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2008 Vol. 28, No. 11
Published: 2008-11-26

 
       光谱学与光谱分析
2465 The Spectra of a Laser-Produced Plasma Source with CO2,O2 and CF4 Liquid Aerosol Spray Target
NI Qi-liang, CHEN Bo
DOI: 10.3964/j.issn.1000-0593(2008)11-2465-04
A laser-produced plasma (LPP) source with liquid aerosol spray target and nanosecond laser was developed, based on both soft X-ray radiation metrology and extreme ultraviolet projection lithography (EUVL). The LPP source is composed of a stainless steel solenoid valve whose temperature can be continuously controlled, a Nd∶YAG laser with pulse width, working wavelength and pulse energy being 7 ns, 1.064 μm and 1J respectively, and a pulse generator which can synchronously control the valve and the laser. A standard General Valve Corporation series 99 stainless steel solenoid valve with copper gasket seals and a Kel-F poppet are used in order to minimize leakage and poppet deformation during high-pressure cryogenic operation. A close fitting copper cooling jacket surrounds the valve body. The jacket clamps a copper coolant carrying tube 3 mm in diameter, which is fed by an automatically pressurized liquid nitrogen-filled dewar. The valve temperature can be controlled between 77 and 473 K. For sufficiently high backing pressure and low temperature, the valve reservoir gas can undergo a gas-to-liquid phase transition. Upon valve pulsing, the liquid is ejected into a vacuum and breaks up into droplets, which is called liquid aerosol spray target. For the above-mentioned LPP source, firstly, by the use of Cowan program on the basis of non-relativistic quantum mechanics, the authors computed the radiative transition wavelengths and probabilities in soft X-ray region for O4+, O5+, O6+, O7+, F5+, F6+ and F7+ ions which were correspondingly produced from the interaction of the 1011-1012 W·cm-2 power laser with liquid O2,CO2 and CF4 aerosol spray targets. Secondly, the authors measured the spectra of liquid O2,CO2 and CF4 aerosol spray target LPP sources in the 6-20 nm band for the 8×1011 W·cm-2 laser irradiance. The measured results were compared with the Cowan calculated results ones, and the radiative transition wavelength and probability for the measured spectral lines were obtained.
2008 Vol. 28 (11): 2465-2468 [Abstract] ( 2400 ) PDF (765 KB)  ( 473 )
2469 Incoherent Broadband Cavity Enhanced Absorption Spectroscopy Based on LED
WU Tao1,ZHAO Wei-xiong1,LI Jin-song1,ZHANG Wei-jun1,CHEN Wei-dong2,GAO Xiao-ming1
DOI: 10.3964/j.issn.1000-0593(2008)11-2469-04
High sensitivity incoherent broadband cavity enhanced absorption spectroscopy based on high power LED was developed. The detection sensitivity was demonstrated by measuring the absorption of NO2 over the wavelength range of 472.3-479.3 nm. A broadband incoherent light (emitting from high power LED peaked at 457 nm) was coupled to a 92.5 cm long high finesse optical cavity consisting of two 30 mm diameter plano-concave mirrors (1.0 m radius of curvature) with reflectivity of ~0.997 (provided by manufacturer). The light leaked out of the cavity was collected by a compact CCD spectrometer (HR 2000). The cavity mirror reflectivity over the wavelength range of 472.3-479.3 nm was determined from the absorption of O2-O2 collisional pair. A series of concentrations of NO2 samples at high dilution were retrieved using differential spectral fitting techniques, with statistical uncertainties approaching 3.1 ppb(ng·mL-1) for a 80 s averaging period.
2008 Vol. 28 (11): 2469-2472 [Abstract] ( 686 ) PDF (1029 KB)  ( 574 )
2473 The Effect of Resolution on the Measurement of Carbon Bisulfide by DOAS
PENG Fu-min1,2, LIN Yi-hui1,XIE Pin-hua1*, WANG Jun-de2,ZHANG Ying-hua1,QIN Min1,LIU Wen-qing1, LI Hai-yang2
DOI: 10.3964/j.issn.1000-0593(2008)11-2473-05
Featuring excellent response characteristics and detection sensitivity and with much lower operational cost, differential optical absorption spectroscopy (DOAS) can be a powerful tool to trace the concentration variation of carbon bisulfide (CS2), a kind of poisonous gas with bad smell. In the DOAS measurement, the accuracy of the carbon bisulfide results is determined by the selected spectral resolution. The present paper focuses on the effect of resolution on the detected characteristic absorption structure of CS2 and the variation in differential cross section of CS2 with the change in resolution, from which the effect of resolution on the detection limit of CS2 is deduced. In the end, the functional dependence of the ratio of signal to noise (S/N) on the resolution is reduced by studying the relationship between light intensity and resolution. And the optimized resolution is determined as 0.41-0.50 nm (FWHM) with the lowest S/N. The optimized resolution range can yield high sensitivity, good selectivity and a reasonable time resolution for the accurate qualitative and quantitative analysis of CS2 (the results of five different concentration cells show linear correlation with r=0.999 9 and all the relative standard deviations are less than 0.3% with n=10). In the end, the long time, real time and continuous monitoring of CS2 was carried out in the Fengtai District of Beijing, and a good result was obtained.
2008 Vol. 28 (11): 2473-2477 [Abstract] ( 2246 ) PDF (1303 KB)  ( 491 )
2478 Monitoring the Change in CO Concentration in Combustion with Tunable Diode Laser Absorption Spectroscopy
XIA Hui, LIU Wen-qing, ZHANG Yu-jun, KAN Rui-feng, CHEN Dong, CUI Yi-ben, HE Ying, CHEN Jiu-ying, WANG Min, WANG Tie-dong
DOI: 10.3964/j.issn.1000-0593(2008)11-2478-04
In the present paper, the technology of tunable diode laser absorption spectroscopy (TDLAS) in conjunction with the open path multi-pass Herriot cell and the new-style detection method of auto-balanced detection combined with wavelength modulation technology were used, and the concentration of CO produced in combustion of alcohol blowtorch was measured. It was found in the measured result that the change in CO concentration in the flame of alcohol blowtorch presented a stated periodicity in the process of combustion and the average concentration of CO was calculated to be 49.4 (10-6 ratio by volume). The experiment is showed that with the conjunction of auto-balanced detection and the second harmonics detection method, adopting the open path multi-pass Herrriot cell to detect the concentration of CO in the combustion of alcohol blowtorch is accurate and contents the detection requirement. It was proved that the system made for measuring the concentration of CO in the flame of alcohol blowtorch in combustion establishes foundation well for developing on-line combustion monitoring based on TDLAS.
2008 Vol. 28 (11): 2478-2481 [Abstract] ( 518 ) PDF (965 KB)  ( 557 )
2482 Spectral Curve Shape Feature-Based Hyperspectral Remote Sensing Image Retrieval
LI Fei1,2,ZHOU Cheng-hu1*,CHEN Rong-guo1
DOI: 10.3964/j.issn.1000-0593(2008)11-2482-05
With the rapid development of technology of sensors and data transmission, using all kinds of airplane sensors and satellite sensors,the authors can get different voluminous remote sensing image data of earth. Those voluminous remote sensing image data bring problems of data storage and management. It is becoming increasingly necessary to retrieve some information the authors need from those voluminous image data. Image retrieval was proposed by CHANG firstly in 1980 and can be regarded as expansion of traditional information retrieval. Oriented to the demands of efficient retrieval for voluminous remote sensing image, and considering that there are many bands in hyperspectral remote sensing image, the authors first analyzed image distance function and similarity measure in image retrieval. The most crucial issues in retrieval are spectral features extraction and similarity measure. In the present paper, the authors used classical Douglas-Peucker algorithm(hereinafter referred to DP algorithm) for curve simplification to extract shape features of spectral curve, in order to speed up hyperspectral remote sensing image retrieval. And the authors proposed a new method of spectral curve and remote sensing image retrieval, called Douglas-Peucker Spectral Retrieval algorithm (hereinafter referred to DPSR algorithm). Spectral shape features were used in image retrieval. DPSR used features of spectral curve, reduced the computation amount, realized match and retrieval efficiently, and is suitable for spectral curve retrieval in hyperspectral remote sensing image. The authors selected four ground features(grass, apple garden, grape garden and pond) in OMISI hyperspectral remote sensing image to compute similarity measure results, in order to test the effect of DPSR algorithm. Compared with traditional analysis method such as spectral angle match (SAM) and spectral information divergence(SID), DPSR can maintain high precision of results with less amount of computation, and then a new efficient image spectral retrieval method is provided. Besides some additional work the authors need to do in the future, for example, the relationship between threshold, retrieval precision rate and retrieval speed.
2008 Vol. 28 (11): 2482-2486 [Abstract] ( 439 ) PDF (581 KB)  ( 573 )
2487 Experimental Investigation of Mechanisms of Forming RbH by Irradiating a Rb+H2 Mixture with Laser Light
SHEN Xiao-yan1,LIU Jing2,DAI Kang2,SHEN Yi-fan2*
DOI: 10.3964/j.issn.1000-0593(2008)11-2487-04
The radiation of a laser photoexcited Rb atoms from the ground state to the 5P3/2 level in a mixture of Rb vapor and hydrogen. The energy-pooling collision 5P3/2+5P3/2→5S1/2+5D producted 5D state. The Rb(5P3/2)density and spatial distribution were mapped by monitoring the absorption of a counter-propagating laser beam, tuned to the 5P3/2→7S1/2 transition, which could be translated parallel to the pump beam. In the presence of radiation trapping, the spontaneous radiation rate is multiplied by the transmission factor T5P3/2→5S1/2, which describes the average probability that photons emitted within the fluorescence detection region can pass through the optically thick vapor without being absorbed. The T5P3/2→5S1/2 is related to the frequency dependent absorption cross section and the density and spatial distribution of atoms in the level of the transition. The effective radiative rates of the Rb D2 line as a function of the H2 pressure were obtained. These quantities were combined with the measured excited atom density and fluorescence ratio to yield absolute energy-pooling rate coefficient. The quenching collision Rb(5P3/2)+H2(v=0)→Rb(5S)+H2(v=2) producted state H2(v=2). This process is at least 16 times faster than the Rb(5P3/2) radiative decay rate. The reverse process of this process is relatively unlikely due to their large translational energy defect. The cross section for the process H2(v=2)+H2(v=0)→H2(v=1)+H2(v=0)+3 920.2 cm-1 is 7.7×10-19 cm2. Hence the relaxation rate of this vibrational level is relatively slow and the nuclear spin statistics is conserved. The H2(v=2) density was determined by using the cross section for Rb(5P3/2)-H2 quenching. RbH was fromed by the Rb(5D)+H2 and Rb(5P3/2)+H2(v=2) reactions and observed by laser absorption. The ratio of 5D→5P3/2 to 5P3/2→5S1/2 fluorescence was measured as a function of the H2 density. The absorption of the laser beam tuned to the X1Σ+A1Σ+ line of RbH was also measured as a function of the H2 density. From these measurements we obtained the cross section of 4.02×10-17 cm2 for the process Rb(5D)+H2→RbH+H. The cross section for Rb(5P3/2)+H2(v=2) →RbH+H is 1.00×10-18 cm2. This experiment showed that under our experimental conditions, RbH molecules are not created by a direct interaction of Rb(5P) with H2 but through a two-step reaction.
2008 Vol. 28 (11): 2487-2490 [Abstract] ( 377 ) PDF (616 KB)  ( 532 )
2491 Study on Energy Transfer in Argon/Air in Dielectric Barrier Discharge by Optical Emission Spectra
DONG Li-fang, QI Yu-yan, ZHAO Zeng-chao,LI Yong-hui, LI Xue-chen
DOI: 10.3964/j.issn.1000-0593(2008)11-2491-03
The energy transfer in dielectric barrier discharge in argon/air mixture in a device with water electrodes was investigated by comparing the optical emission spectra in pure argon, argon/air mixture and air. It was observed that the intensities of argon spectral lines in argon/air discharge are all lower than that in argon discharge, which indicates that the nitrogen in air has a quenching effect on the argon excited states. It was found that the decreasing rate of intensity of spectral lines with increasing the air concentration is different. The intensity of ArI 763.51 nm decreases fastest, the ArⅠ 772.42 nm and ArⅠ 696.54 nm take second place, while the ArI 750.39 nm decreases slowest. Comparing the excitation energy of argon excited state with the excitation energy of nitrogen molecule, the authors found that the smaller the difference between the excitation energy of argon excited state and the excitation energy of nitrogen molecule, the faster the spectral line decreases, implying the stronger the energy transfer. In addition, the additional argon in air makes the emission intensities of nitrogen band of second positive system and band of first negative system increase, which indicates that the excitation of nitrogen is enhanced by the energy transfer from argon through Penning excitation involving argon metastable states. In other words, the component and ratio of gas in the gas mixture influence the optical characteristic and energy transfer peculiarity in the mixed gas discharge. The optical emission spectra measurement as a useful plasma diagnostic tool has been successfully used in the study of energy transfer in the mixed gas discharge, and the results provide a reasonable reference for the underlying industrial applications of different species discharge.
