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2005 Vol. 25, No. 01
Published: 2005-01-26
 
       光谱学与光谱分析
5 The Synthesis and Characteristic of Co3O4 Nanocrystals
TAO Dong-liang1, XU Yi-zhuang2, HUANG Yi1, WEI Fei1*, WU Jin-guang2, XU Duan-fu3
The authors found a new method to synthesize Co3O4 nanocrystals, which were synthesized using Co(CH3COO)2·4H2O and PVP as precursor. The as-prepared products were measured by SEM, TEM and XRD. Co(CH3COO)2·4H2O and PVP were dissolved together in a kind of solvent. Then, the solution was vaporized in water bath at 60 ℃ till the solution became viscid. The viscid solution was transferred into a ceramic boat and was dried in a oven at 110 ℃ for 12 hours. Finally, the dried sample was calcined in tube-like stove at 400 ℃ for 2 hours in air to produce the Co3O4 nanocrystals. To prepare the precursor composed of PVP and Co(CH3COO)2·4H2O, the authors employed two different solvent (ethanol and H2O). It was found that different appearance of Co3O4 nanocrystals was achieved by using different solvent. When ethanol is used as solvent, the prepared spherical particles with diameter of about 1 μm were consisted of Co3O4 nanocrystals with diameter of 20-50 nm. However, only Co3O4 nanocrystals with diameter of 20 nm were synthesized when H2O is used as solvent. This indicated that the solvent played a big role for the final appearance of Co3O4 nanocrystals.
2005 Vol. 25 (01): 5-9 [Abstract] ( 1041 ) PDF (1085 KB)  ( 392 )
10 Studies on Fluorescent Properties of Multi-Walled Carbon Nanotubes before and after Concentrated Nitric Acid Treatment
ＳUN Wen-xiu, HUANG Zhi-peng, ZHANG Lu, ZHU Jing*
Fluorescent properties of multi-walled carbon nanotubes (MWNTs) before and after concentrated nitric acid treatment were studied. The results show that both multi-walled carbon nanotubes (MWNTs) and treated multi-walled carbon nanotubes (t-MWNTs) could emit fluorescence; compared with MWNTs, fluorescence from t-MWNTs is stronger and fluorescent emission peak from t-MWNTs blue shifts slightly to short-wavelength. Luminescence from MWNTs could be related to ｔｈｅ trapping of excitation energy at defect sites and ｔｈｅ energy bandgap between the lowest unoccupied molecular orbital (LUMO) and the highest occupied molecular orbital (HOMO). Treating MWNTs with concentrated nitric acid could introduce more defects on MWNTs and make MWTNs trap more excitation energy, leading to ａ fluorescenｃｅ enhancement of t-MWTNs; ｉｎ addition, ｔｈｅ energy bandgap between LUMO and HOMO increases with length decreasｉｎｇ of MWNT, ａｎｄ the shortening of MWNT caused by concentrated nitric acid treatment could make energy bandgap between LUMO and HOMO increase, resultｉｎｇ in ａ slight blue shift of fluorescent emission peak of t-MWTNs to short wavelength.
2005 Vol. 25 (01): 10-12 [Abstract] ( 1489 ) PDF (269 KB)  ( 412 )
13 Up-Conversion Luminescence and Volumetric Display Research on Er(0.5): FOG Material Excited by 1 520 nm Laser
CHEN Xiao-bo1, SONG Zeng-fu2, N. Sawanobori3
The volumetric display technology is one of the important science frontiers of modern society. Multi-photon up-conversion volumetric 3-D display, attractive especially in its self-spatial vision, has the advantages of total-solidification, high reliability and speedy operation so that it has a broad range of applications. The up-conversion luminescence of oxyfluoride glass material Er(0.5): FOG, when excited by 1 520 nm semiconductor laser, was studied. The common-fluorescence spectra were measured also, in order to know up-conversion sufficiently. It was found that there are several up-conversion luminescence lines (407.43, 411.20 nm), (522.51m, 528.57 nm), (540.53m, 543.70, 549.00 nm), (654.75m, 665.50 nm) and 802.10m nm, which can be recognized as the fluorescence-transitions of (2G4F2H)9/2→4I15/2, 4H11/2→4I15/2, 4S3/2→4I15/2, 4F9/2→4I15/2 and 4I9/2→4I15/2 respectively. It is interesting that the slopes of log F-log P curves, the double logarithmic variation of up-conversion luminescence intensity F with the laser power P, are various for these observed up-conversion luminescences, which are valuable for volumetric display. The comprehensive analysis found that the (2G4F2H)9/2→4I15/2 up-conversion luminescence is a four photon up-conversion luminescence, while {2H11/2→4I15/2, 4S3/2→4I15/2 and 4F9/2→4I15/2} up-conversion luminescence is three-photon up-conversion luminescences, and 4I9/2→4I15/2 up-conversion luminescence is a two-photon up-conversion luminescence. It was found also that the absorption from the ground-state 4I15/2 level to first excited level is very large, resulting in the fact that the sequential energy transfer and step-by-step absorption up-conversion are readily to happen.
2005 Vol. 25 (01): 13-18 [Abstract] ( 641 ) PDF (583 KB)  ( 401 )
19 Luminescence of Eu3+ Ions in Nanocrystalline Zirconia
LIU Huang-qing, QIN Wei-ping, ZHANG Ji-sen
Zirconia doped with 1 mol% Eu3+ and annealed at 600, 800 and 1 000 ℃ and zirconia doped with 1 mol%, 3 mol%, 5 mol% Eu3+ and annealed at 800 ℃ were prepared by co-precipitation method; luminescence of Eu3+ions was investigated under 394 nm excitation, and the emission of 5D0→7F2 was peaked at 604 nm in zirconia annealed at 600 and 800 ℃, however, peaked at 610 nm in the sample annealed at 1 000 ℃. By studying Ω2 of 5D0→7F2, the authors found that Ω2 increased with increasing annealing temperature. When monitored with 604 nm, the authors foundthat the contribution of population of 5L6 level to the luminescence of 5D0→7F2 increased with increasing annealing temperature. By investigating the luminescence in the samples doped with 1 mol%, 3 mol% and 5 mol% Eu3+ions, we found that the emission of 5D0→7F1 transition for the sample doped with 3 mol% Eu3+ions was a broad band peaked at 597 nm.
