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2005 Vol. 25, No. 02
Published: 2005-02-26
 
       光谱学与光谱分析
161 Comprehensive Analysis of Up-Conversion Luminescence Saturation Phenomena of ErYb:Oxyfluoride Vitroceramics
CHEN Xiao-bo1, SONG Zeng-fu2
The saturation phenomenon of the up-conversion luminescence of erbium ytterbium co-doped oxyfluoride vitroceramics (ErYb:FOV), when excited by a 966 nm diode-laser, was investigated comprehensively in the present article. A new kind of “characteristic saturation phenomenon”, which results from energy diffusion, was found, i.e. the slope of logI-logP curve, the double logarithmic variation of up-conversion luminescence intensity I upon laser power P, is increased evidently toward regular multi-photon relation with the increase of laser facula. The “typical saturation phenomenon” resulting from ground state population’s exhaustion has huge influence as well, which causes these logI-logP curves to bend gradually with the increase in laser power. Interestingly, this “typical saturation phenomenon” can be decreased obviously and even vanishes when the pumping laser power density is decreased enough.
2005 Vol. 25 (02): 161-165 [Abstract] ( 1408 ) PDF (583 KB)  ( 375 )
166 Theoretical Analysis of Wavelength Choice in Tri-Wavelength Method of Temperature Measurement
FU Tai-ran, CHENG Xiao-fang, FAN Xue-liang, DING Jin-lei
In this paper, a non-dimensional emissivity model with universality is established. For the tri-wavelength method of temperature measurement, based on the non-dimensional emissivity, the applicable measurement condition and theoretical analysis of wavelength choice are mainly introduced. In the discussion of theoretical analysis of wavelength choice, by optimizing the analysis of measurement method and the concept of isothermal line induced by the measurement coordinates, two kinds of ideal choice rules of measurement wavelength are put forward, which will be necessary to the technology application of this tri-wavelength method. Meanwhile the optimizing idea is also applicable to multi-wavelength method of temperature measurement.
2005 Vol. 25 (02): 166-170 [Abstract] ( 189 ) PDF (517 KB)  ( 337 )
171 Collisional Excitation Transfer between Na2(B 1Πu) and Na2(2 1Σ+g)
LEI Zhen-zhou, LIU Jing , ZHOU Xiao-yan , DAI Kang, SHEN Yi-fan*
The B 1Πu electronic state of Na2 was excited by the 441.6 nm He-Cd laser line. The Na atomic transitions and the A 1Σ+u→X 1Σ+g band of Na2 were recorded. From the intensities and spectra of the Na and Na2 fluorescence several collisional processes in the excited sodium atom-dimer system were identified. The Na atomic lines are the result of collisional energy transfer from Na2(B 1Πu) to Na(3P). Predissociation process may also contribute to atomic fluorescence. The A 1Σ+u→X 1Σ+g band is interpreted through a populating mechanism involving collisional transfer from B 1Πu to 2 1Σ+g followed by a radiative transfer to the A 1Σ+u state. From the decay constants and fluorescence intensities, the rate coefficient at 360 ℃ for collisional energy transfer from Na2(B 1Πu) to Na2(2 1Σ+g) was found to be 5.7×10-10 cm3·s-1. The predissociation rate of the B 1Πu is 2.7×106 s-1.
2005 Vol. 25 (02): 171-173 [Abstract] ( 1528 ) PDF (333 KB)  ( 361 )
174 Electronic Spectral Study on Salicylaldehyde-Amino Acid Schiff Bases in Water
WANG Ming-zhao, NING Ya-lan, MENG Zhao-xing, LIU Bo-li
Seven salicylaldehyde-amino acid Schiff bases in water were investigated by means of electronic spectra, which is helpful to investigate the label of radionuclides with the seven ligands in water for radiopharmaceutical study. Except 10-5 mol·L-1 for Sal-tyr, the minimum concentration of formation is 10-4 mol·L-1 for all other Sal-aas. Only Sal-his is generated at pH 9-10, while the minimum pH conditions for formation are 8 for Sal-gly and Sal-tyr, and 9 for other four. All Sal-aa but Sal-cys, whose concentration at 36 h is higher than that of newly produced one, decompose gradually since generation, with existing time of 24 h for Sal-gly and Sal-glu, and 48 h for other four.
2005 Vol. 25 (02): 174-176 [Abstract] ( 974 ) PDF (323 KB)  ( 364 )
177 Investigation on the Spectral Characteristics and Existing State of a Substituted 3H-Indole Molecular Probe in Triton X-100 Reverse Micelle
LUO Jun-jian, LI Jian, SHEN Xing-hai*,GAO Hong-cheng
The interactions between a fluorescent molecular probe, i. e., [2-(p-hexylamino) phenyl-3, 3-dimethyl-5-ethoxycarbonyl-3H-indole] methyldioctadecylammonium iodide (A) and Triton X-100/heptane/hexanol/water reverse micelle have been investigated by spectroscopy. Micropolarity of the environment, fluorescence anisotropy parameter and the pH effect of A in Triton X-100 reverse micelle were determined. Furthermore, the state of water in reverse micellar systems was studied by FTIR. According to the above experimental results, some information on the structure of Triton X-100 reverse micelle was obtained and the probable site of A in this system was discussed.
2005 Vol. 25 (02): 177-180 [Abstract] ( 1044 ) PDF (528 KB)  ( 359 )
181 S2→S0 Radiative Transition of 2,2’-Bipyridine Doped in Silica Gel Glass
QIAN Guo-dong, CHEN Miao，ZHANG Peng-yue, WANG Zhi-yu,WANG Min-quan
Doping 2,2’-bipyridine molecules in silica gel glass leads to special spectroscopic properties compared to those dissolved in liquid solutions. For the sample without heat treatment, two broad bands centered at 400 nm and 454 nm respectively, induced by the radiative transition from the first excited level S1 to the ground level S0 and attributed to the emission from an excited dimeric 2,2’-bipyridine species respectively, were observed. After heat-treated at 200 ℃, the excimer emission at 454 nm disappeared, and the sample exhibited another emission band centered at 325 nm due to the radiative transition from the second excited level S2 to the ground level. S2→S0 transition resulted from restricting 2,2’-bipyridine molecules in silica networks. Only the structure emission of S2→S0 transition was observed when heat-treated at 550 ℃, which indicates that most of 2,2’-bipyridine molecules were entrapped in the cages of Si—O network. The above results can be used to characterize the microstructural evolution of hybrid organic-inorganic optical materials.
