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2004 Vol. 24, No. 11
Published: 2004-11-26
 
       光谱学与光谱分析
1281 Formation and Emission Spectra of C2 Swan Bands during the Reaction of Laser Ablation Al Plume with CF4，CCl4 and CH2Br2 Beams
ZHANG Shu-dong1, 2, LI Hai-yang1*
The emission spectra of C2 Swan bands transition were observed in 430-600 nm region by Q-switched laser ablation target of Al reacting with CF4，CCl4 and CH2Br2 beams. Five vibration band sequences (Δｖ=2，1，0，-1 and -2) of d3Πｇ-a3Πｇ were identified and the largest vibration number of excited state d is 6. Using a local thermal equilibrium model, the vibrational temperature of d state was determined to be about 6 000 K. Meanwhile, some bumps, separated by about 0.3 nm, were observed between vibrational bands of Δｖ=0 and -1 sequences, which were due to accidental and periodical accumulations of rotational lines belonging to several vibrational bands. The formation mechanism of excited C2 ｄ3Πｇ state is considered as when laser induced Al plasma expansion in the background reaction gas sample, the collisions between metal particles and gas sample molecules cause the dissociation of precursors, so atomic C is produced. Meanwhile, the shock wave induced by plasma expansion might cause molecules dissociation as well. Then C atoms combine to form C2 in the ground state X1Σ＋ｇ(Te=0 cm-1) or first excited state ａ3Πｕ(Te=716 cm-1). The electronic energy transfer between excited state Al (2S1/2)(Te=25 348 cm-1) and C2 ａ3Πｕ state produces the excited state ｄ3Πｇ(Te=20 022 cm-1). Another mechanism that may be possible is that ｂ3Σ-ｇ state of C2 is produced first, then undergoes a radiationless transition into ｄ3Πｇ state through crossing with the ｄ3Πｇ,ｖ′＝6 level. But the vibrational population of ｖ′＜6 levels is formed by collision relaxation.
2004 Vol. 24 (11): 1281-1284 [Abstract] ( 1393 ) PDF (965 KB)  ( 430 )
1285 Synthesis and Spectroscopy of Dawson Molybdovanadophosphoric Acid Charge-Transfer Complexes
GAO Li-hua1, 2, WANG Ke-zhi1*, XIN Xiu-lan2, LI Qian2
A series of organic-inorganic charge-transfer complexes formed by (E)-N-butyl-4-(2-(4-dimethylaminophenyl)ethenyl)pyridinium bromide with Dawson molybdovanadophosphorate have been synthesized and characterized by elemental analyses, thermogravimetric analyses, UV-Vis, IR and X ray photoelectron spectroscopy. IR spectrum confirms the presence of the same type of stacks and presence of the hemicyanine cation and the molybdovanadophosphorate anion in the title complexes. The results show that 6∶1 supramolecular complexes are formed between the hemicyanine cations and the heteropoly anions, and the charge transfer occurs from the hemicyanine cations to the heteropoly anions. The interaction between the hemicyanine cations and the heteropoly anions in the solid powder is stronger than in the fluid solution. The compounds reported in this paper are interesting as catalysts and nonlinear optical materials.
2004 Vol. 24 (11): 1285-1287 [Abstract] ( 1556 ) PDF (863 KB)  ( 351 )
1288 Study of Radicals in Pulsed Corona Discharge by Emission Spectroscopy
WANG Wen-chun, LIU Feng, ZHANG Jia-liang, REN Chun-sheng
The emission spectra of OH(A2Σ→X2Π, O—O), O(3p5P→3s5S02) and Hα(3P→2S) produced by the positive pulsed corona discharge of N2 and H2O mixture in a needle-plate reactor have been successfully recorded against a severe electromagnetic interference coming from the pulsed corona discharge at one atmosphere. The relative populations and the vibrational temperature of N2(C, v′) were determined. The emission intensity of OH(A2Σ→X2Π, 0—0) is obtained through the simulation of the emission spectra of the Δv=+1 vibration transition band of N2(C3Πu→B3Πg). Relative populations of OH(A2Σ), O(3p5P) and Hα(3P) have been obtained by the emission intensity of OH(A2Σ→X2Π, 0—0), O(3p5P→3s5S02) and Hα(3P→2S) and Einstein’s transition probability. The effects of discharge voltage and pulse repetition rate and oxygen flow on the relative populations of OH(A2Σ), O(3p5P) and Hα(3P) are investigated.
2004 Vol. 24 (11): 1288-1292 [Abstract] ( 1735 ) PDF (916 KB)  ( 665 )
1293 Mechanism of Resonance-Enhanced Multiphoton Ionization of NO Molecule
ZHANG Gui-yin1, 2，ZHANG Lian-shui1，YANG Xiao-dong1，SUN Bo1
NO molecule is a diatomic molecule with different nucleus. It is a serious pollutant and is harmful to the health of the generation. It comes mainly from inflammation process using coal as burning material. So researchers have always been interested in it. The Resonance-Enhanced Multi-Photon Ionization (REMPI) spectrum of NO has been obtained in the range of 420-480 nm with a Nd:YAG laser pumped optical parametric generator and amplifier as the radiation source. The ionization pathway of NO molecule was acquired with the assignment of the spectral lines. NO molecules are ionized via the resonant intermediate state Α2Σ＋ and by a (2+2) REMPI process. On the basis of theoretical rate equation and with the condition that the duration of the laser pulse is very short (approximately 35ps), the dependence of ion signals on laser intensity was deduced. The variation of the ionization signal versus laser intensity is near quartic. This is in good agreement with the experimental result.
2004 Vol. 24 (11): 1293-1295 [Abstract] ( 1443 ) PDF (849 KB)  ( 449 )
1296 Comparative Research on Attenuation Characteristics of Human Bladder Cancer Tissue at Different Wavelengths of Laser and Their Linearly Polarized Laser in Vitro
WEI Hua-jiang1, XING Da1*, WU Guo-yong2, JIN Ying1, GU Huai-min1
In this paper, a double-integrating-spheres system, the basic principle of measuring technology of ray radiation, and the optical model of biological tissues were used for the study. Attenuation characteristics of human bladder cancer tissue at 467.5, 488, 496.5, 514.5 and 532 nm laser and their linearly polarized laser irradiation were studied. The results of measurement showed that the attenuation characteristics of human bladder cancer tissue in Kubelka-Munk two-flux model were different at different wavelengths of laser irradiation in the range of five different laser wavelengths. There were significant differences in the total attenuation or effective attenuation coefficients of human bladder cancer tissue at 476.5, 496.5, and 532 nm wavelengths of laser and their linearly polarized laser irradiation(P＞0.05), and there were no significant differences at 488 and 514.5 nm wavelengths of laser and their linearly polarized laser irradiation in two-flux model(P＞0.05). The total attenuation and effective attenuation coefficients of human bladder cancer tissue at 532 nm laser and its linearly polarized laser irradiation were obviously bigger than those at other four different wavelengths of laser and their linearly polarized laser irradiation in two-flux model. The total attenuation and effective attenuation coefficients of human bladder cancer tissue at five different wavelengths of laser and their linearly polarized laser irradiation increased with the decrease of these wavelengths, there were significant differences in those at 476.5, 496.5 and 514.5 nm wavelengths of laser and their linearly polarized laser irradiation(P＜0.05), and there were no significant differences in those at 488 and 532 nm wavelengths of laser and their linearly polarized laser irradiation in light transport theory(P＞0.05).
2004 Vol. 24 (11): 1296-1298 [Abstract] ( 632 ) PDF (832 KB)  ( 369 )
1299 Photolytic Spectroscopy of Cs2 Molecules
LIU Jing, LEI Zhen-zhou, ZHOU Xiao-yan, DAI Kang, SHEN Yi-fan*
Populations of the n2L(nL=7P，6D)states of Cs atoms by photodissociation of Cs2 molecules through the use of the fixed frequence line 441.6 nm of a He-Cd laser radiation are produced. Combining ratios of atomic to molecular fluorescence at the Cs density range between 1 and 9×1015 cm-3, the ratios of collisional rate coefficient to predissociation rates are estimated to be 2.9×10-17 cm3 and 7.4×10-18 cm3, respectively. The branching ratios are defined as the ratios of nLJ to nLJ’ fluorescence. The ratios of the dissociation rates produced in n2L fine-structure states are 0.53 and 0.43, respectively. Fine-structure changing cross section has been measured for far wing excitation, the result is consistent with cross section obtained from other excitation of the n2L states. The cross section for excitation transfer out of the 6D doublet [i.e., Cs(6D)+Cs(6S)→states other than Cs(6D)] is 1.9×10-14 cm2.