2005 Vol. 25 (01): 19-22 [Abstract] ( 1006 ) PDF (509 KB)  ( 358 )
23 Photovoltaic Character of Organic EL Devices MEH-PPV/Alq3
LIN Peng，LIANG Chun-jun，DENG Zhen-bo，XIONG De-ping，WANG Li, ZHANG Zhi-feng，ZHANG XI-qing
An organic photovoltaic(PV) cell, ITO/MEH-PPV/Alq3/LiF/Al，was fabricated. The MEH-PPV and Alq3 are the electron-acceptor and donor in the cell，respectively. The respond region matchs the adsorption of Alq3 film. Under UV light with 0.5 mW·cm-2, the cell shows a short-circuit current of 2.4 μA·cm-2, open-circuit voltage of 2.6 V, a fill factor of 0.71, and a power conversion efficiency of 0.9%。It was found that the PV cell indicates electroluminescence (EL) performance and could emit orange light at DC voltage. The maximum luminance is about 1 000 cd·cm-2 at 15 V.
2005 Vol. 25 (01): 23-25 [Abstract] ( 1080 ) PDF (376 KB)  ( 376 )
26 Photoelectron Decay Time-Resolved Spectrum of AgCl Crystals Doped with K4Ru(CN)6 Complex
YANG Shao-peng, FU Guang-sheng, DONG Guo-yi, DAI Xiu-hong, HAN Li
Microwave absorption and film dielectric spectrum detection technology was used to study the influence of complex K4Ru(CN)6 on the photoelectron decay time-resolved spectrum of cubic AgCl crystals illuminated in this paper. The results indicate that the influence of the doping content and doping position of the complex K4Ru(CN)6 on the photoelectron decay time-resolved spectrum is evident. The photoelectron decay process of this emulsion is slowest, and the photoelectron lifetime is longest when doped with K4Ru(CN)6 of 2.45×10-5 mol·(mol Ag)-1 at doping positions of 75% Ag.
2005 Vol. 25 (01): 26-28 [Abstract] ( 567 ) PDF (360 KB)  ( 370 )
29 Infrared Spectra of Polyoxometalates
FENG Chang-gen1, ZHAO Jun1*，LIU Xia2
The infrared spectra of polyoxometalates are addressed. The vibration frequencies of some synthesized polyoxometalates in recent years are emphasized. It was found that the infrared spectra of polyoxometalates result from stretch vibration frequency of the metal-oxygen, and 1 100-400 cm-1 is the region of the characteristic absorption peak. The infrared spectrum contains information about the symmetry of polyoxoanion as well. As an analytical means，the infrared spectrum can be used to distinguish heteropolyanion and provide information on structure.
2005 Vol. 25 (01): 29-32 [Abstract] ( 1142 ) PDF (455 KB)  ( 459 )
33 Study on Application of Fourier Transformation Near-Infrared Spectroscopy Analysis with Support Vector Machine (SVM)
ZHANG Lu-da1，SU Shi-guang1，WANG Lai-sheng1，LI Jun-hui2，YANG Li-ming1
Support Vector Machine (SVM) is a method for the research oｎ identifying two types of problem. Ｉt is the latest branch in the statistics study theories, and the identifｉｃａｔｉｏｎ model has ａ strict mathematics foundation. In this paper, the basic principle and method of SVM are not only introduced, but also applied to chemometrics. One hundred and three rhubarb samples were ｕｓｅｄ as experimentａｌ materials. The identifｉｃａｔｉｏｎ models ｗｅre established with ｎear-infrared spectroscopy and SVM training method ｗｉｔｈ the intention of identifying whether the rhubarb samples ａｒｅ true or false. The thirty-three samples in training set were identified by the identifying models with the accurate rate ｏｆ 100%, while seventy estimate samples had an accurate rate of 96.77%. The research result provided the method of identifying the traditional Chinese medicine rhubarb quickly. So, it shows the feasibility of establishing the models with ｎear-infrared ｓpectroscopy and SVM method to identify biological samples. This paper introduced the theme of SVM training method in order to beget the attention of the research members who deal with chemometrics.
2005 Vol. 25 (01): 33-35 [Abstract] ( 1663 ) PDF (349 KB)  ( 422 )
36 Quality Control of Corydalis Yanhusuo W. T. Wang by Second Derivative FTIR Spectroscopy Combined with Statistics
CHENG Cun-gui，YING Tao-kai
A new method using single reflection Fourier transform infrared spectroscopy was proposed for direct and fast determination of Corydalis yanhusuo W. T. Wang of traditional Chinese herbal medicines and its confusable varieties. Data were collected directly for Fourier transform infrared spectra with OMNI sampler. Then through converting FTIR spectra of the samples into second derivative spectra by derivative spectra software, it is possible to identify Corydalis yanhusuo W. T. Wang from the confusable varieties with statistics. The result shows that the second derivative FTIR of Corydalis yanhusuo W. T. Wang and its confusable varieties are different in the 2 050-650 cm-1 range. The probability is less than 0.01 and the result is significant. Corydalis yanhusuo W. T. Wang and its confusable varieties can be identified by identifying the inner layer parts of the cuticles of samples by second derivative FTIR spectroscopy with statistics directly, rapidly and accurately.