2005 Vol. 25 (02): 181-183 [Abstract] ( 630 ) PDF (393 KB)  ( 381 )
184 Determination of Nitrite in Water Samples by Sequential Injection Analysis with Chemiluminescence Detection on Chip Flow Cell
WANG Yang, FAN Shi-hua*
A sequential injection chemiluminescence’s system using a chip flow cell was described for the determination of trace amount of nitrite in water samples. Nitride reacted with hydrogen peroxide to form peroxynitrous acid in sulfuric acid medium, which was an unstable in acid medium and subsequently was quenched into peroxynitrite in basic solution. During the composition of peroxynitrite the chemiluminescence intensity was enhanced with the presence of uranin and ethyldimethylcetylammonium bromide. The reaction coil (flow cell) and holding coil was combined for tracking the emission signal. The experimental parameters including physical and chemical parameter were optimized. The interference of cations in water samples was eliminated by passing previously the sample solution through a cation-exchange column. The linear range of the calibration graph was obtained from 1×10-6 to 1×10-4 mol·L-1 with a correlation coefficient of 0.999 8. The detection limit at 95% confidence was 6.8×10-7 mol·L-1. The relative standard deviation at 1×10-5 mol·L-1 nitrite level was 2.7% , and the recovery of 90%-99% and the sampling frequency of 80 h-1 were obtained.
2005 Vol. 25 (02): 184-187 [Abstract] ( 963 ) PDF (460 KB)  ( 335 )
188 Studies on the Effects of Steric Hindrance of Guest Molecule on the Formation of Inclusion Complexes by Molecular Luminescence
MU Jun-ze1，HUANG Gao-ling1, 2，ZHANG Yong1*
Fluorescence and room temperature phosphoresce (CD-RTP) induced by cyclodextrin methods were employed to investigate the effects of steric hindrance of guest molecule on the formation of inclusion complexes of β-cylcodextrin(β-CD) and bromonaphthalene(BrN). It has been found that the RTP intensity of 2-BrN/β-CD/n-Bu/ph was less than one third of that of 1-BrN/β-CD/n-Bu/ph and fluorescence emission spectra of 2-BrN/β-CD/n-Bu/ph had a red shift of 5-10 nm comparing with that of 1-BrN/β-CD/n-Bu/ph under the optimum experimental conditions，respectively. These results exhibited that the steric locations of bromine in BrN strongly influenced the formation of inclusion complexes. The determination of the two quadri-inclusion complexes constants further demonstrated that the steric hindrance has a great effect on the formation of inclusion complexes. According to the above experimental results, the mechanism of formation of inclusion complexes were discussed briefly.
2005 Vol. 25 (02): 188-191 [Abstract] ( 1490 ) PDF (424 KB)  ( 363 )
192 Determination of Total Effective Value of Flavonoids in Propolis by Quenched Electrochemiluminescence Analysis
XU Yang, CHU Hai-hong, QI Ying-ying, DI Jun-wei,TU Yi-feng*
Propolis is a kind of quality health foodstuff containing flavonoids, which is an important clinical effective component in many Chinese traditional medicines. The flavonoids could be used to reduce or clear free radicals, which manifests its medical functions. But there are no satisfactory methods to analyze the content of flavonoids in propolis. This paper reports a new method to determine the total effective value of flavonoids in propolis based on quenched effect for iodide-catalyzed electrochemiluminescence of luminol. It is a sensitive and simple method and might be a probable approach to examining the quality of propolis products.
2005 Vol. 25 (02): 192-194 [Abstract] ( 1132 ) PDF (333 KB)  ( 410 )
195 The Determination of Glutathione by Electrochemiluminescence Quenching Method
QI Ying-ying, WU Ying, DI Jun-wei, TU Yi-feng*
Glutathione is an important active substance in organisms. Its study and determination are very significant to human being’s health and life. In neutral medium, the quenching effect of reduced glutathione on the electrochemiluminescence of luminol-iodide was studied in this paper. Therefore a novel sensitive method for the determination of reduced glutathione was developed based on it. The linear response range of this method is from 3.38×10-13 mol·L-1 to 4.72×10-3 mol·L-1. This method is the most sensitive one and its linear range is the widest among those reported in the literature.
2005 Vol. 25 (02): 195-197 [Abstract] ( 1088 ) PDF (325 KB)  ( 367 )
198 FTIR Spectroscopic Explorations of Clinical Practice of Breast Cancer
LING Xiao-feng1, XU Zhi1, XU Yi-zhuang2*, LI Qing-bo2, ZHOU Su1, ZHANG Li2, ZHAO Hong-mei1, HOU Chun-sheng1, WANG Li-xin1, HOU Kuan-yong1, ZHOU Xiao-si1, WU Jin-guang2
The authors detected ten normal breast tissue samples and eight breast cancer samples by FTIR spectroscopy with an ATR probe. Nineteen variables of thirteen bands in the spectra were compared using standard statistic methods. The results demonstrated that bands of protein, lipid, carbohydrate, and nucleic acid from cancerous samples were significantly different from those from normal ones: (1) The relative intensity of N—H band increased and amide I band shifted to lower wave number significantly; (2)Symmetric and antisymmetric vibrations of —CH2 group, CO vibration, and relative intensity of (—CH2)n decreased; (3)The intensity of 1 160 cm-1 band was much weaker than that of 1 120 cm-1; (4)The band of PO or P—O—C shifted toward lower wave number. The authors believe that FTIR spectroscopy has a promising future in breast cancer diagnosis.
