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2007 Vol. 27, No. 02
Published: 2007-02-26
 
       光谱学与光谱分析
209 The Microscopic Ordering and Macroscopic Disorder Spectra Analysis of X-Band Electronic Paramagnetic Resonance
WU Xue1,2,Edmund Howard3,Yuri Nesmelov3,David D Thomas3
The correlation time and S order parameter are two important parameters to characterize the moving and distribution of the spin labeled macromolecule. It is significant to determine them simultaneously by lineshape analysis with an appropriate physics model for EPR spectrum analysis. In the present paper, the microscopic ordering and macroscopic disorder model (MOMD) was adopted to simulate the X-band EPR spectra of spin label with axial symmetric magnetic tensors. The experimental parameters were measured, and the divergence between the real values and the empirical values was analyzed. For MOMD spectra the authors proposed a criteria to select the experimental parameters. With the selected parameters, the correlation time and the internal S order parameter could be obtained simultaneously. And the valid range determined by the recognition function is presented.
2007 Vol. 27 (02): 209-212 [Abstract] ( 2522 ) PDF (1024 KB)  ( 467 )
213 Multi-Spectral Thermometry Based on GA-BP Algorithm
SUN Xiao-gang, YUAN Gui-bin*,DAI Jing-min
Considering some defects of back-propagation neural network (BP), a new algorithm combining genetic algorithm (GA) with BP was described. The application of GA-BP to the data processing of multi-spectral thermometry was proposed. The simulation experiments, based on GA-BP algorithm and BP neural network respectively, show that the recognition precision of trained emissivity samples is ±5 K and ±10 K respectively, and that of untrained emissivity samples is ±10 K and ±20 K respectively. No matter GA-BP algorithm or BP neural network is used, in general, the recognition precision of trained emissivity samples is higher than that of untrained emissivity samples. The recognition precision of true temperature is lower near the edge of sample sets. The GA-BP algorithm was more efficient than the BP neural network in the true temperature measurement.
2007 Vol. 27 (02): 213-216 [Abstract] ( 1246 ) PDF (875 KB)  ( 549 )
217 A New Measurement Method of Time-Resolved Spectrum
SHI Zhi-gang, HUANG Shi-hua*,LIANG Chun-jun，LEI Quan-sheng
A new method for measuring time-resolved spectrum (TRS) is brought forward. Programming with assemble language controlled the micro-control-processor(AT89C51), and a kind of peripheral circuit constituted the drive circuit, which drived the stepping motor to run the monochromator. So the light of different kinds of expected wavelength could be obtained. The optical signal was transformed to electrical signal by optical-to-electrical transform with the help of photomultiplier tube (Hamamatsu 1P28). The electrical signal of spectrum data was transmitted to the oscillograph. Connecting the two serial interfaces of RS232 between the oscillograph and computer, the electrical signal of spectrum data could be transmitted to computer for programming to draw the attenuation curve and time-resolved spectrum (TRS) of the swatch. The method for measuring time-resolved spectrum (TRS) features parallel measurement in time scale but serial measurement in wavelength scale. Time-resolved spectrum (TRS) and integrated emission spectrum of Tb3+ in swatch Tb(o-BBA)3phen were measured using this method. Compared with the real time-resolved spectrum (TRS). It was validated to be feasible, credible and convenient. The 3D spectra of fluorescence intensity-wavelength-time, and the integrated spectrum of the swatch Tb(o-BBA)3phen are given.
2007 Vol. 27 (02): 217-219 [Abstract] ( 313 ) PDF (887 KB)  ( 537 )
220 Study of Collisional Broadening of Spectral Line by Optical-Optical Double Resonance
LIU Jing1，2,DAI Kang2,SHEN Yi-fan2*
The collisional broadening of the 21Σ＋→61Σ＋ line of NaK molecule was studied using the optical-optical double resonance technique. A single-mode diode laser was set to a particular 11Σ＋(v″，J″)→21Σ＋(v′，J′) transition. Another single-mode diode laser was then used to excite the molecule from 21Σ＋(v′，J′) level to the rovibrational level of 61Σ＋. The two laser beams counterpropagated through the cell. The broadening rate coefficient was determined from the slope of the total linewidth versus potassium density curve. The rate coefficient, kbr=(1.4±0.7)×10-8 cm3·s-1,was obtained. The collisional excitation transfer between rotational levels of the 21Σ＋ state[i.e., 21Σ＋(v＝8，J＝12)→21Σ＋(v＝8，J＝13，14)] was also investigated. The rates can be determined from the relative intensities of the main peak and satellite lines, combined with a rate equation model. The rates are 6.1×106 and 5.2×106 s-1 respectively.
2007 Vol. 27 (02): 220-222 [Abstract] ( 1631 ) PDF (1104 KB)  ( 536 )
223 Establishment and Melting of Charge Ordering in La0.3Ca0.7Mn1-xWxO3 System
CAI Zhi-rang1,GUO Huan-yin1,LIU Ning1，2,ZHANG Yu-heng2
Polycrystalline samples of La0.3Ca0.7Mn1-xWxO3 (0.00≤x≤0.15) were prepared by conventional solid-state reaction method. The influence of W doping at Mn site on the magnetic transition of La0.3Ca0.7Mn1-xWxO3 system was studied by the measurements of magnetization-temperature (M-T) curves，magnetization-magnetic intensity(M-H) curves, and ESR spectra. The results show that, with the increase in W doping amount, the magnetic transition of the system exhibits a complicated charge process, when the doping amount is 0.00≤x≤0.08, the charge-ordering(CO) phase exists in the system, AFM/CO states coexist below the transition temperature, and the charge-ordering temperature(Tco) goes up with the increase in W doping content; when x≥0.12, the charge ordering (CO) state of the system weakens and melts, and paramagnetism-ferromagnetism (PM-FM) transition exists at extremely low temperature.
2007 Vol. 27 (02): 223-227 [Abstract] ( 233 ) PDF (1019 KB)  ( 790 )
228 Emitting Characteristics and Carrier Composite Regions Variety of the Blend of Terbium Complex and Poly-N-Vinylcarbazole
CHENG Bao-mei1,DENG Zhen-bo1*,LIANG Chun-jun1,XU Deng-hui1,WANG Rui-fen2
A new rare earth complex TbGd(BA)6(bipy)2 was synthesized, which was used as an emitting material in electroluminescence. By doping with poly-N-vinylcarbazole(PVK), the stability and conductivity of terbium complex were improved. The photoluminescence of PVK, terbium complex and their blend indicated that energy transfer from PVK to terbium complex occurred. In the present paper, single-, double- and multi- layer devices were fabricated. In the double-layer devices, holes and electrons were recombined at the interface of emitting layer (EML) and electron transporting layer (ETL). With increasing the thickness of Alq3, especially at highly electric field, carrier composite region transferred closely to ETL. However, in multi-layer devices, carrier composite region was restricted at the interface of emitting layer and holes blocking layer (HBL) due to high HOMO level of BCP. Enhancing electric field, emission from terbium complex was getting saturation gradually and weak emission from PVK was observed. From the optimized multi-layer device, bright and green emission from terbium complex was obtained with the highest EL brightness of the device of 213 cd·m-2 at 13.5 V.