2008 Vol. 28 (11): 2491-2493 [Abstract] ( 3839 ) PDF (755 KB)  ( 594 )
2494 Influence of Annealing and Sputtering Ambience on the Photoluminescence of Silicon Nitride Thin Films
JIA Xiao-yun1,XU Zheng1*, ZHAO Su-ling1,ZHANG Fu-jun1,ZHAO De-wei1,TANG Yu2,LI Yuan1,ZHOU Chun-lan2,WANG Wen-jing2
DOI: 10.3964/j.issn.1000-0593(2008)11-2494-04
The radio frequency (r.f.) magnetron sputtering was used for preparing silicon-rich silicon nitride films deposited on polished Si substrates at 80 ℃ substrate temperature. The high-purity Ar was used as a sputtering gas and the high-purity N2 as a reactive gas. The silicon nitride films with different Si-rich degrees were obtained by changing the flow ratio of Ar/N2,and subsequently the samples were annealed at a high temperature in pure N2 ambience. The influence of annealing on the properties of films was investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and photoluminescence (PL). The appearance of Si—N bonds can be confirmed by the XPS, from which the ratio of Si/N can be rough estimated. Therefore, the XPS reveals that the sample before annealing has a high content of Si which is the premise to come into being nanometer Si. However, the PL peak of the films before annealing in the visible light region was not observed obviously. The XRD results indicate that the presence of Si clusters buried in the films after annealing was confirmed by two novel diffraction peaks, which are related to nanometer Si. As the flow ratio of Ar/N2 decreased, the emission intensity of PL peak in the visible light region was enhanced, accompanied with a blue-shift of emission peak. According to the quantum confinement effect, the blue-shift of PL peak should be attributed to the enlarged band gap of Si clusters in the sample, and the increased intensity of the PL peak turns out to be due to the size of nanometer Si. The two important factors of annealing treatment and flow ratio of Ar/N2 were studied, which have an intimate connection with emitting mechanism in PL. The blue-shift of PL peak caused by nanometer Si embodied in the silicon nitride thin films depends on the sputtering condition, such as flow ratio, deposition temperature and sputtering pressure.
2008 Vol. 28 (11): 2494-2497 [Abstract] ( 2000 ) PDF (632 KB)  ( 516 )
2498 Effect of Host MCM-41 on the Luminescence Properties of Tb(aspirin)3phen
PENG Chun-jia,WEI Chang-ping*,ZHU Cui-mei
DOI: 10.3964/j.issn.1000-0593(2008)11-2498-05
Highly ordered mesoporous material MCM-41A(after calcination) and MCM-41B(before calcination) were synthesized in ethylenediamine(EDA) medium at room temperature, and the rare earth complexes Tb(aspirin)3phen which had been heat treated as an active optical guest was incorporated into the one-dimensional channels of MCM-41A(B). The photoluminescence properties of the organic/inorganic composites Tb(aspirin)3phen-MCM-41A(B) were investigated based on the analyses of excitation and emission spectra to provide information about the relationship between the organic host and the inorganic optical guest. The results from the characterization of PL show that the wide excitation band in the range of 240-375 nm of Tb(aspirin)3phen is assigned to the carbonyl group nπ* transition absorption, benzene ring ππ* transition absorption of aspirin, and phenanthrene absorption of phen. As no excitation band appears in ultraviolet ranges, the characteristic emission peaks of Tb3+ in the emission spectra are related to antenna effect. Relative to the excitation band of Tb(aspirin)3phen, the excitation band of Tb(aspirin)3phen-MCM-41B and Tb(aspirin)3phen/MCM-41A splits obviously, and only one narrow excitation peak at 353 nm appears in the excitation spectrum of Tb(aspirin)3phen-MCM-41A. The excitation bands of Tb(aspirin)3phen-MCM-41B and Tb(aspirin)3phen/MCM-41A at short wavelength weakens and disappears gradually, while excitation peaks at long wavelengths is enhanced gradually, and the IL/ILn ratio I, where IL is the emission intensity at 405 nm under 335 nm excitation, and ILn is the emission intensity at 544 nm under 335 nm excitation, also decreases correspondingly. It is suggested that the triplet states and single states of aspirin and phen reduce with different degree after Tb(aspirin)3phen is banded with MCM-41 framework, and the effect of silicon framework on the states of phen is more than that of aspirin. The degree of the effect on the states of organic ligands is in the order of: MCM-41B external surface>MCM-41A external surface>MCM-41A inside surface. In addition, the ratio I also could indicates the degree of the effect of MCM-41 surface lattice field on the ligand energy level and the content of Tb(aspirin)3phen on the MCM-41 surface.
2008 Vol. 28 (11): 2498-2502 [Abstract] ( 2183 ) PDF (979 KB)  ( 468 )
2503 Effect of N+(N=Li, Na, K) on the Spectra of M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ Luminescent Phosphor
LI Pan-lai1,WANG Zhi-jun1*,GAO Hui-ying2,YANG Zhi-ping1
DOI: 10.3964/j.issn.1000-0593(2008)11-2503-04
The M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ red phosphor was synthesized by firing twice at 800 and 1 050 ℃ each for 4 h and 4 h in air, respectively. Y2O3(99.9%), Eu2O3(99.9%), H3BO3(99.9%), CaCO3(99.9%), SrCO3(99.9%), BaCO3(99.9%), Li2CO3(99.9%), Na2CO3(99.9%) and K2CO3(99.9%) were used as starting materials, and the doping Eu3+ concentration was 3 mol%. The excitation spectrum was measured by a SHIMADZU RF-540 ultraviolet spectrophotometer. The emission spectrum was measured by a SPEX1404 spectrophotometer. All the luminescence characteristics of the phosphors were investigated at room temperature. The emission spectrum of M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ phosphor exhibited a 613 nm red emission corresponding to the electric dipole 5D0-7F2 transition of Eu3+ under 365 nm excitation. The excitation spectrum for 613 nm indicates that the phosphor can be effectively excited by ultraviolet (UV) (254, 365 and 400 nm) and blue (470 nm) light. The effect of Li+,Na+ and K+ on the excitation and emission spectra of M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ phosphor was studied. The results show that the location of the excitation and emission spectrum of M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ phosphor was not influenced by Li+,Na+ and K+. However, the excitation and emission spectrum intensities were greatly influenced by Li+,Na+ and K+,and the emission peak intensities were all enhanced. Under the condition of the same Li+,Na+ and K+ concentration, the emission peak intensities of M3(M=Ca, Sr, Ba)Y2(BO3)4∶Eu3+ phosphor were compared, and the result shows that the accretion effect of doping Li+ is the best. The effect of Li+ concentration on the emission peak intensity of Sr3Y2(BO3)4∶Eu3+ phosphor was studied. The results show that the emission peak intensity firstly increased with the increasing Li+ concentration, then decreased, and reached the maximum value at 5 mol% Li+,and the maximum value is about twice as much as the Li-undoped one.
2008 Vol. 28 (11): 2503-2506 [Abstract] ( 853 ) PDF (995 KB)  ( 483 )
2507 The Light Pulses and Spectra of Straight Tube Conical Bubble Sonoluminescence in Glycol
HE Shou-jie1, HA Jing2, DONG Li-fang1, LIU Zhi-qiang1, WANG Long3
DOI: 10.3964/j.issn.1000-0593(2008)11-2507-04
Based on the U-tube, a new type of sonoluminescence apparatus-conical bubble sonoluminescence straight tube apparatus was set up, and the structures and operations were described detailedly. Using the apparatus, the ultrabright cavitation luminescence was obtained in glycol solution. The light pulses of conical bubble sonoluminescence were detected, results show the half width is about 80 μs that is much longer than the results by ultrasound, which should be caused by the fact that the conical bubble can obtain more energy from the flow than the bubbles from the ultrasound. The spectra consist in a broad background ranging from the ultraviolet regioo to the visible region, on which five clear sequences of Swan bands and three sequences of B2Σ+X 2Σ+ transition of CN are superimposed. A band assigned to the A2Δ→X2Π transition of CH was also measured. Specially, the vibrational structures of Swan bands can be resolved. Finally, the achieved molecular vibrational temperature of C2 is estimated to be about (4 200±200) K.
2008 Vol. 28 (11): 2507-2510 [Abstract] ( 1863 ) PDF (897 KB)  ( 466 )
2511 Synthesis and Spectra of Novel Metal Complexes of Multi-Nitrogen Heterocyclic Ligand
JIANG Xin1,2,WU Yi-qun1,3*,HE Chun-ying1
DOI: 10.3964/j.issn.1000-0593(2008)11-2511-04
Novel multi-nitrogen heterocyclic metal complexes M(HMPB)2 (M=Co, Ni) using 2-(2′-hydroxy-5′-methyl phenyl) benzotriazole (HMPB) as ligand, were synthesized by the methanol aqueous solution precipitation method for the first time. The as-prepared samples were characterized by element analysis and laser-desorption ionization time-of-flight mass spectrometry (LDI-TOF-MS). The Fourier transform infrared characteristic spectra (FTIR) and ultraviolet visible electronic absorption spectrum (UV-Vis) of the new complexes were also studied especially. The results show that the HMPB ligand coordinates with the center metal ions by nitrogen and oxygen atoms in the form of bidentate ligand, and the coordination number of the center metal ions is four in the complexes; FTIR characteristic absorption band of the complexes is located in the region of 400-2 500 cm-1. After the complexes formation, the stretching vibration of the hydroxy group of 2-(2′-hydroxy-5′-methyl phenyl) benzotriazole, the vibration peak of CN bond and the characteristic absorption of C─O bond showed distinct changes. The IR characteristic absorption peak positions of M─N and M─O bond were also confirmed. These complexes exhibited a strong absorption in the ultraviolet region and the maximum absorption peak located in the range of 335-345 nm.
2008 Vol. 28 (11): 2511-2514 [Abstract] ( 267 ) PDF (629 KB)  ( 593 )
2515 The Principle and Technical Analysis of Methane Detection Using Infrared Absorption Spectroscopy
ZHANG Yu,WANG Yi-ding*,LI Li,ZHENG Chuan-tao,AN Yu-peng,SONG Zhen-yu
DOI: 10.3964/j.issn.1000-0593(2008)11-2515-05
There has been considerable interest recently in methane sensor based on infrared absorption spectroscopy for industrial detection and environment monitoring. The present paper presents the intensites of methane mid-infrared fundamental absorption bands,near-infrared combination band of ν2+2ν3 and overtone band of 2ν3, and it was found that the absorption strengths of fundamental bands are two orders of magnitude higher than those of overtone bands and three orders of magnitude higher than those of the combinations. Theoretically, mid-infrared detection system is much better. However, because the near-infrared source and detector are more maturely developed and cheaper, near-infrared technology is widely used. Furthermore, the near-infrared radiation can be transmitted through ordinary low-loss silica fiber, suitable for long-distance methane sensing system, meeting the needs of industrial mining and other aspects. But with the development of mid-infrared detector and high-power high-sensitivity devices, low priced micro sensor modules will be more and more developed. The development of optical methane sensors is reported in this paper. Several detection technologies were investigated such as differential absorption, harmonic detection, cavity spectroscopy enhancement and photoacoustic spectroscopy. The theoretical formula,sensitivity and system structure of these technologies are presented.
2008 Vol. 28 (11): 2515-2519 [Abstract] ( 695 ) PDF (1504 KB)  ( 660 )
2520 Passive Remote Measurement of Flame Infrared Image by a FTIR Scanning Imaging System
LIU Zhi-ming,GAO Min-guang,LIU Wen-qing,LU Yi-huai,ZHANG Tian-shu,XU Liang,WEI Xiu-li
DOI: 10.3964/j.issn.1000-0593(2008)11-2520-03
The present paper introduced a FTIR scanning imaging system. This system is based on the combination of a FTIR spectrometer and a scanning mirror. So it has the advantage of FTIR spectrometer: non-contact, real-time, celerity, nicety and high sensitivity. Through scanning mirror, the authors can obtain the space information of targets. The authors used this system to measure the flames infrared emission spectra of three alcohol burners at a flat roof in our laboratory. According to Planck’s law, the authors calculated the relative temperature of from each spectrum. These temperature data formed an array. The authors used matlab software to plot the infrared images of target and contrasted them with video image. They were consistent with each other very well. This experiment allowed us to obtain the temperature distribution of three alcohol burners’ flames, and provide identification, visualization, and quantification of pollutant clouds.
2008 Vol. 28 (11): 2520-2522 [Abstract] ( 1373 ) PDF (798 KB)  ( 526 )
2523 Comparison of PLS and SMLR for Nondestructive Determination of Sugar Content in Honey Peach Using NIRS
XU Hui-rong, WANG Hui-jun, HUANG Kang, YING Yi-bin*, YANG Cheng, QIAN Hao, HU Jun
DOI: 10.3964/j.issn.1000-0593(2008)11-2523-04
Nondestructive fruit quality assessment in packing houses can be carried out using near infrared (NIR) spectroscopy. However, in industrial process, some experimental conditions (e.g. temperature, fruit variety) cannot be strictly controlled and their changes would reduce the robustness of the NIR-based models. In the present paper, a total of 100 honey fruits from two super markets were used as experimental materials. Fifty honey fruits were stored at room temperature and the other fifty samples were stored at 0-4 ℃. NIR diffuse reflectance spectra of the honey peaches were measured in the spectral range of 4 000-12 500 cm-1 using InGaAs detector. After outlier diagnosis using leverage values and Dixon test and spectra data pretreatment with Norris derivative filter (segment length: 5, gap: 5), partial least square (PLS) regression with standard normal variate (SNV) transformation and stepwise multilinear regression (SMLR) with multiplicative scatter correction (MSV) were used to establish calibration models based on first derivative spectra. Comparing the two calibration methods of PLS and SMLR, the performances of the models developed by SMLR were found much better than that by PLS method. The best results for PLS models were: correlation coefficient of calibration (RC)=0.965, root mean square errors of calibration (RMSEC)=0.301° Brix,correlation coefficient of cross-validation (RCV)=0.812, root mean square errors of cross-validation (RMSECV)=0.67° Brix and ratio of standard deviation to root mean square errors of cross-validation (RPD)=1.72, which were slightly worse than those for SMLR: RC=0.929, RMSEC=0.424° Brix of calibration and RCV=0.887, RMSECV=0.532° Brix of cross-validation and RPD=2.16. The RPD values for SMLR models in three different spectral regions 4 290-7 817, 7 817-10 725 and 4 290-10 725 cm-1 were: 1.97, 1.89 and 2.16, respectively. The performance of the model developed by SMLR in the 4 290-7 817 cm-1 region was much better than that in the 7 817-10 725 cm-1 region. The results indicated that the SMLR method could develop a good calibration model by selecting wavelengths insensitive to temperature and NIR spectra could be used for sugar content prediction of fruit samples with varied temperature when developing a global robust calibration model to cover the temperature range.