2005 Vol. 25 (02): 198-200 [Abstract] ( 1533 ) PDF (409 KB)  ( 370 )
201 Studies on Spectral Characteristics of Solid Propellant by Remote Sensing FTIR
LI Yan, HUANG Zhong-hua, ZHOU Xue-tie,WANG Jun-de*
The infrared spectral characteristics of high-intensity IR solid propellant were measured in this paper using a Bruker EQUINOX55 remote sensing FTIR spectrometer. The emission spectra of the combustion flame were recorded in the range of 4 700-1 800 cm-1 with a spectral resolution of 4 cm-1. The combustion temperatures of solid propellant at the burning time of 0, 9, 18, 27 and 36 s calculated from the molecular rotation-vibration spectra were 1 992.5, 1 610.9, 2 294.4, 2 361.1 and 1 916.9 K, respectively. Moreover, the spectral radiance distributions of the high IR flare material at different times were given, and the combustion product concentrations of HCl，HF，CO2 and CO were determined quantitatively. Results showed that remote sensing FTIR is a potential technology that can be applied to the measurement of IR spectral characteristics, especially to the identification of the IR objects, guidance and anti-guidance in the military, and the modification of the make-up of solid propellant.
2005 Vol. 25 (02): 201-203 [Abstract] ( 224 ) PDF (286 KB)  ( 416 )
204 In Situ FTIR Spectroscopic Studies of the Catalytic Combustion of Acid Red B on CuFe2O4 in the Presence and Absence of O2
WU Rong-cheng, QU Jiu-hui*, YU Yun-bo, HE Hong
The reaction process of catalytic combustion of ARB on CuFe2O4 in the presence and absence of O2 was studied by in situ DRIFT spectroscopy. The results showed that the decomposition of the sulfonic group of ARB molecule was not affected by the reaction atmosphere, but the decompositions of azo group and aromatic ring were markedly affected by the presence or absence of O2. The catalytic combustion of ARB was faster in air atmosphere than that in N2 atmosphere, and ARB could be completely oxidized to CO2 and nitrate at 300 ℃. But in N2 atmosphere, it was very difficult for the decomposition of ARB to complete at 300 ℃, even though air was introduced following this process. The temperature required for the rapid and complete decomposition would be as high as 500 ℃.
2005 Vol. 25 (02): 204-206 [Abstract] ( 1454 ) PDF (314 KB)  ( 370 )
207 Fast Outlier Detection for Milk Near-Infrared Spectroscopy Analysis
LIU Rong, CHEN Wen-liang, XU Ke-xin*, QIU Qing-jun, CUI Hou-xin
Near-infrared spectroscopy is a fast and efficient analytical technique based on multivariate calibration model, which correlates near-infrared spectra with the property of samples (such as concentration). The reliability of analytical results depends mostly on the accuracy of measured spectra. But outliers do not make for reliable data. The authors combined RHM (Resampling by Half-Means) with SHV (Smallest Half-Volume) method to detect the outliers of the near-infrared spectra of milk samples, and the results were satisfactory. The performance of the new method is superior to the traditional outliers detecting algorithms such as Mahalanobis distances and hat matrix leverage. And this combined method is simple and fast to use, conceptually clear, and numerically stable, so it is recommended to be used for the detection of multiple outliers in multivariate data, especially the online measurement and discriminant analysis.
2005 Vol. 25 (02): 207-210 [Abstract] ( 2024 ) PDF (524 KB)  ( 377 )
211 Spectral Analysis of Dissolved Organic Matter Derived from Rice Straw after Chemical Treatment
SHEN Qi-rong1, XU Yong1, YANG Hong2, ZHOU Li-xiang1, YU Qing3, ZHOU Zhi-ping3
Fourier transform infrared spectroscopy (FTIR), ultraviolet spectroscopy (UV)，and nuclear magnetic resonance spectroscopy (NMR) were used to study the chemical composition of Dissolved Organic Matter (DOM) derived from rice straw in the hydrolysis process with a dilute complex acid solution. The results obtained are as follows. FTIR spectra could indicate the changes of DOM during the hydrolysis process of rice straw. With the progress of rice straw hydrolysis, methyl, methylene, aromatic compounds and carbonhydrates decreased，most of aliphatic compounds were oxidized to CO2 and H2O, and others were turned into carbonates. Most of the organic silicon was hydrolyzed into inorganic silicon. The proteins, amino acids and other nitrogen were hydrolyzed to NH+4. All the recalcitrant fractions of rice straw, such as hemi-cellulose, cellulose and silicon sharply decreased during the process of chemical treatment. The results obtained in this paper proposed that the changes of DOM of rice straw in the hydrolysis could be an indication in the changes of chemical composition of rice straw during the hydrolyzation，and FTIR, UV and NMR were good methods to study the changes in the structure of organic compounds.
2005 Vol. 25 (02): 211-215 [Abstract] ( 1567 ) PDF (579 KB)  ( 378 )
216 Synthesis, Spectral Characterization and Bioactivity of Complexes of Furoylpyrazolone-Thiosemicarbazone
LI Jin-zhou, ZHANG guang-lin,SHA Jing-quan, AN Yu-mei
A new Schiff base containing sulphur, 1-phenyl-3-methyl-4-(α-furoyl)pyrazolone-5-thiosemicarbazone (HL) and its Zn(Ⅱ), Cd(Ⅱ) and Co(Ⅱ) complexes have been synthesized. On the basis of elemental analysis and molar conductance, the general formulae of the complexes, [ZnL2]·1.5H2O, [CdL2]·C2H5OH and [CoL2]·H2O, were given. They were characterized by IR, UV-Visible, 1H NMR, 13C NMR and magnetic moments. The results show that the metal ions exhibit coordination of six in the complexes. The antibacterial experiments indicate that they have high antibacterial activities against S. aureus, B. subtilis, E. coli, E. carotovora, and C. flaccumfaciens.
