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2005 Vol. 25, No. 03
Published: 2005-03-26
 
       光谱学与光谱分析
321 The Study on the Growth Process of ZnO Nanorods
QI Xiu-qin1, TAO Dong-liang1, HUANG Yi1，LING Chen1, XU Yi-zhuang2, WEI Fei1*, WU Jin-guang2, XU Duan-fu3
The authors synthesized ZnO nanorods by calcining the precursor composed of PVP and Zn(CH3COO)2·2H2O at 300 ℃. In order to investigate the growth process of ZnO nanorods, the precursor was calcined for different time (0.5, 3, 12, 24 h) and the corresponding products were measured by TEM, HR-TEM (high-resolution transmission electron microscopic)，SAED (selected-area electron diffraction pattern) and XRD. The result showed that there were ZnO crystallites in the precursor of PVP and Zn(CH3COO)2·2H2O, which was dried at 110 ℃. When the precursor was calcined at 300 ℃ for 0.5 h, ZnO nanorods could be observed with diameter of 50 nm and the nanorods consisted of two parts. One was compact nanorod with diameter of about 30 nm and the other part was ZnO crystallites attaching around the nanorod. This phenomenon indicated that there might be a transverse growth direction of ZnO nanorods at early time of crystal growth. When the precursor was calcined for 3 h, the products were direct and smooth single crystal ZnO nanorods. Further increasing the calcining time at 300 ℃ could improve the length of the ZnO nanorods in a certain extent while the diameter changed a little. The HR-TEM results showed that the growth direction of ZnO nanorods was along c axis.
2005 Vol. 25 (03): 321-325 [Abstract] ( 1889 ) PDF (1714 KB)  ( 379 )
326 Selective Excitation Spectroscopy of Eu[Cr0.1Al0.9(OH)6Mo6O18]·11H2O
YIN Min1，Krupa JC2, Yusov A B3，Fedosseev A M3
Following the previous work, luminescent properties of Eu3+ ions in powder sample Eu[Cr0.1Al0.9(OH)6Mo6O18]·11H2O was studied in detail. Experimental results revealed that there were three Eu3+ centers in the system. The dominant one can transfer its excitation energy to Cr3+ ions, as studied before. By conducting site-selective excitation at low temperature, emission spectra from the three centers were separated clearly. The fluorescence decay curves for different centers were also measured. Lifetime values 107 and 599 μs for 5D0 energy level of center 1 (main site) and center 3 were obtained respectively, showing that the main site is in a lower symmetry.
2005 Vol. 25 (03): 326-328 [Abstract] ( 1110 ) PDF (780 KB)  ( 362 )
329 Judd-Ofelt Spectral Theory
ZHANG Qing-li1, HE Wei2, SUN Duen-lu1，WANG Ai-hua1, YIN Shao-tang1
In this article, the development and application of Judd-Ofelt spectral theory(J-O theory) was reviewed briefly. J-O theory was used to analyze the absorption and emission spectra of rare earth ions in solids, and compute their transition probabilities, line strengths, energy lifetimes, emission cross sections, and so on. When J-mixing was considered in J-O theory, the theoretical and experimental results were more consistent. The spectra of Pr3+ can be analyzed relatively accurately with modified J-O theory. The spectral properties of anisotropic crystal can be analyzed from the unpolarized-light transmission spectrum of a quadratic sample without special-orientation processing. The overlapped absorption bands can be treated as one band approximatively. The J-O parameters can also be calculated with fluorescence lifetimes.