2004 Vol. 24 (11): 1299-1301 [Abstract] ( 1393 ) PDF (854 KB)  ( 415 )
1302 Concentration Dependence of Luminescence under Different Excitation Wavelength in Y2O2S:Sm3+ Phosphor
LEI Bing-fu1, 2, LIU Ying-liang2, TANG Gong-ben1, YE Ze-ren1, SHI Chun-shan1*
The concentration dependence of luminescence under different excitations in Y2O2S:Sm3+ phosphor has been studied. The optimum activator concentration was found to be a function of the number of excited activator ions as well as the excitation wavelength. The concentration dependence curve of Y2O2S:Sm3+ phosphor under 413 nm excitation was different from the curve obtained with 263 nm excitation. For excitation radiation having longer wavelength (413 nm), the concentration quenching of Y2O2S:Sm3+ phosphor occurred at about 2%, which is ten times as the result with shorter wavelength (263 nm) excitation (-0.2%). Fitting the concentration dependence curve and the result shows that the cross-relaxation caused by the dipole-quadrupole interaction of neighboring Sm3+ ions results in the concentration quenching.
2004 Vol. 24 (11): 1302-1305 [Abstract] ( 998 ) PDF (871 KB)  ( 339 )
1306 Influence of Pr3+ on Eu3+ Luminescence in Three Component Complex System of Eu(ClO4)3-DPSO-Phen
LI Wen-xian，ZHONG Rui-xia，LUO Qing-shan
Different nuclear [(Eu1-xPrx)(DPSO)(phen)3(ClO4)2]ClO4·nH2O(x=0.000-0.200，DPSO as the abbreviation for diphenyl sulfoxide and phen for 1,10-phenanthroline，n=1-6) coordination compounds were synthesized，and were studied by means of composition analysis, conductance, IR spectra and fluorescence excitation and emission spectra. In the fluorescence spectra it was found that Pr3+ has a great influence on the luminescence of Eu3+. The fluorescence emission intensity of europium perchlorate was enhanced when doped with 0.001→0.100 mol Pr3+. The local symmetry of Eu3+ site is low in this coordination compounds.
2004 Vol. 24 (11): 1306-1308 [Abstract] ( 936 ) PDF (844 KB)  ( 380 )
1309 In-Situ Transient DRIFTS Studies of the Reaction Pathway of n-Butane Selective Oxidation over (VO)2P2O7 Catalysts
LIANG Ri-zhong1，2，LI Ying-xia1，LI Cheng-yue1，CHEN Biao-hua1
The reaction pathway of n-butane selective oxidation to maleic anhydride (MA) over vanadium phosphorous oxide (VO)2P2O7 catalysts was systematically probed using in situ transient Diffuse Reflectance Infrared Fourier-Transform Spectroscopy (DRIFTS) in high temperature/high pressure chamber. The unsaturated and saturated noncyclic carbonyl species were determined to be intermediates in n-butane selective oxidation to MA. Furan was detected on the surface of the (VO)2P2O7 catalysts in 1-butene, 1, 3-butadiene selective oxidation. It was deduced that furan ring was cleaved to form unsaturated noncyclic carbonyl species before its conversion to MA. Based on these results and in comparison with the literature, a simplified scheme of the reaction network structure can be proposed for n-butane selective oxidation to maleic anhydride.
2004 Vol. 24 (11): 1309-1314 [Abstract] ( 1833 ) PDF (1014 KB)  ( 348 )
1315 Preparation and FTIR Properties of Amino Compounds Modified Glutaraldehyde Crosslinked Chitosan Resin Activated with Cyanuric Chloride
FENG Chang-gen1, BAI Lin-shan1，REN Qi-sheng2
The preparation and IR properties of 1-butylamine, dimethylamine, trimethylamine, triethylamine, benzylamine, 4-methylaniline and 4-aminobenzenesulfonic acid modified glutaraldehyde crosslinked chitosan activated with cyanuric chloride were studied. The absorption of ν(O—H) and ν(N—H) at 3 430-3 440 cm-1, ν(C—O—C) at 1 155 cm-1, ν(C—OH) at 1 030 cm-1 and ν(C—O) of β-D-glucose at 899 cm-1 were not shifted obviously. The absorption of δ(C—H) at 1 400-1 384 cm-1 and ν(C—OH) at 1 095 cm-1 varied markedly. The ν(CN) absorption of crosslinked chitosan was at 1 640-1 650 cm-1. The skeleton vibration absorption of 1,3,5-triazine ring was at 803-812 cm-1 and 1 584-1 590 cm-1. With different deacetylation or substitution, the amide Ⅰ, Ⅱ, Ⅲ absorption at 1 650, 1 600 and 1 310 cm-1 varied obviously. When modified with 1-butylamine, dimethylamine, benzylamine, 4-methylaniline and 4-aminobenzenesulfonic acid, strong absorption of δ(NH+3) appeared at 1 517-1 530 cm-1, which was weakened or disappeared when modified with trimethylamine or triethylamine, but a series of new absorption of ν(C—N) appeared at 1 400-1 500 cm-1.
2004 Vol. 24 (11): 1315-1318 [Abstract] ( 1839 ) PDF (941 KB)  ( 634 )
1319 Near-Infrared Spectral Studies of Hydrogen-Bond in Water-Methanol Mixtures
YUAN Bo, DOU Xiao-ming
Investigations of hydrogen bond in a water-alcohol mixture were carried out with the near-infrared (NIR) spectra of water-methanol solutions over a concentration range of 0-100 wt% with an interval of 5 wt% by analyzing the concentration-dependent variations of OH bands due to combination and overtone modes. Since the OH bands strongly overlapped in the NIR region, various spectral analysis methods, such as second derivatives, principal component analysis (PCA), and two-dimensional (2D) correlation analysis, were employed to improve the spectral resolutions and obtain the effective information from the NIR spectra of water-methanol mixtures. The possible combined modes between water and alcohol in the system of water-alcohol mixture were qualitatively described. The present study provides a new possibility for investigating the hydrogen bond in water-alcohol mixtures.
2004 Vol. 24 (11): 1319-1322 [Abstract] ( 1121 ) PDF (942 KB)  ( 631 )
1323 A Novel Calibration Technique for Quantitative Analysis of FTIR Spectra
LIAN Chen-zhou, Lü Zi-an, JI Chun-sheng, LI Ding-kai, XU Xu-chang
Fourier transform infrared spectroscopy(FTIR)can be used for the continuously on-line quantitative determination of the concentrations of several gas components in smoke gas. The process of acquiring accurate calibration of spectra is one of the most important steps in the quantitative analysis. In the present paper, a novel calibration technique was proposed and evaluated by the results of CO and HCl. Data obtained by this new technique were compared to those of conventional concentration-based calibration. The results showed that this calibration technique is feasible, and its reliability and validity were also confirmed. Further more, it has several other advantages, which will also be discussed here. Finally, the calibration problem that the substances are liquid at ambient temperature was solved by this technique.
2004 Vol. 24 (11): 1323-1326 [Abstract] ( 1633 ) PDF (860 KB)  ( 795 )
1327 Rapid and Non-Destructive Identification of Calligraphies by Fourier Transform Infrared Spectroscopy and Fourier Transform Raman Spectroscopy
NA Na1, OUYANG Qi-ming2, QIAO Yu-qing1, OUYANG Jin1*，WANG Ya-hui1
A rapid and non-destructive method was used to discriminate between calligraphies by means of Fourier transform infrared (FTIR) and FT-Raman spectroscopy in this paper. In order to discriminate two real calligraphies of Ouyang Zhong-shi from two counterfeit ones, the authors investigated the inkpad and the rice paper of the calligraphies by means of FT-Raman spectroscopy and tested the inkpad and the ink mark of the calligraphies by means of FTIR spectroscopy. It could be seen that the tiny, delicated varied chemical components of the real and the counterfeit calligraphies lead to different characters in vibration frequencies of IR and Raman functional groups and also the real calligraphies have the perfect reiteration. So the authors can discriminate between the real and the counterfeit calligraphies. It is proved that FTIR and FT-Raman are useful in the non-destructive identification of calligraphies and more precise and quicker than traditional approaches.