2005 Vol. 25 (01): 36-38 [Abstract] ( 1114 ) PDF (391 KB)  ( 404 )
39 Raman Spectra and Photoluminescence Spectra of InGaN/GaN Multiquantum Wells Annealed
Lü Guo-wei, TANG Ying-jie, LI Wei-hua, LI Zi-lan, ZHANG Guo-yi,DU Wei-min*
InGaN/GaN multiquantum well, grown by MOCVD on a sapphire substrate and annealed under the conditions of 700 and 900 ℃·(20 min)-1, was studied by means of mirco-Raman spectroscopy and photoluminescence. The Raman peak of E2, A1 showed red shift after multiquantum were wells annealed, and the HWHM of Raman peak decreased imperceptibly. Moreover, the photoluminescence peak of the sample annealed under the condition of 700 ℃·(20 min)-1 showed a red shift, then appeared a blue shift under the condition of 900 ℃·(20 min)-1. These results clearly showed that the sample annealed induced strain stress relief that could explain Raman peak shift, but the piezoelectric field induced the quantum-confined Stark effect, which can’t agree with the photoluminescence experiment. Sample annealed could change the width of quantum well and InGa phase segregated; these factors influencing structure of quantum well could explain the results of photoluminescence ｓpectra.
2005 Vol. 25 (01): 39-43 [Abstract] ( 1707 ) PDF (586 KB)  ( 421 )
44 Raman Spectra Study on the GeS2-Ga2S3-KCl System Glasses
TAO Hai-zheng, ZHAO Xiu-jian*, JING Cheng-bin, TONG Wei
Raman spectra of GeS2-Ga2S3-KCl pseudo-ternary system glasses at room temperature in the air were probed systematically in the region of 150-500 cm-1. Based on the results of Raman spectra and preparing procedure in pseudo-binary systems GeS2-KCl and Ga2S3-KCl, the sole interaction of Ga2S3 and KCl was identified and new units GaS3/2Cl were produced in GeS2-Ga2S3-KCl glasses. That K+ ions in the form of Cl as the nearest coordination were homogeneously dispersed in the polymeric network was confirmed by the Raman spectra evolution of samples on the serials Ⅰ and Ⅲ. Raman spectral evolution of three composition serials can be successfully interpreted using a localized model considering the effect of K+ ions on the structural units GaS3/2Cl and Ga2S4Cl2.
2005 Vol. 25 (01): 44-47 [Abstract] ( 1043 ) PDF (540 KB)  ( 366 )
48 Raman Spectroscopic Analysis of Dissolution and Phase Transformation of Chloropinnoite in the Boric Acid Aqueous Solution
LI Xiao-ping1, GAO Shi-yang2, LIU Zhi-hong2, HU Man-cheng2, XIA Shu-ping2*
Raman spectroscopy of dissolution and transformation of chloropinnoite in 4.5%(w.t.%) boric acid aqueous solution at 30 ℃ has been recorded. The Raman spectra of kinetics process have been obtained. The phase transformation product is kurnakovite(2MgO·3B2O3·15H2O). The main polyborate anions and their interaction in aqueous solution have been proposed according to the Raman spectrum. Some assignments were tentatively given and the relations between the existing forms of polyborate anions and the crystallizing solid phases have been gained. Ａ mechanisms of dissolution and crystallization reactions and the formation condition of kurnakovite in Qinghai-Tibet plateau were proposed and discussed.
2005 Vol. 25 (01): 48-50 [Abstract] ( 1049 ) PDF (373 KB)  ( 592 )
51 Application of Depth-Analysis of Confocal Raman Micro-Spectroscopy to Chirography Identification
LIN Hai-bo1, XU Xiao-xuan1, WANG Bin1, YANG Yan-yong1, YU Gang1, ZHANG Cun-zhou1,LI Jie2
Depth analysis of confocal Raman micro-spectroscopy was applied to chirography identification. The result indicated that depth analysis has potential application to forensic science field, especially in longitudinal identification of ink and inkpad. No matter what the spatial distributions of the signature pen and inkpad are, confocal Raman micro-spectroscopy can longitudinally distinguish those spatial differences. All those suggested that confocal Raman micro-spectroscopy is a fast, simple, high sensitive and non-destructive technique.
2005 Vol. 25 (01): 51-53 [Abstract] ( 1448 ) PDF (436 KB)  ( 386 )
54 Raman Spectrum of Nano-Graphite Synthesized by Explosive Detonation
WEN Chao1，2, LI Xun2, SUN De-yu2, GUAN Jin-qing2, LIU Xiao-xin2, LIN Ying-rui2 , TANG Shi-ying2, ZHOU Gang2, LIN Jun-de2, JIN Zhi-hao1
The nano-graphite powder synthesized by the detonation of explosives with negative oxygen balance is a new powder material with potential ａｐｐｌｉｃａｔｉｏｎｓ. In this work, ｔｈｅ preparation of nano-graphite powder in steel chamber by pure TNT (trinitrotoluene) explosives has been introduced. In the synthesiｓ process, ｔｈｅ protective gasｅｓ in the steel chamber are N2, CO2 ａｎｄ Ar, and the pressure is 0.25-2 atm. Raman spectrum of ｔｈｅ nano-graphite was measured. The characteristic Raman band assigned to sp2 ｏｆ graphite has been observed at about 1 585 cm-1 with half-peak width of 22 cm-1. The peak shifted to ａ higher frequency by 5 cm-1 compared with that of bulk graphite. The authors explain this blue shift phenomenon by size effect. The average size of nano-graphite from Raman measurement is 2.97-3.97 nm. X-ray diffraction (XRD) and ｔransmission electron microscopy (TEM) were used to measure the structure and particle size of ｔｈｅ nano-graphite. The crystallite size of nano-graphite estimated from XRD and TEM are 2.58 nm(acid untreated) and 1.86 nm(acid treated) respectively, which is in accord with the results of ｔｈｅ measurement approximately.