2005 Vol. 25 (03): 329-333 [Abstract] ( 1699 ) PDF (1440 KB)  ( 452 )
334 Study on the Emission Spectrum of B3Πg State of N2 Molecule
ZHAO Xiao-hui, ZHANG Lian-shui, ZHANG Gui-yin,SUN Bo, LI Xiao-wei
DC glow discharge was used to study N2 molecule at low pressure(4 Torr). The emission spectrum was examined in the range of 320-470 nm in the discharge plasma of N2, which showed that the emission was composed of a series of spectral lines equidistant, and the relative emission intensity became weaker with longer wavelength, whose distribution accorded with Frank-Condon rule. It is attributed to the transition of C3Πu→B3Πg. On this base, the authors have calculated the vibrational frequency of B3Πg state to be 1 738.50 cm-1. The Frank-Condon factor about C3Πu(v′=0)→B3Πg(v″=0-5) was calculated, which is consistent with the results of experiment.
2005 Vol. 25 (03): 334-336 [Abstract] ( 1597 ) PDF (773 KB)  ( 398 )
337 Research on Energy Transfer between Riboflavin and Anthrone Derivative
WANG Jing，XU Bing-ming，WANG Jin，MENG Ji-wu
According to Frster’s theory about energy transfer, the energy transfer between riboflavin and anthrone derivative was investigated. It was found that there is a notable energy transfer between riboflavin and anthrone derivative, and the energy transfer efficiency is affected by the following factors: heating temperature, heating time, and mass ratio. And the best ratio of riboflavin and anthrone derivative is 1∶3. At the same time the energy transfer efficiency drops with increasing heating temperature and time.
2005 Vol. 25 (03): 337-340 [Abstract] ( 429 ) PDF (847 KB)  ( 384 )
341 Effects of Gas Composition and Pressure on the Intensity and Quality of the Plasma Induced by a High-Energy Neodymium Glass Laser
CHEN Jin-zhong, ZHAO Shu-rui, WEI Yan-hong, GUO Qing-lin，HUAI Su-fang
In this experiment, the effects of gas composition and pressure on the intensity and quality of the plasma induced by a high-energy neodymium glass laser were studied. The experimental results show that the spectral intensity of the plasma in the argon atmosphere is stronger than that in the air when the pressure is the same. For the steel alloy sample, the intensities of the emission spectrum reach the maximum values when the argon pressure is 0.8×105 Pa. The self-absorption phenomena of AlⅡ308.22 and AlⅡ309.27 nm lines strengthen with the increase of the pressure, and even serious self-reversal appears when the pressure is (0.8-0.9)×105 Pa. The temperature of plasma also raises with the increase of the pressure. When the argon pressure is 0.93×105 Pa, the temperature is about 1 500 K higher than that when the argon pressure is about 0.43×105 Pa.
2005 Vol. 25 (03): 341-345 [Abstract] ( 989 ) PDF (905 KB)  ( 361 )
346 Reducing the Influence Non-Linearity of Detecting Array on Absorption Spectrum with Curve Fitting
CHEN Gang, WEN Zhi-yu, LIANG Yu-qian, JIANG Zi-ping, HUANG Jian, XIONG Yu-hong
In a micro spectral analytical system, the non-linearity response of the photoelectronic detecting array pixel will cause the deformation of the spectrum, especially in the measurement of absorption spectrum. In this paper, the factors that cause the deformation were studied and a corresponding solution was proposed to reduce such deformation. By using curve fitting, the non-linearity of the pixel can be corrected. This method was adopted to correct the absorption spectrum obtained by a micro spectral analytical system and the result showed that it is a efficient way to correct the non-linearity in the pixel of photoelectronic detecting array.
2005 Vol. 25 (03): 346-350 [Abstract] ( 945 ) PDF (873 KB)  ( 507 )
346 Reducing the Influence Non-Linearity of Detecting Array on Absorption Spectrum with Curve Fitting
CHEN Gang, WEN Zhi-yu, LIANG Yu-qian, JIANG Zi-ping, HHANG Jian, XIONG Yu-hong
In a micro spectral analytical system, the non-linearity response of the photoelectronic detecting array pixel will cause the deformation of the spectrum, especially in the measurement of absorption spectrum. In this paper, the factors that cause the deformation were studied and a corresponding solution was proposed to reduce such deformation. By using curve fitting, the non-linearity of the pixel can be corrected. This method was adopted to correct the absorption spectrum obtained by a micro spectral analytical system and the result showed that it is a efficient way to correct the non-linearity in the pixel of photoelectronic detecting array.