2004 Vol. 24 (11): 1327-1330 [Abstract] ( 1099 ) PDF (963 KB)  ( 706 )
1331 Raman Analysis of Conformation Changes of Insulin Solvent after Being Exposed to ELF Pulsed Electric Field
TIAN Bing1, 2, JIA Cai-li1, XIA Ruo-hong1, CHEN Shu-de1
Raman spectra of insulin solvents are presented before and after being exposed to the pulsed electric field with extremely low frequency 50 Hz(ELF). The covalences of the molecule were not affected and the changes of some secondary bonds such as hydrogen bonds and salt bonds were observed. Detailed analysis of these spectra indicates that the α-helix of insulin molecule was destroyed after the exposure, which is proved by the shift of the peak of the amide Ⅰ region toward higher wave number and by the appearance of several new peakss: 1 561 and 1 594 cm-1 . Uhe disulfides were affected by the weaken α-helix, and their vibrational moees were changed. Meanwhile the hydrogen bonding between the dimer are broken down which leads to the increase in the peak intensities at 1 002 and at 1 602 cm-1.
2004 Vol. 24 (11): 1331-1333 [Abstract] ( 1420 ) PDF (881 KB)  ( 579 )
1334 Studies on the Reactions of Unsaturated Chloride Polyether Polyol with Trimethyl Phosphite by FTIR
ZHANG Tian-lin1，LI Zai-feng2，JIA Zhen1，WANG Jun-hong1
The reactions of unsaturated chloride polyether polyol with trimethyl phosphite have been studied by FTIR, which was prepared by copolymerization of ethanediol, allyl glycidyl ether and epoxychloropropane. The experimental results showed that the reaction included ester-exchange reaction, ester-exchange polymerization and Arbuzov rearrangement. The process conditions such as catalyst，mass rate and reaction time were determined through the experiments. The analytic results indicated that the reaction temperature was the key controling the process and the reaction products are suitable for reactive multifunctional flame retarders.
2004 Vol. 24 (11): 1334-1337 [Abstract] ( 1928 ) PDF (971 KB)  ( 550 )
1338 Identification of Wheat Varieties by FTIR Spectrum
ZHAO Hua-rong, WANG Xiao-yan, CHEN Guan-hua, WEN Shu-min
The spectra of eight kinds of wheat roots were determined by FTIR spectrometry and the absorption peaks were analyzed. Results from the comparison of the spectra showed that there were some differences in the shape, wave number and the number of absorption peaks of their spectra within the same range of wave number. The spectra of different wheat varieties exhibited remarkable differences. The first difference was in the region of 2 800-2 980 cm-1 which mainly reflected the stretching vibration of methyl and methylene, the length of molecular chain of compound, and the molecular weight. The second difference existed in the region of 1 510-1 730 cm-1, which mainly reflected the substituent nature of amide N and α-C. The major differences of spectra in this region might result from the differences in genes. So FTIR spectra could be used for the identification of wheat varieties.
2004 Vol. 24 (11): 1338-1341 [Abstract] ( 1018 ) PDF (922 KB)  ( 559 )
1342 FTIR Study on Normal and Cancerous Lung Tissues
CHENG Cun-gui1, SHI Hong-qi2, ZHU Xiao-jun2, ZHENG Rong-quan1，ZHU Shou-tian2
Tissues of cancerous and normal lungs were analysed directly and fast by Fourier transform infrared spectroscopy with OMNI-sampler. The result indicated that some remarkable spectral differences were among normal and cancerous lung tissues in frequency, intensity and shape of the absorption peaks. These facts indicated significant differences of content, structure and conformation of proteins, nucleic acids and lipids in different types of lung tissues. The present results suggested that Fourier transform infrared spectrometry(FTIR) could show the properties of normal and cancerous lung tissues at the molecular level. It was able to provide rich and reliable information for investigation of normal and cancerous lung tissues and could be used as a convenient and reliable diagnostic tool for some tumors.
2004 Vol. 24 (11): 1342-1344 [Abstract] ( 1046 ) PDF (839 KB)  ( 507 )
1345 Prediction of NDF and ADF Concentrations with Near Infrared Reflectance Spectroscopy (NIRS)
BAI Qi-lin1, 4, CHEN Shao-jiang1*, DONG Xiao-ling2, MENG Qing-xiang2, YAN Yan-lu3, DAI Jing-rui1
The NDF (Neutral Detergent Fiber) and ADF (Acid Detergent Fiber) concentrations in maize stalk were analyzed with 147 samples selected from 600 samples of different eco-environments, hybrids and inbred lines, development stages, and various parts of the plants in two years. 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+vector normalization, and the first derivative+multivariate scattering correction were the best for NDF and ADF with the same spectral regions (7 501.7-5 449.8 cm-1 and 4 601.3-4 246.5 cm-1). All these models yielded coefficients of determination of calibration (R2cal) for NDF and ADF that are higher than 0.94, while R2cv and R2val ranged from 0.92 to 0.96 for cross and external validation. The root mean square error of estimation, root mean square error of cross validation, and root mean square error of prediction (RMSEE，RMSECV and RMSEP) for NDF and ADF ranged from 1.49 % to 1.81%. The models can be used to measure various samples in screening and evaluating quality constituents of silage maize.
2004 Vol. 24 (11): 1345-1347 [Abstract] ( 2016 ) PDF (849 KB)  ( 449 )
1348 Identification of Official Rhubarb Samples Based on NIR Spectra and Neural Networks
TANG Yan-feng1, ZHANG Zhuo-yong1*, FAN Guo-qiang2
Rhubarb is one of the most widely used Chinese medicinal herbs in China. Fast and accurate identification of official and unofficial rhubarb samples is most critical for quality control of Chinese medicine production. In the present paper near-infrared reflectance spectrometry (NIRS) and artificial neural network (ANN) were combined to develop classification models for identifying 52 official and unofficial rhubarb samples. The measured spectra were compressed by wavelet transformation (WT) and then the ANN classification models were trained with the reduced-variables spectral data. The rate of correct classification was over 96%. The effects of neurons in hidden layer and the momentum were also discussed. Owing to its fast and nondestructive properties, NIRS is a promising approach to identifying Chinese medicinal herbs.
2004 Vol. 24 (11): 1348-1351 [Abstract] ( 1099 ) PDF (861 KB)  ( 442 )
1352 A Rapid and Nondestructive Analysis of Red Wines of Different Manufacturers
XIAO Pu1, SUN Su-qin1*, ZHOU Qun1, WANG Jing2，WU Fang-di2
Alcohol and sugar are two main components in wine. We applied ATR Fourier Transform Infrared(FTIR) spectra and second derivative spectra to analyze the alcoholicity and content of sugar of red wines produced by different manufacturers for the first time. For wines with less sugar, the intensity of absorption peaks assigned to C—O bond at 1 120-1 000 cm-1 becomes stronger when the alcoholicity is higher. For wines with more sugar, we can confirm the content of sugar by the intensity of absorption peaks and the number of peaks during the range from 1 200 to 830 cm-1, which includes many the characteristic absorptions of sugar. FTIR spectra not only can show clearly the relationship between the intensity of peaks and content of alcohol and sugar, but also are so rapid and convenient that it can be used to analyse samples directly.
2004 Vol. 24 (11): 1352-1354 [Abstract] ( 1033 ) PDF (861 KB)  ( 562 )
1355 Studied on the Identification of Fructus Amomi from Its Confusable Varieties by Fourier Transform Infrared Spectroscopy
CHENG Cun-gui1, RUAN Yong-ming1, LI Bing-lan2
This paper uses Fourier transform infrared spectrometer with OMNI sampler to distinguish fructus amomi from their confusable varieties, i.e. Amomum aurantiacum H.T.Tsai et S.W.Zhao, Amomum chinense Chun ex T.L.Wu, Alpinia chinensis (Ketz.)Rosc and Alpinia japonica (Thunb.) Miq. IRs of Amomum villosum Lour., Amomum longiligulare T.L.Wu and Amomum villosum Lour. Var xanthioides T.L.Wu et Senjen are resemble, and they are markedly different from the FTIR of the confusable varieties. Repeat experiments were processed with different samples of the same set, and the probability is 1.000. The result shows that FTIR can be directly used to distinguish fructus amomi from their confusable varieties.