2005 Vol. 25 (01): 54-57 [Abstract] ( 206 ) PDF (512 KB)  ( 390 )
58 Raman Spectra of Cell from Breast Cancer Patients
YAN Xun-ling1，DONG Rui-xin1, 2，WANG Qiu-guo1，CHEN Shuang-feng3，ZHANG Zong-wang4，ZHANG Xue-jun4，ZHANG Lei4
Raman spectra of normal and cancer cell from breast cancer patients are presented. It is reported that all of the Raman lines become weak. The intensitｉｅｓ of Raman lines 782 ａｎｄ 1 084 cm-1 of DNA phosphate group and 1 155 ａｎｄ 1 262 cm-1 of deoxyribose-phosphate decrease. The spectral lines 812 cm-1of A-type DNA and 979 ａｎｄ 668 cm-1 disappear, ａｎｄ the 905 cm-1 peak is shifted to lower frequency by 6 cm-1. This means that ｔｈｅ phosphate backbone of DNA is destroyed to a certain extent and ｔｈｅ fissipariｔｙ of cancer cell can’t be controlled effectively. In addition, the authors found a kind of Raman line 960 cm-1 concernｉｎｇ calcifiｃａｔｉｏｎ and sclerosis of cancer cell. The results indicate that Raman spectra may offer the experiment basis for the cancer diagnosis and treatment.
2005 Vol. 25 (01): 58-61 [Abstract] ( 308 ) PDF (403 KB)  ( 395 )
62 Preparation and Properties of Organobentonites
ZHENG Yu-ying，ZHANG Han-hui，CAI Wei-long, FU Ming-lian, WANG Liang-en*
The chemistry organobentonites were synthesized by means of the ionexchange reaction between single-octadecyl trimethyl ammonium chloride(SOAC), di-octadecyl dimethyl ammonium chloride (DOAC) , tri-octadecyl methylammonium chloride (TOAC) quaternary ammonium salts and sodium base bentonites, respectively. The authors used FTIR, X-ray diffraction diagram and DSC thermograms to characterate the structure of the modified bentonites, and discussed the effect of different quaternary ammonium salt on the properties of organobentonites. The results showed that ion of the surfactants had entered into the chip layer of the bentonites, and changed the hydrophilic environment of the chip layer into hydrophobic environment and increased the distance among the chip layer, all of these had laid a base for the preparation of the nanometer composite material of high polymer/bentonite.
2005 Vol. 25 (01): 62-64 [Abstract] ( 1582 ) PDF (393 KB)  ( 405 )
65 Investigation of the (6, 1) and (7, 2) Bands in the A 2Пi—X 2Σ+ Red System of CN Radical
AN Li-qiong, YANG Xiao-hua, GUO Ying-chun, XU Yi-min, XU Chao-xiong, CHEN Yang-qin*，LIU Yu-yan
The CN radical was produced by Penning AC discharge of the mixture of trace acetonitrile (36 Pa) and helium (660 Pa) and the ro-vibrational spectra were measured by optical heterodyne magnetic rotation enhanced concentration modulation spectroscopy in the range of 16 850-17 480 cm-1. 138 lines and 118 lines were assigned to the (6, 1) and (7, 2) bands in red system A 2Пi—X 2Σ+ of CN respectively, while others were due to (8, 3) band in CN red system and C2 Swan band system. More accurate molecular constants of A 2Пi(ν=6, 7) state and perturbation parameters ξ and η between A and X states were derived based on nonlinear least-square fitting, individually, by diagonalizing the effective Hamiltonian matrix involving the perturbation elements of two electronical states and the standard deviation of fitting was less than the experimental uncertainty 0.007 cm-1, which implied the accuracy of our results.
2005 Vol. 25 (01): 65-68 [Abstract] ( 548 ) PDF (511 KB)  ( 445 )
69 Synthesis and Photoluminescence Properties of Tb3+-Acetylacetone Ternary Complexes Doped with La3+ or Y3+
WU Hui-xia，XU Li-xia，XIN Chi-yang，YU Xi-bin，WANG Ze-min
Four series of solid complexes including RExTb1-x(acac)3phen and RExTb1-x(acac)3bipy (RE=La, Y;x=0, 0.10, 0.20, 0.30, 0.50, 0.70, 0.90, 1.00) were synthesized. These complexes were characterized by IR spectra and XRD. Photoluminescence (PL) properties of these complexes were studied. The relation between their fluorescence intensities and the content of doped ions was also discussed. The experimental results show that the PL intensity of Tb3+ was sensitized by La3+ or Y3+, and La3+ is better than Y3+ in enhancing the fluorescence of Tb3+. When x=0.1-0.3, the fluorescence intensities of most doped complexes are stronger than their corresponding pure Tb3+ complex.
2005 Vol. 25 (01): 69-72 [Abstract] ( 1441 ) PDF (425 KB)  ( 411 )
73 Studying on the Relationship between the Fluorescence Occurring Time and Fluorescence Summit Wavelength
LIU Jie1，YU Chang-qing2
The authors have detected the fluorescence characteristic of aromatic pollution material-anthracene by OMA and obtained its 3-D(time-wavelength-fluorescence intensity) fluorescence diagrams, three summit wavelengths’s fluorescence time spectra, equal high spectra. By analyzing these spectra properties, the authors find that there is a clear order with the occurring time among the three fluorescence summit wavelengths (399 nm, 423 nm, 445 nm). Long fluorescence wave occurs earlier than short fluorescence wave. This solution is also analyzed and explained by atomic energy levels theory.