2005 Vol. 25 (03): 346-350 [Abstract] ( 525 ) PDF (873 KB)  ( 356 )
351 Investigation of the Layers Doped with Rare Earth Elements in Si Substrate and It’s Key Problems
CHENG Guo-an
The photoluminescence properties of rare earth doped silicon were investigated with ion beam technique. The photoluminescence spectra in the layers doped with ions of La, Ce and Nd were obtained at room temperature. At the same time, the up-conversion luminescence in the doped layers was observed. The intensities of both the luminescence and the up-conversion luminescence increased with increasing the doping dose and the treatment temperature. However, the intensities of the luminescence decreased with increasing the exciting wavelength between 220 nm and 300 nm; the intensities of the up-conversion luminescence increased with increasing the exciting wavelength between 600 nm and 800 nm. It was indicated that the luminescence and the up-conversion luminescence in the layers doped with ions of La, Ce and Nd depended on the doping dose, the heat treatment temperature and the exciting wavelength.
2005 Vol. 25 (03): 351-355 [Abstract] ( 1000 ) PDF (850 KB)  ( 330 )
356 Observation of IR Spectra from Doped SO2-4/ZrO2 Nanosolid Superacid
JIAN Pan-ming, XU Lin, GAO Qiang, SHEN Chang-mei, SUN Rong-fu
In this paper, ZrO(OH)2 was prepared with sol-gel method, then a series of metal-ions-doped SO2-4/ZrO2 nanosolid superacids were prepared by impregnated ZrO(OH)2 using diluted H2SO4 and Ni2+, Al3+, Sn4+, Ag+, Sn2+ etc. salt solutions. The samples were characterized by IR, XRD, TEM and chemical analysis method. The result shows that the IR spectra of samples are the characteristic spectra of the solid superacids. The stretching frequencies of Zr—O and SO in Ni2+ and Sn4+ doped samples are obviously increased, the νZr—O values of Zr—O increase from 485 cm-1 for SO2-4/ZrO2 to 500 cm-1 for both Ni2+ and Sn4+ doped samples, the νas values of SO increase from 1 390 cm-1 for SO2-4/ZrO2 to 1 405 and 1 400 cm-1 for Ni2+ and Sn4+ doped samples respectively, but that in Sn2+ doped sample increases a little. It is indicated that the samples doped by Ni2+ and Sn4+ show higher super acidity than SO2-4/ZrO2. The IR spectra of samples were determined at different calcination temperatures. It was found that the stretching frequencies of Zr—O and SO in Ni2+ and Al3+ doped samples are obviously increased with the increase in calcination temperature, but that in Ag+ doped sample is not.
2005 Vol. 25 (03): 356-359 [Abstract] ( 1087 ) PDF (1481 KB)  ( 373 )
360 Development of Soft X-Ray and Vacuum Ultraviolet Spectrum Sources
CHEN Bo, NI Qi-liang, CAO Jian-lin, LI Fu-tian，CHEN Xing-dan
The soft X-ray and vacuum ultraviolet sources developed in CIOMP are presented. The wall-stabilized argon arc source with spectrum stability and repeatability of ±0.3% is applied to the calibration of spectrum intensity distribution of the vacuum ultraviolet instruments as an absolute standard source. The Penning source, duobplasma source and hollow cathode source are able to produce atomic and ionic line spectra as a wavelength standard source, which covers a few nanometers to several tens nanometers with spectrum radiation stability and repeatability of ±1.0%. In particular, the low debris laser produced plasma source with liquid aerosol spray target recently developed can emit stronger soft X-ray for soft X-ray lithography and metrology, which has a transfer efficiency as high as 0.75%/2π·sr/2% bandwidth.