2007 Vol. 27 (02): 228-231 [Abstract] ( 1178 ) PDF (954 KB)  ( 764 )
232 Hydrothermal Preparation and Luminescence of LaF3∶Ce, Tb Nano-Sized Phosphor
ZHANG Mao-feng, MENG Jian-xin*,LIU Ying-liang, MAN Shi-qing
Green-emitting LaF3∶Ce, Tb phosphor nanoparticles were synthesized by a simple hydrothermal method and characterized by XRD, TEM and fluorescence spectra. The prepared samples had a hexagonal shape, fine size (30 nm), and high brightness under ultraviolet, and the structure of LaF3 remained unchanged after being doped with Ce3+ and Tb3+ ions. The blue Ce3+ emission centered at 261 nm is efficiently quenched in the samples of LaF3∶Ce, Tb, in which the dominant emission is in the green at 544 nm, originating from the doped Tb3+ ions’ transition of 5D4 to 7F5. Excitation spectra of the LaF3∶Ce, Tb, observed at 544 nm, consist of both contributions from Ce3+ and Tb3+ ions. There is energy transfer of Ce3+→Tb3+ in this system. The energy transfer mechanism was discussed. Above all, the phosphor nanoparticles have high photoluminescence intensity even without any calcination, about twice that of bulk materials prepared by high temperature solid synthesis, and the intensity is also stronger than calcined phosphor nanoparticles.
2007 Vol. 27 (02): 232-235 [Abstract] ( 1686 ) PDF (949 KB)  ( 784 )
236 Effect of PEG400 on the Luminescent Eu(BA)3/SiO2
ZENG Dong-ming1,LI Yan-hua1, 2,FU Chang-cheng1,LIU You-nian1,SHU Wan-gen1
Rare earth organic complexes combined with inorganic compounds can enhanced thermal stability, but inorganic compounds matrix has great influence on the luminescence characteristic of rare earth organic complexes. The luminescence characteristic of organic and inorganic compound material was improved by PEG doping in the material. Eu(BA)3/SiO2 and Eu(BA)3/PEG400-SiO2 were synthesized by Sol-Gel method. The result of luminescence analysis showed that the excitation spectra and emission spectra of Eu(BA)3 accorded with those of Eu(BA)3/SiO2 and Eu(BA)3/PEG400-SiO2, but the luminescence intensity of Eu(BA)3/SiO2 was improved by PEG 400-SiO2 in SiO2 gel. This was because PEG400 as a hard Lewis base, could be combined with rare earth ion and increase the luminescence intensity of Eu(BA)3. It was shown that the amount of PEG400 in Eu(BA)3/SiO2 had influence on luminescence intensity of Eu(BA)3, namely there was better luminescence intensity in Eu(BA)3/SiO2 with increment of the PEG400 addition, but when the amount of PEG400 exceeded 50 wt% of that of SiO2, the luminescnece intensity of Eu(BA)3 hardly increased. When the amount of PEG400 exceed 15 wt% of that of SiO2, PEG400 had little influence on the content of water and hydroxy in the matxix, as verified by IR spectrum. The surface characteristic of SiO2 gel was investigated by atomic force microscopy(AFM).
2007 Vol. 27 (02): 236-239 [Abstract] ( 250 ) PDF (1393 KB)  ( 489 )
240 Luminescence Properties of White LED Blue Light Conversion Materials
HAO Hai-tao1,ZHOU He-feng1,LIANG Jian1,LIU Xu-guang2,XU Bing-she1*
Using rare earth oxides as raw materials, yttrium aluminum garnets activated by cerium and gadolinium ions were prepared by high energy ball milling and solid-state reaction at 1 300 ℃. The crystal structures of the products were studied by XRD, and the luminescence characteristics of Ce ion and the influence of Gd ion were studied by emission and excitation spectra. The results indicated that the products were yttrium aluminum garnet crystals of cubic system, and they were excited by blue light chips effectively. The emission peak of phosphors could change among 530-560 nm by adjusting the mole density of doping ions. The red shift of emission spectra could be interpreted with the configuration coordination figure. White LEDs were fabricated by phosphor conversion. When electric current is 20 mA, and the working voltage is 3.5 V, the white light LED chromaticity coordinates are x=0.310 and y=0.323, the lumen efficiency is 26.131 m·W-1,the color rendering index is 81.8, and the color temperature is 6 605 K.
2007 Vol. 27 (02): 240-243 [Abstract] ( 1669 ) PDF (1687 KB)  ( 676 )
244 Study on Electro-Optical Performance of Frequency Driven Liquid Crystal Light Valve
HUANG Chong, LIU Ji, ZHOU Xue-ping, OUYANG Yan-dong
The electro-optical characteristic and principle of frequency-driven liquid crystal light valve were discussed and analyzed. Under different electric field frequency and certain AC voltage, the electro-optical characteristic of frequency-driven TB3639 liquid crystal light valve was measured. The results show that it can display gray scale in visible light region, and it can not only display black and white, but also can display different gray scale. The influence of frequency-driven way to the transmission spectrum change tendency of different wavelength in visible light is approximately same, which will avoid high chromatism in application. The new frequency-driven liquid crystal light valve can improve display quality of liquid crystal display device. It will develop new application of liquid crystal display device and has practical application value.
2007 Vol. 27 (02): 244-246 [Abstract] ( 1188 ) PDF (923 KB)  ( 649 )
247 Ion-Conducting Mechanism of Composite Polymer Electrolyte: An Emission FTIR Spectroscopy Study
XU Jin-mei, JIANG Yan-xia*,ZHUANG Quan-chao, ZENG Dong-mei, SUN Shi-gang
Solvent-free, composite electrolytes based on poly(ethylene oxide) (PEO) were prepared by using mesoporous silica SBA-15 with surface modification of (trimethylchlorosilane) as the filler. The samples were explored by emission FTIR spectroscopy at elevated temperatures. The results of emission FTIR spectra illustrated the dependence of crystalline PEO phase on temperature. On the basis of electrochemistry, SEM, and emission FTIR studies, the effect of inorganic filler on the ionic conductivity was analyzed, and a conclusion concerning the ion-conducting mechanism of composite polymer electrolyte was drawn. The exploratory experiments demonstrated that the emission FTIR spectroscopy is an important method to be applied in the study of lithium batteries.
2007 Vol. 27 (02): 247-249 [Abstract] ( 1184 ) PDF (910 KB)  ( 574 )
250 The Identification of Several Saturated Fatty Acids and Their Salts by Means of Infrared Spectrometry
LUO Man1,GUAN Ping1*,LIU Wen-hui2
It is considered that saturated fatty acids and their salts may be potential hydrocarbon-generation matters in carbonate rocks. However, there is no effective method to distinguish them from natural sediments, making recognizing their distribution in sediments a challenge. Formic acid, acetic acid, stearic acid, calcium formate, calcium acetate, magnesium acetate, calcium stearate, and magnesium stearate from some chemical plants were investigated by means of Fourier transform infrared spectroscopy. Their infrared spectra were obtained and the distinctions of the infrared spectra between saturated fatty acids and their salts were studied in detail. The differences in the group’s electron-releasing ability, molecular reduced mass, ion configuration and the length of carbon chain can cause wavelength shifts of infrared absorption peaks of the saturated fatty acids and their salts. The research provides a method for the identification of saturated fatty acids and their salts in samples from nature.
2007 Vol. 27 (02): 250-253 [Abstract] ( 1196 ) PDF (873 KB)  ( 796 )
254 Application of IR Spectrum to the Research on Coordination Mechanisms of Organic Carboxylic Acid during Homogeneous Precipitation
MEI Yan,NIE Zuo-ren*,WANG Wei
Infrared (IR) spectrum, X-ray diffraction (XRD) and transmission electron microscope (TEM) were used to study and characterize the coordination mechanisms, products and morphology of organic carboxylic acid during homogeneous precipitation in the system of Ce(NO3)2·6H2O and urea solution. The results showed that monocarboxylic acid stearic acid played a role of surfactant, and the product was still orthorhombic Ce2O(CO3)2·H2O with a high crystallization degree. In turn, duality-carboxylic acid tartaric acid and tri-carboxylic acid citric acid were combined with Ce3+ to form chelate citric acid and cerium tartaric acid, respectively. The results were caused by different mechanisms of reaction in the solution.