2005 Vol. 25 (01): 73-75 [Abstract] ( 994 ) PDF (397 KB)  ( 373 )
76 Preparation and Fluorescence Study of Anthracene, Perylene and 1-Aminoanthraquinone Colloids
LIU Jin-shui, LI Yong-xin, GAO Feng, WANG Lun*
Anthracene, perylene and 1-aminoanthraquinone colloids have been prepared by reprecipitation method. In comparison with the fluorescence emission spectra of colloids and molecules (in acetone solution), it was indicated that collids fluorescence spectra are red-shifted and easy emission. Base on the fluorescence emission and molecular structure theory, the authors conclude that these molecules overlap when they form particles. At the same time they are planar molecules. This results in the strong stacking electronic properties. So fluorescence excitation and emission become easy.
2005 Vol. 25 (01): 76-78 [Abstract] ( 1509 ) PDF (518 KB)  ( 419 )
79 Study on the Effect of Aluminum (Ⅲ) on NADH in the Presence of NH4Ac in Aqueous Solution
YANG Xiao-di1, 2, MIAO Qiang1, QIAN Sheng-li1, BI Shu-ping1*
This paper studied the interactions of Al (Ⅲ) and dihydronicotinamide adenine dinucleotide (NADH) in nearly neutral aqueous solutions (pH 6.5) by means of UV-Vis and 1H, 13C-NMR techniques. The results suggested that Al (Ⅲ) interacts with NADH to form Al-NADH complexes by occupying the binding sites of phosphate oxygen atoms O1N and O1A and ribose ring hydroxyl groups, which are the potential recognition sites for substrates, coenzyme and enzyme. In the presence of NH4Ac salt buffer and with Al (Ⅲ) salt solution, NADH will be marked with structural changes at the nicotinamide moiety in contrast with almost no structural changes in Tris-HCl buffer solution with Al (Ⅲ) salt.
2005 Vol. 25 (01): 79-82 [Abstract] ( 982 ) PDF (470 KB)  ( 338 )
83 UV-Vis Spectroscopic Study of Aluminum-Manganese Cooperative Effect on the Melanin Formation from DOPA Oxidation
DI Jun-wei1, 2，BI Shu-ping1*
The effect of aluminum and manganese ions on the melanin formation from oxidized DOPA was investigated by UV-Vis spectroscopy. In the weak acidic buffer solution (pH 5.5), aluminum and manganese ions have cooperative effect on the melanin formation. Aluminum is not a transition metal and therefore cannot initiate oxidative effect. However, manganese ions initiate the oxidation of DOPA to yield dopachrome. Aluminum ions can greatly catalyze the conversion reaction of dopachrome to form 5,6-dihydroxyindole，which is a key step in the biosynthesis of melanin. Its product is further oxidized and polymerized immediately to produce melanin. Therefore, the cooperative effect of manganese and aluminum ions increases the melanin formation from DOPA and enhances the oxidative stress.
2005 Vol. 25 (01): 83-85 [Abstract] ( 1053 ) PDF (369 KB)  ( 441 )
86 Ultraviolet Absorption Spectra of Iodine, Iodide Ion and Triiodide Ion
WEI Yong-ju, LIU Cui-ge, MO Li-ping
Ultraviolet absorption spectra of iodine I2, iodide ion I- and triiodide ion I-3 were studied, and molar absorptivities of these species were determined. Absorption spectrum of I2 aqueous solution appears as an absorption peak at 203 nm with ａ molar absorptivity of 1.96×104 L·mol-1·cm-1. Absorption spectrum of I- appears as two absorption peaks at 193 and 226 nm with molar absorptivities of 1.42×104 and 1.34×104 L·mol-1·cm-1, respectively. When I2 aqueous solution ｉｓ mixed with KI solution, two absorption peaks appear at 288 and 350 nm, ｒｅｓｐｅｃｔｉｖｅｌｙ，indicating the formation of I-3. Using saturation method, molar absorptivities of I-3 at 288 and 350 nm were determined to be 3.52×104 and 2.32×104 L·mol-1·cm-1, respectively.
2005 Vol. 25 (01): 86-88 [Abstract] ( 3301 ) PDF (313 KB)  ( 1718 )
89 Determination on Conditional Equilibrium Constants of the Complexes of Gd(Ⅲ) and Yb(Ⅲ) with HBED by UV Difference Spectra
WANG Jin-ling1，BI He-ping2，YANG Bin-sheng1*
In 0.01 mol·L-1 Hepes, pH 7.4 and at room temperature the binding of HBED with Gd(Ⅲ) or Yb(Ⅲ) was monitored by UV difference spectrum. The results show that the molar ratio of the complexes is most likely 1∶1. Gd-HBED or Yb-HBED complex produced peaks at 237 nm and 291 nm. The molar absorptivities of Gd-HBED and Yb-HBED at 237 nm are ΔεGd= (22.52±0.20)×103 cm-1·mol-1·L, ΔεYb=(27.15±0.11)×103 cm-1·mol-1·L, respectively. The conditional equilibrium constants for the complexes were measured to be lgKGd-HBED=13.56±0.28 and lgKYb-HBED=16.06±0.03. A linear free energy relationship for the complexes of Yb(Ⅲ) and Gd(Ⅲ) has been established by using equilibrium data on 18 complexes. The HBED binding constants for Yb(Ⅲ) and Gd (Ⅲ) are in agreement with the linear free energy relationship.