2005 Vol. 25 (03): 360-364 [Abstract] ( 1026 ) PDF (1472 KB)  ( 419 )
365 A Theoretical Study of the Influence of Interaction between Transition Metal Atoms and Carbon Monoxide on Infrared and Raman Intensities of the C—O Stretching Vibration
WU De-yin, ZHENG Jian-zhou, REN Bin, XU Xin, TIAN Zhong-qun*
The structures and the spectral properties of the transition metal M-CO complexes have been investigated by performing the calculation of the hybrid density functional theory approach. The calculated results show that for each M-CO complex the infrared intensity of the C—O stretching mode is significantly larger than that of the M-C stretching mode and the bending modes. The Raman scattering factor of the C—O stretching mode is the largest among three modes. Comparison of the calculated results indicates that the C—O modes of M-CO complexes, the metal atom of which belongs to the fourth periodic metals and the Cu group, have larger Raman scattering factors than those in the other M-CO complexes.
2005 Vol. 25 (03): 365-368 [Abstract] ( 1744 ) PDF (789 KB)  ( 384 )
369 Spectral Study of Some Polyoxovanadium Borates
ZHANG Han-hui1, 2, LIN Zhi-hua1, HUANG Chang-cang1, 2, WANG Yong-jing1, SUN Qiao-zhen1, CHEN Yi-ping1， WU Xiao-yuan1, 2，SUN Rui-qing1, CAO Yan-ning1
Four novel polyoxovanadium borates with [(VO)12O6B18O42], namely (enH2)6H3[(VO)12O6B18O42]·13H2O(1), [Ni(en)2]6H3[(VO)12O6B18O42]·8H2O(2), [Cu(en)2]5H3[(VO)12O6B18O42][B(OH)3]2·16H2O(3) and(enH2)4Na4H3[(VO)12O6B18O42]·8H2O(4)，were synthesized. The relationship between their properties and structures were studied by using FTIR，UV-Vis DRS and fluorescence etc. Among these compounds, compound (1) possesses isolated [(VO)12O6B18O42] cage, there is a ring of B18O42 sandwiched between two vanadium-oxygen clusters V6O18 by eighteen B—(μ3—O)—V bonds, while compound (2) is rather six [Ni(en)2]，each connected with the B18O42 ring by two Ni—(μ3—O)—B. In compounds (3) and (4), the anion clusters [(VO)12O6B18O42]13- are connected with [Cu(en)2]2+ and Na+, respectively. Thus, the compounds (3) and (4) are extended to an infinite two-dimensional network structure, respectively. These characteristic vibrational frequencies of polyoxovanadium borates are related to the structures of these compounds. In UV/Vis DRS spectra, there are two characteristic peaks of polyoxometalates at 205 and 260 nm, respectively. The fluorescence spectra of these four compounds have been studied, and they have emission peaks at 415 nm excited by 310 nm which are caused by Oμ→Mo. The fluorescence lifetimes of these compounds have been studied.
2005 Vol. 25 (03): 369-373 [Abstract] ( 1699 ) PDF (872 KB)  ( 496 )
374 Study on D-Glucosamine-Zn(Ⅱ) Complexes by IR Spectral Analysis
SUN Sheng-ling1，2, WANG Ai-qin1*, GAO Yi-ci2
In this paper, a series of glucosamine-Zn(Ⅱ) complexes were synthesized by the reaction of D-glucosamine hydrochloride with ZnSO4 at different pH values. The physical properties and the IR spectra of glucosamine-ZnSO4 complexes were investigated. The absorption at 3 346 and 3 292 cm-1 shifted to 3 300 cm-1 due to O—H and N—H stretching, one at 1 617 cm-1 shifted to 1 530 cm-1 due to N—H stretching, and one at 1 094 cm-1 disappeared due to secondary alcohol —OH stretching. But 1 033 cm-1 with primary alcohol —OH did not shift, suggesting that both the amino and secondary hydroxyl groups of glucosamine are coordinated to Zn(Ⅱ). The results showed that the coordination ability of Zn(Ⅱ) to glucosamine was enhanced with the pH value increasing, however, the coordination ability weakened when pH value was more than 6.5. So pH 6.5 is an optimal coordination condition for glucosamine-ZnSO4 complexes. The complexes of D-glucosamine with different zinc salts (zinc sulfate, zinc nitrate, zinc acetate, and zinc chloride) were also synthesized at the same pH value, and zinc chloride had weaker coordination ability than other zinc salts. Their IR spectra indicated that glucosamine-Zn(Ⅱ) complexes with different zinc salts had different coordination model, and only glucosamine-ZnSO4 complex had fixed ratio of coordination under the condition of pH 6.5. The structure of the complex seems to correspond to [Zn(glucosamine) ]SO47H2O at pH 6.5.