2007 Vol. 27 (02): 254-258 [Abstract] ( 1701 ) PDF (1957 KB)  ( 962 )
259 Infrared Spectroscopic Studies of the Effect of Hydrotalcite on the Capability of Agricultural Film
WANG Liang-yu1,CUI Hai-long1, 2,JIAO Hong-wen2
Different kinds of hydrotalcite and their effects on the optic capability, transmittance, infrared anti-transmittance and heat preservation of agriculture film were studied by IR spectroscopy. It was found that the haze degree of the film decreased about 1.5% because the diameter of the hydrotalcite made in Dalian was bigger than those made in Japan. Compared to the french chalk, the hydrotalcite had much better capability of infrared anti-transmittance. But from the spectra of hydrotalcite, whichever made in Dalian or in Japan, there was no infrared absorption in the region of 1 100-1 200 cm-1. Compared with the wavelength of 9-11 μm, the absorbance band at 1 360 cm-1 had a little shift. Hence, the capability of heat preservation of hydrotalcite-added agriculture film would be studied in the future work.
2007 Vol. 27 (02): 259-261 [Abstract] ( 2298 ) PDF (1461 KB)  ( 849 )
262 Influence of LPLS Algorithm Parameters on NIR Veracity
LI Jun-hui1,QIN Xi-yun2,ZHANG Wen-juan1,CAI Gui-min1,YANG Yu-hong2,ZHAO Long-lian1,CHANG Zhi-qiang1,ZHAO Li-li1,ZHANG Lu-da3
The theory of local partial least square (LPLS) algorithm was described based on locally weighted regression algorithm(LWR). The influence of data processing parameters, such as principal component numbers and local set-up sample number in LPLS mode, on the NIR veracity was studied with homemade grating diffuse NIR instrument using Yunnan flue-cured tobacco. Results showed that for nicotine model, the principal component number decided by cross validation was not the best choice, and better results could be achieved by reducing the principal component number; using 30-50 samples to set up NIR model, the veracity of total sugar, total nitrogen, and nicotine could be improved by 7%, 14% and 10%, respectively. So, LPLS algorithm can effectively improve NIR model’s veracity, and is a good method to set up robust NIR models.
2007 Vol. 27 (02): 262-264 [Abstract] ( 1953 ) PDF (849 KB)  ( 941 )
265 Structure Analysis of Benzoic Medicines by Near Infrared and Two Dimensional Correlation Spectroscopy
LIU Hao1,XIANG Bing-ren2*,QU Ling-bo3,XU Jian-ping2
The structure analysis of benzoic medicines by Fourier transform near infrared spectroscopy and generalized two dimensional correlation spectroscopy was performed. Three kinds of medicines showed unconspicuous changes in one-dimensional near infrared spectra, while the two dimensional correlation spectra showed high resolution，and were more explicable. By the comparison and analysis of raw near infrared spectra and 2D-correlation spectra, the near infrared absorption peaks of benzoic acid medicines were assigned，and their structure characteristics were analyzed, the results affirmed the six-membered ring intramolecular hydrogen bond especially. The study is helpful to the in-depth understanding of benzoic medicines, and provides information for the future study and utilization of benzoic medicines.
2007 Vol. 27 (02): 265-269 [Abstract] ( 1829 ) PDF (1150 KB)  ( 495 )
270 Study on the Relation between Ginkgolide B and Water by FTIR
YUAN Chuan-xun, PAN Jian, HU Xue-qiao, XU Jing
The method of IR was used to study GB spectrum variety with different water ratio, and it was showed that GB IR spectrum only changed in the absorption strength at 3 452, 1 793, 1 780 and 1 630 cm-1. The reason is that the water was concealed by GB cage skeleton and formed hydroxyl bond with GB hydroxyl groups, and the structure of GB remained unchanged and accorded with standardized GB. With the help of DSC and LC-MS, the subtle relations between GB and water were explained, GB is lipophilic and can not be dissolved by water, but in general, GB is easy to absorb the water of environment, and can be dehydrated under particular conditions.
2007 Vol. 27 (02): 270-274 [Abstract] ( 2463 ) PDF (922 KB)  ( 573 )
275 Prediction of Maize Stover Components with Near Infrared Reflectance Spectroscopy
LIU Li-ying, CHEN Hong-zhang*
The components concentrations in maize stover were analyzed with 67 samples selected from 380 samples of different provinces and varieties in order to serve the biomass utilization of our country. The technique of near infrared reflectance spectroscopy (NIRS) and partial least square (PLS) regression were used to establish the models. The results showed that the calibration models developed by the spectral data pretreatment of the first derivative+Karl Norris derivative filter were the best for ash, hemicellulose, cellulose, Klason lignin, acid unsolvable ash, and water in the spectral region of 4 100-7 500 cm-1. The root mean square error of cross validation (RMSECV) for the above six components was 0.991, 1.27, 1.44, 0.599, 0.090 3 and 0.547, respectively; the root mean square error of prediction (RMSEP) was 0.774 6%, 1.807 2%, 0.256 9%, 2.581 9%, 0.515 8% and 1.032 5%, respectively. The models can be used to measure various samples in biomass transformation industry.
2007 Vol. 27 (02): 275-278 [Abstract] ( 1788 ) PDF (898 KB)  ( 669 )
279 Application PCA-ANN Method to Fast Discrimination of Tea Varieties Using Visible/Near Infrared Spectroscopy
LI Xiao-li, HE Yong, QIU Zheng-jun*
A new method for the discrimination of varieties of tea by means of visible/near infrared spectroscopy (Vis/NIRS) (325-1 075 nm) was developed. A relation has been established between the reflectance spectra and the tea varieties. The data set consists of a total of 150 samples of tea. First, the data was analyzed with principal component analysis(PCA). It appeared to provide the reasonable clustering of the varieties of tea. Meanwhile PCA compressed hundreds of spectral data into a small quantity of principal components which described the body of the spectra; the first 6 principal components computed by PCA were applied as inputs to a back propagation neural network with one hidden layer. One hundred twenty five samples from five varieties were selected randomly, then they were used to build BP-ANN model. This model has been used to predict the varieties of 25 unknown samples; the residual error for the calibration samples is 1.267×10-4. The recognition rate of 100% was achieved. This model is reliable and practicable. So this paper could offer a new approach to the fast discrimination of varieties of tea.
2007 Vol. 27 (02): 279-282 [Abstract] ( 1297 ) PDF (880 KB)  ( 984 )
283 Application of HATR-FTIR Spectroscopy to the Analysis of Quality Mensuration of Rhizoma Atractylodes
HONG Qing-hong1，2,CHENG Cun-gui2*,CHENG Ze-feng2,LI Dan-ting2
The present paper used many kinds of mensuration of FTIR spectroscopy to determine traditional Chinese drugs-Rhizoma Atractylodis Macrocephalae. Comparing the horizontal attenuated total reflection-Fourier transform infrared spectra(HATR-FTIR) of xylem and outer layer parts of cuticle indicates that there are more butenolide and its derivatives in outer layer parts of cuticle. Much more chemical materials could be found in fresh sample than in drying sample, possibly due to the decreased amount of naphtha in the drying sample. The HATR-FTIR of xylem of Rhizoma Atractylodis Macrocephalae and its confusable varieties were transformed into second derivative FTIR to make sure whether the peak location is consistent. As a result, the difference is significant.