2005 Vol. 25 (01): 89-91 [Abstract] ( 1076 ) PDF (366 KB)  ( 367 )
92 Spectrophotometric Determination of Albumin with Acid Brown SR
ZHAO Chang-rong, LIU Bao-sheng*, ZHANG Hong-yi
A new method for the determination of albumin in human serum and mouse serum has been developed by spectrophotometry coupled with acid brown SR(ASR) as probe molecule. The maximum absorption wavelength of ASR was at 445 nm, while the maximum absorption wavelength of their product was at 610 nm. However, the reaction of ASR with albumin such as BSA or HSA was so strong that parts of their product were undissoluble in water. The addition of gum water into the system effectively eliminated the deposition. Under optimum reaction conditions, the ranges of working lines for BSA and HSA were 0-91.0 mg·L-1 and 0-95.2 mg·L-1, respectively. The detection limits were 5.72 mg·L-1 for BSA and 5.15 mg·L-1 for HSA. The relative standard derivation and the recovery of the method for the determination of total proteins in 6 human serum samples were 1.8%-4.4% and 93.6%-109.1%, respectively. The proposed method has been employed in the assay of protein of human serum and mouse serum. The results of this work were in agreement with those ｏｂｔａｉｎｅｄ by Biuret method.
2005 Vol. 25 (01): 92-94 [Abstract] ( 1410 ) PDF (363 KB)  ( 358 )
95 Review of Atomic Spectroscopy
LIU Ke-ling
The content of this review covers atomic absorption spectroscopy, atomic fluorescence spectroscopy, atomic emission spectroscopy, inductively coupled plasma mass spectroscopy, sampling systems and preconcentration systems of spectrochemical analysis, speciation of inorganic elements, process analytical chemistry，and sensors of inorganic elements.
2005 Vol. 25 (01): 95-103 [Abstract] ( 1192 ) PDF (1267 KB)  ( 428 )
104 Temperature-Dependence Emission Properties of Eu3+-Doped in LiNbO3 Single Crystal
XIA Hai-ping1, SONG Hong-wei2, WANG Jin-hao1, ZHANG Jian-li1, WANG Tie2, ZHANG Yue-pin1
The temperature-dependence emission spectra of lower and upper part of Eu3+-doped LiNbO3 crystals from 77 to 600 K were investigated under the excitation of a 488 nm light. The results show that, for upper part of crystal, the fluorescence intensity of Eu3+ ions increases with the temperature increase, however, for lower part, the intensity first increases with the temperature increase, and then decreases obviously with temperature increase. The variations of fluorescence intensity for lower and upper part of crystals are explained. The emission intensity of Eu3+ ions in LN is the total effect of thermally excited emission, phonon-assistant absorption and temperature-quenching effect.
2005 Vol. 25 (01): 104-107 [Abstract] ( 1098 ) PDF (521 KB)  ( 363 )
108 Emission Spectra of Hydroxyl Radical Generated in Air Corona Discharge
SUN Ming1, WU Yan1, ZHANG Jia-liang2, LI Jie1, WANG Ning-hui1, WU Jiang1, SHANG Ke-feng1
In this paper, the relative emission intensity of the 309 nm transition band of hydroxyl radical (OH) was measured by a CCD imaging spectrometer in a pin-plane corona discharge scheme of one atmosphere pressure air injected with unsaturated water vapor from the central hole of the used pins. The influences of several factors on the OH radical production were investigated by relative emission intensity measurement. The production of OH radical increased with a limited increment of water vapor concentration in the mixed gas. Compared with positive DC corona discharges, more OH radicals were generated in positive pulsed corona discharges and less in negative DC corona discharges. The spatial distribution of OH radical production was also observed. Most OH radicals were produced within the range of 5 mm off the discharge pin electrode. In conclusion, this means of optical emission spectroscopy, compared with more sophisticated laser fluorescence measurements used for plasma OH production diagnostics investigation, is simpler and more effective for characterizing the OH radical potential for pollutant oxidation.
2005 Vol. 25 (01): 108-112 [Abstract] ( 1186 ) PDF (546 KB)  ( 554 )
113 Quantitatively Determining Trace Elements Co and Bi in Gelatin by Inductively Coupled Plasma Atomic Emission Spectrometry Method ——Applying IEC Model to Correct the Spectral Interference of Fe to Co
DU Bao-an1, SHEN Shi-gang1, LI Zhi-ting1, XU Jian-zhong1, MA Li-qian2, SUN Han-wen1
By ICP-AES, the authors established the method to quantitatively determine the trace elements Co ａｎｄ Bi in gelatin. The authors processed the unknown sample with wet digesting method. Trace elements in gelatin could be quantitatively determined at the same time. Ｔo correct the spectral interference of Fe to Co at specific wavelength，ｔhe Ｉｎｔｅｒｅｌｅｍｅｎｔ Ｃｏｒｒｅｃｔｉｏｎ(ＩＥＣ) ｍｏｄｅｌ ｗａｓ ｅｓｔａｂｌｉｓｈｅｄ. Ｔｈｅ results of the experiment showed that the ＩＥＣ ｍｏｄｅｌ ｃｏｕｌｄ ｅｆｆｅｃｔｉｖｅｌｙ ｅｒａｓｅ ｔｈｅ ｓｐｅｃｔｒａｌ ｉｎｔｅｒｆｅｒｅｎｃｅ ｏｆ Ｆｅ to Ｃｏ. Ｔｈｅ result of the ｓｐｅｃｔｒａｌ ｃｏｒｒｅｃｔｉｏｎ ｗａｓ ｇｒｅａｔｌｙ ｓｕｐｅｒｉｏｒ ｔｏ ｔｈｅ ｒｅｓｕｌｔ ｗｈｅｒｅ ｔｈｅ ｓｐｅｃｔｒａｌ ｉｎｔｅｒｆｅｒｅｎｃｅ ｗｅｒｅｎ′ｔ ｃｏｒｒｅｃｔｅｄ ｂｙ ｔｈｅ ＩＥＣ ｍｏｄｅｌ. Ｔｈｅ method was accuraｔｅ, quick ｗｉｔｈ high performance ａｎｄ ｗｉｄｅ lineａr range. The lineａr correlation coefficient of the tested elements was over 0.999 90. The relative standard deviation (RSD%) wａｓ less than 2.00％. Ｔｈｅ ｒｅｃｏｖｅｒｙ ｒａｔｅｓ ｗｅｒｅ ｉｎ ｔｈｅ ｒａｎｇｅ ｏｆ ９８％-10７％.