2005 Vol. 25 (02): 216-218 [Abstract] ( 1528 ) PDF (352 KB)  ( 371 )
219 Study on an Unknown Complex by Gas Chromatography/Infrared Spectrometry
CHEN Rui-ping1, YU Jun-qiang2, ZHENG Yu1*, REN Qing1
If the authors use normal infrared spectrometry, a lot of mixture compounds are difficult to characterize, because most of the peaks are overlapped in the spectra. Gas chromatography/Infrared spectrometry (GC-IR) are widely used in the separation and identification of organic complexes. The GC-IR can characterize the ingredients quickly and correctly that are difficult to do for normal infrared spectrometry. The technique also can be used to quantitatively analyze the ingredients by integral. The authors studied an unknown complex by GC-IR here.
2005 Vol. 25 (02): 219-221 [Abstract] ( 1004 ) PDF (288 KB)  ( 323 )
222 High Temperature Raman Spectra and Structure Character Study of BSO Crystal
QIU Huai-li1，WANG Ai-hua1，YOU Jing-lin2，LIU Xiao-jing1，CHEN hui2，YIN Shao-tang1
The structure character of BSO crystal at room temperature was generalized. The main Raman shifts of lattice vibration at room temperature were interpreted. The Raman spectra of BSO crystal were measured in a temperature range from 293 K to 1 123 K with high temperature Raman spectroscopy and time-resolved detection techniques. Temperature-dependence character of the Raman spectra of the crystal was investigated. The vibration mode of the longest bond Bi—O(1) in crystal shifts from 542 cm-1 to 512 cm-1 with the temperature increasing from room temperature to 1 123 K. It can be attributed to the fact that oxygen atoms are electrostatic bond to Bi atoms. The intensity of 88 cm-1 modes, which belongs to combination mode of bending and stretching in Bi3O4 unit, changes not so noticeably as other modes, and even the 58 cm-1 mode of Bi atoms motions in crystal lattice decreases rapidly when the temperature is higher than 873 K, which indicates that the framework structure of the crystal is broken down at high temperature, while the Bi3O4 unit still exists.
2005 Vol. 25 (02): 222-225 [Abstract] ( 396 ) PDF (414 KB)  ( 400 )
226 Spectroscopy Studies on the Interaction of Bis(p-Nitrophenyl) Esters and β-Cyclodextrin
LI Hong, HU Dao-dao, FANG Yu*, LIU Ya-ling
The bis(p-nitrophenyl) esters of succinic acid, adipic acid and sebacic acid have been synthesized, respectively, by employing 1,3-dicyclohexylcarbodiimide (DCC) as a dehydration agent. The composition and structure of the esters have been characterized by elemental analysis, FTIR, 1H NMR and DSC. Furthermore, the host-guest interactions of the esters with β-cyclodextrin (β-CD) have been studied systematically by using fluorescence quenching, fluorescence spectroscopy and UV-Vis spectroscopy measurements. It was demonstrated that the chain of the esters was longer, the interactions was weaker between the esters and the β-CD. Both p-nitrophenyl groups in bisp-nitrophenyl) esters of succinic acid can enter the inner cavity of β-CD. In contrast, only one of the groups in bis(p-nitrophenyl) esters of adipic acid can enter the cavity. For bis (p-nitrophenyl) esters of sebacic acid, however, both groups can not enter the cavity of the β-CD. The difference in the host-guest interactions of the three esters with β-CD has been attributed to the difference in the conformations adopted by the esters. Based upon these observations, it is proposed that the esters with short linker may be more suitable for construction of new networks, which are based upon, in concept, host-guest interactions.
2005 Vol. 25 (02): 226-231 [Abstract] ( 1640 ) PDF (754 KB)  ( 373 )
232 Study on the Interaction of Anticancer Drugs and DNA Using Fluorescence Spectroscopy
SHEN Jing-shan1, SUN Dan-dan2, FU Lian-chun4, Lü Wen-bo1, Lü Guo-wei1, YE Xue-min1, MENG Guang-zheng3, SONG Zeng-fu1*
Fluorescence spectroscopy has achieved great successes in the study on the interaction of drugs and DNA in both quantitative analysis and qualitative analysis. While the fluorescence probe technique can be used to measure the intensity of drugs-DNA interaction, because the injected drugs can change the fluorescence intensity of the probe. In this paper, the authors use berberine as a probe to measure the interaction intensity between some anticancer drugs and DNA, calculate the constant D and determine the effects of those drugs. In addition, the authors point out that this method can not be efficient for certain drug solution.
2005 Vol. 25 (02): 232-234 [Abstract] ( 1153 ) PDF (317 KB)  ( 429 )
235 Ultraviolet and Blue-Violet Photoluminescence of Gold Nanoparticles
ZHU Jian，WANG Yong-chang
Suspended gold nanoparticles (size range 20-30 nm) have been synthesized via electrochemical method. The emission spectra of gold colloidal nanoparticles were studied at room temperature. Fluorescence occurs at ultraviolet and blue-violet wavelengths. Two emission peaks were observed at 377 nm and 459 nm, respectively, when the corresponding excitation wavelength was at 220 nm. The emission peak at 377 nm increases with increasing particle density or excitation intensity, whereas the emission peak at 459 nm decreases with decreasing excitation intensity or increasing the particle density, and disappears below the threshold. With increasing the slit width, the intensity difference between these two emission peaks decreases and the ratio approaches 1. All these observed results are in agreement with the theory of self-organized random micro-cavity. It is indicated that the fluorescence emissions in ultraviolet and blue-violet wavelength regions are induced by the multiple scattering in a disordered gold nanoparticles system. And these photoluminescence features suggest the possible future applications in the areas of optical data storage and full color display.
2005 Vol. 25 (02): 235-238 [Abstract] ( 976 ) PDF (570 KB)  ( 379 )
239 The Research on the Quenching of Fluorescence Spectra of TOPⅠ by Iodine Anion
XIA Bing-le1, PENG Dun-geng1, LI Min-li1, XIAO Hong2, WANG Kai-bao3
Comparing the fluorescence spectra of tobacco peroxidaseⅠ(TOPⅠ) solution and the solutions titrated by iodine anions，the number of binding locus and the binding constant of iodine anion to TOPⅠ were calculated by using the modified Stern-Volmer equation. The mechanism of the quenching of fluorescence spectra and the distribution of tryptophane residues in the TOPⅠ molecule were discussed.