2007 Vol. 27 (02): 283-286 [Abstract] ( 1266 ) PDF (948 KB)  ( 682 )
287 The Spectrum Characterization of Non-Stoichiometry Potassium Lithium Niobate Crystals
WAN You-bao1, 2,YUAN Guo-xiang2,WU Yu-rong2,YANG Pei-zhi3,XIN San-fa2,ZHU Hai-bin2,HUANG Xue-jun2,YANG Hui1
A batch of potassium lithium niobate(KLN) crystals with different compositions were grown by using TSSG technique. Samples with three different compositions were well polished. By using near infrared cw: Ti-sapphire laser，their Second Harmonic Generation (SHG) properties were investigated. The results showed that the SHG effect is related to the composition of the samples, and their frequency-doubling efficiency enhanced with the raise of Li ions content in the crystal. By using infrared Raman technique, the properties of nonlinear lattice vibration of thee samples were investigated, and the character of Raman spectrum were analyzed, as well the effect of composition on the SHG properties were discussed. The analysis results showed the striking effects of Li content for these Raman peaks. For KLN sample with small Li content, the three character peaks belonged to [NbO6]7- octahedron show simple peak. With the raise of Li content in crystal, the peaks belonged to ν2 mode were partly split, and the peak belongs to ν5 mode was broadened. When the Li content approach to the chemical composition KLN crystal, and the structure of [NbO6]7-octahedron is almost to be disorganized, the peaks belonged to ν5 mode were split, and the peaks belonged to ν1 mode and ν2 mode were partly split also, with more distinct weak peaks in the wavelength range of 100-400 cm-1. These effects were caused by the raise of Li content, which leads to the severer aberrance of [NbO6]7-octahedron in KLN crystal, and disturbing the lattice vibration of the octahedron. This phenomenon is agreed with the nonlinear properties of potassium lithium niobate crystal.
2007 Vol. 27 (02): 287-291 [Abstract] ( 2387 ) PDF (1119 KB)  ( 434 )
292 Raman Spectra Analysis of DKDP Crystal
ZHAO Peng1，2,XIA Hai-rui2,LING Zong-cheng2,WANG Pei-ji1,SU Yan1,ZHANG Zhong1
Based on the space group theory, the normal vibration modes of DKDP crystal were analyzed and the assigned. Raman spectra were measured at the room temperature. Results show that the lattice vibration spectra of DKDP arise mainly from the internal vibrations of D2PO-4 anionic cluster. Compared with the Raman spectra of an aqueous solution of KH2PO4 and an NaD2(PO4)2 crystal, the four internal vibration models of the D2PO-4 in DKDP were assigned as 881 cm-1(ν1)，357 cm-1(ν2)，514/541 cm-1(ν3)，965 cm-1(ν4), respectively.
2007 Vol. 27 (02): 292-294 [Abstract] ( 1679 ) PDF (1100 KB)  ( 781 )
295 Study of Human Tumor Tissues by Raman Imaging Spectra
YU Ge1,ZHANG Pan2,TAN En-zhong1,ZHANG Cun-zhou2
The Raman mapping spectra were collected from the samples of fresh human breast tumor tissues with the excitation wavelength at 633 nm, their correlation coefficients with the reference spectra of chemical DNA, cytoplasm and extra-cellular matrix etc. were calculated, and the images were created based on these correlation coefficients. Examining these images, the authors found that they show approximately the distribution of the corresponding reference chemicals in human tissues and that the DNA spectrum correlation images reflect the DNA distribution quite well because of its much lower correlation with the spectra of other morphological chemicals. This work is helpful in understanding the chemical/morphological basis of the breast tissue Raman spectra and in developing the Raman diagnostic method for breast tumor.
2007 Vol. 27 (02): 295-298 [Abstract] ( 1197 ) PDF (992 KB)  ( 777 )
299 Comparative Study on SERS and Stability of Negative Silver Colloids
LI Qing-yu1,LI Shi-rong2,SI Min-zhen2*,ZHANG Peng-xiang3
Negatively charged colloidal nano-silver particles were prepared by the colloidal chemical method. A 1.7% solution of silver nitrate(2 mL) was diluted with deionized water to 100 mL. A 1% solution of tannic acid(1 mL) was added dropwise to the solution stirring, then a 1% solution of potassium carbonate anhydrous(3-4 drops) was added to the mixed solution. Finally, a red-brown silver sol was obtained. It was testified that the silver sol is a negatively charged colloid by experiment of electrophoresis. The negative silver colloids (for short, old NCS) were kept on at the room temperature two year ago in order to test its SERS and stability. The sizes of particles were determined by Hitachi H-800 transmission electron microscope. Absorption spectroscopy and SERS were used to determine the main properties. Absorption spectra were obtained with UV-2401PC. Raman spectra were recorded with RENISHAW MIK 2000 Raman micro-spectroscopy. The 514.5 nm line of an argon ion laser with about 3 mw was used. Compared with the newly perpared negative silver colloids (for short, new NCS). It was found that the mean diameter of the old NCS was larger than the new NCS; old NCS had absorption maximum at 431 nm but new NCS at 418 nm, the absorbance spectrum of old NCS had a 12 nm red shift, and the red shift rate is about 0.5 nm/month; Both strong SERS spectra were observed when cationic molecules of fuchsine basic and neutral molecules of alcidine orange adsorbed on old NCS and new NCS; For cationic molecules of methylene blue, the SERS is stronger on new NCS than old NCS; but no SERS was observed for the anionic molecule of benzoic acid both on new NCS and on old NCS.
2007 Vol. 27 (02): 299-301 [Abstract] ( 239 ) PDF (1059 KB)  ( 739 )
302 Synthesis and DNA Binding Spectroscopic Studies of Cu(Ⅱ)-HAsp-Im Complexes
ZHANG Fang, ZHANG Qian-qian*,LU Xiao-lan, JIANG Tao, WANG Xiu-lin
Two novel complexes of [Cu(HAsp)ImH2O]SO4·4H2O and [Cu(Asp)Im(OH)]·4H2O (HAsp=Aspartic acid molecule, Asp=Aspartic acid ion, Im=Imidazole) were synthesized and characterized by elemental analysis, IR spectroscopy and TG-DTA. The interactions of the complexes with sperm DNA were studied by electronic absorption and fluorescence spectra. Results showed that the reactions of the two complexes with DNA are obviously different: for [Cu(HAsp)ImH2O]SO4·4H2O, it is intercalation companied by electrostatic effect, while [Cu(Asp)Im(OH)]·4H2O mainly cooperates with the nitrogen atom of the DNA base pair, which induces the breakage of DNA double helix. The reasons for these differences in their DNA binding modes were also discussed.
2007 Vol. 27 (02): 302-305 [Abstract] ( 704 ) PDF (927 KB)  ( 653 )
306 Study on the Interaction between BSA and Nicotine
SHENG Liang-quan1,YAN Xiang-yang2,XU Hua-jie1,TONG Hong-wu2,LIU Shao-min2*
The interaction of BSA and NIC was investigated by absorption spectra，fluorescence spectroscopy and synchronous fluorescence spectroscopy. In the system of sodium phosphate dibasic-citric acid of 0.1 mol·L-1,fluorescence titration showed that the fluorescence intensity of BSA at 342 nm was quenched when NIC was added, NIC was capable of binding with BSA to form a 1∶1 complex and the quenching mechanism of BSA affected by NIC was shown to be a static quenching procedure by calculating the binding number n and binding constant K. NIC decreased the intensity of the characteristic absorption peak of BSA, showing that the binding of NIC to BSA had strong impact on protein conformation with the decrease in a-helicai content of the protein. Synchronous fluorescence indicated that the binding of NIC to BSA is near tryptophan subunit.