2004 Vol. 24 (11): 1355-1358 [Abstract] ( 1466 ) PDF (919 KB)  ( 658 )
1359 Studies on Human Breast Cancer Tissues with Raman Microspectroscopy
YU Ge1, XU Xiao-xuan1, NIU Yun2, WANG Bin1, SONG Zeng-fu3,ZHANG Chun-ping1*
The microscopic Raman spectra from normal and malignant human breast tissues have been measured and investigated. The spectral differences and changes between normal and malignant breast tissue samples mainly involve: (1) the band from the symmetric stretching modes of PO-2 group in the DNA shifts from 1 082 to 1 097 cm-1 and becomes stronger. The intensity of the symmetric stretching modes of O—P—O at 817 cm-1 in RNA increases greatly. (2) The bands of Amide Ⅰ and Ⅲ at 1 657 and 1 273 cm-1 change to 1 662 and 1 264 cm-1 respectively with their intensity and band width increasing. The peak of the C—O stretching modes in the amino acids shifts to higher wave number. The tryptophane band at 1368 cm-1 almost disappears. (3) Fewer characteristic Raman bands from lipids are observed. These spectral changes indicate that nucleic acids increase in contents relatively, while their conformation changes in cancer tissues. The proteins show various conformations and disorder structures with their molecular hydrogen bonds nearly broken. The contents of lipids decrease obviously. This investigation shows that Raman microspectroscopy is useful to biochemical study and vivo diagnosis of human breast cancers.
2004 Vol. 24 (11): 1359-1362 [Abstract] ( 1588 ) PDF (867 KB)  ( 739 )
1363 Elementary Investigation on the Application of Laser Raman Microprobe in Petroleum Exploration
HE Mou-chun, Lü Xin-biao, LIU Yan-rong
Laser Raman Microprobe (LRM) is a micro-analytical technique for determining molecular components. Base on the summarization of the applications of LRM in petroleum exploration, the authors analyzed fluid inclusions(FI) and organic matters, and found that this technique could not only research qualitatively different phase components of single fluid inclusions and the types of organic substances, but also determine quantitatively each phase component of single fluid inclusions and the indexes of maturation of vitrinite. It is concluded that it is feasible to calculate the salinity of single FI by ωB% NaCl=61.183S-22.173 and the reflectance(R0) of vitrinite by R0(%)=0.69 ln(82.12 D-16 054.49)-4.88.
2004 Vol. 24 (11): 1363-1366 [Abstract] ( 556 ) PDF (982 KB)  ( 584 )
1367 Temperature Dependence of Collagen by Raman Spectra
DONG Rui-xin1，2, YAN Xun-ling1, JIANG Shan2, LIU Mei-jie2, LIU Sheng-gang2
Raman spectra of collagen Ⅰ at different temperature were obtained. There was no change at 1 003 cm-1 line, 1 302 cm-1 line moved to a higher wave number, but other lines moved to lower wave number when temperature increased. In addition, the authors observed the temperature dependence of Raman intensity and four denaturation points at 0, 40, 68 and 90 ℃ respectively. The points at 40 and 68 ℃ are in agreement with the experimental data by DSC and SHG. The point at 0 ℃ might be frozen transition; the point at 90 ℃ might be related to the damage of secondary structure. When heated to 150 ℃, the Raman intensity of all bands decreased rapidly and many lines disappeared.
2004 Vol. 24 (11): 1367-1369 [Abstract] ( 1111 ) PDF (846 KB)  ( 402 )
1370 Raman Spectroscopic Study on the Influence of Ultraviolet Radiation on Calf Thymus DNA in Aqueous Solution
ZHOU Dian-feng，KE Wei-zhong*
The Raman spectra of calf thymus DNA in aqueous solution and at 9, 20 and 40 min after ultraviolet radiation were reported. The experimental results proved that though the ultraviolet radiation time was not long, it had a serious influence on the DNA. Only through 9 min of ultraviolet radiation, the peak of 1 094 cm-1 changed into a few weaker peaks，and it was proved that the molecular conformation was changed and the hydrogen bonds were damaged. Some kinds of nucleotides came into being because of the damage to the DNA molecular. Ultraviolet radiation also had influence on adenine, guanine, cytosine and thymine. Among them the purine and pyrimidine were badly damaged. At the same time, our experiment proved that DNA in aqueous solution possesses both A-type structure and B-type structure.
2004 Vol. 24 (11): 1370-1372 [Abstract] ( 1667 ) PDF (839 KB)  ( 466 )
1373 TLC-FT-SERS Study on a Pair of Optic Isomers in Ephedra
WANG Yuan1，ZHANG Jin-zhi2，MA Xin-yong1
A new method for analyzing the ingredients of a pair of optic isomers in ephedra, nor-ephedrine and nor-pseudoe-ephedrine, using hyphenated high-efficiency thin layer chromatography (TLC) and surface-enhanced Raman spectroscopy (SERS) techniques, is reported. The results show that the characteristic spectral bands of nor-ephedrine and nor-pseudo-ephedrine can be obtained from the TLC spot with 8 μg sample of about 2.0 mm in diameter. The difference between the SERS and solid spectra was found. Spectral bands at 1 004 cm-1 and 1 605 cm-1 were found greatly enhanced. Molecule was absorbed in surface silver sol by π electrons in ring. Under similar experimental conditions the spectral information of Levo-nor-ephedrine ramifications TLC-SERS is rich with strong credibility, whereas dextral-nor-ephedrine ramifications show a relatively strong fluorescence backdrop with less spectral information and weak credibility. The effective combination of TLC and SERS can be used to analyse the chemical ingredients with high sensitivity.
2004 Vol. 24 (11): 1373-1375 [Abstract] ( 970 ) PDF (854 KB)  ( 535 )
1376 SERS Spectra of Vitamin A Acid in Silver Solution
WANG Yu1, LI Ying-sing2, ZHANG Zheng-xing3, AN Deng-qui3
Vitamin A acid (VAA) was firstly dissolved in chloroform, and then the organic solution containing the samples was mixed with silver sol at the desired concentration. After sufficient shaking, collect SERS spectra of VAA with silver sol layer solution. The attribution of the peaks was illustrated by comparing SERS spectra with NR(Normal Raman) spcetra, and the mechanism and orientation of adsorption were also discussed according to the peaks which was absent in NR spectrum but observed in SERS spectrum. To verify the feasibility of the method for the quantitative analysis, SER spectra at different concentration of VAA were collected. The intensities measured with the band at 1 583 cm-1 were plotted as a function of concentration. It was found that an effective limit for the detection of VAA could be as low as to 1.0×10-7 mol·L-1, the calibration curve was linear in the range from 1.0×10-6-5×10-5 mol·L-1. The proposed method has the potential to quantitative assay of the drugs having SERS effects but undissolvable in water.
2004 Vol. 24 (11): 1376-1378 [Abstract] ( 1909 ) PDF (841 KB)  ( 611 )
1379 Fluorescence Fluctuation Spectroscopy with Strong Background Fluorescence——An Monte Carlo Approach
LIU Guang, CHEN Bo, MENG Fan-bo, MA Hui*, CHEN Die-yan
Fluorescence fluctuation spectroscopy is a method in which fluorescence fluctuations arising from a very small sample volume are analysed to obtain brightness, diffusion coefficient and concentration of particles. Using Monte Carlo simulation, the influences of background autofluorescence and noises on fluorescence fluctuation spectroscopy are studied. Results show that a two- component photon counting histogram can effectively remove the effects due to background autofluorescence from low brightness and high concentration components and uniform noise. The result will help to bring applications of fluorescence fluctuation spectroscopy to intracellular environment.
2004 Vol. 24 (11): 1379-1383 [Abstract] ( 1442 ) PDF (893 KB)  ( 467 )
1384 Constant-Energy Synchronous Fluorescence Spectrometry for Simultaneous Determination of Anthracene and 9,10-Dimethylanthracene
HE Li-fang1,2, LIN Dan-li1, LI Yao-qun1*
A new method of constant-energy synchronous fluorimetry to determine anthracene and 9,10-dimethylanthracene simultaneously is suggested. The spectral resolution of the constant-energy synchronous fluorescence spectra of these two compounds was much higher than that of conventional spectra. The linear ranges for anthracene and 9,10-dimethylanthracene were 0-2 μg·mL-1 and 0-5 μg·mL-1 respectively. The detection limits of anthracene and 9,10-dimethylanthracene were 2.2 ng·mL-1 and 1.7 ng·mL-1 respectively，and the relative standard deviation was less than 2%. When the new method was used for the determination of anthracene and 9,10-dimethylanthracene in water samples, the recoveries were in the range of 85% to 103%. This method has proved to be simple and rapid.