2008 Vol. 28 (11): 2523-2526 [Abstract] ( 284 ) PDF (711 KB)  ( 540 )
2527 Study on Discrimination of Tea Based on Color of Multispectral Image
CHEN Xiao-jing1,WU Di2,HE Yong2*,LI Xiao-li2,LIU Shou1
DOI: 10.3964/j.issn.1000-0593(2008)11-2527-04
Tea is one of the most popular beverages worldwide. Its categories have a great relationship to its beneficial medicinal properties. The present work attempted to study the feasibility to use multispectral imaging technique as a rapid and non-destructive method to discriminate tea varieties. Two categories of tea discriminated hardly by naked eye were sorted. The images were 1 036 pixels vertically by 1 384 pixels horizontally with 24-bit depth, and were captured using a red (R) waveband, near infrared (NIR) waveband and green (G) waveband multispectral digital imager, MS3100 (Duncan Technologies, Inc., CA, USA). The three wavebands of image (Red, Green, NIR) can be composed into one image which contains more information than images recorded by ordinary digital cameras, especially, the NIR image is more sensitive to the color of organic matter than visible spectrum. The three images of one sample can be obtained simultaneously. The color features of tea were calculated using the standard notations: mean and mean square deviation. Then, the two color features of 3CCD and ordinary digital cameras were extracted and calculated by Matlab 7.3 software respectively, and were contrasted. A total of 60 samples were adopted, and the features of mean and mean square deviation of NIR waveband image were applied as inputs to a back propagation neural network (BP-ANN) with one hidden layer. The forty samples (twenty for each category) were selected randomly to build BP-ANN model, and this model was used to predict the varieties of 20 unknown samples (ten for each category). The two categories of tea can be discriminated by the information of color of images of 3CCD, but can not by the ordinary digital cameras. The result indicted that the discrimination rate of classification set of BP-ANN model was up to 100% within 0.3 of threshold. It concluded that multi-spectral imaging technique has a high potential to identify categories of green tea fast and non-destructively.
2008 Vol. 28 (11): 2527-2530 [Abstract] ( 2671 ) PDF (933 KB)  ( 607 )
2531 The Clinical Detection of Breast Cancer by Spectrum Method
GAO Tian-xin1,3,FAN Xiao-fei1,XUAN Li-xue2,ZHANG Bao-ning2, LI Xia1,BAI Jing1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2531-05
Breast cancer is one of the most frequently encountered malignant tumors of women. Early detection can save lives successfully. A safe, effective detection method is needed. The detection of breast cancer based on the laser-tissue interactions is an international research focus. The prototype of the detection system in the authors’ lab uses a 780 nm low frequency modulated laser to penetrate breast tissue. Two-dimensional scan is processed under the control of computer. A photomultiplier tube (PMT) is used to get the penetrated light and convert it to electrical signal. The signal of light intensity is sampled by the system and used to get the near infrared penetrating image of breast after data processing. In the present paper the signal processing method is discussed and the data processing results in the lab experiments are given. Clinical trials were carried out in the Cancer Institute and Hospital, Chinese Academy of Medical Sciences and Peking Union Medical College, using NIR (near infrared light) breast scanner developed by the authors’ lab. The investigations were performed after approval by the ethic committee of Cancer Institute and Hospital, Chinese Academy of Medical Sciences. Written informed consent was obtained from each subject. None of the patients’ names, initials, or hospital numbers was used in this paper. Fifty patients underwent the examination. Thirty four of them were malignant, and 13 were benign. The other 3 lacked pathology results. Analysis and comparison were executed to evaluate the result. NIR images, mammographs, and the ultrasound images were compared with both the pathology results and each other. The accuracy percentage of NIR image reaches 72.5%, which is between the accuracy percentage of ultrasound (77.50%) and that of mammography (71.88%). In this paper, the characteristics of different breast diseases were found in NIR images, which offers criterion for NIR diagnosis method in detail. The typical NIR images of different diseases, such as papillomatosis with local cancer and cancer, were shown. The clinical trial verified the validity of tumor diagnosis with the special absorption of NIR light by hemoglobin. Both the position and the benign/malignant property of tumor can be detected by NIR method. The improving aspects of the prototype were proposed. A new approach was put forward to the optical method.
2008 Vol. 28 (11): 2531-2535 [Abstract] ( 2362 ) PDF (1043 KB)  ( 446 )
2536 Online Detection of Soluble Solids Content of Pear by Near Infrared Transmission Spectrum
SUN Tong1, YING Yi-bin1*, LIU Kui-wu1, HU Lei-xiu2
DOI: 10.3964/j.issn.1000-0593(2008)11-2536-04
The research was to detect soluble solids content (SSC) of pear online by near infrared transmission spectrum. The movement speed of pear was 0.5 m·s-1 the power of light source was 300 W, and semi-transmission was used to collect the spectrum of pears. The total experiment samples were 187 pears, with a calibration set of 147 pears and a validation set of 40 pears. Partial least squares (PLS) and principal component regression (PCR) technique were used to develop the calibration model for online detection. Spectral ranges of 550-700 nm, 700-850 nm, 550-850 nm were used to establish the calibration models, and it was found that the model with 550-850 nm was better than others whether for PLS or for PCR. Also, the models based on different pretreatment methods such as Savitzky-Golay smooth, first derivative, second derivative and so on were compared, and the result showed that the five point Savitzky-Golay smooth could increase S/N ratio and improve performance of the model, whereas first derivative and second derivative could do little to improve performance of the model. The best model had the satisfactory calibration and prediction abilities, with the correlation coefficient (RC)=0.948 8, root mean square error of calibration (RMSEC)=0.236 and root mean square error of validation (RMSEP)=0.548. The result in this study shows that the detection of SSC of pear online is feasible.
2008 Vol. 28 (11): 2536-2539 [Abstract] ( 2444 ) PDF (626 KB)  ( 500 )
2540 Study on Influence of Gamma-Ray Treatment on Spectral Characteristic of Rapeseed
HUANG Min1,WANG Zun-yi2,HE Yong1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2540-05
After being treated by gamma-ray, the spectral characteristic of rapeseed would be changed. Based on the principle, a rapid and nondestructive method by using visible and near infrared spectroscopy was proposed to discriminate rapeseeds (Brassica nupus) treated by different dosages of gamma-ray. Partial least square (PLS) method and BP neural network (BPNN) were applied to establish the discrimination model, and the influences of different pretreatment methods of original spectra data, data transformation methods of PLS principal components and the selection of node number of hidden layers of BP neural network model on prediction precision were compared and discussed. In the experiment, 184 samples were treated by gamma-ray with 5 different dosages (50, 100, 150, 200 Gy, and the samples without gamma-ray treatment). Then spectra tests were performed on the 184 samples using a spectrophotometer (325-1 075 nm). One hundred thiry five samples were selected randomly for model calibration and the left 49 samples were used for prediction. As a result, the optimal model was established and the parameters of the model were shown as follows. The original spectra data were pretreated by smoothing media filter, multiplicative scatter correction and Savitzky-Golay derivatives, then 6 PLS principal components were selected by using partial least square method. After being transformed by using natural logarithm transformation method, the 6 PLS principal components were used as the input layer factors to establish the BP neural network model and the node number of hidden layers was selected as 4 or 9. The prediction precision of the optimal model to distinguish the untreated samples from gamma-ray treated samples was 100%. The precision of predicting the dosages of gamma-ray treatment of all samples achieved 85.71%. It can be concluded that the proposed method for estimating the influence of different gamma-ray dosages on the spectral characteristic of treated rapeseeds was feasible.
2008 Vol. 28 (11): 2540-2544 [Abstract] ( 1915 ) PDF (896 KB)  ( 501 )
2545 The Correlation between Postmortem Interval and Fourier Transform Infrared Spectra in Rat’s Brain
KE Yong1,WANG Shi-wei2,LU Qing-yang1,HUANG Ping1,XING Bo1,WANG Zhen-yuan1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2545-05
In the present study, FTIR spectroscopy was applied to observe the process of postmortem degradation in rat’s brain and a lot of useful data for the estimation of postmortem interval (PMI) were provided. Sprague-Dawley male rats (weight 240±10 g) were chosen and sacrificed by cervical dislocation. The bodies were kept in a controlled environmental chamber set at (20±2) ℃, and their brain cortex as the measuring sample which was extracted at 0, 12, 24, 48, 72, 96, 120, 144 and 168 h from the 8 rats. The tissues were freeze dried in a vacuum at -50 ℃ overnight in order to dehydrate them. About 2 mg freeze dried tissues were mixed with 200 mg KBr and then ground in an agate mortar for 5 min. The mixture then was pressed into a pellet with a thickness of 0.4 mm and a diameter of 12 mm. The FTIR spectra were quantitatively recorded at room temperature in the range 4 000-400 cm-1 on a Shimadzu 8400S spectrometer (Shimadzu, Japan). IR solution 1.10 software (Shimadzu, Japan) was used for the analysis of the FTIR spectra and for recording the data from the spectra. With the PMI increasing, the peak position of main absorbance bands in the FTIR spectra showed no significant difference, but there was a dramatic variance in the intensity: (1) The relative intensity at 1 080 and 1 238 cm-1(I1 080/I1 398 and I1 238/I1 398) related with nucleic acid tended to decrease obviously. (2) The intensity ratio at amide Ⅱ and Ⅰ(I1 541/I1 647) increased with the PMI increasing. The intensity at 1 338 and 1 313 cm-1 varied slightly, but their intensity ratio to 1 398 cm-1 decreased. (3) The intensity at 1 456 and 1 398 cm-1 showed a trend of decreasing and increasing respectively. (4) Compared with the intensity at 2 871 cm-1,the intensity at 2 852, 2 871, 2 923 and 2 958 cm-1 tended to increase, but the increasing tendency at 2 871 cm-1 was slight. It is concluded that FTIR spectroscopy is going to be an effective method for estimating the PMI in medicolegal practice and the brain tissue may be a suitable marker as a potential sample.
2008 Vol. 28 (11): 2545-2549 [Abstract] ( 320 ) PDF (1223 KB)  ( 480 )
2550 The Quantified Analysis of Fresh Mutton Tenderness Using PLS Methods and Fourier Transform Near-Infrared Spectroscopy
ZHANG De-quan1,CHEN Xiao-na2,SUN Su-qin3,LI Chun-hong1,ZHANG Bo-lin2,LI Yong1,LI Shu-rong1, LI Qing-peng1,ZHOU Hong-jie1
DOI: 10.3964/j.issn.1000-0593(2008)11-2550-04
Ninety eight representative fresh mutton samples from Neimeng, Ningxia, Gansu, Xinjiang province were selected for this study, the nondestructive measurement of the fresh mutton tenderness by Fourier transform near infrared (FT-NIR) spectroscopy was discussed. Partial least squares(PLS) algorithm was used to build the model between the shear force value of the fresh mutton tenderness measured by the texture machine and the FT-NIR spectra. The influence of different processing method of spectra, factors and wave regions on the determination coefficients (r2), root mean square error of cross validation (RMSECV) and root mean square error of prediction (RMSEP) was studied. The result showed that the shear force value of ninety eight representative fresh mutton samples was 1.673-6.631 kg, and the shear force value above 75% samples was 2-5 kg, almost covering the fresh mutton tenderness of our country’s sheep, the r2 of the calibration could reach 86.2% and the RMSECV was up to 0.445 in the wave number range 11 995-5 446 cm-1 and 4 601-4 246 cm-1 with vector normalization when the PLS factors was ten. The correlation coefficient(R), RMSEP and average bias between value measured by the texture machine and predicted value of model based on validation samples were 0.87, 0.524 and 0.385 respectively. The result indicates that FT-NIR spectroscopy is capable of predicting tenderness value of fresh mutton.
2008 Vol. 28 (11): 2550-2553 [Abstract] ( 311 ) PDF (746 KB)  ( 458 )
2554 Characterization of Oxidation on Pyrite by In Situ Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy
ZHANG Ping, CHEN Yong-heng, LIU Juan, WANG Chun-lin
DOI: 10.3964/j.issn.1000-0593(2008)11-2554-03
Pyrite is one of common natural minerals in the environment, which is easily oxidated and is the main source of acidity mine drainage (AMD). The study on the oxidation of pyrite is helpful to comprehend the mechanism of its pollution. In the present paper, the oxidation of pyrite under the condition of air and water was respectively investigated by the attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) through the designing experiment on the formation of carbon dioxide by the reaction of carbonate in pyrite with sulfuric acid formed by the oxidation of pyrite. The CO2 measurement by in situ ATR indicated that the oxidation rate of pyrite both in the air and in water both reduced by time and the latter reduced more obviously than the former, which indicates that the oxidation rate of pyrite in water is slower than that in the air. In the ATR measurement, the double absorption peaks at 2 350 cm-1 that indicates CO2 have high selectivity, and permits the in situ analysis.
2008 Vol. 28 (11): 2554-2556 [Abstract] ( 1233 ) PDF (842 KB)  ( 489 )
2557 Study on IR Fingerprint Spectra of Alpinia Oxyphylla Miq
LIU Hong1,HAN Chang-ri1*, LIU Hong-xia2,LIU Yuan-feng1,HE Meng-xiong1
DOI: 10.3964/j.issn.1000-0593(2008)11-2557-04
Fourier transform infrared spectrum has been developed for application in the quality control of traditional Chinese medicine, and two new indexes, including common peak ratio and variant peak ratio, were applied, and their values were calculated by means of the sequential analysis for eight kinds of essence oil of Alpinia oxyphylla Miq from different cultural areas (Hainan, Guangxi and Guangdong), in which each sample’s IR fingerprint spectra were set up and the common peak ratio and variant peak ratio sequences were arranged in the order of size in comparison with other samples. It can be seen that Alpinia oxyphylla samples from Guangxi, Hainan and Guangdong provinces could be successfully revealed directly by the common peak ratio and variant peak ratio sequences. In comparison with their conventional IR spectra, the primary difference in Alpinia oxyphylla is the intensity of characteristic peaks at 1 710 and 1 666 cm-1. Considering the spectral range of 400-4 000 cm-1,the common peak ratio of the spectra between Hainan and Guangdong was 62%, while the common peak ratio between Hainan and Guangxi was 52%. But the mix common peak ratio of the spectra in Hainan is 66%. The fingerprint characters of IR can not only identify the main chemical constituents in medicinal materials, but also compare the components differences among the similar samples. The analytical method is an rapid, effective, fast and advanced to evaluate the production area for pharmaceutical market.