2005 Vol. 25 (03): 374-376 [Abstract] ( 1094 ) PDF (827 KB)  ( 507 )
377 Application of Near-Infrared Spectroscopy to Postoperative Monitoring of Flap in Plastic Surgery
LI Yue1, DING Hai-shu1*, HUANG Lan1, TIAN Feng-hua1, CAI Zhi-gang2
As a non-invasive technique for the measurement of blood and oxygen in tissue, the near-infrared spectroscopy (NIRS) has an increasing application to the postoperative monitoring of plastic surgery. In authorial research, a set of NIRS oximeter has been used in 6 successful flap-transplantation operations to monitor and contrast the oxygen saturation in the free flap side and in the normal opposite side. It was found in the research that there is a notable difference in the oxygen saturation between those two sides. Another research has been done in an unsuccessful operation. In this experiment, several points in the mandible were measured and the result shows that the oxygen saturation is at an obviously lower level in the anoxic position than in the normal ones. In the above several researches, near infrared spectroscopy showed a high sensitivity to detect the dynamic changes in flaps induced by inhalation of pure oxygen. Therefore, NIRS can be a valuable aid in the post-operative monitoring of free flap after the operation, and must have a great practical future in this field.
2005 Vol. 25 (03): 377-380 [Abstract] ( 1072 ) PDF (1358 KB)  ( 401 )
381 Improving Partial Least Square Regression Precision in NIR Multi-Component Analysis Using Artificial Neural Network
BAI Ying-kui1，MENG Xian-jiang1，DING Dong1，SHEN Xuan-guo2
The present paper presents a new NIR multi-component analysis method with Artificial Neural Network(ANN) and Partial Least Square Regression(PLS). First, this method divides the concentration range of training samples into some sub-ranges, and respectively computes a PLS correlation model in each sub-range with the sub-range’s training samples. Then, the authors classify prediction samples according to its concentration sub-range with ANN and judge which sub-range the prediction sample belongs to. Finally, the authors compute the concentration of prediction component with the PLS correlation model of the sub-range according to ANN. The experiment and the result of data processing show that this method improves the model’s applicability, and evidently enhances prediction precision compared to traditional PLS.
2005 Vol. 25 (03): 381-383 [Abstract] ( 1625 ) PDF (803 KB)  ( 655 )
384 Study on the Peaks Linked to the Crystalline of L-LA with Variable Temperature FTIR Spectra Method
CHU Yan-hong1, 2，ZHANG Guo-bao2*，ZHAO Gen-suo2，YU Shou-zhi2
Variable temperature FTIR spectra method was used to study the crystalline spectra of crystal compounds. In the present paper, the sample of L-LA was synthesized and characterized by FTIR, NMR and DSC. It was found that the two peaks in the range of 800-770 cm-1 changed sharply at 95 ℃ after being investigated by FTIR spectra between 15-120 ℃. When the temperature increased, these peaks remained almost unchanged, but they returned to the original state after annealing. It was deduced that these two peaks are linked to the crystalline of L-LA.