2005 Vol. 25 (02): 239-241 [Abstract] ( 994 ) PDF (378 KB)  ( 381 )
242 Influence of Excitation Light Wavelength on the Fluorescence Spectra of Ethanol Solutions
LIU Ying1, 2, LAN Xiu-feng1, SHEN Zhong-hua1, LU Jian1, NI Xiao-wu1*
Ethanol solution can emit visible fluorescence when induced by UV light. With emission spectral profiles similar on the whole, the peaks are red-shifted distinctly when the excitation light alters from 200 to 250 nm. And the spectral profiles of ethanol solutions with different concentrations are also red-shifted when induced by the same wavelength of excotation light. A thorough analysis of the rule of spectrum peaks that are red-shifted is carried out and discussed in theory and in experiment. Investigation on the intrinsic fluorescence spectrum of ethanol solution and its characteristics will contribute to the study of the fluorescence spectra when ethanol serves as a solute and hydrolysis catalyst. Especially, this study will also help to offer a sensitive method of the determination of ethanol.
2005 Vol. 25 (02): 242-245 [Abstract] ( 1041 ) PDF (456 KB)  ( 406 )
246 Study on the Interaction of Pb2+ and Bovine Serum Albumin by Fluorescence
WU Gen-hua1，WANG Chun-hua2
The interaction of Pb2+ and bovine serum albumin(BSA) was studied under conditions similar to those in human bodies by fluorescence spectra. The results indicated that tryptophan and tyrosine, which were located in BSA, had a max fluorescence emission peak at 341 nm with an excitation wavelength of 283 nm. It was shown that Pb2+ had a powerful ability to quench the BSA fluorescence with a mechanism of a static process rather than a dynamic one. The apparent quenching constant Kq was obtained to be 9.5×1012 L·mol-1·s-1 by Stern-Volmer equation. The apparent complexation constant of Pb2·BSA is lgK=11.61. The nitrogen in BSA could coordinate with lead in Pb2-BSA.
2005 Vol. 25 (02): 246-248 [Abstract] ( 1061 ) PDF (392 KB)  ( 346 )
249 Inhibitory Kinetic Fluorimetric Determination of Trace Aniline
FENG Su-ling, WANG Jin, FAN Jing, CUI Feng-ling
An inhibitory kinetic fluorimetric method is reported for the determination of trace aniline. The proposed method is based on the inhibitory effect of aniline on the reaction of potassium periodate oxidation of rhodamine 6G in phosphoric acid medium. The detection limit is 7.2 ng·mL-1，the linear range of the determination is 0.010-0.183 μg·mL-1. This method has been applied to the determination of trace aniline in phenolic tubes and water samples with satisfactory results.
2005 Vol. 25 (02): 249-251 [Abstract] ( 1617 ) PDF (420 KB)  ( 369 )
252 Assay of Three Kinds of Aluminum Fractions (Ala, Alb and Alc) in Polynuclear Aluminum Solutions by Al-Ferron Timed Spectrophotometry and Demarcation of Their Time Limits
WANG Chen-yi1,2, ZHANG Cai-hua1, BI Shu-ping1*, ZHANG Zhen-chao3, YANG Wei-hua3
Al-Ferron timed spectrophotometry assay is a basic method in the study on the formation of polynuclear hydroxyl aluminum species and their transformation laws in aqueous systems. In actual working process, this methodology has some dogmatism and arbitrariness in the time limits demarcation of the three kinds of aluminum fractions (Ala, Alb and Alc) in polynuclear aluminum solutions, which makes this kind of classification rougher, and the experimental results non-reproducible. The reason for this difference is that the specific species within Ala, Alb and Alc have different reaction mechanism and dynamics, and that specific species of Alb having different OH／Al ratios have different reaction rates with ferron. In this paper, the ExpAssoc distribution was applied to quantitatively fit the Al-Ferron reaction dynamics curve, and the extrapolation method was used to survey the 1 min measured value [Ala] of monomeric Al, which is hard to obtain in manual manipulation. The time demarcation between Alb and Alc should reach the point of the experimental data curve up to horizontal platform. The microwave-radiated technology was used to fast assay the total aluminum concentration [AlT]. With these methods, the contents of monomeric Ala, polynuclear Alb and gel Alc can be conveniently and quantitatively measured. It offers a novel method for surmounting the arbitrariness in the measurement of the three kinds of aluminum fractions and the repetitive calculation of Ala and Alb.
2005 Vol. 25 (02): 252-256 [Abstract] ( 424 ) PDF (537 KB)  ( 398 )
257 Synthesis of 2,3,4-Trihydroxyacetophenone Hydrazones and Study on Their Spectral Properties
LIU Jian-ning, WU Bo-wan, ZHANG Bing, YU Xin-qiao
2,3,4-trihydroxyacetophenone was synthesized with pyrogallol. Benzoylhydrazone and p-hydroxybenzoylhydrazone were synthesized using the reaction of ethyl benzoate and methyl p-hydraxy benzoate with hydrazine hydrate. Three novel 2,3,4-trihydroxyacetophenone hydrazones were synthesized using the reaction of 2,3,4-trihydroxyacetophenone with benzoylhydrazone, p-hydroxybenzoylhydrazone and phenylhydrazine. IR, UV and the fluorescence spectrum of 2,3,4-trihydroxyacetophenone hydrazones were studied.
2005 Vol. 25 (02): 257-259 [Abstract] ( 1220 ) PDF (313 KB)  ( 410 )
260 Analysis of Spectral Properties of Oil Matrix Raw Materials in Skin Care Products
HUANG Chong1, OUYANG Yan-dong1*, FANG Yi-wen2
There are many kinds of oil matrix raw materials used in skin care products. Their spectral properties are different. The matrix raw material that has better ultra-violet absorption will enhance the sun-screening agent effect obviously. In the present article the spectral properties of six oil matrix raw materials often used in skin care products were mainly measured and analyzed by spectrophotometer. The analysis of T-λ spectra shows that castor oil can absorb ultraviolet as well as near infrared light. It was shown that castor oil chosen as the matrix raw material will improve the effect of sun-screening agent and enhance the products. The function of sun-screening agent and skin health care product will stand out clearly.