2008 Vol. 28 (11): 2557-2560 [Abstract] ( 2514 ) PDF (541 KB)  ( 487 )
2561 A Local Regression Method for Near-Infrared Spectral Quantitative Analysis of Tobacco Samples
SHI Xue, CAI Wen-sheng, SHAO Xue-guang*
DOI: 10.3964/j.issn.1000-0593(2008)11-2561-04
A local regression method based on distance criterion in principal component (PC) space for near-infrared (NIR) spectral quantitative analysis was proposed. In this method, principal component analysis (PCA) is firstly utilized to extract the information of the NIR spectra, and then, the calibration subsets are individually selected for each prediction sample according to the distance between the sample and calibration samples in the PCs space. Finally, the PLS local model for every prediction sample is established individually and the prediction of the sample is done with the local model. It was found that the Euclidean distance can more effectively measure the similarity of the samples than Mahalanobis distance. With an application of the local regression method to the quantitative determination of chlorine and nicotine in tobacco samples, it is proved that the prediction precision of local regression method is better than that of global regression methods, especially in the situation of predicting the low concentration components.
2008 Vol. 28 (11): 2561-2564 [Abstract] ( 1308 ) PDF (762 KB)  ( 541 )
2565 Determination of Adulteration in Honey Using Near-Infrared Spectroscopy
CHEN Lan-zhen1, 2,ZHAO Jing1,YE Zhi-hua2*,ZHONG Yan-ping3
DOI: 10.3964/j.issn.1000-0593(2008)11-2565-04
The objective of the present research is to study the potential of using Fourier transform near-infrared spectroscopy (FT-NIR) in conjunction with discriminant partial least squares(DPLS) chemometric techniques for the discrimination of honey authenticity. First, seventy one commercial honey samples from Chinese market were analyzed to detect the levels of honey adulteration by stable carbon isotope ratio and the chemical result showed that the samples include unadulterated (n=27) and adulterated (n=44) products. The samples were scanned in the spectral region between 4 000 and 11 000 cm-1 by FT-NIR spectrometer with an optic fiber of 2 mm path-length and an InGaAs detector and then divided randomly five times into two sets, namely calibration sets and validation sets, respectively. Five kinds of mathematic models of honey samples were established for classification of honeys as authentic or adulterated by using DPLS. Different spectra pretreatment methods, spectral range and different principal component factors were selected to optimize the calibration models. The calibration models were successfully validated with exterior cross-validation methods. Through comparison analysis of the results, the overall corrected identification rate of authentic and adulterated honey samples in five calibration models were 91.49%, 94.68%, 92.98%, 93.86% and 94.87%, respectively. The correct classification rate of the validation samples was 93.75%, 89.58%, 89.29%, 92.31% and 86.96% from model one to model five, respectively and 100% of adulterated honey samples were correctly identified and classified in validation models 2, 3 and 4. The results demonstrated that FT-NIR together with DPLS could be used as a rapid and cost-efficient screening tool for discrimination of commercial honey adulteration, and the analytical technique would be significant to Chinese honey quality supervision.
2008 Vol. 28 (11): 2565-2568 [Abstract] ( 2717 ) PDF (503 KB)  ( 609 )
2569 A Raman Study of ZnO Powders with ZnO2 as Precursor
ZHANG Sheng-rui,CHEN Yi-ting,SONG Sheng-hua,JIN Yuan-hao,DU Wei-min*
DOI: 10.3964/j.issn.1000-0593(2008)11-2569-05
Raman spectra of ZnO powders prepared by firing ZnO2 precipitate were reported in detail for the first time. By comparing the spectra with that of the sample fabricated by another method and analyzing frequency difference between the focused-laser irradiated samples with different firing temperature in preparation, it was concluded that the ~333 cm-1 peak is ascribed to E2(high)-E2(low) and the ~661 cm-1 peak to its overtone. In addition, a new interpretation for the observed Raman peaks between 400 and 500 cm-1 in ZnO2 powders was presented based on the IR data and ab initio calculation.
2008 Vol. 28 (11): 2569-2573 [Abstract] ( 2000 ) PDF (1503 KB)  ( 509 )
2574 Raman Spectroscopic Investigation on the Interactions between Liver Cancer Cells (SMMC-7721) and Fufang Luxiancao Particles
ZHANG Jin-yan, GUO Jian-yu, CAI Wei-ying, SUN Zhen-rong*
DOI: 10.3964/j.issn.1000-0593(2008)11-2574-05
Luxiancao is a new medicine for liver cancer, and is purely natural botanical. It has good curative effects and few side effects. The curative mechanism of Luxiancao is unknown. In the present paper, the authors used a 514.5 nm laser to measure the changes in the Raman spectrum of liver cancer cells (SMMC-7721) treated by Luxiancao at different concentrations. The study can help us know more about the mechanism, efficiency and side effects of Luxiancao. The results show that significant changes were observed in the cells’ Raman spectra after reacting with Luxiancao. The intensities at 785 and 1 092 cm-1,corresponding to DNA phosphate backbone vibration, were reduced; and the Raman bands for the bases A and G at 1 312 and 1 585 cm-1 also decreased, indicating that Luxiancao may be inserted in DNA bases and influence the DNA replications, resulting in the reduction in DNA content and breaking of the DNA strands. Besides, the intensity of 1 360 cm-1,belonging to Trp, decreased gradually and disappeared in the end, indicating the Trp of cancer cells began to be exposed when adding in Luxiancao. The bands at 1 004 cm-1 for Phe and 1 656 cm-1 for proteins α-helix also decreased, suggesting that there were changes in the structure of protein and circumstance of amino acid. Moreover, the effects on cancer cells were enhanced gradually with the HCPT concentration increasing. Since a Raman spectrum is a chemical fingerprint of a sample, the different concentration dependent changes in the Raman spectra of individual cells due to reacting with Luxiancao can overcome the limitations of other detection systems used for quantitative and qualitative analysis of the drug.
2008 Vol. 28 (11): 2574-2578 [Abstract] ( 509 ) PDF (1310 KB)  ( 505 )
2579 Effect of Fluorine in Mould Fluxes on Microstructural Units of Silicates Slag
HE Sheng-ping1,YOU Jing-lin2,WANG Qian1,XU Chu-shao1
DOI: 10.3964/j.issn.1000-0593(2008)11-2579-04
In the continuous casting of steel, mold fluxes play an important role in improving surface quality of casting strands and maintaining the continuous casting process. The physiochemical property of mold fluxes is definitely correlated with the microstructure. Fluorides play an important role in modifying the high temperature properties of mold fluxes. So, studying the effect of fluoride on multicomponent silicate structure is helpful to understanding the performance of fluoride in mould fluxes. In the present paper, effects of fluorine on melt, glass and crystal structure of silicate were studied by using Raman spectroscopy and in situ high temperature technique. The results were as follows: While the content of CaF2 increased, the varieties and relative quantities of microstructural units of silicates changed, the polymerization of the silicate network decreased, and the viscosity of the melt decreased; comparing non-fluoride with high-fluorine mold fluxes, the main kind of microstructure of silicates in mold fluxes with high fluorine was mostly monomer, while in fluorine free mold fluxes it was mainly chain of microstructure. It would help to develop fluorine free mold fluxes.
2008 Vol. 28 (11): 2579-2582 [Abstract] ( 3552 ) PDF (1050 KB)  ( 743 )
2583 Study on Spectral Characteristic of Dissolved Organic Matter Fractions Extracted from Municipal Solid Waste Landfill Leachate
ZHANG Jun-zheng1,YANG Qian1*,XI Bei-dou2,WEI Zi-min3,HE Xiao-song3,LI Ming-xiao3,YANG Tian-xue3
DOI: 10.3964/j.issn.1000-0593(2008)11-2583-05
In the present study, the samples of landfill leachate of 0, 5, 10-year-old were respectively taken from landfill plant. Based on a modified Leenheer fractionation scheme, dissolved organic matter (DOM) extracted from landfill leachate of three different ages was fractioned according to their polarities and charge characteristics by using XAD-8 resin, and the fractions of hydrophobic acid (HOA), neutral (HON) and hydrophilic matter (HIM) were obtained, Then the fluorescence and UV spectra of DOM fractions were determined. The fluorescence synchronous scan spectra of DOM fractions exhibited a primary peak at 280 nm for 0-year-old, while the primary peak exhibited at 340nm for 5 and 10 year-old, suggesting that DOM fractions contained mainly protein-like matter at initial stage of landfill, and with the increase in landfill ages, aromatic structures of DOM fractions in leachate were enriched. Among the DOM fractions of HOA, HON and HIM at different ages of landfill leachate, the fluorescence and UV spectra all indicated that the molecular weight, content of aromatic compounds and degree of condensation were all in the order of HOA>HON>HIM. The ratio of UV absorbance at 253 nm to that at 203 nm (A253/A203) showed, that the substituent on the aromatic ring of HOA and HON fractions consisted mainly of carbonyl, carboxyl and hydroxyl; while that of HIM consisted of aliphatic chains, and the content of aromatic compounds was lower than that of HOA and HON; which implied that the HIM displayed a lower molecular weight and simpler structure compared to HOA and HON. Altogether, the results obtained from fluorescence and UV spectra indicate that the degree of aromatization increased in DOM fractions of leachate with the landfill ages, in the following order: HOA>HON>HIM.
2008 Vol. 28 (11): 2583-2587 [Abstract] ( 2690 ) PDF (1137 KB)  ( 572 )
2588 Spectra Characteristics of an Aminated Glucose and Its Complex with Cu(Ⅱ)
LIAO Qiang-qiang1,2, LI Yi-jiu1, XIANG Bo1,CHENG Ru-mei1,CHEN Lin1,HE Wei-na1
DOI: 10.3964/j.issn.1000-0593(2008)11-2588-04
Characteristics of an aminated glucose and its complex with Cu (Ⅱ) were investigated by FTIR, 1H-NMR and UV spectroscopy, respectively. Compared with glucose, the FTIR spectrum of an aminated glucose showed a moderate peak at 1 629-1 608 cm-1 which was attributed to δNH vibration, suggesting that glucose reacted with ethylenediamine. The 1H-NMR spectrum of an aminated glucose demonstrated the signal of the C1 hydroxy proton and one of the amino proton at 4.82-4.79 ppm, illustrating that the amino of ethylenediamine was substituted for the hydroxy group of C1. As for UV spectra, an aminated glucose did not show absorbance in the ultraviolet region while its complex with Cu(Ⅱ) had obvious absorption peak at about 236 nm. The complex ratio of the aminated glucose to Cu(Ⅱ) was about 1 to 1 and the stability constant of its Cu(Ⅱ) complex was 6.8×107 L·mol-1.
2008 Vol. 28 (11): 2588-2591 [Abstract] ( 1341 ) PDF (885 KB)  ( 529 )
2592 Synthesis and Spectral Characterization of Ce(Ⅲ)and Dy(Ⅲ)Complexes with Tetraisopropylmethylenediphosphonate
GAO Hong-wei1,DONG Jia-cui1,ZHAO Xing-e2,YANG Liang1,JIN Qiong-hua1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2592-04
Three rare-earth complexes [CeL4](OTf)3·2H2O(L=tetraisopropylmethylene -diphosphonate; OTf=trifluoromethanesulfate), [Dy(OTf)2L2(H2O)2](OTf)(CH3CN) and [DyL4](OTf)3·L·2H2O were prepared by the reaction of Ln(OTf)3(Ln=Ce,Dy) and (iPrO)2P(O)CH2P(O)(iPrO)2 in CH3CN. Their compositions were confirmed and their properties were characterized by elemental analysis, infrared spectra, 1H and 31P NMR spectroscopy, fluorescence spectra and DTA-TGA. The data of elemental analysis of these complexes are in good agreement with the formula given above. In the infrared spectra of all these complexes, there are obvious shifts of some important absorption bands, such as the PO or S—O bands, illustrating that the ligands L or OTf ions were coordinated to the lanthanide ions. The signals in 1H NMR spectrum at approximately 1.2, 2.4 and 4.5 have been assigned to the resonance of H atoms in the ligand L, and these signals in the spectrum of complexes are highfield shifted compared to that of free ligand due to the electron cloud of Ln—O band moving towards to P—O band. The sharp single peaks were found in the 31P NMR spectrum, and the chemical shifts are at 18.705 6 for free ligand L, 18.543 5 for complex Ⅰ, 18.273 1 for complex Ⅱ, and 18.489 4 for complex Ⅲ. The excitation and emission signals of Ce(Ⅲ) ion were in view of electric dipole transition from 4f15d1 to 4f7. The fluorescence spectroscopy shows that the excitation peak of [CeL4](OTf)3·2H2O is at 249 and 300 nm, and a strong emission peak is at 641 nm. The existence of two coordination water molecules in [Dy(OTf)2L2(H2O)2](OTf)(CH3CN) makes both the excitation and emission peaks weaker than that of [DyL4](OTf)3·L·2H2O. The coordination model of rare-earth with diphosphonic ligand was also discussed. All of these complexes are eight-coordinated. The complexes [CeL4](OTf)3·2H2O and [DyL4](OTf)3·L·2H2O are highly-symmetrical, in which four bidentate ligands L are coordinated to Ce and Dy atoms respectively while the OTf ions and the water molecules are not coordinated. In the complex [Dy(OTf)2L2(H2O)2](OTf)(CH3CN), two L molecules, two water molecules and two OTf ions are coordinated to Dy atom while one OTf ion and one solvent molecule CH3CN are not coordinated.