2005 Vol. 25 (03): 384-386 [Abstract] ( 989 ) PDF (828 KB)  ( 517 )
387 Synthesis, Characterization and NIR Luminescence Properties of Erbium Organic Complexes
WANG Huai-shan1, QIAN Guo-dong1*, WANG Min-quan1，LUO Yong-shi2, LIN Jiu-ling2
Several erbium organic complexes, hydrated erbium binary complexes with acetylacetone (AcAc) or dibenzoylmethane (DBM), erbium ternary complexes derived from 1,10-phenanthroline (Phen) with acetylacetone (AcAc), dibenzoylmethane (DBM) or trifluoroacetylacetone (TFA), were synthesized and identified by elemental analysis. The UV-Vis absorption and FTIR spectra measurements have been employed for all the erbium complexes. Near infrared (NIR) photoluminescence properties, such as luminescence intensity and effective bandwidth, of the erbium complexes were also studied. As a result, the erbium ternary complex with AcAc and Phen exhibits the most excellent luminescence properties among those investigated complexes.
2005 Vol. 25 (03): 387-390 [Abstract] ( 1051 ) PDF (858 KB)  ( 393 )
391 Synthesis of Byrazoline Fluorescent Compounds and Studies by Infrared Spectroscopy
XIAN Yuan-fang1, LI Dong-feng2, LI Hai-dong1, YU Bao-hui3
Benzothiazole compounds with byrazoline group or benximidazole group are new fluorescent compounds. The fluorescent compounds have been used in many fields, but their development has beeo slow. According to Schellhammer theory on the relation between chemical structure and fluorescent quality, the authors designed now fluorescent compounds with benximidazole group or the byrazoline group in the 1-benzothiazole and with biphenyl in the 3,5-benzothiazole, and their possess fluorescent nature. Two new benximidazole and benzothiazole fluorescent compounds were synthesized. All these compounds were characterized by elemental analysis and infrared spectroscopy. The excitation wavelength of the two compounds is about 441-446 nm. The fluorescence spectra show that the compounds have good blue and green fluorescence. The characteristic peaks of the absorption spectra of these compounds were found by IR spectral analysis, which can be used to deduce the structures of chemical compounds.
2005 Vol. 25 (03): 391-394 [Abstract] ( 1027 ) PDF (846 KB)  ( 376 )
395 Preparation and Spectroscopic Study of Two New Charge Transfer Salts
CHEN You-cun, LIU Guang-xiang*, WANG Ming, ZHANG Ming-tian, REN Xiao-ming
TCNQ (TCNQ＝tetracyanoquinodimethane) salts have good conductivity. The magnetic properties of substituted benzylpridiniums，such as ferromagnetism, antiferromagnetism and spin Peierls transition，have widely been investigated. In order to obtain some new materials with both conductivity and magnetism, two new organic salts, [NO2BzPy]Cl (1) and [NO2BzPyNH2]Cl (2), were synthesized and characterized. Further more, two new charge transfer salts, [NO2BzPy] [TCNQ]2 (3) and [NO2BzPyNH2][TCNQ]2 (4) were synthesized and characterized. The tested results of elementary analysis of charge transfer salts (3) and (4) were consistent with theoretical values, and the results of IR indicated that there exist TCNQ and TCNQ anions. One-dimensional molecular column of TCNQ has been formed. Partial charge transfer takes place from [TCNQ]-2 to cation.
2005 Vol. 25 (03): 395-397 [Abstract] ( 1561 ) PDF (784 KB)  ( 381 )
398 A New Calibration Transfer Method Based on Target Factor Analysis
WANG Yan-bin, YUAN Hong-fu, LU Wan-zhen
A new calibration transfer method based on target factor analysis is proposed. The performance of the new method is compared with the piecewise direct standardization method. This method was applied to two data sets, of which one is a simulation data set, and the other is an NIR data set composed of benzene, toluene, xylene and isooctane. The results obtained with this new method are at least as well as those obtained by PDS with the biggest improvement occurring when the spectra have some non-linear responses.