2005 Vol. 25 (02): 260-262 [Abstract] ( 1568 ) PDF (345 KB)  ( 363 )
263 Speciation Analysis of Selenium by Flow-Injection Catalytic Spectrophotometry
FAN Jing, Lü Hui-xiong, YE Cun-ling,CUI Feng-ling
A new flow-injection catalytic spectrophotometric method was proposed for the determination of Se(Ⅳ) based on its catalytic effect on the reduction reaction of azure I by Na2S in pH 7.0 citric-acid sodium-hydrogen-phosphate buffer solution. Some different schematic diagrams of FIA were compared. Effects of the flow rates of reagents and sample, the medium and its acidity, the temperature, and coexistent substances were studied respectively. The amount of used reagents and the experimental conditions for sampling volume and coil length were optimized by using the controlled and weighed centroid simplex method. The Linear range of the determination is 0.1-2.0 mg·L-1, the detection limit is 0.015 mg·L-1, the relative standard deviation is less than 3.1%, and the sampling frequency is 120 samples per hour. The method has been applied to the determination of organic selenium and inorganic selenium in garlic and selenium-yeast. It was found that garlic had a strong enriching effect for selenium, and the conversion ratio of organic selenium decreased with increasing the concentration of selenium in the environment. The recovery of this method is 97.1%-104.3%.
2005 Vol. 25 (02): 263-265 [Abstract] ( 400 ) PDF (366 KB)  ( 388 )
266 Quantitative Determination of Total Flavonoids in Sea-Buckthorn Fruit Juice by Three Wavelength Spectrophotometry
HUI Rui-hua，HOU Dong-yan，GUAN Chong-xin，LIU Xiao-yuan
Numerous studies dealing with the quantitative determination of total flavonoids in sea-buckthorn fruit juice by spectrophotometry are presented. The flavonoids in sea-buckthorn fruit juice and aluminate produce stable complex whose absorption occurred at longer wavelength. To determine the total flavonoids in sea-buckthorn fruit juice by traditional spectrophotometry method，baseline shift and asymmetric absorption peak occurred on the absorption curve. Quantitative determination of flavonoids in sea-buckthorn fruit juice by three wavelength spectrophotometry method can eliminate the absorbance error caused interfering components in turbid solution and the scattering effect. Back ground changing with the concentration change and asymmetric absorption peak problems can also be solved. The regression equation of concentration vs ΔA was obtained：ΔA=-0.007 03+0.000 48ｃ with a relation coefficient γ=0.999 1. The experimental results demostrate the total flavonoids concentrations in 0-800 μg·mL-1 with ΔA obeying linear relation when the absorbance was measured at wavelength λ1=495 nm, λ2=415 nm and λ3=368 nm. The recovery is 97.0%-101.0% and the coefficient of variation is 0.058%(n=9). The method is more advantageous than tranditional spectrophotometry method.
2005 Vol. 25 (02): 266-269 [Abstract] ( 381 ) PDF (423 KB)  ( 362 )
270 Study on the Measurement of Residual Stresses around Indentations in SiC/Al2O3 Nanocomposite Using Fluorescence
TAO Jie，CUI Yi-hua，LI Yang
The residual stresses induced by an indentation were studied in 5% SiC/Al2O3 nanocomposite using fluorescence spectroscopy in this work. It was found that within the indentation and the region of about 10 μm outside the impression, the broadening of the R-lines is obvious, and that the compression shift is a strong function of the distance from the indentation centre. From the observed frequency shifts, the hydrostatic stresses in regions sampled in the indentation, and in the complex stress field surrounding it were measured. The same variation regularity of stresses exists along the diagonal direction and the side vertical bisector direction. The symmetry of the residual stress field around the indentation was also found.
2005 Vol. 25 (02): 270-273 [Abstract] ( 1398 ) PDF (501 KB)  ( 345 )
274 Preparation of Ce-Loaded Nano-TiO2 and Study on Its UV-Vis Reflective Spectrum
LIU Xue-feng1, 3, ZHANG Li2, TU Ming-jing3
Ce-loaded nano-TiO2 was prepared by the loading technology of metallic ions, and was characterized by XRD and TEM. The UV-Vis reflective spectra of nano-TiO2 and Ce-loaded nano-TiO2 were analyzed. The result shows that after loading rare earth element Ce the reflective spectral characteristic of nano-TiO2 moves to the visible region with a red shift to 500 nm, and the obvious change takes place in the absorbance in the visible spectral range with a three-fold enhancement. It is indicated that the load of rare earth element Ce is favorable to enhancing the absorption of visible and UV light of anatase nano-TiO2, and thereby greatly increases its photocatalytic activity.
2005 Vol. 25 (02): 274-276 [Abstract] ( 1049 ) PDF (478 KB)  ( 390 )
277 Ultraviolet Spectral Characteristics of Charge-Transfer Reaction Complex in Micellar System and Its Application
DU Li-ming, CHEN Cai-ping,LI Jian-hua
Charge-transfer (CT) reaction of chloranil (TCBQ) as a π-electron acceptor with fleroxacin (FLX) as an electron donor has been studied by ultraviolet spectrophotometry method. Experiment showed that FLX reacted with TCBQ in sodium dodecyl sulfate(SDS)micellar systems, and a stable complex was formed and the absorbency was remarkably enhanced. Therefore, a simple, rapid, accurate and sensitive method for the determination of FLX has been developed. Beer’s law is obeyed in the range of 0.6-24 mg·L-1 of FLX and r=0.999 3. The apparent molar absorptivity of CT complexes at 326 nm is 3.3×104 L·mol-1·cm-1. The composition of CT complex was found to be 1∶1 by Bent-French and curved intersection methods. The proposed method has been applied to the determination of ESL in tablets. The recoveries are 99.2%-99.7%. The relative standard deviation is 0.7%-2.1%. The proposed methods are suitable for the routine quality control of drug alone and in tablets or capsules without fear of interference caused by the excipients expected to be present in tablets or capsules.