2004 Vol. 24 (11): 1384-1387 [Abstract] ( 1563 ) PDF (956 KB)  ( 370 )
1388 Spectroscopic Analysis of the Interaction of Ethanol and Acid Phosphatase from Wheat Germ
XU Dong-mei，LIU Guang-shen，WANG Li-ming，LIU Wei-ping*
Conformational and activity changes of acid phosphatase from wheat germ in ethanol solutions of different concentrations were measured by fluorescence spectra and differential UV-absorption spectra. Ｔｈｅ ｅｆｆｅｃｔ ｏｆ ｅｔｈａｎｏｌ ｏｎ ｋｉｎｅｔｉｃｓ ｏｆ ａｃｉｄ ｐｈｏｓｐｈａｔａｓｅ ｗａｓ ｄｅｔｅｒｍｉｎｅｄ ｂｙ ｕｓｉｎｇ ｔｈｅ ｄｏｕｂｌｅ ｒｅｃｉｐrｏｃａｌ ｐｌｏｔ. The results ｉｎｄｉｃａｔｅ ｔｈｅ ｅｔｈａｎｏｌ ｈａｓ ａ ｓｉｇｎｉｆｉｃａｎｔ ｅｆｆｅｃｔ ｏｎ ｔｈｅ ａｃｔｉｖｉｔｙ ａｎｄ ｃｏｎｆｏｒｍａｔｉｏｎ ｏｆ ａｃｉｄ ｐｈｏｓｐｈａｔａｓｅ. Ｔｈｅ activity of acid phosphatase decreased linearly with increasing ｔｈｅ concentration of ethanol. Differential UV-absorption spectra of the enzyme denatured in ethanol solutions showed two positive peaks at 213 and 234 nm，ｒｅｓｐｅｃｔｉｖｅｌｙ. The peaks on the differential UV-absorption spectra suggested that the conformation of enzyme molecule changed from orderly structure to out-of-order crispation. The fluorescence emission peak intensity of the enzyme gradually strengthened with increasing ethanol concentration, which is in concordance with the conformational change of the microenvironments of tyrosine and tryptophan residues. Ｔｈｅ ｒｅｓｕｌｔｓ ｉｎｄｉｃａｔｅ ｔｈａｔ ｔｈｅ ｅｘｐｒｅｓｓｉｏｎ ｏｆ ｔｈｅ ｅｎｚｙｍｅ ａｃｔｉｖｉｔｙ ｃｏｒｒｅｌａｔｅｓ ｗｉｔｈ ｔｈｅ ｓｔａｂｉｌｉｔｙ ａｎｄ ｉｎｔｅｇｒｉｔｙ ｏｆ the ｅｎｚｙｍｅ ｃｏｎｆｏｒｍａｔｉｏｎ ｔｏ ａ ｇｒｅａｔ degree. Ethanol is uncompetitive inhibitor of acid phosphatase.
2004 Vol. 24 (11): 1388-1390 [Abstract] ( 917 ) PDF (854 KB)  ( 419 )
1391 Speciation of Aluminum in Natural Waters by Fluorimetry
LIAN Hong-zhen1, 2, KANG Yu-fen1, ARKIN Yasen1, BI Shu-ping1*, LI Dan-ni1, MEI Si-zhu1, WU Xiao-jiang1, TAO Xian-cong2, CHEN Yi-jun2, DAI Le-mei2, GAN Ning1，TIAN Li-qing2
Fluorimetric method has been proposed for the speciation of Al in natural waters, based on the different competitive complexation behavior of analytical reagent and natural organic matter to Al. With eriochrome blue black R (EBBR) or morin, the monomeric inorganic Al (Ali) was determined, while with 8-hydroxylquinoline, the total monomeric Al (Ala) was obtained. The analytical results of Al speciation in natural water are close to those by Driscoll’s method. The method is simple and reliable. Fractionation of Al was realized by selecting appropriate reagents under the pH of natural water determined. The merits of this novel strategy are that the disturbance to original equilibrium of Al species is minimized and the results conform to the actual situation of natural waters.
2004 Vol. 24 (11): 1391-1394 [Abstract] ( 601 ) PDF (857 KB)  ( 1020 )
1395 Study of Direct Fluorophotometric and Flow-Injection Fluorophotometric Methods Based on the Inhibitory Effect for the Determination of Trace Formaldehyde
OUYANG Xiao-qing，XIE Zeng-hong*，GUO Zu-feng，LIN Xu-cong，GUO Liang-qia
Sulfite reacts with o-phthalaldehude in the presence of ammonium forming the highly fluorescing isoindole-1-sulfonate in neutral or weakly acid solution, and formaldehyde has inhibitory effect on it. Based on this principle, the authors developed the direct fluorophotometric and flow-injection fluorophotometric methods for the determination of trace formaldehyde. The maximum excitation wavelength and the maximum emission wavelength are 320 and 390 nm respectively. With the direct fluorophotometric method, formaldehyde in the concentration range of 0.10-1.60 μg·mL-1 can be determined with a detection limit of 0.046 μg·mL-1. With the flow-injection fluorophotometric method, formaldehyde in the concentration range of 0.10-2.00 μg·mL-1 can be determined with a detection limit of 0.085 μg·mL-1. The methods were applied respectively to the analysis of river water with satisfactory results.
2004 Vol. 24 (11): 1395-1399 [Abstract] ( 1457 ) PDF (895 KB)  ( 717 )
1400 Spectrophotometric Determination of Tace Amount of Lead with Trimethoxyphenylfluorone in Microemulsion after Using Sulphydryl Dextran Gel for Preconcentration and Separation
WEI Qin1, DU Bin1, WU Dan1, OU Qing-yu2
In this paper, the color reaction of lead with trimethoxyphenylfluorone (TM-PF) in microemulsion has been studied. Lead (Ⅱ) reacts with TM-PF to form a stable 1∶2 complex at pH 9.1. Its apparent molar absorptivity is 5.32×104 L·mol-1·cm-1 at 565 nm. Beer’s law is obeyed in the range of 0-1.5 μg·mL-1. Sulphydryl dextran gel (SDG), in which sulphydryl group has a big share, is a new type of metallic ion adsorbent. It presents the advantage of higher adsorption capacity, better reuse ability and higher mechanical stability. So the coexistent metal ions can be separated effectively and lead can be enriched by SDG, greatly improving the selectivity and sensibility of the system. The method was used to determine trace amount of lead in blood, hair and urine samples with satisfactory results.
2004 Vol. 24 (11): 1400-1403 [Abstract] ( 1520 ) PDF (863 KB)  ( 393 )
1404 Determination of Trace Germanium in Coal by Spectrophotometry with 2,4-Dichlorophenylfluorone
SAI Yin, LI Sheng, HAN Fu-bin
A method for the determination of germanium in coal samples by spectrophotometry has been developed. The color reaction of germanium with 2,4-dichlorophenylfluorone(2,4-DClPF) in the presence of cetyltrimethylammonium bromide(CTMAB) has been studied. The results show that Ge(Ⅳ) reacts on 2,4-DClPF and CTMAB to form a multicomponent complex in a 1.8-2.5 mol·L-1 H2SO4 medium. The complex has the maximum absorption wavelength at 516 nm and its apparent molar absorptivity ε is 1.38×105 L·mol-1·cm-1. Beer’s law is obeyed in the range of 0-12.5 μg·(25 mL)-1 for Ge(Ⅳ). The recovery of standard addition is 103%-106% and the relative standard deviation(RSD) is 1.1%-1.7%. This method has been applied to the determination of Ge(Ⅳ) in coal samples with satisfactory results.