2008 Vol. 28 (11): 2592-2595 [Abstract] ( 269 ) PDF (891 KB)  ( 528 )
2596 Metamerism Breakdown Characteristic and Its Application in Detection of Foreign Materials
JIA Dong-yao1,YANG Wen-kao2,LIU Ze1
DOI: 10.3964/j.issn.1000-0593(2008)11-2596-05
Spectrum imaging detection techniques currently face the new challenge that it’s difficult to detect similar foreign materials for their same appearance as the background. To resolve the problem of detection of similar foreign materials in the complex background, the objective of the present research was to develop a transmission/reflection spectrum image detection method based on metamerism breakdown characteristic. In the discrete spectrum wavelength region from 370 to 1 100 nm, this method is based on the principle that different materials have different spectral transmission and reflectance characteristic. When submitted to a source of illumination at different wavelength, foreign materials present different transmission and reflectance values in comparison to those from background. In the present paper, for simultaneously discriminating several types of foreign materials from background, the transmission and reflectance characteristic discrimination between foreign materials and background in the metamerism breakdown process was analyzed, then the optimal wavelength evaluation function for describing the background/foreign materials transmission and reflectance discrimination was set up to seek an optimal transmission/reflection illumination wavelength. Through the spectrum imaging experiment, the optimal operating condition including optimal detection wavelength and optimal illumination energy for these detected foreign materials was determined and accordingly an optimal wavelength imaging system was developed. In the actual application to the detection of foreign materials in cotton, the foreign material image features were acquired using the optimal wavelength transmission/reflection imaging system, also the image features were enhanced using image decision band fusion, then the targets of foreign materials were extracted effectively from image using binary processing. The experiment result indicated that the image features of similar foreign materials acquired by imaging system were obvious, and the detection result consisted with the fact in the double wavelength image detection system, which include 390 nm reflection wavelength and 580 nm transmission wavelength. This method provided an effective way for the detection of white fiber foreign materials in cotton and a novel practical means to solve the current problem of foreign material detection.
2008 Vol. 28 (11): 2596-2600 [Abstract] ( 438 ) PDF (883 KB)  ( 427 )
2601 Improved Data Processing Method of Fluorescence Correlation Spectroscopy
WANG Shuo1,JIN Lei2*,CHEN Die-yan1
DOI: 10.3964/j.issn.1000-0593(2008)11-2601-04
By the unique ability of measuring concentration and diffusion coefficient, fluorescence correlation spectroscopy (FCS) has kept enlarging and deepening its application fields which need measuring physicochemical properties in complex mixtures. However, the classical data processing method in FCS generally induces errors in the fitting parameters, and the intuitionistic information in the chart is little or confused. Aiming at the above problems, we tried a new data processing method with differential treatment to find out whether it has multi-fluorescent-components and estimate the parameters intuitionally in the chart. The differential curves of treated autocorrelation curves have various positions, depths and full widths at half depth of the trough, by which the characteristic diffusion time and the number of the fluorescent components are decided. This improved processing method provides help for the FCS measurement in complex environment of life.
2008 Vol. 28 (11): 2601-2604 [Abstract] ( 2004 ) PDF (929 KB)  ( 447 )
2605 Study on Fluorescence Characteristic of Dissolved Organic Matter from Municipal Solid Waste Landfill Leachate
XI Bei-dou1,WEI Zi-min1,2*,ZHAO Yue2,LI Ming-xiao2,LIU Hong-liang2,JIANG Yong-hai1,HE Xiao-song2, YANG Tian-xue2
DOI: 10.3964/j.issn.1000-0593(2008)11-2605-04
In the present study, the samples of leachate of 0, 5, 10-years-old landfill were respectively taken from landfill plant, the dissolved organic matter (DOM) was extracted from landfill leachate, and the fluorescence spectra of DOM were determined. The fluorescence synchronous scan spectra of DOM in 0-year-old leachate exhibited a primary peak at 335 nm, a secondary peak at 455 nm, and a shoulder peak at 385 nm. While the fluorescence intensities of DOM at different peaks were decreased for 5-year-old leachate, especially those of the peaks at shorter wavelengths (335 and 385 nm) which may be ascribed that the simpler structural components were decreased sharply. Compared with 5-year-old leachate, the fluorescence intensity of DOM in 10-year-old leachate decreased slightly. Three-dimensional excitation emission matrix fluorescence spectra (3DEEM) of DOM in 0-year-old leachate exhibited two peaks at Ex/Em wavelength pairs of 270/355 and 220/350, respectively, which were all associated with protein-derived compounds, while the peaks of protein-like disappeared in 5-year-old leachate, and new peaks of complex structural fulvic acid-like were formed at Ex/Em wavelength pair of 330/412.5 and 250/416.5, respectively. This indicated the component of DOM in the leachate of 5-year-old landfill led to a decrease in low molecular compound, and an increase in high molecular compound compared to that of the 0-year-old. 3DEEM of DOM of 10-year-old leachate was similar to that of DOM in the 5-year-old, but the fluorescence intensity of the peaks of fulvic acid-like in DOM was different, and compared with that of 5-year-old leachate, the peak of DOM in 10-year-old leachate shifted from Ex/Em wavelength pair of 250/416.5 to 250/427.5. This indicated that the DOM formed similar structures, but the structure of fulvic acid-like in DOM of 10-year-old leachate had a greater degree of aromatization and quantity than that of 5-year-old leachate. The results obtained from fluorescence synchronous scan spectroscopy and 3DEEM indicate that aromatic structures of DOM are enriched with the age of landfill leachate.
2008 Vol. 28 (11): 2605-2608 [Abstract] ( 471 ) PDF (868 KB)  ( 494 )
2609 Studies on Interaction of Sinafloxacin with Bovine Serum Albumin and Effect of the Coexistent Metal Ions on the Reaction
FEI Yan1,LU Guo-cai2,FAN Guo-rong1*,QI Yun-peng1,WU Hui-ling1,WU Yu-tian1
DOI: 10.3964/j.issn.1000-0593(2008)11-2609-06
Serum albumin is the most abundant protein in plasma. It can bind with many intrinsic and extrinsic materials. The study of the interaction between serum albumin and drugs is a very important task in life science and chemistry. Quinolone drug is a kind of antibacterial drugs which have been used widely in clinical medicine, but its pharmacology and toxicology still have to be studied further. Sinafloxacin is a new quinolone antibiotics. The interaction between sinafloxacin and bovine serum albumin (BSA) at different temperatures and pH was investigated by fluorescence and UV absorption spectroscopy. The experimental results demonstrate that the fluorescence quenching of BSA by sinafloxacin is a result of the formation of sinafloxacin-BSA complex and the quenching mechanism is mainly static quenching. The interaction association constants of BSA and sinafloxacin were determined from the double reciprocal Lineweaver-Burk plot. The binding distance(r=3.64 nm)and energy transfer efficiency (E=0.163) between donor(BSA)and acceptor (sinafloxacin) were obtained based on Fōrster’s non-radiative energy transfer theory. There is a strong interaction between sinafloxacin and BSA. From thermodynamic coordination it can be judged that the binding force between sinafloxacin and BSA is mainly electro-static force. The effect of sinafloxacin on the conformation of BSA was analyzed by synchronous fluorescence spectrometry and three-dimensional fluorescence spectrometry. The emission maximum of tyrosine residues does not show a significant shift, while the small blue shift of tryptophan residues indicates that the hydrophobicity of microenvironment was increased. In addition, in the plasma,there are some metal ions, which can participate in many important vital actions and affect the reactions of the drugs with the serum albumins. So the effect of Cu(Ⅱ), Fe(Ⅲ), Zn(Ⅱ) and Mg(Ⅱ) on the binding constant of sinafloxacin to BSA was also discussed and it was shown that the interaction between BSA and sinafloxacin was decreased. In short, the results offer a reference for the studies on the biological effects and action mechanism of sinafloxacin with albumins in vivo.
2008 Vol. 28 (11): 2609-2614 [Abstract] ( 1747 ) PDF (1585 KB)  ( 490 )
2615 Determination of Protein by Synchronous Fluorometric Method with a New Indole Homodimeric Cyanine as Fluorescence Probe
LIN Xu-cong,YAN Jin,GUO Liang-qia,XIE Zeng-hong*
DOI: 10.3964/j.issn.1000-0593(2008)11-2615-04
Using a new homodimeric hydrophilic indole dye (Dye-I) as fluorescence probe, a sensitive synchronous spectrofluorometric determination for protein was developed. Characteristics of the fluorescence reaction between DYE-1 and BSA protein were investigated. Effects of the concentration of the hydrophilic dye, pH value of the buffer solution, and ion-intensity of NaCl were also studied and the optimum condition was gained. At pH of 2.50, electrostatic interactions of positive charges of the BSA chain and negative charges on the sulfonic groups of DYE-1 were carried out. The interactions of the indole group of DYE-1 and some active groups of BSA (viz. amido, carboxyl or sulfhydryl) were also achieved, and resulted in the combination of indole group of dye at the chain of BSA, which caused a notable increase in synchronous fluorescence with an observable shift to the longer emission wavelength. Effects of the concentration of indole dye on the determination of BSA were also investigated. With the augmentation of BSA, the α-helix structure of BSA molecular would change from the unwrapped state to the enfolded state, which was in favor of restraining free-oscillation of fluorescence probe in the solution and maintaining a high energy transfer efficiency. Such a fact would fuel a high fluorescence enhancement. and the change in fluorescence intensity (ΔF) gained the peak at 3.00 μmol·L-1. The influences of ion-intensity of NaCl on the fluorescence of BSA-DYE-1 system was visible. Effects of coexistent substances such as amino acid and metal ions such as Cu2+, K+, Ca2+, Mg2+, Al3+, and Zn2+ were also investigated. Most substances showed no notable influences on the determination of BSA except Zn2+ and Cu2+ ions. Under the optimum conditions, good calibration curves of the protein were also obtained in the range of 5.00×10-7-2.50×10-5 g·mL-1 (BSA) with a detection limit of 3×10-8 g·mL-1. Applied to simulant protein samples at the level of 1.00, 2.00, and 5.00 μg·mL-1 of BSA, the recoveries were in the range of 98.6%-103.0% with the RSD of 1.1%-1.9%。Compared with the UV standard method, the relative deviation was obtained in the range of 0.4%-3.9%.
2008 Vol. 28 (11): 2615-2618 [Abstract] ( 1873 ) PDF (680 KB)  ( 450 )
2619 Influence of Rutin on Conformation of Serum Albumin
WU Jin-xiu1,ZHANG Yin1,LI Mei1,SONG Yu-min2
DOI: 10.3964/j.issn.1000-0593(2008)11-2619-04
We studied the effect of the rutin on the conformation of bovine serum albumin (BSA) and human serum albumin (HSA) by synchronous fluorescence spectrum(Δλ=λemex=15 nm and Δλ=λemex=60 nm) and circular dichroism spectra. The results showed that rutin had hardly effect on the serum protein conformation, but influenced the secondary structure of serum albumin (SA) molecule with the addition of rutin into BSA and HSA solution. The α-helix structure of BSA and HSA was decreased and the β-sheet was increased with the increase in rutin concentration. At the same time, we studied the binding of rutin and bovine serum albumin (BSA) and human serum albumin (HSA) by electrochemistry under physiological condition. Cyclic voltammograms of rutin demonstrated a pair of well-reversible peaks in the solution of Tris-NaCl buffer at pH 7.38(sweep rate: 50 mV·s-1; a glassy carbon working electrode, a platinum auxiliary electrode, and a saturated calomel reference electrode). Both peak potentials of rutin were Epc=0.103 2 V and Epa=0.150 6 V, ipc∶ipa=1∶1.2, the dispersion of peak potential was 47.4 mV (ΔEprutinEpc-Epa=47.4 mV). In addition, with the addition of BSA and HSA into the rutin solution, both the reduction and oxidation currents decreased only at the peak potentials of rutin (BSA:Epc=0.114 1 V, Epa=0.168 5 V, ipc∶ipa=1∶1.2;HSA:Epc=0.114 2 V, Epa=0.168 8 V, ipc∶ipa=1∶1.1),the dispersions of peak potential were changed: for BSA ΔEprutin=Epc-Epa=54.4 mV, and for HSA: ΔEprutin=Epc-Epa=54.6 mV. The results showed that there was an interaction of rutin with BSA and HSA, forming a kind of nonelectroactive supramolecular complex, and indicated that rutin could be deposited and transported by serum protein in vivo.
2008 Vol. 28 (11): 2619-2622 [Abstract] ( 702 ) PDF (968 KB)  ( 623 )
2623 Fluorescence Analysis of Taxol-Induced Paraptosis-Like Independent of Caspase-3 Activation
CHEN Tong-sheng1,WANG Xiao-ping2,SUN Lei1,WANG Hui-ying1,WANG Long-xiang1
DOI: 10.3964/j.issn.1000-0593(2008)11-2623-05
In the present report, the authors for the first time described the characteristics of taxol-induced paraptosis-like for the human lung adenocarcinoma cells (ASTC-a-1). CCK-8 was used to assay the inhibition of taxol on the cells viability. Cell viability was inhibited obviously 24 h after taxol treatment. Confocal fluorescence scanning microscope was used to monitor the morphology changes in cells with taxol treatment. Fluorescence resonance energy transfer (FRET) and acceptor photobleaching techniques were used to analyze the caspase-3 activation in the taxol-induced cell swelling and cell dearth. Taxol induced cell swelling, cytoplasmatic vacuolization and cell death without cell shrinkage, an apoptotic feature, and membrane rupture, a necrotic feature. The emission spectra of scat3 inside living cells expressed stably with scat3 were the same for control (without taxol). Further analysis with FRET and acceptor photobleaching techniques showed that the caspase-3 was not activated by taxol for the cytoplastic vacuoliazation cells expressed stably with scat3 plasmid, suggesting that caspase-3 is not involved in the taxol-inducecd cell swelling, cytoplasmatic vacuolization and cell death. These results show that taxol can induce a novel nonapoptotic PCD resembling the paraptosis in ASTC-a-1 cells.
