory analysis and experiments demonstrated the feasibility of the spectra detection system. It could give theoretical and experimental guidance to the design and fabrication of miniature near-infrared spectrometer based on grating light modulators.
2010 Vol. 30 (03): 846-850 [Abstract] ( 1695 ) PDF (1404 KB)  ( 464 )
851 Simultaneous Discriminating Measurement of Temperature and Strain Based on a Long Period Grating’s Spectrum
HU Xing-liu1,2, LIANG Da-kai1*, LU Guan1, ZENG Jie1
DOI: 10.3964/j.issn.1000-0593(2010)03-0851-04
The new scheme of using a long period grating for simultaneous discriminating measurement of temperature and strain is proposed. The scheme is based on the long period grating’s spectrum characteristics. The spectrum is composed of multiple and different loss peak. The resonant wavelength of the first and fourth-order loss peak with different temperature and strain sensitivity was selected in this experiment. The wavelength shift resulting from parameter variation can be obtained by observing its corresponding spectrum. The temperature was acquired by a study on the temperature characteristic of a LPG. The strain sensitivity was obtained by the research on the strain characteristic of a LPG. The standard matrix equation was set up and solved according to the corresponding parameter. The authors know by calculating the standard matrix equation that the cross-sensitivity has little influence on the measurement of the parameter. As the effect of cross-sensitivity is lower than the resolution of the LPG in this case, we can eliminate the deviation due to the cross-sensitive by appropriate compensation. The errors of temperature and strain were calculated to be ±0.92 ℃ and ±22 με respectively. The cross-sensitivity between temperature and strain was decreased and the measuring precision of the system was improved by using this scheme in which a single long period grating was used to test two measurands. By comparison between the applied and the calculated temperature and strain of a LPG, the experiment results showed that the methods are feasible.The experimental system is small and the cost is relatively low. The experimental device is simple and practical and has good application prospect.
2010 Vol. 30 (03): 851-854 [Abstract] ( 2149 ) PDF (999 KB)  ( 405 )
855 Research on Spatially Modulated Fourier Transform Imaging Spectrometer Data Processing Method
HUANG Min1,2, XIANGLI Bin1,3*, Lü Qun-bo1,ZHOU Jin-song1,2, JING Juan-juan1,2, CUI Yan1,2
DOI: 10.3964/j.issn.1000-0593(2010)03-0855-04
Fourier transform imaging spectrometer is a new technic, and has been developed very rapidly in nearly ten years. The data catched by Fourier transform imaging spectrometer is indirect data, can not be used by user, and need to be processed by various approaches, including data pretreatment, apodization, phase correction, FFT, and spectral radicalization calibration. No paper so far has been found roundly to introduce this method. In the present paper, the author will give an effective method to process the interfering data to spectral data, and with this method we can obtain good result.
2010 Vol. 30 (03): 855-858 [Abstract] ( 1217 ) PDF (891 KB)  ( 431 )
859 Electro-Optic Modulation Based Study on Spectrum Resolution of Static Fourier Transform Spectrometer
YANG Zheng-min, LIU Zhi-chao*, LI Xiao, CHEN Yuan-yuan, WANG Zhi-bin, TIAN Er-ming
DOI: 10.3964/j.issn.1000-0593(2010)03-0859-04
In the static interferometer system, the variable refractive crystal LiNbO3 with electro-optic modulation was used in static Fourier transform interferometer, where both sides load phase opposite modulation signal separately so to raise the spectrum resolution in the same size of the instrument by the increment of optical path difference. According to the derivation of the optical path difference function with refraction modulation, the maximum optical path difference was calculated and the spectrum resolution was analyzed to be 16.7 times previous one when the refraction modulation was 0.030 in the same size of interferometer. The simulation result indicated that the refractive modulation would be reduced when the wavelength increased, and the value of optical path difference will be bigger when the x′ increased. In actual detection process, because spectral region 500-1 100 nm is relatively narrow, the spectrum distortion by the wavelength change is not big and may be compensated through the demarcation. This method can increase the optical path difference without mechanical scanning, and possibly raises spectrum resolution of the static interferometer.
2010 Vol. 30 (03): 859-862 [Abstract] ( 1722 ) PDF (985 KB)  ( 389 )