2004 Vol. 24 (11): 1404-1406 [Abstract] ( 1002 ) PDF (834 KB)  ( 369 )
1407 A Novel Catalysis Kinetics Fluorimetry System for the Determination of Eliminating Ratio of Chinese Traditional Medicine for ·OH
QU Peng，LI Guan-liang，XU Mao-tian
Benzoic acid with weak fluorescence may react on ·OH, and then products with intense fluorescence are made. Extractives of Chinese traditional medicine may eliminate ·OH in solution, and reduce the amounts of the products. Then, the increased level of fluorescence of the products in solution will be lowered. Based on this principle, a novel catalysis kinetics fluorimetry system for the determination of eliminating ratio of Chinese traditional medicine for ·OH was developed. When the concentration of traditional Chinese herbal drugs was 4.0 mg(dry weight )·mL-1, the eliminating ratios of Viola yedoensis, Atrctylodes chinensis and Paeonia veitchii were 60.8%, 40.1% and 94.3%, respectively. The results obtained by this method are in good agreement with those obtained by spectrophotometry.
2004 Vol. 24 (11): 1407-1409 [Abstract] ( 999 ) PDF (835 KB)  ( 488 )
1410 Synthesis and Characterization of Mixed Ligand Complexes Rare Earth with 2,3-Dimethoxylbenzoic Acid and 1,10-Phenanthroline
LI Xia，REN Gui-fen，LIU Meng-you，SONG Bao-hua
The quaternary mixed anion of rare earth with 2,3-dimethoxylbenzoic acid and 1,10-phenanthroline has been synthesized from the water-ethanol solution. Elemental analysis shows that the complexes general formula is RE(2,3-DMOBA)2NO3Phen(RE=La, Nd, Eu, Dy). The complexes are characterized by IR, UV, TG-DTA analysis. ν2+ν5，ν2+ν6 of NO-3 are observed in 1 772 and 1 737 cm-1 in IR spectra of complexes, it shows that NO-3 group is in a bridging-chelating mode in which two O atoms chelate to RE3+ ions. UV spectra of ligand and complexes are different, it shows that ligand 2,3-dimethoxylbenzoate and 1,10-phenanthroline coordinate to RE3+ ions. Visible absorption spectra of Nd(2,3-DMOBA)2NO3Phen show that hypersensitive transition of neodymium.
2004 Vol. 24 (11): 1410-1411 [Abstract] ( 1473 ) PDF (826 KB)  ( 457 )
1412 The Pattern of Levenberg-Marquardt Backpropagation Algorithm for Recognition of Coronary Heart Disease Patients Based on Microamount of Elements in Human Blood
KAI Xiao-ming
The contents of four microamount elements (Sr, Cu, Mg and Zn) in human blood were chosen as recognition index of coronary heart disease patients and normal persons. The recognition pattern of Levenberg-Marquardt Backpropagation algorithm has been established. The first-layer transfer function is Tansig function; the second-layer transfer function is linear Purelin function. There are four input vectors, eight neurons on hidden layer, and one neuron of output vector. Four samples were chosen as a teat group and 22 samples as a training group. The weights and biases of the neural network were given. The given data could be completely identified, which predicted that this method could be a supplementary tool to diagnose this kind of disease with the determined contents of microamount of elements in human blood.
2004 Vol. 24 (11): 1412-1414 [Abstract] ( 897 ) PDF (827 KB)  ( 343 )
1415 Determination and Pharmacokinetics of Photosensitizer ZnPcS2P2 Uptaken by K562 Cells
XIE Bao-gang1，HUANG Hui-fang2，HUANG Jian-dong1*，CHEN Nai-sheng1，HUANG Jin-ling1
The di-sulfonated di-phthalimidomethyl phthalocyanine zinc(ZnPcS2P2) was an amphiphilic photosensitizer for photodynamic therapy of cancer. According to fluorescence analytical method, extracting efficiencies of 2.0% SDS(Wt%), 1.5% Triton X-100(φ) and DMF for ZnPcS2P2 in K562 cells were compared. The results showed that 1.5% Triton X-100 was the most efficient reagent for the first time extracting. Using 1.5% Triton X-100 as extracting reagent, the kinetic curves of cellular uptake of ZnPcS2P2 as well as LDL-ZnPcS2P2 complex by K562 cells were determined.Compared with ZnPcS2P2，the maximum cellular uptake of LDL-ZnPcS2P2 by K562 was doubled, which indicated that LDL was an effective targeting delivery vehicle for ZnPcS2P2.
2004 Vol. 24 (11): 1415-1418 [Abstract] ( 1382 ) PDF (875 KB)  ( 376 )
1419 Spectrophotometry Determination of Trace Selenium(Ⅳ) in Chinese Herbal Medicine by Catalytic Kinetics Ⅰ. RDB and Potassium Bromate
DING Liang1，2, SHAN Jin-huan2*, WANG Xiu-mei2, YAO Zi-hua2，WANG Yu2
Trace Se(Ⅳ) can catalyze the discolouring oxidizing reaction of RDB with potassium bromate in nitric acid medium, and the conditions of kinetics has been studied in detail. A new method of kinetics spectrophotometry for determination of trace(Ⅳ) is established. The sensitivity of the method is 0.905 μg·L-1. The range of measurement is 0-9.6 μg·L-1. The method has been used for determining trace Se(Ⅳ) in Chinese herbal medicine with satisfactory results.
2004 Vol. 24 (11): 1419-1421 [Abstract] ( 1108 ) PDF (894 KB)  ( 692 )
1422 Determination of Microamounts of Palladium by Triple-Wavelength Overlapping Spectrophotometry
LIU Gen-qi1, HAN Ling2*, ZHANG Xiao-ling2, ZHANG Guang2
The method for the determination of microamounts of palladium with 2-(3, 5-dichlolor-2-pyridylazo)-5-dimethylaminoaniline (3, 5-diCl-PADMA) by triple-wavelength overlapping spectrophotometry has been developed. It’s shown that in the medium of 0.02-1.6 mol·L-1 H2SO4, Pd reacts with 3, 5-diCl-PADMA to form a stable 1∶1 green-blue complex, which has two different positive absorption peaks and one negative absorption peak at 621 nm, 574 nm and 434 nm respectively, and their absorbance sum showed good linearity with Pd concentration. The apparent molar absorptivity is 2.03×105 L·mol-1·cm-1, which is twice as high as that of single-wavelength spectrophotometry. Beer’s law is obeyed in the range of 0-1.2 mg·L-1 for palladium. Relatively large amounts of co existing elements, including other precious metal ions，can be tolerated. The method is simple, highly sensitive and selective，and has been used to the determination of microamounts of Pd in ore，alloy and molecular sieve with satisfactory results.
2004 Vol. 24 (11): 1422-1424 [Abstract] ( 1001 ) PDF (840 KB)  ( 675 )
1425 Study on Spectral Properties of Natural Plant Ultraviolet Absorbent
HUANG Chong1, FANG Yi-wen2, OUYANG Yan-dong1, YU Yun-peng1
Natural plant ultraviolet absorbent is a safe cosmetic-typed ultraviolet additive, with no side-effect and bright future. Natural plant ultraviolet absorbent is grｏｕnd from ultraviolet absorbing plant into organic solvent ｕｎｄｅｒ dry-vacuum condition. This new type of ultraviolet absorbent has brown colour in solid form，but when it mixes with alcohol and water, its colour changes to light yellow in liquid form. This paper focuses mainly on using ultraviolet／visible spectrometer to examine its spectral properties under ultraviolet light. The result shows that this absorbent has a relative transmittance below 0.2% in the UVC and UVB zones，while in the UVA zone around 375 nm, the ｖａｌｕｅ raiseｓ up only to 2.1%. This concludes that the natural plant ultraviolet absorbent has a high absorbing ability under ultraviolet light and can withstand ultraviolet light with long wavelength.
2004 Vol. 24 (11): 1425-1427 [Abstract] ( 1476 ) PDF (829 KB)  ( 392 )
1428 Determination of Impurities in K2Cr2O7 by an Inductively Coupled Plasma Spectrometer
LI Yu-ping1，2，ZHANG Yi1*，QI Tao1，LIU Ke-ling1
The trace elements Si, Al, Fe, Ca, Mn, Mg, and Cl in the K2Cr2O7 produced by chromate cleaner production were determined by a sequential inductively coupled plasma spectrometer in this paper. Matrix effect was studied and eliminated through matrix matching. The analytical conditions for the elements were optimized. Incident power of the RF generator was 0.95 kW. Pressure of carrier gas flow was 0.13 MPa, and its flow rate was 1.2 L·min-1. Auxiliary gas flow rate was 0.2 L·min-1. The element Cl was indirectly determined by the method of AgCl precipitation. The ion Cl- can be completely precipitated in 6% nitric acid system, and then determined after keeping the solution at 50 ℃ for two hours. The recoveries of the studied impurities range from 95% to 104%, and the relative standard deviations are lower than 4% (n=10). Detection limits of these impurities are in a range 0.000 1%-0.000 01% (w/w). The analytical results of random samples agree well with the results using the standard-adding method, and the relative error varies from -4.27% to +5.26%. The developed method has been applied to the determination of impurities in K2Cr2O7 product with satisfactory results.