2008 Vol. 28 (11): 2623-2627 [Abstract] ( 2005 ) PDF (974 KB)  ( 493 )
2628 Simultaneous Determination of 1-Naphthol and 2-Naphthol in Water by Spectrofluorimetry
ZHOU Chun1,WANG Qiong-e2,ZHUANG Hui-sheng1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2628-05
A simple and sensitive method for the simultaneous determination of trace amounts of 1-naphthol and 2-naphthol by fluorescence spectrofluorimetry was established based on the fact that the excitation and emission wavelengths are different between 1-naphthol and 2-naphthol. The influencing factors, such as pH temperature and surface activator were synthetically considered in the present paper. Interference of similar organic matters and inorganic ions were also taken into account. Compared with traditional methods, the method discussed here needs no complex pretreatments and expensive equipment. So it is convenient, quick and cheap yet with a satisfactory precision and accuracy. The accuracy and precision of results obtained are satisfactory when the concentration ratio (CR) of 1-naphthol to 2-naphthol is in the range of 1:19-19:1; the detection limit (DL) of both naphthols is 8.6×1 0-3 ng·mL-1; the relative standard deviation (RSD) of 1-naphthol and 2-naphthol is 1.26% and 1.45% respectively; and the recovery ratio (RR) of both naphthols is between 95% and 105%. This proposed method has been applied to the determination of trace amounts of 1-naphthol and 2-naphthol in the man-made sample water and environmental imitative water simultaneously, and obtained a satisfactory result, showing that the method discussed here is simple, sensitive and reliable in the future use.
2008 Vol. 28 (11): 2628-2632 [Abstract] ( 2293 ) PDF (866 KB)  ( 489 )
2633 Detection of Singlet Oxygen and Superoxide Anion with the Fluorescence of FCLA
WEI Yan-chun,LUO Shi-ming*,XU Wei
DOI: 10.3964/j.issn.1000-0593(2008)11-2633-03
Reactive oxygen species (ROS) plays a major role in various life systems and is critical in understanding the mechanisms of photodynamic therapy (PDT), seed vigour and plant stress, and so on. Researchers have dedicated much effort for detecting singlet oxygen and suqeroxide anion. FCLA (the fluoresceinyl cypridina luciferin analog) is a singlet oxygen and superoxide anion specific chemiluminescence probe. Typical chemiluminescence signal is relatively weak and its detection at single cell level is rather difficult. In the present study, the fluorescence of FCLA at 515 nm was investigated and was found to increase significantly during the ROS oxidative reaction. With fluorescence imaging technique, ROS can be detected by evaluating the spatial distribution and the dynamic changes in FCLA fluorescence. The technique is proved to have high sensitivity and excellent signal-to-noise ratio compared to direct CL measurement. With minimal cytotoxicity and excellent ROS selectivity, the FCLA fluorescence imaging technique can be a powerful new means in real-time in vivo and in situ single oxygen detection at the single cell level.
2008 Vol. 28 (11): 2633-2635 [Abstract] ( 1810 ) PDF (749 KB)  ( 441 )
2636 Two-Photon Excitation Fluorescence of 5-ALA Induced PpIX in DHL Cells
HUANG Zu-fang1,CHEN Rong1*,LI Yong-zeng1,CHEN Guan-nan1,CHEN Xian-ling2,FENG Shang-yuan1, JIA Pei-min3
DOI: 10.3964/j.issn.1000-0593(2008)11-2636-04
Two-photon fluorescence microscopy is a novel imaging technique, which is primarily sensitive to a specimen’s response coming from an in-focus plane, thus has low photo-bleaching and photo-damage to biological samples. 5-ALA induced production of PpIX in DHL cells was excited by 820 nm femtosecond laser; two-photon excitation fluorescence of single cell was obtained in Lambda mode of laser scanning confocal microscope. The specific fluorescence intensity of PpIX which accumulated in DHL cells was measured at 2,4 and 10 mmol·L-1 concentration of 5-ALA with different incubation time, which reflected the kinetics of 5-ALA accumulated in DHL cells. Accumulation of PpIX in DHL cells was a dynamic change process. Biphasic alterations of PpIX accumulation were noted: PpIX content enhanced with the increasing time and reached the maximal value around 3 h, however PpIX content decreased in the subsequent incubation time. Results indicate that two-photon fluorescence based on laser scanning microscope can be a useful technology for studying the kinetics of 5-ALA induced PpIX production in DHL cells and other leukemia cells.
2008 Vol. 28 (11): 2636-2639 [Abstract] ( 2199 ) PDF (693 KB)  ( 505 )
2640 Studies and Application of Fluorescence of Metacycline Enhanced by Synergetic Effect of β-Cyclodextrin and DBS
AO Deng-gaowa,SI Qin
DOI: 10.3964/j.issn.1000-0593(2008)11-2640-04
The fluorescence of metacycline enhanced by the synergetic effect of β-cyclodextrin with anion surfactant sodium dodecylbenzene sulfonate (DBS) was studied. It was found that the fluorescence intensity of metacycline was greatly enhanced in the system of β-CD-DBS. Based on this a new sensitive method for the determination of metacycline was established. The experiments indicated that MTC-β-CD-DBS can form 1∶1∶1 ternary inclusion complex with apparent stability constant of 1 294 L2·mol-2,respectively. The fluorescence intensity was linearly related to the metacycline concentration in the range of 1.7×10-7 to 8.8×10-5 mol·L-1 with a correlation coefficient of 0.996 6. The detection limit was 7.4×10-9 mol·L-1 this method was satisfactorily applied to the determination of metacycline in pharmaceutical preparations. The recovery was within the range of 95% to 106%.
2008 Vol. 28 (11): 2640-2643 [Abstract] ( 537 ) PDF (593 KB)  ( 477 )
2644 Study on Apparent Kinetics of Photocatalytic Oxidation Degradation Rhodamine B by Photo-Fenton Reaction
LI Hong1,2,ZHENG Huai-li1*,LI Xiao-hong2,XIE Li-guo1,TANG Xue3
DOI: 10.3964/j.issn.1000-0593(2008)11-2644-05
The Fenton process, mixed by hydrogen peroxide and iron salts with highly oxidative effect, is recognized as one of powerful advanced oxidation technologies available and can be used to destroy a variety of persistent organic pollutants. The oxidation power of Fenton reagent is due to the generation of hydroxyl radical (·OH) during the iron catalysed decomposition of hydrogen peroxide in acid medium. The hydroxyl radical with a high oxidation potential (2.8 eV) attacks and completely destroys the pollutants in Fenton process. The degradation of pollutants can be considerably improved by using sunlight radiation, which is due to the generation of additional hydroxyl radicals. This photo-Fenton process had been effectively used to degrade the pollutants. In this paper, the definite quantity of Fenton reagent was added in the definite concentration of Rhodamine B solution. The degradation reaction was carried out at pH 3.5 under natural sunlight. The factors influencing on photocatalytic oxidation degradation rate of Rhodamine B were studied following: the initial concentration of Rhodamine B, initial concentrateions of Fe2+ and H2O2. The orders of degradation reaction were obtained by solving exponential kinetics equations of curve fitting, thereby gaining the kinetic parameters and reaction dynamics equation of the reaction system. The research contents included mainly: the UV-Vis spectra of Rhodamine B solution, the concentration-absorbency work curve of Rhodamine B solution, the analysis of the reaction system at various initial Rhodamine B concentrations, the analysis of the reaction system at various initial Fe2+concentrateions, the analysis of the reaction system at various initial H2O2 concentrations, and the calculation of the apparent kinetics parameters in reaction dynamics equation. The reaction dynamics equation from experiments was constructed: V=5×10-9P1.28F0.366E0.920, and overall reaction order was 2.57.
2008 Vol. 28 (11): 2644-2648 [Abstract] ( 652 ) PDF (870 KB)  ( 519 )
2649 Study on the Degradation of Phenol Wastewater Using Hydroxyl Radical Produced by Plasma and the Course by UV Spectra
YANG Xian-li, BAI Min-dong, HAN Feng, GU Jian-long
DOI: 10.3964/j.issn.1000-0593(2008)11-2649-04
The phenol wastewater with high concentration was treated by hydroxyl radical produced by a strong ionization discharge plasma in the present article. Salicylic acid used as molecular probe to determine the concentration of hydroxyl radical. The phenol elimination efficiency of wastewater whose initial concentration was 1 21 5 mg·L-1 could reach 99.11% when the concentration of hydroxyl radical was 1 037 mg·L-1; while the initial concentration of 8 853 mg·L-1 of phenol wastewater dropped to 6 250 mg·L-1 under the same conditions, that is, 1 mg hydroxyl radicals could oxidize 2.5 mg of phenol. The smaller the initial phenol concentration, the higher the removal. However, the higher the initial concentration, the greater the absolute quantity of treatment. And the relation between the changes including pH value and the conductivity and the concentration of hydroxyl radical was stated and explained. With the concentration of hydroxyl radicals increasing, the pH value of wastewater changed from close to neutral to acidity gradually. The higher the concentration of hydroxyl radical, the stronger the acidity of wastewater. When continuing the increase in the concentration of hydroxyl radical, the change began to smooth. With the addition of hydroxyl radical, as is different from other phenomena, there was a tiny descending stage before ascending as shown on the conductivity curve, indicating that phenol had been oxidized and generated the organic acids continuously. Catechol, hydroquinone and benzoquinone are the important compounds of the intermediate products as shown by the analysis of UV spectra and chromatography. The final UV spectra curve indicated that there were little organic compounds containing conjugated structure in the treated wastewater.
2008 Vol. 28 (11): 2649-2652 [Abstract] ( 2144 ) PDF (810 KB)  ( 534 )
2653 Immunonanogold Catalytic Spectrophotometric Determination of Trace Complement 3
HUANG Wen-xin1,JIANG Zhi-liang1, 2*,LIANG Ai-hui2
DOI: 10.3964/j.issn.1000-0593(2008)11-2653-03
Gold nanoparticles about 10 nm in size were prepared by improved trisodium citrate reduction procedure, and were used to label goat anti-human C3 to obtain a sensitive spectral probe for complement 3 (C3) in the condition of pH 7.5. The immune reaction between nanogold-labeled C3 antibody (anti-C3) and the antigen C3 took place to form the nanogold immune complex in pH 5.6 Na2HPO4-C6H8O7 buffer solution and in the presence of polyethylene (PEG). The optimal immunoreaction conditions were pH 5.6-9.7 μg·mL-1 nanogold-labeled anti-C3, 6.0% PEG 6000 and incubation time 15 min under ultrasonic irradiation. After centrifuging for 10 min at 12 000 r·min-1, the excess nanogold-labeled anti-C3 in the upper solutions was obtained, and was used to catalyze the colored particle reaction between HAuCl4 and NH2OH·HCl to produce gold particles with bigger size. The influence on the immunonanogold catalytic reaction was considered spectrophotometrically. A pH 2.97 Na3C6H5O7-HCl buffer solution, 53.33 μg·mL-1 HAuCl4, 74.13 μg·mL-1 NH2OH·HCl, and reaction time of 3 min at 37 ℃ water bath were chosen for use. Results demonstrated that with increasing C3, the concentration of gold labeled anti-C3 in the upper solution decreased, and the absorbance decreased linearly. Linear relationships between the decreased absorbance and the C3 concentration in the range of 0.025-0.60 ng·mL-1 were obtained by spectrophotometry at 760 nm. The regress equation was ΔA760 nm=0.276c+0.025 4, the correlation coefficient was 0.990 3, and the detection limit reached 0.007 2 ng·mL-1 of C3. The influence of foreign substances such as HAS, BSA, and ammonia acid on the determination of 0.2 ng·mL-1 of C3 was examined. Results showed that this assay has high selectivity. The sensitive, rapid and highly specific assay was applied to the quantification of C3 in human sera, with satisfactory results.
2008 Vol. 28 (11): 2653-2655 [Abstract] ( 272 ) PDF (573 KB)  ( 431 )
2656 Determination of Dextran Sulfate Sodium with Ethyl Violet by Resonance Rayleigh Scattering
WANG Xiao-zhou1,2,LI Nian-bing1,LUO Hong-qun1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2656-04
In the Britton Robinson buffer medium (pH 9.0-10.5), either dextran sulfate sodium (DSS) or ethyl violet (EV) showed very faint resonance Rayleigh scattering (RRS) spectra. However, when DSS and EV were mixed together, the interaction between DSS and EV by virtue of electrostatic and hydrophobic forces occurred, which greatly enhanced the RRS intensity and a new RRS spectrum for the DSS-EV system appeared with three obvious scattering wavelengths at 348.0, 509.8 and 680.0 nm, respectively. All these RRS peaks increased with the increase in DSS concentration. The maximum scattering wavelength appeared at 509.8 nm; and therefore was selected as the determination wavelength for the system. The RRS intensity was directly proportional to the concentration of DSS in the range of 0.005-2.4 μg·mL-1, and the detection limit was 3.25 ng·mL-1. The characteristics of RRS and absorption spectra of the DSS-EV system, the influencing factors, such as solution pH, EV concentration, reaction time, temperature, and ion strength, and the optimum conditions for the reaction were investigated. The influence of foreign substances on the DSS-EV system was also studied. The method was sensitive and selective, and has been applied to the determination of DSS in synthetic samples with satisfactory results.A new method for the determination of trace amounts of DSS based on the RRS method has been developed.
2008 Vol. 28 (11): 2656-2659 [Abstract] ( 343 ) PDF (829 KB)  ( 401 )
2660 Measurement of Steel Corrosion in Concrete Structures by Analyzing Long-Period Fiber Grating Spectrum Character
WANG Yan1,2,LIANG Da-kai1*,ZHOU Bing1
DOI: 10.3964/j.issn.1000-0593(2008)11-2660-05
The consideration on the durability of concrete structures with reinforcement corrosion has become a most urgent problem. A new technique to measure the corrosion of steel in concrete structures was proposed in the present paper. It is based on the microbending characteristic of long period optical grating (LPFG). The temperature spectum character and curvature spectrum character of long period optical fiber grating were studied first. It was shown that the transmission spectrum of long period optical fiber grating shifted right and the transmission of the resonance wavelength was invariable when the temperature increased, while the transmission spectrum of long period optical fiber grating became shallow when the curvature increased, the transmission of the resonance wavelength would increase and it was linear with the curvature. On the basis of the characteristic, a notch shaped pedestal was designed and a long period optical fiber grating was laid on the steel surface. With this method the radial expansion of the steel resulting from the steel corrosion would translate into the curvature of the long period optical fiber grating. The curvature of long period optical fiber grating could be obtained by analyzing the change of spectrum, and then the steel corrosion depth could be measured. This method is simple and immediate and is independent of the variety in temperature, strain and refractive index owing to the inimitable spectrum characteristic of long period optical fiber grating. From the experiment it was found that the precision of the corrosion depth was better than 1.2 μm, and the corrosion depth of 3 mm could be achieved. This measurement could be used to monitor the early to metaphase corrosion of reinforcing steel in concrete structures.