2005 Vol. 25 (01): 113-115 [Abstract] ( 278 ) PDF (473 KB)  ( 656 )
116 Determination and Correlation Analysis of Trace Elements in Hair of Dependence Drug Addicts
CHENG Fa-liang，WANG Hong，WU Jian，NING Man-xia，HU Ling-feng，SU Ya-ling
The concentrations of Al, Ba, Ca, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sr and Zn in the human hair of dependence drug addicts and healthy contrast were determined by ICP-AES. The RSD of the method was 1.3%-4.9%, and recovery was 89%-129%. Correlation of the trace elements was analyzed by SPSS software. The contents of Zn and Ca in the hair of dependence drug addicts were lower, while those of Pb, Fe and Mg were higher than healthy contrasts. The result provided a foundation for improving immune function of dependence drug addicts and enhancing the effect of giving up taking addictive drugs.
2005 Vol. 25 (01): 116-118 [Abstract] ( 1987 ) PDF (412 KB)  ( 401 )
119 Visible Spectra Analysis on Edge Recycling in HT-7 Tokamak
HUANG Juan, WAN Bao-nian, WU Zhen-wei, ZHOU Qian
The main efforts of HT-7 superconducting tokamak were directed to quasi-steady state discharges and their relevant physics. Significant progress in obtaning high-performance discharges under quasi-steady state in HT-7 has been realized. The long pulse discharges have been obtained with a duration up to 63.95 s. The edge recycling was studied by the ratio of H to D through OSMA(Optical Spectroscopy Multichannel Analyzer) system. During the discharge, recycling dominated the particle balance. In the steady state, when the density was controllable, the deuterium(hydrogen) recycling played an important role and the recycling coefficient R≤1. During the later time, R＞1 and the density was uncontrollable. The main contribution was from the D(H) recycling and impurity from the surfaces of the limiter and the first wall due to the increased surface temperature and radiation power, and these limited the duration of long duration discharges. The influence of wall conditioning on the edge recycling was also studied through the ratio of H to D.
2005 Vol. 25 (01): 119-123 [Abstract] ( 440 ) PDF (567 KB)  ( 342 )
124 A New De-Noising Technique for Spectra Based on Mexican Hat Wavelet
WANG Ying, MO Jin-yuan*
Signals in spectral analysis often have random noise, which has negative influence on the accuracy and detection limit of analysis. A new chemometrics method named Mexican Hat Wavelet De-noising Arithmetic (MWDA) is presented, which can be used to remove noise in analytical chemical signals. In this method, Mexican Hat wavelet is chosen to construct de-noising function because of its excellent properties, then the de-noising function is used to extract useful information from noisy signals. MWDA is effective for signals with either wide peaks or very sharp peaks. Many processing results of simulated and experimental signals indicate that MWDA is a simple and powerful de-noising method, even when the signal has very high noise (whose signal to noise ratio is 1). After processed, the relative errors of peak position, peak height and peak area are less than 0.2%, 3.2% and 1.1% respectively. When it is applied to experimental spectra, the results are also satisfactory. This new method can increase the accuracy of spectral analysis, and the result is credible and satisfying.
2005 Vol. 25 (01): 124-127 [Abstract] ( 1001 ) PDF (440 KB)  ( 390 )
128 Determination of Relative Error of Pressure-Broadening Linewidth for the Experimentally Indistinguishable Overlapped Spectral Lines with Voigt Profile
LIN Jie-li, HUANG Yi-qing, LU Hong
The simulation and fitting of the overlapped spectral lines with Voigt profile were presented in this paper. The relative errors ε of the fitted pressure-broadening linewidth when taking the overlapped spectral line as one spectrum were discussed in detail. The relationship between such error and the two spectral lines center distance δν0, and theoretical pressure-broadening linewidth δν0Ｌ were analyzed. ε is found to be very large and the relationship between ε and δν0, δν0Ｌ is very complicated when the value of pressure-broadening linewidth is considerably less than that of Dopplerian one δνＤ. When δν0Ｌ is comparative to δνＤ the relationship between ε and δν0 is close to the smooth two-order polynomial curve. However, the slop of this curve is negative while δν0Ｌ is smaller than δνＤ and is positive when larger. Generally, ε decreases with the increase of proportion of δν0Ｌ to the whole spectral linewidth. All the above conclusion and corresponding data are the significant reference to determine the precise pressure-broadening coefficient from the experimentally indistinguishable overlapped spectrum, as well as to correct the fitted pressure-broadening linewidth.
2005 Vol. 25 (01): 128-132 [Abstract] ( 1419 ) PDF (491 KB)  ( 358 )
133 The Influence of Dissolved Oxygen on Sonoluminescence
LIU Yan1，WANG Jun2
Ultrasound at frequency of 1.1 MHz was used to study the sonoluminescence(SL) in air-saturated water at temperature ranging from 283 to 313 K. It was found that the logarithm of the detected SL intensity increases linearly with the dissolved oxygen(DO) concentration. The waters with five kinds of anions in different concentration (mg·L-1): Cl-(5-25)，NO-3(0.2-1.8)，F-(0.1-2.7)，HCO-3(8-15)，SO2-4(0.4-40) were used to simulate natural environmental chemistry background. The experimental results show that the anions in the simulated water have no influence on the SL intensity.