2004 Vol. 24 (11): 1428-1431 [Abstract] ( 1508 ) PDF (888 KB)  ( 515 )
1432 Studies on Organic Protective Coatings for Anti-Atomic Oxygen Effects by Spectrum Analysis
ZHANG Lei
This paper describes organic protective coatings on space material for anti-AO effects and the experiments to assess the properties of the coatings. Organic protection waｓ analyzed after exposures to ground state fast atomic(AO) radiation in the atomic oxygen beam facility for ground simulation experiments. The tests results have been analyzed with advanced FTIR，XPS and SEM. The test indicated that epoxy，alkyd and urethane organic coatings were highly reactive to AO with a strong degradation and changed in morphology of the surface layer. It is evident that siloxane coatings have excellent properties for anti-AO effects. The erosion product haｓ SiO2 left on the surface, thus providing protection from further attack by the energetic oxygen atoms.
2004 Vol. 24 (11): 1432-1436 [Abstract] ( 995 ) PDF (1314 KB)  ( 432 )
1437 Spectral Diagnosis of Dielectric Barrier Plasma Discharge at Atmospheric Pressure and Its Application to Surface Modification of Materials
TANG Xiao-liang, FENG Xian-ping, LI Zhi-guang, YAN Yong-hui, QIU Gao
The spectral lines of air and argon plasma emission at atmospheric pressure were recorded and analyzed. Plasma parameters such as discharge current, discharge gap and electron temperature were measured. The purpose of the study is to control the process of materials’ surface modification promptly. The experimental results indicate that a critical discharge gap is an important parameter to improve the quality of materials’ surface modification, and spectral diagnosis has been proved to be a workable method by choosing a suitable discharge gap.
2004 Vol. 24 (11): 1437-1440 [Abstract] ( 1097 ) PDF (883 KB)  ( 526 )
1441 Direct Determination of Trace Elements in Human Serum by Electrothermal Vaporization ICP-AES
CHEN Shi-zhong
A method for direct determination of trace elements in human serum by electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES) with slurry samplimg was developed. A polytetrafluoroethylene (PTFE) emulsion was used as a fluorinating agent to promote the vaporization of the analytes from graphite furnace, resulting in a remarkable improvement of analytical performances for the recommended method. The main factors affecting emission signals of the interested elements were investigated. The detection limits of 1.4 ng·mL-1 for Cu and 2.9 ng·mL-1 for Fe were achieved, and the precisions expressed as relative standard deviation (RSD) were less than 6.0% after optimization of the operating conditions.
2004 Vol. 24 (11): 1441-1443 [Abstract] ( 592 ) PDF (848 KB)  ( 336 )
1444 Study on the Adsorption Behaviors of Cadmium and Lead Ions on Green Tea and Black Tea by ICP-AES
LI Gui-zhi1，LIU Yong-ming1，LI Gai-zhi2
The adsorption behaviors of Cd(Ⅱ) and Pb(Ⅱ) on green tea and black tea in aqueous solution as well as the influences of time，acidity and temperature on the adsorption have been studied. It was found that Cd(Ⅱ) and Pb(Ⅱ) can been adsorbed strongly by green tea and black tea samples. The adsorption effects depend on the pH strongly when pH＜4. The recovery of Pb(Ⅱ) on tea samples is more than that of Cd(Ⅱ) when pH＜6 and it is opposite when pH＞6. It is difficult to elute Cd(Ⅱ) and Pb(Ⅱ) from tea samples by water at 25 ℃.
2004 Vol. 24 (11): 1444-1446 [Abstract] ( 990 ) PDF (840 KB)  ( 359 )
1447 Determination of Selenium in Rat′s Organs by Graphite Microwave Dissolution
WANG Li-xin1, 3，HU Xiao-rong2，3，LI Hui3*
The content of selenium in rat′s ten organs was determined by graphite furnace atomic absorption spectrometry with microwave dissolution. Inorganic palladium modifier was added into the sample to solve the problems of selenium volatilization and matrix disturbance as selenium in the sample is liable to receive serious loss during the course of digestion and cineration. The optimistic determination conditions were shown as follow, digestion reagent of 4 mL (10∶3)HNO3/H2O2, matrix modification of 50 μg·mL-1 palladium chloride, cineration temperature of 1 200 ℃ and atomization temperature of 1 800 ℃. Under such optimum conditions, the linear range is 0-80 ng·mL-1 and the detection limit is 1.83 ng·mL-1. The RSD is less than 8% and the average recovery rate is 97.6%. The method was shown to be precise, reliable, convenient and quick in selenium determination of various organism organs.
2004 Vol. 24 (11): 1447-1450 [Abstract] ( 431 ) PDF (882 KB)  ( 374 )
1451 Determintion of Trace Lead in the Traditional Chinese Medicine Using Hydride Generation Atomic Fluorescence Spectrometry
SHI Jie, GONG Xue-yun, ZHU Yong-qin
A hydride generation atomic fluorescence spectrometry method has been developed for the determination of trace lead in traditional Chinese medicines. A high pressure digestion using HNO3-H2O2 system was applied for the pretreatment of traditional Chinese medicine samples and the interval flow precedure was used. The experimental conditions and instrumental operatinｇ parameters such as KBH4 concentration, flow rateｓ of carrier and shield gasｅｓ, current of the lamp and height of the atomizer, have been optimized. Under the optimum conditions the detection limit is 0.08 μg·L-1. The ｒｅｌａｔｉｖｅ ｓｔａｎｄａｒｄ ｄｅｖｉａｔｉｏｎ is 0.34%. This method is simple, rapid ａｎｄ sensitive, so it can be successfully used for the determination of lead in traditional Chinese medicines.
2004 Vol. 24 (11): 1451-1453 [Abstract] ( 1614 ) PDF (871 KB)  ( 717 )
1454 Determination of 14 Trace Elements in Soybean and Its Products by Atomic Absorption Spectrometry
LIU Yan-ming, WANG Hui, LIU Yan-fu, ZHAO Ya-mei, ZHAN Bao-hua
Fourteen trace elements in soybean and its products were determined by atomic absorption spectrometry. The effects of cinefaction temperature, cinefaction time, and the concentration of HNO3 as a digestion solution were investigated in detail. The effect of the concentration of SrCl2 on the determination of Ca and Mg was also studied. The results obtained show that the soybean and its products contain higher amounts of K, Na, Ca, Mg, Fe, Cu, Zn and Mn than other elements.
2004 Vol. 24 (11): 1454-1457 [Abstract] ( 1030 ) PDF (891 KB)  ( 400 )
1458 FAAS Determination of Trace Elements in Tea-Leaves Using Suspension Sampling with Ultrasonic Agitation
WENG Di
It is known that some minerals and trace elements such as Cu, Fe, Zn and Mn are the necessary elements in human body. The lack of these elements can cause various diseases. Because tea contains all kinds of minerals and trace elements, drinking tea is healthy for people. In order to contrast teas of different sort grades and producing areas the minerals and trace elements in the tea have been determined using suspension sample introduction technique. To determine the content of trace elements in tea-leaves, samples were powdered and sieved after being heated at (80±2)℃ for 4 hours. 5 mL 0.15 % agar solution was added and mixed thoroughly with the samples by ultrasonic agitation. Then the prepared suspension of sample was directly introduced to FAAS for determination. The results of this method are consistent with those obtained by wet treatment method, and the relative deviation of treatment method is less than ±0.96%. The t-test shows that no difference was found. The present method is convenient, rapid and accurate.