2007 Vol. 27 (02): 306-308 [Abstract] ( 1721 ) PDF (1116 KB)  ( 845 )
309 Interaction of Tributyltin (TBT) Compound and Bovine Serum Albumin (BSA)
ZHANG Zhao-hong1,DONG Dian-bo1,ZHAO Zhe1,ZANG Shu-liang1, 2*,CHEN Zhong-lin1,WANG Jie1, ZHANG Hua-chun1
Tributyltin (TBT) compound is one of the main components of antifouling paint for boats and ships. The interaction of TBT compound and bovine serum albumin (BSA) was investigated by ultraviolet, fluorescence and circular dichroism (CD) spectra. The influences of concentration, acidity and organic solvent were also studied. The results showed that the interaction of TBT and BSA was dual, showing not only the hydrophobic actions of butyl groups but also the coordination action of tin cation with BSA molecule, which resulted in the exposures of aromatic amino acids residues of tryptophane and tyrosine in BSA molecule, the destruction of BSA secondary structure, the decrease in α-helix content, and the transformation of the conformation.
2007 Vol. 27 (02): 309-312 [Abstract] ( 1165 ) PDF (935 KB)  ( 552 )
313 Spectroscopic Study on the Binding of Mn(Ⅱ) to EHPG
LI Hai-peng, ZHAO Chun-gui*,LI Xiao-li, YANG Bin-sheng
Under the conditions of 0.05 mol·L-1 Hepes buffer at room temperature and pH 7.4, the interaction of ethylene-N, N’-bis(o-hydioxyphenylglycine) (EHPG) and Mn(Ⅱ) was investigated by both fluorescence and UV difference spectra. Results showed that the molar ratio of the complex is 1∶1. With the addition of manganese ions, the fluorescence peak of EHPG at 310 nm decreased, while the peaks of UV absorptivity at 238 and 291 nm increased. The molar absorptivity of Mn(Ⅱ) to EHPG at 238 nm is (1.31±0.02)×104 cm-1·mol-1· L. The disassociation constant for Mn-EHPG was determined to be (1.36±0.21)×10-5. It can be concluded that the binding of Mn(Ⅱ) to EHPG is not a strongly binding reaction.
2007 Vol. 27 (02): 313-316 [Abstract] ( 221 ) PDF (934 KB)  ( 464 )
317 Study on the Interaction between Alginic Sodium Diester and Azur A and the Application
LIU Yong-ming, LI Gui-zhi, PAN Fei
The interaction of alginic sodium diester (ASD) and azur A (AA) was studied by absorption spectra. The influence of pH and the molar ratio of AA/ASD on the spectra was investigated. The maximum binding number (N=168) and the binding equilibrium constant (K=3.25×106) of the alginic sodium diester and azur A were obtained by the theoretical model. The new method for the determination of ASD was developed by the formation of ASD-AA ion-association complex that caused the fading of the AA. The detection limit is 0.009 μg·mL-1. The method has the advantages of simplicity, stable system, good accuracy and selectivity, and was applied to the determination of alginic sodium diester in tablets with satisfactory results.
2007 Vol. 27 (02): 317-320 [Abstract] ( 1210 ) PDF (930 KB)  ( 472 )
321 Spectroscopic Study on the Effect of Crystallization of the Hydroxyapatite on the Secondary Structure of Bovine Serum Albumin
YE Feng, AN Ying-ge, QIN De-zhi, YANG Lin*,SHE Lan, XING Rui-min
The effect of crystallization of hydroxyapatite on the secondary structure of bovine serum albumin(BSA) was studied by circular dichroism spectrum, Fourier transform infrared spectroscopy, derivative, deconvolution and curve-fitting techniques in the present paper. The CD results show that pure bovine serum albumin is composed of 56.8% α-helices, 5.8% β-sheets, 14.1% β-turns and 23.9% random structures, while the bovine serum albumin in the Ca10(PO4)6(OH)2/bovine serum albumin solution is composed of 25.4% α-helices, 25.0% β-sheets, 20.0% β-turns and 29.7% random structures. The results of Fourier transform infrared spectroscopy are in good agreement with those from the CD spectra. From these results it can be seen that the percentage of α-helix decreased, while that of the β-sheet increased with the formation of the crystal of hydroxyapatite, and with the reaction time increasing, the percentages of α-helix obviously dropped and those of β-sheet markedly rose. These results showed that α-helix transformed into β-sheet. Furthermore the essence of these changes is discussed.
2007 Vol. 27 (02): 321-324 [Abstract] ( 1172 ) PDF (902 KB)  ( 504 )
325 Ultraviolet-Visible Absorption Spectral Properties of Sudan Ⅲ in Different Solvents
YANG Sheng-ke, ZHANG Jin-ping, XU Yong-hua, DENG Xiao-ni
Ultraviolet-visible absorption spectral properties of Sudan Ⅲ in different solvents were studied. The results show that the main absorption peaks are located in 200-230 nm，340-360 nm and 490-510 nm. When Sudan Ⅲ is in polar solvent, two absorption peaks appear in the mid-ultraviolet region, 200-230 nm. And when it is in nonpolar solvent, the absorption changes from two peaks to one peak with the concentration of Sudan Ⅲ increasing. When it is in composite solvent, the two absorption peaks disappear, but one absorption peak appears at 310 nm. Molar absorptivities of Sudan Ⅲ in the five solvents were determined, whose order of magnitude was 104.
2007 Vol. 27 (02): 325-328 [Abstract] ( 1858 ) PDF (900 KB)  ( 964 )
329 The Spectroscopic Study on the Interaction between Edible Pigment and Human Serum Albumin in Two-Phase Aqueous Systems
DENG Fan-zheng, GUO Dong-fang, WANG Hai-rong
In polyethylene glycol 2000(PEG)-(NH4)2SO4-edible pigment two-phase aqueous systems, the spectroscopic behaviour of the complexes of edible pigment and human serum albumin in PEG phase was investigated. Effects of different acidity, quantities of PEG and salt, reaction time, and coexistent matter on the determination of systems were discussed. Experimental results show that compared to BS spectra, the maximum wavelength of the complex of human serum albumin shifted to the red by 13 nm in buffer solution at pH 8, the maximum binding number of 40 was measured by molar ratio method, and the apparent molar absorptivity was 9.4×104 L·mol-1·cm-1. The linear range was 0-21.07 mg·L-1. With different surfactant, the interaction mechanism of protein and edible pigment was discussed.
2007 Vol. 27 (02): 329-331 [Abstract] ( 2229 ) PDF (852 KB)  ( 740 )
332 Study on Fluorescence Property of DCM with SDS in Water Solution Excited by 532 nm Laser
LIANG Hui-min, LUO Shi-rong*,WANG Zhi-hua, ZUO Hao-yi, WANG Hong-bo, ZHAO Xiao-yan, YANG Jing-guo
The fluorescence property of DCM in water solution with added different concentration of SDS is reported. With increasing the concentration of SDS in water, the solubility of DCM and the fluorescence intensity increase. When the concentration of SDS increases from 0.025 to 0.5 mol·L-1,the maximum fluorescence relative intensity is enhanced by a factor of 95. A powerful dye laser at wavelength of 648 nm was generated in the solution of DCM in water with SDS exited by a 532 nm laser. It shifts 13 nm compared with the dye laser wavelength of the solution of DCM in ethanol. And enhancement of SRS of C6H6 was achieved both in the solution of DCM in water with SDS and in the solution of DCM in ethanol. The result is that the second, the third and the forth order Stokes of C6H6 are all enhanced. But the former mainly enhances the forth order Stokes(632 nm) and the enhancement gain coefficient is 8.5, while the latter mainly enhances the third order Stokes(595 nm) and the enhancement gain coefficient is 2.5. The mechanism of solubility, fluorescence enhancement and its possible application are discussed.