2005 Vol. 25 (02): 277-279 [Abstract] ( 1645 ) PDF (363 KB)  ( 385 )
280 Determination of Twenty One Elements in Lithium Hexafluorophosphate by ICP-AES
FANG Yi-wen，HAO Zhi-feng，SONG Yi-bing，SUN Chang-yong，YU Jian，YU Lin
One gram (±0.000 1 g) of lithium hexafluorophosphate was weighed exactly under dry atmosphere and was dissolved with an adequate amount of dimethyl carbonate(DMC). After the sample solution was pretreated with a series of methods, Be, Cu, Pb, Ca, Zr, Co, Mg, V, Ti, Mo, Ni, Mn, Sr, Zn, K, Al, Ba, Cd, Fe, Cr and Na were determined by ICP-AES. The results show that the recoveries of standard addition were 93.3%-102.1%, and the relative standard deviations(n=11)were 0%-3.56%. The method is efficient, accurate and easy to operate. It has been applied to the determination of lithium hexafluorophosphate products with satisfactory results.
2005 Vol. 25 (02): 280-282 [Abstract] ( 1471 ) PDF (322 KB)  ( 386 )
283 Determination of Trace Zirconium and Hafniumin Sample by Atomic Emission Spectrometry
LI Hui-zhi，YANG Chun-xia，ZHAI Dian-tang
This paper describes the determination of trace Zr and Hf in the sample using carbon powder and titanium oxide as the buffer by Atomic Emission Spectrometry(AES). Titanium was selected for the internal standard line. Sample separation and chemical treatment were not required. The sample was directly loaded into an ordinary electrode. The method is simple, rapid and accurate. The conditions for the determination, and the factors of influence have been studied. A new method has been developed for the determination of zirconium and hafnium. The analytical lines of Zr and Hf were 327.3 and 286.6 nm respectively. The internal standard line of Ti was 308.8 nm. The linear range of the determination of Zr and Hf was 0-0.50% and 0-0.25% respectively. The detection limit of Zr and Hf was 0.001 0% and 0.010% respectively. The range of the recovery of zirconium and hafnium was 96.67%-105.0%. The results for these elements in standard sample are in agreement with certified values with a precision of 3.61% RSD for Zr(n=9), and 4.82% RSD for Hf(n=9). The method has been applied to the determination of Zr and Hf with satisfactory results.
2005 Vol. 25 (02): 283-285 [Abstract] ( 556 ) PDF (332 KB)  ( 341 )
286 Speciation Analysis of Mercury in Traditional Chinese Medicine by Vapor-Generation Atomic Fluorescence Spectrometry
YANG Li-li1, LI Na2, ZHANG De-qiang3*, GAO Li-rong2，KANG Hai-yan2
A sensitive method has been proposed for the determination of inorganic mercury and total organic mercury in traditional Chinese medicine(Wanshi Niuhuang Qingxin) by vapor-generation atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity of Hg and the oxidization of organic mercury were investigated and optimized. Thiourea citric acid was selected as a sensitization agent, which greatly enhanced atomic fluorescence signal intensity of mercury. The influence of foreign ions and their elimination were studied. The detection limit of the method for Hg was 7.6 ng·L-1 and the relative standard deviation was 1.56%-3.28% for Hg. The proposed method was successfully applied to the determination of mercury speciation in real samples with a recovery range of 90.3%-110.3%.
2005 Vol. 25 (02): 286-289 [Abstract] ( 1585 ) PDF (463 KB)  ( 396 )
290 Determination of Trace Silver by Flame Atomic Absorption Spectrometry Using Chitosan Enriching Method
SUN Jian-min, XU Peng, HAN Xue-tao, SUN Han-wen
A method for the determination of trace silver by flame atomic absorption spectrometry using chitosan enriching method has been investigated. The conditions that influence the adsorption of silver by chitosan were studied. The optimal flow rate of the sample solution was 1 mL·min-1, and the optimal sorption (96.7%) was possible by using the systems with pH 6.0 for silver. The amount of saturated adsorption of silver in the chitosan was 97.8 mg·g-1. Silver was eluted from the chitosan by 1 mol·L-1 H2SO4. 100 mg·mL-1bp>b2+ and Zn2+ did not disturb the determination of silver. K+, Na+, Ca2+, Mg2+ and Mn2+ did not disturb the determination of silver because they were not adsorbed by chitosan. The method has been applied to the determination of silver (1.83 μg·mL-1) in waste water sample with a recovery of 94.3%.
2005 Vol. 25 (02): 290-292 [Abstract] ( 196 ) PDF (308 KB)  ( 355 )
293 Determination of Eight Trace Elements in the Flowers of Hylocereus Undatus by FAAS
WANG Xin-ping
The effects of different sample digestives for the flowers of hylocereus undatus are compared. Eight trace elements in the flowers of hylocereus undatus were determined by flame atomic absorption spectrophotometer. The result shows that the RSD and recovery are better if the flowers of hylocereus undatus was digested with HNO3-HClO4(5∶1) mixed acid, and the flowers of hylocereus undatus contains many essential elements among which the contents of Fe, Mn and Zn are higher than those of Ni and Cu. Co and Cd were not determined, but Pb was determined. The experimental results showed that the detection limits were all smaller than 0.086 μg·mL-1, the RSDs (n=8) all smaller than 8.37%, and the addition standard recovery(ASR)(n=8) was 79.69%-118.6% for all elements.
2005 Vol. 25 (02): 293-295 [Abstract] ( 1446 ) PDF (333 KB)  ( 368 )
296 Analysis and Separation of Organic and Inorganic Speciations of Soluble Zinc in Edible Flowers
PENG Shan-shan，HUANG Guo-qing
Considering the medicinal effects of the edible flowers, the authors studied the separation of trace element zinc’s soluble organic and inorganic speciations in water decoction of three edible flowers: Chrysanthemum, Cottonrose hibiscus and Honeysucker by using the 0.45 μm membrane filter and amberlite XAD-2 macroreticular resins. And trace element zinc contents were determined by atomic absorption spectrometry. The optimal conditions for separation had been established. This study verifies the economic value of developing edible flowers, and provides theoretical basis for developing edible flowers as the third functional food materials.