2005 Vol. 25 (03): 398-401 [Abstract] ( 954 ) PDF (771 KB)  ( 431 )
402 Research on the Modification of Kevlar Fiber by Polypropylene Glycol and Cis-2-Butene-1,4-Diol
ZHENG Yu-ying,WANG Can-yao,FU Ming-lian, CAI Wei-long, WANG Liang-en*
The mechanism of the modification of Kevlar fiber by polypropylene glycol(PPG) and cis-2-butene-1, 4-diol was studied in the paper, the authors learned the esterification of toluene-2, 4-diisocyanate (TDI) onto Kevlar fiber by infrared spectrum. In the mean time, the infrared spectrograms of the productions which steadily disposed by PPG and butendiol were analysed respectively, the result showed that the intensity of the bands was reinforced at about 1 700-1 720 cm-1 after the samples were steadily disposed, that is to say, the group of —NCO has been stabilized into —NHCO group, the effect of steady disposal was obvious; but the disposal effect of butendiol was apparently better than PPG’s at the same condition. Finally, the authors compared the influence of different mol rates between TDI and butendiol on the productions. Based on the consequence, excessive butendiol would prevent the Kevlar fiber from farther reaction, therefore, the mol rate between TDI and butendiol should approach 1∶1.
2005 Vol. 25 (03): 402-404 [Abstract] ( 1616 ) PDF (849 KB)  ( 386 )
405 Raman Spectral Study of Nitrosyhemoglobin and Several Other Hemoglobins
CEN Yan1,2, ZHANG Ren3, YAO Wen-hua3, MA Jiong1,2, CHEN Ji-yao1, 4*
The Raman spectra of nitrosyhemoglobin(NOHb), methemoglobin(MetHb), oxygenated hemoglobin(oxyHb)，and deoxygenated hemoglobin(deoxyHb) were comparatively studied. The results show that the Raman spectra with 632.8 nm excitation can be used to detect the R state (oxyHb) to T state (deoxyHb) transition. The difference of NOHb and MetHb in their electron spin state was clearly demonstrated in their Raman spectra with 632.8 nm excitation, suggesting that Raman spectra provide a new simple way to measure and distinguish NOHb and MetHb.
2005 Vol. 25 (03): 405-408 [Abstract] ( 1134 ) PDF (872 KB)  ( 476 )
409 Studies on FT-Raman Spectra of ⅡB-Metal Complexes with Ligand Dmit and Dmid
BIAN Guo-qing, ZHU Qin-yu, LI Xiao-wei, DAI Jie*, GU Ren-ao*
The powder solid state FT-Raman spectra of four unsymmetric dithiolate complexes with formulas (Me4N)2[M(Ln)(SPh)2] (M=Cd and Zn, L1=dmit=1,3-dithiole-2-thione-4,5-dithiolate, L2=dmid=1,3-dithiole-2-one-4,5-dithiolate, SPh= thiophenolate) (2-5) and [Bu4N]2[Zn(dmit)2] (1) were studied and characterized by changing the structures of ligands or the metals of the complexes. The blue shift of the CC peak around 1 420 cm-1 is about 38 cm-1 when the dmit2- is replaced by dmid2-. When Zn2+ is replaced by Cd2+, or dmit2- is replaced by dmid2-, the 990 cm-1 peaks of the pentacyclic ring shift to red by about 11 and 7 cm-1 respectively. Two peaks at 463 and 300 cm-1 were assigned to stretching vibration and bending vibration respectively for the S—C—S bond of S2CCS2 in dmit2-or dmid2-. Red shifts of those two peaks are found when dmit2- is replaced by SPh-, or Zn2+ is replaced by Cd2+; but they will shift to blue when dmit2- is replaced by dmid2-. There are two peaks of Cd—S vibrations with the sulfur atom from thiophenolate and from the ligands dmit2- or dmid2-, which are at about 180 and 140 cm-1 respectively. Just like Cd—S, the vibration of Zn—S has two peaks as well, which are at about 193 and 155 cm-1, respectively.