2007 Vol. 27 (02): 332-334 [Abstract] ( 1255 ) PDF (874 KB)  ( 739 )
335 Synthesis，Characterization and Fluorescence Property of An Unsymmetrical Schiff Base and Its Copper Complex
ZHANG Dong-mei, FAN Yu-hua*,BI Cai-feng, AI Xiao-kang, HE Xue-tao, SUN Feng
An unsymmetrical tetradentate Schiff base ligand (H2L) was synthesized using 5-chloro-2-hydroxybenzophenone, o-phenylenediamine and salicylaldehyde. A solid complex of this ligand CuL was prepared and characterized by elemental analyses, IR spectra, UV spectra, TG-DTG and molar conductance. Possible structure of this complex was proposed. The fluorescence property of the ligand and complex was also studied. The result indicates that the Schiff base reagent exhibits a maximum of fluorescence emission spectrum at 385 nm. At pH 9.62, the copper complex of this reagent can cause fluorescence quenching of the reagent.
2007 Vol. 27 (02): 335-338 [Abstract] ( 1212 ) PDF (940 KB)  ( 809 )
339 A Fluorescence Quenching Method for the Determination of Trace Chlorite in Water with Rhodamine B
KANG Cai-yan1，2,JIANG Zhi-liang2，3*,XI Dan-li1*
In acidic sodium acetate-HCl buffer solution containing KI, Rhodamine B(RhB) has a fluorescence peak at 580 nm. When ClO-2 exists fluorescence quenching occur. The fluorescence quenching intensity is linear with the concentration of ClO-2 in the range of 0.021 8-0.51 μg·mL-1. Based on this, a new, simple, sentisive fluorescence method has been proposed for the determination of ClO-2 in water, with satisfactory results.
2007 Vol. 27 (02): 339-341 [Abstract] ( 2349 ) PDF (891 KB)  ( 546 )
342 Fluorescence Spectra of Dichroa Febrifuga Aqueous Extraction
ZHANG Ying-hua, SHI Xun-li, LIU Ya-lan, LIU Cui-ge, WEI Yong-ju*
Fluorescence spectra of chang shan (Dichroa febrifuga Lour) aqueous extraction were studied. In the three-dimensional fluorescence contour spectrum, three fluorescence peaks of quinazoline alkaloids, which are the active components of chang shan, were observed. The excitation wavelengths of the peaks were 235, 270 and 320 nm, respectively, and the emission wavelength of all the peaks was 430 nm. Three-dimensional fluorescence contour spectrum is the very image of fingerprint, suitable for qualitative identification of traditional Chinese medicine. In the range of pH 3 to pH 6, the fluorescence spectrum of chang shan aqueous extractions changes with the variation in pH value. The reason for this spectral change might be the protonation of N-1 in quinazolone ring of β-dichroine (febrifugine) molecule. There is an excellent linear relationship between the fluorescence intensity and the concentration of chang shan under nearly neutral conditions, thereby a quantitative method for the determination of quinazoline alkaloids may be established.
2007 Vol. 27 (02): 342-345 [Abstract] ( 1863 ) PDF (938 KB)  ( 700 )
346 Study on the Role of Polysaccharide and Flavone in Chinese Herbs in Protecting DNA with Fluorescence Probe
ZHANG Hai-rong,WU Xiao-yan
The aim of the present work is to study the role of polyaccharide and flavone compounds of Flos lonicerae, Ganoderma lucidum etc. in protecting DNA with EB as a probe to determine the fluorescence integration intensity of DNA and EB mixture. D is defined as the interaction constant between different extracts from traditional Chinese herbs and DNA. The bigger the D,the stronger the interaction of drugs and DNA. According to the definition of D,the impact of polysaccharide and flavone compounds on the protection of DNA is discussed. The results show that all the extracts from traditional Chinese herbs can interact with DNA, but the degree of interaction is different. The order is as follows: Folium hippophae rhamnosides＞Rhizoma anemarrhenae＞Radix acanthopanacis senticosi＞Ganoderma lucidum＞Radix achyranthis bidentatae＞Fructus lycii＞Flos lonicerae＞Rhizoma atractylodis＞Astragalus membranaceus＞Flos chrysanthemi in the presence of polysaccharide compounds，while Folium hippophae rhamnosides＞Flos lonicerae＞Fructus lycii＞Rhizoma atractylodis＞Astragalus membranaceus＞Rhizoma anemarrhenae＞Radix acanthopanacis senticosi＞Ganoderma lucidum＞Radix achyranthis bidentatae(Flos chrysanthemi, with no signals) in the presence of flavone compounds.
2007 Vol. 27 (02): 346-349 [Abstract] ( 206 ) PDF (1135 KB)  ( 729 )
350 Rapid Simultaneous Analysis of Fluorene, Carbazole, Benzo[α]pyrene, and Perylene by Derivative-Constant Energy Synchronous Fluorescence Spectroscopy
ZHANG Ru-ping, HE Li-fang*
A new method of derivative constant-energy synchronous fluorescence (CESF) spectroscopy for the simultaneous determination of fluorene，carbazole, benzo[α]pyrene and perylene was developed. The comparison and explanation of its performance are presented. The derivative CESF spectra are apparently more structured than the direct CESF. The scanning of derivative CESF is more effective than derivative constant-wavelength synchronous fluorescence spectroscopy. By using this method, real samples (tap water, seawater and airborne particulates) were determined directly and good results were obtained. The recoveries in tap water, seawater and airborne particulates were 90.0％-108.0％, 90.0％-104.0％ and 90.0％-102.0％ respectively.
2007 Vol. 27 (02): 350-354 [Abstract] ( 592 ) PDF (964 KB)  ( 615 )
355 Simultaneous Spectrophotometric Determination of Certain β-Lactam Antibiotics in Rabbit Serum Using Multivariate Calibration Methods
NI Yong-nian, GE Cheng-xiang
Cefuroxime sodium, ceftriaxone sodium, cefotaxime sodium and cefazolin sodium have absorption in ultraviolet region, and their absorption spectra are overlapping. So they can not be determined individually by spectrophotometry without prior separation. In this paper, the chemometric multivariate calibration method was applied to the simultaneous determination of these four compounds in a Britton-Robinson buffer solution (pH 2.09), and the analytical results were compared with those by classical least squares (CLS), principal components regression (PCR) and partial least squares (PLS). The linear ranges of cefuroxime sodium, ceftriaxone sodium, cefotaxime sodium and cefazolin sodium are 1.0-20.0, 2.0-20.0, 2.0-20.0 and 1.0-18.0 μg·mL-1,respectively. The proposed procedure was successfully applied in the determination of these drugs in rabbit serum, and the result obtained from spectrophotometry was compared with the one by HPLC with no significant difference found.
2007 Vol. 27 (02): 355-359 [Abstract] ( 1676 ) PDF (934 KB)  ( 548 )
360 Study on Solid Phase Extraction and Spectrophotometric Determination of Palladium with MCI-GEL Resin
ZHONG Yi-hui1, 2,HUANG Qi-lin1, 2,ZHANG Xin1,HUANG Zhang-jie2,HU Qiu-feng2,YANG Guang-yu2*
Based on the color reaction of 2-(2-quinolinylazo)-5-diethylaminoaniline (QADEAA) with palladium(Ⅱ) and the solid phase extraction of its colored complex with MCI-GEL reversed phase cartridge, a new method for the determination of trace palladium was established. In the presence of 0.2-2.0 mol·L-1 of hydrochloric acid solution and CTMAB medium, QADEAA reacts with palladium(Ⅱ) to form a stable 2∶1 complex. The colored complex can be enriched by MCI-GEL reversed phase cartridge, and the retained chelates was then eluted by acetone. The eluant was determined by spectrophotometry at 615 nm. Beer’s law is obeyed in the range of 0.01-1.5 mg·L-1. This method was applied to the determination of palladium with good results.