2005 Vol. 25 (01): 133-135 [Abstract] ( 1751 ) PDF (287 KB)  ( 359 )
136 Adopting the Method of Correlation Coefficient to Improve the Accuracy of the Xylene Isomer’s Prediction Model
WU Zhong-chen1, XU Xiao-xuan1, YANG Ren-jie1, YU Gang2, ZHANG Cun-zhou1
This paper focuses on the detailed researches on the correlation coefficient in near infrared spectrum and points out its characteristics in multi-component solution; the paper also proves the principle of obtaining more accurate results when using high correlation coefficient for model building, and presents a practical experiment to test the conclusions by using para-xylene, meta-xylene, and ortho-xylene’s mixture.
2005 Vol. 25 (01): 136-140 [Abstract] ( 1131 ) PDF (582 KB)  ( 428 )
141 Spectroscopy of α-Isoxazoleazoxyl-β-Diketone Derivatives and Their Tautomers
HUANG Fu-xin1, WU Yi-qun1, 2, GU Dong-hong1, GAN Fu-xi1
In this paper, the IR and UV-Vis spectroscopy of five novel α-isoxazoleazoxyl-β-diketone derivatives with different structures have been studied, and their keto-enol and azo-hydrazone tautomeric phenomena have been discussed. It was found that all compounds, which are in the solid or in the solution, exist in the form of hydrazodiketo and azoenol isomers. The authors can also see that there are two absorption bands which are in the range 246-262 nm and 326-339 nm, respectively, for all compounds in the UV spectra, and the intensities of long wavelength absorption bands which are attributed to azoenol forms are stronger than short wavelength absorption bands which are attributed to hydrazodiketo forms. This shows that the quantities of azoenol forms in the compounds are more than hydrazodiketo forms, and it may be due to that the varieties of the azoenol isomers can easily form six-membered rings structure in the form of intramolecular hydrogen bonding, and make chemical structures more stable.
2005 Vol. 25 (01): 141-144 [Abstract] ( 1082 ) PDF (426 KB)  ( 398 )
145 Synthesis of a Novel Rare Earth Light Conversion Agent and Study on Its Compatibility in Plastics
XIAO Zun-hong1，2, TAN Song-ting2, WANG Xia-yu2, ZOU Ying-ping2
2-octyl-1, 3-diphenol-1, 3-propdione was synthesized by phase transfer catalysis and its Sm complexes were prepared. These compounds were characterized by IR，EA，UV and 1H NMR; Sm complex and its mixture doped with PE and PVC show photoluminescence at 650 nm. There is excellent compatibility between Sm complex and plastics by the addition of long carbon chain. Therefore, Sm complex with long carbon chain is a superior light conversion agent with good compatibility in resins with emission wavelength suitable to the 643 and 660 nm for plants’ photosynthesis.
2005 Vol. 25 (01): 145-148 [Abstract] ( 1624 ) PDF (606 KB)  ( 345 )
149 Studies on Properties of Aggregates and Langmuir-Blodgett Films for Centrosymmetric Naphthalocyanine Molecules
WANG Wen-jun1, ZHANG Shan-biao1,MENG Xiang-guo1, LIU Yun-long1, WANG Gong-ming2, WANG Wen-cheng2
Deposition of Langmuir-Blodgett films and the aggregative properties of three centrosymmetric naphthalocyanine derivatives were investigated by using linear absorption spectra. Good LB films could be formed for all the three compounds. In dilute solution, the monomers are the main formation for the tetra-tert-butyl-cyan naphthalocyanine. Due to atomic zinc action, the tetra-tert-butyl naphthalocyanine zinc molecules could not only form H-aggregates, but also form J-aggregates. The tetra-tert-butyl naphthalocyanine zinc molecules mainly are aggregates in dilute solution. In the Langmuir-Blodgett films, both tetra-tert-butyl-cyan naphthalocyanine and tetra-tert-butyl-cyan naphthalocyanine zinc formed H-aggregates. The monomers are the main formation for the bi-(tetra-tert-butyl-naphthalocyaninato)-orbium in dilute solution and Langmuir-Blodgett films.
2005 Vol. 25 (01): 149-152 [Abstract] ( 1011 ) PDF (413 KB)  ( 380 )
153 Wavelet Transform Zero-Crossing Method for Auto-Extraction of Spectral Lines
ZHAO Rui-zhen1, HU Zhan-yi1,ZHAO Yong-heng2
Wavelet transform method is used in this paper. The authors firstly studied the properties of spectral lines in the wavelet domain. By introducing the items of up-zero-crossings and down-zero-crossings, the authors concluded that absorption lines and emission lines correspond to different kinds of zero-crossings. Therefore the authors presented a new wavelet transform zero-crossing method for the extraction of spectral lines and the normalization of continuum spectra. The useful spectral lines can be obtained together with the continuum spectra. The extraction of spectral lines in this paper is a direct method, which avoids the errors caused during the process of noise reduction. The experiments both on stars and nearby galaxies show that our method can be used to accurately extract the spectral lines, which is helpful to the computation of characteristic parameters and the automatic classification of spectra based on spectral lines.
2005 Vol. 25 (01): 153-156 [Abstract] ( 466 ) PDF (442 KB)  ( 360 )
157 The Properties of Energy Upconversion of Yb3+-Doped Materials Based on ZrF4
YUAN Fang-cheng
There have been few reports on studies of energy upconversion from Yb3+-doped materials based on oxide, fluoride or oxyfluoide, because researches commonly considered that Yb3+ was only a good sensibilizer. This paper reports the properties of energy upconversion of Yb3+-doped materials based on ZrF4. The rare earth Yb3+ was doped in the ZrF4 glass under the specific condition. Using 980 nm laser as an excitation light, the upconversion fluorescence spectra of the sample were measured, and the red band, green band, blue band and purple band observed, respectively. The peaks were at 412, 478, 558 and 671 nm，respectively. This paper reports the upconversion from Yb3+ standard energy level to Yb3+ energy level 2F7/2.
2005 Vol. 25 (01): 157-158 [Abstract] ( 1040 ) PDF (289 KB)  ( 372 )

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