2004 Vol. 24 (11): 1458-1460 [Abstract] ( 330 ) PDF (833 KB)  ( 599 )
1461 Determination of Fifteen Metal Elements in Cynomorium Songaricum by Flame Atomic Absorption Spectrophotometry(FAAS)
XUE Guo-qing1, LIU Qing2, REN Xue-feng1, HAN Yu-qi1
A FAAS method was established for the determination of Na, K, Mg, Ca, Cu, Zn, Fe, Mn, Ni, Co, Pb, Cr, Cd, Ag and Au in Cynomorium Songaricum after digestion with HNO3-HClO4(φ 4∶1) at 90-95℃ and at normal pressure. In this paper, the parameters in FAAS were studied. The analytical results of Na, K, Mg, Ca, Fe, Zn, Cu, Mn, Pb, Ni and Ag were 13 572.0, 14 260.0, 358.3, 168.3, 238.5, 19.4, 5.9, 3.4, 2.6, 1.3 and 0.4 μg·g-1 respectively and Co, Cr, Cd and Au were not found in the samples. The results showed that the recovery of standard addition was 97.8%-104.5%, and the relative standard deviation (n=9) was 0.2%-5.0%. The method is fast, simple and convenient. The results were satisfactory.
2004 Vol. 24 (11): 1461-1463 [Abstract] ( 907 ) PDF (833 KB)  ( 1006 )
1464 Study of Determination Method for Zinc in Semen and Liquor Folliculi of Artificial Fecundation
YU Jian-qiao1，SHI Xiao-yong1，YANG Ming-ming2，PAN Li2, LIU Ning-kai1
Zinc one of the key elements that influence huma genetic health, was selectively determined in this paper. In the area of metal elements determination in body fluid，most samples used in the study are blood，plasma and saliva. No literature about genetic fluid determination has been found so far. In this paper the preparation of samples，volume of samples and determination parameters were investigated. An easy reliable method of determining zinc in semen and liquor folliculi was established. The recoveries are 92.0%-107.6%, the detection limit is 0.002 mg·L-1 and the relative standard deviations (RSD)(n=5) are 1.3%-10.0%.
2004 Vol. 24 (11): 1464-1466 [Abstract] ( 1454 ) PDF (817 KB)  ( 307 )
1467 Flame Atomic Absorption Spectrophotometry for Measurement of Iron, Manganese and Zinc Contents of Wheat Seeds
WANG Xiu-min1, CHEN Yan-chang2，XIE Ling-qin1, FAN Zhong-liang3，WU Tong-yan1
The iron, manganese and zinc trace element contents of six different ｋinds of winter wheat seeds ｗｅｒｅ studied by flaｍe atomic absorption spectrophotometｒｙ. As a result, the rates of recovery of iron, manganese and ziｎc are 103.09%，102.90% and 101.19%，respectively，ａｎｄ the relative standard deviations (RSDｓ) of Fe，Mn ａｎｄ Zn are smaller than 3.94%, 1.67% and 2.69%，respectively. Taking GBW08503 ｗheat fｌour ａｓ standard sample and cａrrying out comparative determination，ｔhe successful results ｗｅｒｅ achiｅved. This method is very simple, rapid and accurate.
2004 Vol. 24 (11): 1467-1469 [Abstract] ( 1660 ) PDF (827 KB)  ( 456 )
1470 Non-Invasive Determination of Bone Lead in Human Body Using X-Ray Fluorescence Excited by 109Cd
HUANG Shi-bin1, TIAN Lin2, CHENG Huan-sheng3, PEI Peng1
A measurement system of X-ray fluorescence excited by 109Cd was set up for the in vivo measurement of bone lead. In the system, a HPGe detector (10 mm×7 mm) was used to detect the characteristic K X-rays of lead in tibia excited by γ rays of 88.0 keV from 109Cd. By the normalization of lead X-rays to the coherent scatter, the content of bone lead was calculated from the calibration curves of the ratio (X-ray intensity: coherent intensity) against the lead concentration in tibia phantoms. The normalization technique rendered the measurement accuracy independent of tissue overlay thickness, bone shape, size, mass, and subject motion. Calibration curves obtained from a set of tibia phantoms with lead-doped plaster of Paris were linear. The results of pilot measurements showed that the contents of bone lead in the occupationally exposed workers were higher than those in the control group.
2004 Vol. 24 (11): 1470-1472 [Abstract] ( 973 ) PDF (860 KB)  ( 343 )
1473 Improvement of Grating Spectrograph and Its Application to Frequency-Doubling in PPLN
ZHOU Jun1, 2，3，LOU Qi-hong1，ZHU Xiao-zheng1，DONG Jing-xing1，YE Zhen-huan1，WEI Yun-rong1
Charge-coupled device (CCD) has been widely used in spectral detection and spectral imaging fields, which has a number of benefits: broad spectral range response, low detection limit, wide dynamic range, minimal dark current and readout noise as well as the abilities of signal integration, simultaneous multichannel detection, and real-time detection. The combination of a traditional one meter grating spectrograph and a science charge-coupled device (CCD) led to a real-time grating spectrograph for laser spectrum detection developed in this paper. Based on the new grating spectrograph, the spectral characteristic of frequency-doubling of a broad band double-cladding fiber laser in polarized lithium niobate (PPLN) has been investigated. Dynamic spectrum of the second harmonic with varying temperature of PPLN has been observed and analyzed in detail.
2004 Vol. 24 (11): 1473-1475 [Abstract] ( 1400 ) PDF (864 KB)  ( 371 )
1476 NMR Study on the Determination of Structure in the Protected Glucosamineoside
GUO Zhen-chu, HAN Liang, HU Bo, XIONG Xing-quan
The protected glucosamines 5,8,9,12,13 and the protected diglucosamines 10 and 11 were prepared from D-glucosamine hydrochloride, trichloroacetonitrile, trichlorocthoxycarbonyl chloride and trimethylsilyl trifluoromethanesulfonate(TMSOTf). They were new products and their structures were characterized by means of 1H NMR and 13C NMR. The data of 1H NMR indicated that the chemical shift of NH of them were moved remarkably to the low field 5.07-5.26 compared with that of D-glucosamine hydrochloride. The data J1, 2 of the compounds 9,10,11,12,13 were between 7.2 and 8.8 Hz, which showed their structures were β configuration, while the data J1, 2 were between 3.00 and 4.96 Hz in the compounds 5 and 6, which showed their structures were α configuration. H-2 was situated in the higher field, which δ was between 3.10 and 4.30. The data of 13C NMR showed that the δ of C-1 laid in the lowest field and the δ of C-2 laid in the higher field, as were the δ of H-1 and H-2 in NMR . Commonly speaking, if the δ of C-1 was greater than 100, the structure of the compound was β configuration such as compound 9 (δ=101.9). On the contrary, if the δ of C-1 was less than 100, the structures were α configuration like compound 5 (δ=95.20)and 6(δ=97.21) . The chemical shift of other carbon and hydrogen in the ring were discussed. The progression of Carbon in the compound 6 were distinguished conveniently and clearly by using DEPT (Distortionless Enhancement by Polarization Transfer)and 13C NMR.
2004 Vol. 24 (11): 1476-1481 [Abstract] ( 1483 ) PDF (934 KB)  ( 612 )
1482 The Analysis of Trace Elements in Corn Beard for Uighur Medicine
MAIMAITI Tuerxun, ABULAITI Abudourexiti
Some elements such as K, Na, Ca, Fe, Cu, Co, Ni, Zn, Mg, Mn and Cr in corn beard were determined by atomic absorption spectrometry. The results show that the corn beard is rich in micro elements which human body needs. Our study provides new scientific foundation for further study and general application of corn beard.
2004 Vol. 24 (11): 1482-1483 [Abstract] ( 933 ) PDF (848 KB)  ( 343 )
1484 Catalytic Kinetic Spectrophotometric Determination of Nickel in Alloys
XIA Chang-bin，HUANG Nian-dong，WANG Hong-jun，HE Xiang-zhu
In (CH2)6N4-HCl buffer solution and in the presence of OP emulsifier trace Ni(Ⅱ) catalyzes strongly the decolorization reaction of Rhodamine B (RhB) by oxidizing with H2O2，and its catalytic extent is linear with the contents of Ni(Ⅱ) in a certain range. Based on this study，a novel spectrophotometric method for determining Ni(Ⅱ) was developed. The results show that the maximum absorption of the complex is at 550 nm，the detection limit of the method is 0.4 μ g·L-1for Ni(Ⅱ)，and Beer’s law is obeyed for Ni(Ⅱ) in the range of 0-0.3 mg·L-1. The method has been applied to the determination of Ni in FeNiCr alloys with satisfactory results.
2004 Vol. 24 (11): 1484-1485 [Abstract] ( 1468 ) PDF (822 KB)  ( 716 )

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