2005 Vol. 25 (02): 296-298 [Abstract] ( 391 ) PDF (406 KB)  ( 359 )
299 Characterization of Dinosaur Fossils and Their Surrounding Rocks by Atomic Emission Spectrometry and X-Ray Powder Diffractometry
YANG Qun1, WANG Yi-lin1，LI Chao-zhen2，YUAN Bo3
More dinosaur fossils have been found in the Laochangqing valley, Lufeng county than anywhere else in the world, and the dinosaur fossils found here cover the longest time span (including the early and middle Jurassic ages). This excavation offers an ideal experimental base for prehistoric biology studies. This paper presents an elementary analysis of the components and structure of the dinosaur fossils in three different geologic-layers and their surrounding rocks in the above mentioned area. Atomic emission spectrum shows that the fossils are rich in the contents of calcium (＞5%) and phosphor, but low in the content of silicon (3%-8%), while the surrounding rocks are high in the content of silicon (＞10%). Furthermore, XRD results show that the major compound of the fossils is CaCO3(66%), followed by SiO2(17%); while that of the surrounding rocks is SiO2(＞80%), followed by CaCO3(＜12%). The most important difference between the fossils and the surrounding rocks is, according to the experiment, that phosphate has been identified in the former but not in the latter. This is a characteristic that can be used to distinguish the dinosaur fossils from other rocks. This paper provides valuable data for further zoological studies on the living conditions and evolution of the dinosaurs in the Laochangqing valley, Lufeng county.
2005 Vol. 25 (02): 299-301 [Abstract] ( 2027 ) PDF (354 KB)  ( 365 )
302 Investigations on the Movement of Pigment Particles in the Electrophoretic Liquids
ZHANG Yan-fen, TENG Feng*, XU Zheng, DUAN Xiao-xia, LIANG Chun-jun, BING Xiu-hua
In the present report, the authors studied the movement of pigment particles which decide the display status, enduced the equation of the motion and the expression of reflectivity, and estimated the value of the delay time. Combining the above theoretical conclusion with the experimental results, the authors discussed the feasibility of the passive matrix addressing of electrophoretic image displays, and provided good advice on how to acquire display devices of good quality.
2005 Vol. 25 (02): 302-306 [Abstract] ( 1365 ) PDF (609 KB)  ( 339 )
307 Spectral Similarity Measure and Retrieval Based on the Complete Spectral Reflectance and Absorption Feature ——Nonlinear Spectral Angle Mapper
TANG Hong, FANG Tao, SHI Peng-fei
A novel method for spectral similarity measure, which is called nonlinear spectral angle mapper, is presented. In this method, on one hand, nonlinear transformation and removing high relativity among bands are used through kernel PCA; on the other hand, the feature of both spectral reflection and absorption are combined in transformed space. At last, spectral angle mapper is used to measure spectral similarity. The authors′ experiments show that this method is effective in spectral similarity retrieval.
2005 Vol. 25 (02): 307-310 [Abstract] ( 1053 ) PDF (361 KB)  ( 344 )
311 A New Method of Avoiding Entrainment Swelling in Liquid Surfactant Membrane for the Determination of Trace Hg(Ⅱ)
YU Hui-fen，XU Lin-lin，DING Peng
Entrainment swelling consists of occlusion swelling and reliquefaction swelling. Entrainment swelling is significant to industrialized liquid surfactant membrane in the process of operation. The present study based on the life-span of W/O emulsion and O/W emulsion discussed the process of forming entrainment swelling. The result shows that no matter what surface-active agent was used, the life-span of W/O emulsion is 20-88 times longer than that of O/W emulsion. After oil drop was dispersed in water，no swelling was discovered, thus, the ratio of swelling is less than that by other method. The new method of determination of trace mercury by avoiding entrainment swelling in liquid surfactant membrane and FAAS is described. The precision(RSD) and recovery are 1.9%-2.3％ and 99.8％-101.1% respectively. Hg2+ at ng·g-1 level can be enriched and determined. This method can be used in the determination of trace mercury in waste water.
2005 Vol. 25 (02): 311-313 [Abstract] ( 1459 ) PDF (305 KB)  ( 366 )
314 Studies on the Constituents of Polysaccharide and the Content of Saccharide from Mongolian Medicine Hara Buri-16
ZHAO Yu-ying
This article describes the extraction of dissolvable polysaccharide from Hara Buri-16, and using phenyl hydrate-sulfuric acid to determine the content of dissolvable polysaccharide. The average recovery is 101.1% and RSD is 0.94%. The components of water soluble polysaccharide were identified by gas chromatography as：fucose, arabinose, xylose, mannose, galactose and glucose in the molar ratio of 0.57∶6.67∶0.46∶6.61∶2.47∶4.80 respectively.
2005 Vol. 25 (02): 314-316 [Abstract] ( 1311 ) PDF (417 KB)  ( 360 )
317 Determination of Lead and Cadmium Contents in Chicken Granules and Gourmet Powder
SHI Min1, HAO Ai-guo1, ZHU Li-zun2
Through atomic absorption detector, the contents of Pb and Cd in chicken granules and gourmet powder were determined. From the result it was found that there are differing contents of pollutant elements, i.e. 0.00-10.00 μg·mL-1 for Pb and 0.00-4.00 μg·mL-1 for Cd, respectively. The relative standard deviations of Pb and Cd are 3.15% and 4.26%，respectively. At the same time, a recovery experiment for Pb and Cd in chicken granules and gourmet powder were performed, and the recoveries are 96.7%-102.1% for Pb and 91.9%-107.6% for Cd, respectively.
2005 Vol. 25 (02): 317-318 [Abstract] ( 1039 ) PDF (221 KB)  ( 369 )

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