2007 Vol. 27 (02): 360-363 [Abstract] ( 1834 ) PDF (1047 KB)  ( 747 )
364 Spectrophotometric Determination of Codeine Through Charge-Transfer Reaction
DU Li-ming, LI Li, WU Hao
The charge-transfer reaction of 7,7,8,8-tetracyano-quinodimethane(TCNQ)as a π-electron acceptors with codeine as electron donors was investigated by spectrophotometry. TCNQ was found to react with codeine to produce stable charge-transfer complexes in acetone. Meanwhile, the studied drugs suffer a considerable bathochromic shift (from 216 to 843 nm ). The influential factor of charge-transfer reaction and the optimum conditions for the determination of codeine were investigated in detail. Therefore a simple, rapid and accurate method with a good selectivity for the determination of codeine has been developed. The results show that Beer’s law is obeyed in the ranges 0.1-1.6 μg·mL-1 for codeine. The apparent molar absorptivity of the complex at 843 nm is 1.7×104 L·mol-1·cm-1. Furthermore, the association constants and standard free energy changes were studied, and the mechanism of charge-transfer reaction was explored elementarily. The proposed method has been applied successfully to the determination of codeine in pharmaceutical preparations. The recoveries are from (98.94±0.96)% to (99.12±1.21)%.
2007 Vol. 27 (02): 364-366 [Abstract] ( 1543 ) PDF (866 KB)  ( 651 )
367 Characterization and Heavy Metal Adsorption Properties of Schwertmannite Synthesized by Bacterial Oxidation of Ferrous Sulfate Solutions
ZHOU Shun-gui, ZHOU Li-xiang*,CHEN Fu-xing
An amorphous ferric hydroxysulfate named schwertmannite was synthesized by using bacterial oxidation of ferrous iron by resting A. ferrooxidans cells in acid ferrous sulfate solution (pH 2.5). The identification of the bacterially oxidized iron precipitate was carried out by SEM, XRD, FTIR and chemical analysis. Results showed that resting cells of A. ferrooxidans LX5 could completely oxidize ferrous ions to ferric ions in the FeSO4-H2O system after 2 days of incubation. The solution pH decreased from an initial 2.5 to 2.10, and about 15% of the ferrous iron was transformed into the red-brown precipitates. The subsequent characterization of the precipitates showed that the biotic, synthetic ferric hydroxysulfate was schwertmannite. Sorption edge measurement showed that the adsorption behavior of metal cations (e.g., Cu2+,Zn2+ and Cr3+) was pH-dependent. The adsorption increased with an increase in pH, and the maximum was found in a pH range of 6.0-7.0. For solution concentration of 50 mg·L-1,the maximum adsorption efficiencies of Cu2+,Zn2+ and Cr3+ were 99.3%, 99.4% and 87.6%, respectively.
2007 Vol. 27 (02): 367-370 [Abstract] ( 1617 ) PDF (995 KB)  ( 645 )
371 Analysis of Trace Elements in Corn Stover by ICP-AES
SUN Yong1, 2,YANG Gang1, 2,ZHANG Jin-ping1, 2,LI Zuo-hu1
The contents of trace elements of Zn，Mg，Mn，Sr，Fe，Co，Ni and Se in the corn stover collected from Shanxi, Beijing, Xinjiang, Shandong, Neimeng, Gansu, Shaanxi, Jilin, Yunnan and Jiangsu, 10 different provinces in China, were determined by ICP-AES using nitrifying method of high pressure nitrifying pot. This method proved to be easily operational, rapid, highly sensitive, and accurate, and can be adopted as the method of determining many elements simultaneously. The recovery yields of Zn, Mg, Mn, Sr, Fe, Co, Ni and Se are 96.5%-103.8%, 98.0%-102.5%, 95.7%-104.1%, 97.1%-103.2%, 95.1%-101.3%, 95.1%-104.5%, 97.0%-103.5% and 95.9%-104.6%, respectively, and the relative standard deviation of all the elements is all below 5.00%.
2007 Vol. 27 (02): 371-373 [Abstract] ( 1341 ) PDF (837 KB)  ( 613 )
374 CAIS Correction for Blood Matrix Effect on Determination of Lead Concentration and Isotope Ratio by ICP-MS
ZENG Jing1,WANG Xiao-yan1, 2,LIU Hu-sheng1,DUN Zhe3,ZHAI Lei3,WANG Jing-yu1, 2*
The research studied the influence of matrix effect on the determination of lead concentration and isotope ratio through simulating blood matrix, and its correction by common analyte internal standardization (CAIS) method. The experiment results showed that CAIS method was suitable for the multi-element-matrix. The relative errors between the determined and the true concentration values are 20%(without correction), 8%(by conventional internal reference correction) and 2% (by CAIS correction), respectively. Otherwise, the influence of matrix effect and its correction for isotope ratio determination are not that obvious. Similarity of the mass number and properties between internal reference and analyte elements seems not important for CAIS correction, since very close correction results were obtained by using Tl and Dy as internal reference elements. Besides, correction results are not affected by different matrix dilution. Reliability and practicality of CAIS were proved by bovine blood standard material determination.
2007 Vol. 27 (02): 374-377 [Abstract] ( 2297 ) PDF (899 KB)  ( 833 )
378 Study on Elemental Speciation Analysis and Transference Characteristics of Arnebia Euthroma (Royle) Johnst by ICP-MS
SHI Yu-feng1,XIE Ming-yong1*,NIE Shao-ping1,JING Miao2,WANG Xiao-ru2, 3
The elemental transference characteristics and primary speciation analysis of Arnebia euthroma (Royle) Johnst were investigated in the present paper. The results showed: sealed digestion at high temperature was more efficient and thorough than microwave-assisted process(MAP) digestion in the preparation of speciation analysis; Most of the elements analyzed, excluding potassium and zinc, exist in particulate speciation in the plant; The transference characteristics of elements were associated with the polarity of extraction solvents. Contents of all 22 elements basically were directly proportional to the polarity of solvents varying from almost no polarity to strong, especially for 7 elements: magnesium, potassium, calcium, manganese, cobalt, thallium and lead.
2007 Vol. 27 (02): 378-382 [Abstract] ( 1108 ) PDF (877 KB)  ( 608 )
378 Study on Elemental Speciation Analysis and Transference Characteristics of Arnebia Euthroma (Royle) Johnst by ICP-MS
SHI Yu-feng1,XIE Ming-yong1*,NIE Shao-ping1,JING Miao2,WANG Xiao-ru2, 3
The elemental transference characteristics and primary speciation analysis of Arnebia euthroma (Royle) Johnst were investigated in the present paper. The results showed: sealed digestion at high temperature was more efficient and thorough than microwave-assisted process(MAP) digestion in the preparation of speciation analysis; Most of the elements analyzed, excluding potassium and zinc, exist in particulate speciation in the plant; The transference characteristics of elements were associated with the polarity of extraction solvents. Contents of all 22 elements basically were directly proportional to the polarity of solvents varying from almost no polarity to strong, especially for 7 elements: magnesium, potassium, calcium, manganese, cobalt, thallium and lead.
2007 Vol. 27 (02): 378-382 [Abstract] ( 1067 ) PDF (877 KB)  ( 434 )
383 HG-AFS Determination of Selenium in Moringa Oleifera
HUANG Guo-qing1, 2,XIAO Zi-jun2
The Se content in Moringa oleifera was studied by hydride generation atom fluorescence spectrometry(HG-AFS) with wet digestion. The effects of the way of digestion, the work condition of apparatus, the reaction medium and acidity, and the reducing agent and masking agent on the determination of Se were investigated. And the operating condition of apparatus was optimized. The results showed that the detection limit of Se in this method was 0.42 ng·mL-1 in the linear ranger of 0-120 ng·mL-1,the relative standard deviation was 3.53%(n=11), and the recovery of the method was 95.2%-104.6%. It was showed that the method was very sensitive, simple, rapid and accurate.