2008 Vol. 28 (11): 2660-2664 [Abstract] ( 2384 ) PDF (1040 KB)  ( 511 )
2665 Determination of Heavy Metals for RoHS Compliance by ICP-OES Spectrometry Coupled with Microwave Extraction System
HUA Li1,2,WU Yi-ping1*,AN Bing1,LAI Xiao-wei1
DOI: 10.3964/j.issn.1000-0593(2008)11-2665-06
The harm of heavy metals contained in electronic and electrical equipment (EEE) on environment is of high concern by human. Aiming to handle the great challenge of RoHS compliance, the determinations of trace or ultratrace chromium (Cr), cadmium (Cd), mercury (Hg) and lead (Pb) by inductively coupled plasma optical emission spectrometry (ICP-OES) was performed in the present paper, wherein, microwave extraction technology was used to prepare the sample solutions. In addition, the precision, recovery, repeatability and interference issues of this method were also discussed. The results exhibited that using the microwave extraction system to prepare samples is more quick, lossless, contamination-free in comparison with the conventional extraction methods such as dry ashing, wet-oven extraction etc. By analyzing the recoveries of these four heavy metals over different working time and wavelengths, the good recovery range between 85% and 115% showed that there was only tiny loss or contamination during the process of microwave extraction, sample introduction and ICP detection. Repeatability experiments proved that ICP plasma had a good stability during the working time and the matrix effect was small. Interference was a problem troublesome for atomic absorption spectrometry (AAS), however, the techniques of standard additions or inter-element correction (IEC) method can effectively eliminated the interferences of Ni, As, Fe etc. with the Cd determination. By employing the multi-wavelengths and two correction point methods, the issues of background curve sloping shift and spectra overlap were successfully overcome. Besides, for the determinations of trace heavy metal elements, the relative standard deviation (RSD) was less than 3% and the detection limits were less than 1 μg·L-1(3σ, n=5)for samples, standard solutions, and standard additions, which proved that ICP-OES has a good precision and high reliability. This provided a reliable technique support for electronic and electrical (EE) industries to comply with RoHS directive.
2008 Vol. 28 (11): 2665-2670 [Abstract] ( 2008 ) PDF (1305 KB)  ( 512 )
2671 Application of ICP-AES to Detection of Inorganic Elements in Roots Bleeding Sap from Maize and Soybean Plants
DUAN Liu-sheng,ZHANG Ming-cai,DONG Xue-hui,TIAN Xiao-li,LI Zhao-hu
DOI: 10.3964/j.issn.1000-0593(2008)11-2671-03
The constituents of the roots bleeding sap are an important index characteristic of roots activity and roots-shoots relationship. To compare the differences between the constituents of roots bleeding sap from maize and soybean plants, roots bleeding saps were collected from maize (Zea mays L. cultivar 3138) and soybean [Glycine max (L.) Merr. cultivar Ludou 11] plants at different growth and development stages under field condition, and the inorganic elements were determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). The results indicated that both the constituents of inorganic elements and flow intensities were various between roots bleeding saps from maize and soybean plants at different growth and development stages. The flux of inorganic elements in roots bleeding sap showed different trends with progress in plants growth and development. In the roots bleeding sap from maize, the predominant inorganic elements were K,Ca,Mg,P,Na, Si,Zn,Mn and Fe, with flux ranging from 1 to 1 851.5 μg·h-1·plant-1. The flux of B,Cu and Mo was relatively lower and less than 1 μg·h-1·plant-1,while none of the elements of Co,Cd,Ba,Pb,Sr and As could be detected, and was estimated to be lower than 0.01 μg·h-1·plant-1 based on the detection limit. The flow of most inorganic elements showed decreasing trends with plant development progressing from booting to grain filling stage. In the roots bleeding sap from soybean, Ca,Mg,K,P,Na,Zn,Mn,Fe and Cu were found as predominant inorganic constituents, ranging from 1 to 1 158 μg·h-1·plant-1. The flow of both B and Mo was found lower than 1 μg·h-1·plant-1,and none of Si,Co,Cd,Ba,Pb,Sr and As could be found. With the growth and development,different inorganic elements showed various changing pattern.
2008 Vol. 28 (11): 2671-2673 [Abstract] ( 2445 ) PDF (357 KB)  ( 479 )
2674 Determination of Total Mass and Morphology Analysis of Heavy Metal in Soil with Potassium Biphthalate-Sodium Hydroxide by ICP-AES
QU Jiao1,2,YUAN Xing1*,CONG Qiao2,WANG Shuang2
DOI: 10.3964/j.issn.1000-0593(2008)11-2674-05
Blank soil was used as quality controlling samples, soil sample dealt by potassium biphthalate-sodium hydroxide buffer solution was used as check sample, mixed acid HNO3-HF-HClO4 was chosen to nitrify soil samples, and plasma emission spectrometer (ICP-AES) was used as detecting method. The authors determined the total metal mass of Mo, Pb, As, Hg, Cr, Cd, Zn, Cu and Ni in the extracted and dealt soil samples, and determined the mass of Mo, Pb, As, Hg, Cr, Cd, Zn, Cu and Ni in the three chemical morphologies, including acid extractable morphology, oxide associated morphology, and organics associated modality. The experimental results indicated that the different pH of potassium biphthalate-sodium hydroxide buffer solution had obvious influence on the total mass of heavy metal and morphology transformation. Except for metal element Pb and Zn, the addition of different pH potassium dihydrogen phosphate-sodium hydroxide buffer solution could accelerate the soil samples nitrification and the total mass determination of heavy metal in the soil samples. The potassium biphthalate-sodium hydroxide buffer solution could facilitate the acid extractable morphology of Cr, Cu, Hg and Pb, oxidation associated morphology of As, Hg, Pb and Zn and the organic associated morphology transforming of As and Hg. At pH 5.8, the maximum acid extractable morphology contents of Cu and Hg were 2.180 and 0.632 mg·kg-1,respectively;at pH 6.2,the maximal oxidation associated morphology content of Pb could achieve 27.792 mg·kg-1;at pH 6.0,the maximum organic associated morphology content of heavy metal Hg was 4.715 mg·kg-1.
2008 Vol. 28 (11): 2674-2678 [Abstract] ( 2222 ) PDF (457 KB)  ( 445 )
2679 Determination of Trace Elements in Mongolian Medicine Zidianling Curing Allergic Purpura Disease by ICP-AES
E Er-deng-sang1,HANG Gai-ba-te-re2,BA Tu1
DOI: 10.3964/j.issn.1000-0593(2008)11-2679-05
During the study of the Mongolian medicine Zidianling, the authors found that the Mongolian medicine Zidianling contains great amount of trace elements in which human-body-needed trace elements are fairly much but the heavy metals are very little. A method using ICP-AES with microwave digestion was studied for the determination of 15 elements including Ca, Mg, Sr, Fe, Mn, Zn, Cu, Pb, etc. in Mongolian medicine-Zidianling. The major function of this medicine is clearing away heat and removing toxic substances, and cooling blood to stop bleeding. To explain the Zidianling’s clinical effects, the authors chose 260 allergic purpura patients with 140 male and 120 female. The youngest was 6 years old, the oldest was 62 years old. Most of patients were between 6 and 16, accounting for nearly 90%. The results of clinical effects show that 234 patients were cured, roughly 90% of the total number Thirteen patients showed obvious effects (5% of the total number) and 11 had effective cures of illnesses (4.23% of the total number). Two patients had no cures of illnesses (0.77% of the total number). And the integrated effective rate may reach 99.23%. The results show that Mongolian medicine Zidianling has great amount of trace elements and its Sr content is different from other Mongolian medicines and is especially high. The recoveries of standard addition are in the range of 94.63%-106.40%. The relative standard deviation RSD≤3.17%, and the detection limit is in the range of ≤0.009 μg·mL-1.
2008 Vol. 28 (11): 2679-2683 [Abstract] ( 2294 ) PDF (488 KB)  ( 449 )
2684 Investigation of Enhancing Effect for Hydride Generation-Atomic Fluorescence of Transition Metal Elements
SUN Han-wen1,SUO Ran1,2
DOI: 10.3964/j.issn.1000-0593(2008)11-2684-07
A mechanism of hydride generation based on disassembly reaction of hydrogen-transferred interim state [M(BH4)m]* was developed by investigating the effect of reaction medium acidity on hydride generation. The effects of Co2+ and Ni2+,phenanthroline and 8-hydroxyquinoline on hydride generation-atomic fluorescence signals of Zn, Cd, Cu and Ni were studied, respectively, and their enhancing mechnism was discussed. The enhancing effect Co2+ and Ni2+ on the fluorescence signals of Zn and Cd was due to the increase in transmission efficiency of hydride of Zn and Cd. There was a synergic enhancing effect between phenanthroline or 8-hydroxyquinoline and Co2+ on the fluorescence signals of Zn and Cd, however no synergic enhancing effect between phenanthroline and 8-hydroxyquinoline on the fluorescence signals of Zn and Cd. The simulative action of cationic surfactant, anion surfactant and non-ionic surfactant surfactant to hydride generation was investigated. It is shown that both cationic surfactant and non-ionic surfactant have obvious enhancing effect on the fluorescence signals of analytes because of the decrease in surface tension of reaction solution. The release characteristics of hydride from the absorption solution containing surfactant was ulteriorly examined by using graphite furnace atomic absorption spectrometry, and the mechanism of enhancing effect of surfactant on hydride generation and transmission was proposed.
2008 Vol. 28 (11): 2684-2690 [Abstract] ( 4582 ) PDF (1637 KB)  ( 771 )
2691 Determination of Total Arsenic and Mercury in the Fucoidans by Hydride Generation Atomic Fluorescence Spectroscopy
LIU Yi-xiang,WU Yong-pei*,WANG Li,HUANG Zhi-yong
DOI: 10.3964/j.issn.1000-0593(2008)11-2691-04
In the present article, the method of high pressure microwave digestion and hydride generation atomic fluorescence spectroscopy (HG-AFS) was used for the determination of total arsenic and mercury in fucoidans, and the detecting conditions were optimized, including instrument working parameters, such as atomic temperature, lamp current, high voltage of PMT etc, and the conditions of hydride generation, such as the acid concentration of loading fluid, speed of carrying gas, the concentration of KBH4 etc. The result shows that there are good linear relations between fluorescence intensity and the concentrations of arsenic and mercury where their concentrations are 0-200 μg·L-1 and 2.0-10.0 μg·L-1,respectively, and the related coefficient of arsenic is 0.999 9 and that of mercury’s is 0.999 8. The blanks of samples were detected constantly (n=10), and the detection limit of this method is 0.173 ng·kg-1 for total arsenic and 0.012 2 ng·kg-1 for mercury. In order to do precise analysis, the samples were detected constantly (n=8), and the relative standard deviations (RSDs) of arsenic and mercury are 1.09% and 1.69%, severally. The quantitative arsenic and mercury were added into the samples before they were digested, and the recovery range is 93.31%-100.9% for arsenic and 91.21%-106.1% for mercury. The contents of total arsenic and mercury in fucoidans before desalted by ultrafiltration are 2.78 mg and 0.125 mg·kg-1,respectively. Nevertheless, the contents of total arsenic and mercury in fucoidans desalted by ultrafiltration are 2.26 mg·kg-1 and 0.119 mg·kg-1,severally.
2008 Vol. 28 (11): 2691-2694 [Abstract] ( 1678 ) PDF (589 KB)  ( 472 )
2695 A Flow Injection On-Line Unequal Flow Complexation Preconcentration Procedure Coupled with Flame Atomic Absorption Spectrometry for Determination of Lead in Tap Water
WANG Zhong-yuan,SU Yao-dong*,LI Shuang, GAN Li-hua
DOI: 10.3964/j.issn.1000-0593(2008)11-2695-04
A simple, environmentally friendly, cost-effective, and sensitive method was developed for the determination of trace lead in tap water by flow injection (FI) on-line unequal flow complexation preconcentration procedure coupled with flame atomic absorption spectrometry (FAAS). Compared with conventional preconcentration method, the unequal flow complexation preconcentration procedure, increased the flow rate of sample while decreased the flow rate of complexing agent. The new method decreased the dilution effect of sample caused by the chelating agent, increased the sorption preconcentration effect, and increased the enhancement factor. The decrease in the flow rate of chelating agent will not result in a deficient complex formation because the concentration of APDC is much higher than that of the sample’s. Compared with other sorption preconcentration methods, such as, multiplexed sorption preconcentration procedure, the unequal flow complexation preconcentration procedure need not to prolong the preconcentration time, but received even better results. Taking lead as a model element, ammonium pyrrolidine dithiocarbamate (APDC) as the chelating agent, and ethanol as the eluent, the proposed FI on-line KR unequal flow complexation preconcentration procedure was coupled with FAAS for the determination of trace lead in tap water. With a sample loading flow rate of 10.4 mL·min-1 and preconcentration time of 60 s, the enhancement factor increased from 30 (conventional equal flow complexation preconcentration procedure) to 59 (unequal flow complexation preconcentration procedure), the detection limit (3σ) of 5.6μg·L-1 was obtained at a sampling frequency of 40 samples·h-1. The relative standard deviations (n=11) were found to be 2.1% at the level of 0.5 mg·L -1. The recovery ranged from 98.5% to 102%. The proposed method has been successfully applied to the determination of lead in tap water samples.