2007 Vol. 27 (02): 383-385 [Abstract] ( 547 ) PDF (849 KB)  ( 563 )
386 Application of High Performance Liquid Chromatography and Hyphenated Techniques in Analysis of Arsenic Species
ZHANG Hua1,WANG Ying-feng1,SHI Yan-zhi1*,CHEN Yu-hong2
Arsenic is a very important nonmetal element in the environment and is vitally related to human lives. It is well known that the biological availability and toxicological effects of arsenic compounds depend upon their chemical forms, so it is necessary to detect the species of arsenic in some environmental samples, food, medicine, and body fluids. High performance liquid chromatography (HPLC) is widely used in the research on arsenic species because of its high separation capability. The detection techniques used for arsenic species analysis have been improved rapidly with the gradually increasing demand for sensitivity and accuracy. Various hyphenated techniques have also been developed. Inductively coupled plasma mass spectrometry has many advantages, such as high sensitivity, simultaneous multi-element detection, wide linear range and so on. Therefore, high performance liquid chromatography-inductively coupled plasma mass spectrometry is widely used in the analysis of arsenic species.
2007 Vol. 27 (02): 386-390 [Abstract] ( 1191 ) PDF (880 KB)  ( 869 )
391 Calculation of the Contributions of Scattering Effects to the X-Ray Fluorescence Intensities
HAN Xiao-yuan1, 2,ZHUO Shang-jun1*,SHEN Ru-xiang1,WANG Pei-ling1
The contribution of scattering effects to the X-ray fluorescence intensity was studied for pure element samples, BaB binary samples and fused disk samples by theoretic calculation and experiment. Three scattering effects were considered in the present study, i.e. coherent scattering effect, incoherent scattering effect, and primary fluorescence that was scattered into the direction of detector. The study shows that the contribution of scattering effects to the intensity of fluorescence is related to the energy of the atomic absorption edge, and the sample’s matrix. The higher the energy of the atomic absorption edge, the more the contribution of scattering effects to the intensity of fluorescence. The contribution of scattering effects to the fluorescence intensity is larger for light matrix samples than heavy matrix samples. The results of experiment show that the accuracy of theoretic calculation was evidently improved when the scattering effects were considered in the theoretic calculation for the intensity of fluorescence.
2007 Vol. 27 (02): 391-394 [Abstract] ( 255 ) PDF (1234 KB)  ( 691 )
395 Application of X-Ray Photoelectron Spectroscopy to the Study of Complexes and Its Progress
YUAN Huan-xin, OUYANG Jian-ming*
X-ray photoelectron spectroscopy (XPS) provides information about the core-level binding energies and oxidation states of complexes. It can be used to identify the species and valence states of elements, measure the relative content of elements, investigate the interaction between ligands and central ions, and verify the results obtained by quantum chemistry theory. XPS has been found to be a powerful tool for identifying coordination site, evaluating charge redistribution, and characterizing geometry of complexes.
2007 Vol. 27 (02): 395-399 [Abstract] ( 485 ) PDF (994 KB)  ( 819 )
400 XPS Research on Thymine Implanted by Low Energy N+
GU Yun-hong, WANG Wei-dong, QIN Guang-yong*,HUO Yu-ping
The induced variation mechanism of low energy ion beam implantation into a creature has attracted a great attention. DNA was the target of radiation. XPS analysis of thymine sample implanted by low energy N+ was studied. It was found that the relative content of C, N and O changed in the implanted samples. The content of N and O decreased, while that of C increased. Subtle structure of C, N and O was studied. It was found that the peak location of O(1s) shifted. The peak number of N(1s) changed from one to three, while that of C(1s) changed from two to one. The results indicated that the chemical environment and physical structure changed greatly by implantation. N+ implantation could lead to destruction and change of thymine molecular structure.
2007 Vol. 27 (02): 400-403 [Abstract] ( 1621 ) PDF (886 KB)  ( 457 )
404 Method of Fused Sample Preparation after Nitrify—Determination of Primary and Minor Elements in Manganese Ore by X-Ray Fluorescence Spectrometry
SONG Yi, GUO Fen, GU Song-hai*
Eight components, i.e. Mn, SiO2, Fe, P, Al2O3, CaO, MgO and S, in manganese ore were determined by X-ray fluorescence spectrometer. Because manganese ore sample releases a lot of air bubbles during fusion which effect accuracy and reproducibility of determination, nitric acid was added to the sample to destroy organic matter before fusion by the mixture flux at 1 000 ℃. This method solved the problem that the flux splashed during fusion because organic matter volatilized brought out a lot of air bubbles, eliminated particle size effects and mineral effect, while solved the problem of volatilization of sulfur during fusion. The experiments for the selection of the sample preparation conditions, i.e. fusion flux, fusion time and volume of HNO3, were carried out. The matrix effects on absorption and enhancement were corrected by variable theoretical alpha coefficient to expand the range of determination. Moreover, the precision and accuracy experiments were performed. In comparison with chemical analysis method, the quantitative analytical results for each component are satisfactory. The method has proven rapid, precise and simple.
2007 Vol. 27 (02): 404-407 [Abstract] ( 2223 ) PDF (913 KB)  ( 610 )
408 Spectra Study on the Influence of Drying Process on Palygorskite Structure
HUANG Jian-hua, LIU Yuan-fa, JIN Qing-zhe, WANG Xing-guo*
There are four different types of molecules of hydroxyl groups of the natural attapulgite. The band at 3 614 cm-1 was attributed to the stretching modes of hydroxyls coordinated with the magnesium. The band at 3 415 cm-1 is associated with the hydroxyl streuching vibrations of absorbed water. The bands at 3 581 and 3 552 cm-1 were attributed to the symmetric and antisymmetric stretching modes of molecular water coordinated with the magnesium at the edges of the channels. The band at 1 653 cm-1 is associated with the hydroxyl stretching vibrations of zeolitic water. The structures of the natural palygorskite and its products dried at different temperatures for 30 min were analysed by Fourier transform infrared spectroscopy(FTIR) and X-ray diffraction(XRD). The absorbed, zeolitic and co-ordinated water decreased during the drying process at the same time. The absorbed water was completely-dehydrated firstly, then the zeolitic water, and lastly the co-ordinated water. And the hydroxyl groups remained until about 600 ℃. When the co-ordinated water was dehydrated completely at 450 ℃, the crystalloid was destroyed. The mechanism of the palygorskite structure change was also discussed in detail.
2007 Vol. 27 (02): 408-410 [Abstract] ( 1235 ) PDF (889 KB)  ( 757 )
411 Influence of Spectrometer Scanning Requirements in Homemade Grating Diffuse NIR Instrument on NIR Veracity
QIN Xi-yun1,LI Jun-hui2*,YANG Yu-hong1,CAI Gui-min2
The influence of instrument parameters, such as scan internal, length of instrument run, frequency of scan background etc, on NIR veracity was studied with a homemade grating diffuse NIR instrument using Yunnan flue-cured tobacco. Results showed that scan interval, such as 8 nm or 16 nm, had no evident influence on NIR quantitative analysis. To improve scan speed, the scan interval the authors decided to use was 16 nm. NIR model was set up which could revise the influence of the length of instrument run. This instrument can clue on baseline shift to decide the frequency of background scanning, which can deduce NIR analysis error and improve NIR veracity.
2007 Vol. 27 (02): 411-413 [Abstract] ( 1447 ) PDF (841 KB)  ( 704 )

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