2008 Vol. 28 (11): 2695-2698 [Abstract] ( 1150 ) PDF (723 KB)  ( 468 )
2699 Comparative Study on Trace Elements in Elsholtzia bodineri Vaniot. from Honghe by FAAS
ZHANG Ju-cheng, LIU Wei*,YI Zhong-zhou, QIU Cheng-shu, LI Ying, YAN He-ping
DOI: 10.3964/j.issn.1000-0593(2008)11-2699-04
In the present paper, the authors prepared all the samples by the same method, and optimized the work conditions for flame qtomic absorption spectrometry. FAAS was applied to determine the trace elements, such as Pb, Cr, Cd, Cu, Zn, Hg, Se etc, in Elsholtzia bodineri Vaniot. from Mengzi, Shiping, Mile and Jianshui located in Honghe state. The method is simple, rapid and accurate, and allows simultaneous determination of many elements. The recoveries were in the range of 98.7%-116.4%,and RSD was 0.07%-1.69%. The contents of Pb, Cd and Hg were 53.47, 6.03 and 7.68 μg·g-1,respectively, in the sample from Jianshui, and were higher than those from other areas. The content of Mn was the highest, and was higher in Mengzi than in other areas, and the average content in the four samples was 913.48 μg·g-1,which was higher than the content in the soil. Fe is the semi-microelement whose average content in Elsholtzia bodineri Vaniot. from Honghe was 688.46 μg·g-1,the high-to-low content sequence of Fe in terms of location was Mengzi, Mile, Shiping and Jianshui. The average content of Zn was 116.64 μg·g-1,and the highest one was from Shiping. But we did not obtain the data of Se in the Elsholtzia bodineri Vaniot. from Honghe state by AAS, and did not detect Hg in samples from Shiping and Mile. The content of the detected elements in Mengzi’s sample had the sequence as follows; Mn>Fe>Zn>Pb>Cu>Cr>Cd>Hg>Se, while the sequence was Mn>Fe>Zn>Pb>Cu>Hg>Cd>Cr>Se in the sample of Jianshui, Mn>Fe>Zn>Pb>Cu>Cd>Cr>Hg>Se in Shiping, and Fe>Mn>Zn>Pb> Cu>Cd> Cr>Hg>Se in Mile. The results show that the content of the trace elements is high, especially, Mn, Fe and Zn, in Elsholtzia bodineri Vaniot. in Honghe. Therefore, Elsholtzia bodineri Vaniot., which can be used as drug or beverage, is worth exploitation.
2008 Vol. 28 (11): 2699-2702 [Abstract] ( 2384 ) PDF (467 KB)  ( 450 )
2703 Determination of Major Elements in Superphosphate by X-Ray Fluorescence Spectrometry
RUI Yu-kui1,LI He2,SHEN Jian-bo1,ZHANG Fu-suo1*
DOI: 10.3964/j.issn.1000-0593(2008)11-2703-03
Phosphate fertilizer is one of the most important fertilizers. The authors determined nine kinds of major elements in superphosphate, the most important phosphate fertilizer, by X-ray fluorescence spectrometry. The detection range of SiO2,Al2O3,TFe2O3,MnO, MgO, CaO, Na2O, K2O and P2O5 is 15.0%-90.0%, 0.20%-25.0%, 0.20%-25.0%, 0.01%-0.35%, 0.20%-40.0%, 0.10%-35.0%, 0.10%-7.50%, 0.05%-7.50% and 1.00%-100.00% respectively, and the precision of the method for SiO2,Al2O3,TFe2O3,MnO, MgO, CaO, Na2O, K2O and P2O5 range from 0.20% to 0.005%, so the method of X-ray fluorescence spectrometry is a fast and effectual method for detecting the composition of phosphate fertilizer. The contents of the above elements showed (1) the detected superphosphate content is 18.101% of P2O5,which is accordant to the labeled level (≥16%); (2) the detected superphosphate contains much SiO2,TFe2O3,MgO, CaO and K2O, which are necessary for plant growth and the content of which is 16.954%, 1.495%, 1.580%, 21.428% and 1.585% respectively. These data showed that phosphate fertilizer sometimes can supply some trace elements for plants, but we should eliminate the interference effect of these elements when we research the role of phosphorus; (3) superphosphate contains 3.225% of Al2O3,so the authors should attention to the aluminium poison when superphosphate is used chronically.
2008 Vol. 28 (11): 2703-2705 [Abstract] ( 1235 ) PDF (348 KB)  ( 512 )
2706 Determination of Major Elements in Soil from Cancer Village by X-ray Fluorescence Spectrometry
WEI Zhen-lin1,LI He2,RUI Yu-kui3*
DOI: 10.3964/j.issn.1000-0593(2008)11-2706-02
Many social problems arise from environmental pollution, cancer village is one of the many important problems caused by pollution. The authors selected a typical cancer village where 80-100 people died of cancer in the last five years, but there are only a total of 1 200 people in this village. The authors sampled soils from crops-planted areas and detected the major elements by X-ray fluorescence spectrometry. The results showed that the contents of SiO2, TiO2, Al2O3, Fe2O3, MnO, MgO, CaO, Na2O, K2O and P2O5 in soil of this village were 66.05%, 0.66%, 11.37%, 3.93%, 0.075%, 1.97%, 5.47%, 1.90%, 2.11% and 0.20% respectively; with the precision being ±0.20%, ±0.005%, ±0.10%, ±0.10%, ±0.005%, ±0.05%, ±0.04%, ±0.08%, ±0.02% and ±0.005% respectively, which showed that X-ray fluorescence spectrometry is a good method.
2008 Vol. 28 (11): 2706-2707 [Abstract] ( 1344 ) PDF (278 KB)  ( 530 )
2708 A Microfabricated ICP Source Base on Planar Spiral-Shaped Coil
WANG Yong-qing1,2,LOU Jian-zhong1,SUN Rong-xia1,MA Wen3,TANG Yu-jun1,PU Yong-ni1
DOI: 10.3964/j.issn.1000-0593(2008)11-2708-05
Along with the development of micro-electromechanical system technology, the reports on the optical splitting systems and the photoelectric detection systems of spectrometer based on micro-electromechanical system have become increasingly popular, whereas the reports on micro excitation source in the development of micro spectrometer are few. In other words, the development of micro excitation source is the most important part in the development of the micro spectrometer. A novel low-pressure microfabricated inductively coupled plasma source is introduced, which is an emission spectrum excitation source based on surface-micromaching technology. Its radio frequency power consumption is much lower than the general inductively coupled plasma source. The source can work at an argon gas pressure of 100 Pa, and thus consumes less argon. The principle of operation for a microfabricated inductively coupled plasma source is illustrated. The layout of the planar spiral-shaped coil, the matched capacitor and the resonant capacitor is given. The fabrication process and properties of the plasma source are described. Meanwhile a novel inductively coupled plasma based on the technology of printed circuit board is introduced. In the experiment, the planar spiral-shaped coil and interdigatial capacitor were used. When the pressure of argon was 100 Pa and the radio frequency power was 3.5 W at 13.56 MHz the novel inductively coupled plasma was ignited. The photo of the argon ignition is given. Finally the potential application of the micro inductively coupled plasma in spectrometers is presented.
2008 Vol. 28 (11): 2708-2712 [Abstract] ( 2275 ) PDF (1193 KB)  ( 479 )
2713 Determination of Optical Parameters in Thin Films by Transmittance Spectra
WANG Keng1,JIA Hong-zhi1*,XIA Gui-zhen2
DOI: 10.3964/j.issn.1000-0593(2008)11-2713-04
The high tin-doped SiO2 films prepared by CVD will bring some crystals, but sol gel can control the accurate chemical component of the films. So it can produce high tin-doped materials. In the present paper, the tin-doped SiO2 films were prepared by a sol gel dip-coating process on glass substrates at concentrations of 66 mol% and 75 mol%. Then dipping was performed several times to enhance the thickness of the films. The transmittance spectrum was obtained by spectrophotometer. Compared with the films prepared in a thin film on a thick substrate previously, the model here has been modified to describe the transmittance of a thick film (substrate) sandwiched between two thin films (coating method). The authors used the curves method to calculate the film’s parameters. The result showed that uhe refractive index of different samples was increased with the wavelength. And the film thickness was about 900 nm.
2008 Vol. 28 (11): 2713-2716 [Abstract] ( 2527 ) PDF (644 KB)  ( 445 )
2717 Comparison of Two Methods to Solve AR Model Parameters of Line Shape Optimized Maximum Entropy Spectral Estimation
GAO Xiao-feng,XU Zhi-hai*
DOI: 10.3964/j.issn.1000-0593(2008)11-2717-04
Line shape optimized maximum entropy spectral estimation (LOMEE) is to remove the influence resulting from line shape by Fourier self-deconvolution and to model interferogram data in order to substitute AR model parameters for the spectral estimator. The proper calculation of AR model parameters in LOMEE is very important to the quality of recovered spectrum. Modified covariance method (MCOV) and Burg method were used to solve AR model parameters under different noise level. The simulation results of recovered spectrum were acquired with the two methods. The influences of AR order and signal-to-noise ratio on the simulation were compared. It is shown that MCOV is more excellent than Burg in LOMEE.
2008 Vol. 28 (11): 2717-2720 [Abstract] ( 2391 ) PDF (771 KB)  ( 396 )
2721 Superficial Bladder Cancer Detection Using Diffuse Reflectance Spectral Ratio R540/R575 of Oxygenated Hemoglobin Bands
WEI Hua-jiang1,XING Da1*,WU Guo-yong2,LU Jian-jun2,WU Rong-hai3,GU Huai-min1,HE Bo-hua4, CHEN Xue-mei5
DOI: 10.3964/j.issn.1000-0593(2008)11-2721-05
A low-cost, fast, and noninvasive method for early diagnosis of malignant lesions of mucosa tissue based on diffuse reflectance spectra was applied in the study of the optical biopsy of superficial human bladder cancer. In the present paper, differential diagnosis of superficial human bladder cancer was studied using the diffuse reflectance spectral ratio (R540/R575) of the oxygenated hemoglobin absorption bands at 540 and 575 nm in vitro. Diffuse reflectance spectra for mucosa/submucosa tissues of normal bladder and superficial bladder cancer were measured using a spectrophotometer with an integrating sphere attachment. The results of measurement showed that there were three the diffuse reflectance spectral dips at 415, 542 and 577 nm respectively for mucosa/submucosa tissues of normal bladder and superficial bladder cancer in the spectral range from 400 to 600 nm. The mean diffuse reflectance spectral ratio (R540/R575) of normal bladder mucosa/submucosa tissue decreased slowly with time increase after surgical excision, and the mean diffuse reflectance spectral ratio (R540/R575) of superficial bladder cancer mucosa/submucosa tissue also decreased slowly with time increasing after surgical excision. The mean diffuse reflectance spectral ratios (R540/R575) of normal bladder mucosa/submucosa tissue were 111%, 107%, 104% and 102% after 2, 3, 4 and 5 h after surgical excision respectively, and those of superficial bladder cancer mucosa/submucosa tissue were 98.4%, 95.5%, 93.1% and 91.6% after 2, 3, 4 and 5 h after surgical excision respectively. There were significant differences in mean diffuse reflectance spectral ratio (R540/R575) for mucosa/submucosa tissues between normal bladder and superficial bladder cancer after 2, 3, 4 and 5 h after surgical excision respectively(p<0.05). Differences in mean diffuse reflectance spectral ratio (R540/R575) for mucosa/submucosa tissues between normal bladder and superficial bladder cancer were 12.6%, 11.5%, 10.9% and 10.4% after 2, 3, 4 and 5 h after surgical excision respectively. It is obvious that pathological changes in bladder mucosa/submucosa tissues induced changes in the component and structure of the tissues, and especially quantitative changes in oxyhemoglobin and de-oxyhemoglobin of tissues obviously. Conclusion of the study provides a new method that can be applied to rapid, low-cost and noninvasive optical biopsy of superficial bladder cancer.
2008 Vol. 28 (11): 2721-2725 [Abstract] ( 2797 ) PDF (682 KB)  ( 518 )
2726 Optimizing Algorithm Design of Piecewise Linear Classifier for Spectra
LAN Tian-ge, FANG Yong-hua, XIONG Wei, KONG Chao, LI Da-cheng, DONG Da-ming
DOI: 10.3964/j.issn.1000-0593(2008)11-2726-04
Being able to identify pollutant gases quickly and accurately is a basic request of spectroscopic technique for envirment monitoring for spectral classifier. Piecewise linear classifier is simple needs less computational time and approachs nonlinear boundary beautifully. Combining piecewise linear classifier and linear support vector machine which is based on the principle of maximizing margin, an optimizing algorithm for single side piecewise linear classifier was devised. Experimental results indicate that the piecewise linear classifier trained by the optimizing algorithm proposed in this paper can approach nonolinear boundary with fewer super_planes and has higher veracity for classification and recognition.
2008 Vol. 28 (11): 2726-2729 [Abstract] ( 1321 ) PDF (759 KB)  ( 482 )
2730 Development of Multi-Target Multi-Spectral High-Speed Pyrometer
XIAO Peng, DAI Jing-min, WANG Qing-wei
DOI: 10.3964/j.issn.1000-0593(2008)11-2730-05
The plume temperature of a solid propellant rocket engine (SPRE) is a fundamental parameter in denoting combustion status. It is necessary to measure the temperature along both the axis and the radius of the engine. In order to measure the plume temperature distribution of a solid propellant rocket engine, the multi-spectral thermometry has been approved. Previously the pyrometer was developed in the Harbin Institute of Technology of China in 1999, which completed the measurement of SPRE plume temperature and its distribution with multi-spectral technique in aerospace model development for the first time. Following this experience, a new type of multi-target multi-spectral high-speed pyrometer used in the ground experiments of SPRE plume temperature measurement was developed. The main features of the instrument include the use of a dispersing prism and a photodiode array to cover the entire spectral band of 0.4 to 1.1 μm. The optic fibers are used in order to collect and transmit the thermal radiation fluxes. The instrument can measure simultaneously the temperature and emissivity of eight spectra for six uniformly distributed points on the target surface, which are well defined by the hole on the field stop lens. A specially designed S/H (Sample/Hold) circuit, with 48 sample and hold units that were triggered with a signal, measures the multi-spectral and multi-target outputs. It can sample 48 signals with a less than 10ns time difference which is most important for the temperature calculation.
2008 Vol. 28 (11): 2730-2734 [Abstract] ( 729 ) PDF (1178 KB)  ( 549 )