2005 Vol. 25 (03): 409-411 [Abstract] ( 626 ) PDF (797 KB)  ( 364 )
412 Research on the Mechanism of Fluorescence Quenching of HRP by NaN3
XIA Bing-le, PENG Dun-geng, NIU Hai-xia, LIU Qing-liang
The fluorescence and synchronous fluorescence spectra were employed to study the binding between sodium azide(NaN3) and horseradish peroxidase (HRP), which was affected by the molecular conformation and the microenvironment of the fluorescence residues. The mechanism of the fluorescence quenching of HRP by NaN3 was discussed and the binding constant and the number of binding sites of non-covalent bond between them were calculated.
2005 Vol. 25 (03): 412-415 [Abstract] ( 1104 ) PDF (879 KB)  ( 474 )
416 Laser Induced Dispersed Fluorescence Spectra of NO2 in the Range of 550-740 nm
ZHANG Lian-shui1, SUN Bo1, ZHANG Gui-yin1,2，ZHAO Xiao-hui1
Laser induced dispersed fluorescence spectra (LIDFS) of NO2 molecules, excited by second harmonic lines (the output wavelength is 532 nm) of a pulsed Nd: YAG laser at room temperature and at low and high NO2 pressures, were obtained and analyzed. The authors got vibronic progressions in the range of 550-740 nm at low pressure and ascribed them to the transitions from the first excitation electronic state A2B2 to the vibrational levels of the ground electronic state X2A1, and then calculated the harmonic frequencies of symmetry stretch and bond stretch: ω1=1 300.72 cm-1 and ω2=744.14 cm-1, respectively. On the basis of what was above-mentioned, the authors compared the spectra at low pressure with those at high pressure and pointed out the difference between them. Then the authors also interpreted the obvious red shift of fluorescence spectra at high NO2 pressures in terms of a step-ladder model of vibrational deactivation and obtained significative results.
2005 Vol. 25 (03): 416-419 [Abstract] ( 1024 ) PDF (832 KB)  ( 378 )
420 Study on the Interaction Mechanism of Antibacterial Peptide MDL-1 in Musca Domestica L and E. coli DNA by Fluorescence Spectra
GONG Xia，SHI Yong-hui，LE Guo-wei*
In this paper, the interaction of the antibacterial peptide MDL-1 of Musca domestica L and E. coli DNA was investigated by fluorescence spectra. The interaction mode was studied by using ethidium bromide (EB) as an extrinsic fluorescence probe. The result of fluorescence spectra and Scatchard plot indicate that the binding constant and the number of binding sites between DNA and EB decrease with increasing concentration of MDL-1. The change in binding constant and binding sites showed that the conformation of DNA transformed. When the EB molecule just fitted into the interval, the fluorescence intensity was maximum. When MDL-1 was present in the system, the EB molecules was excluded from DNA, then the fluorescence intensity decreased. The result showed that the style was eletrostatic binding, groove binding and intercalation in the interaction of MDL-1 and double helix DNA. The binding constant of MDL-1 complex with DNA was determined. Meanwhile, it helped to explain the molecule mechanism of antibacterial peptides from the interaction style and structure characteristic of antibacterial peptide and bacterial DNA.
2005 Vol. 25 (03): 420-423 [Abstract] ( 409 ) PDF (778 KB)  ( 451 )
424 Effect of Pb2+ on Spectral Characteristics of DNA from Fish Intestines
HONG Fa-shui, CAI Shu-ming, LIU Chao, ZHENG Lei, Lü Shi-peng
The interaction of Pb2+ and DNA of fish intestines was investigated using absorption spectrum, fluorescence emission spectrum, and electrophoresis. Ultraviolet absorption spectra indicated that with the addition of Pb2+, the DNA generated obvious hypochromic effect, and the absorption peak at 207 nm of DNA was blue-shifted. The fluorescence emission spectra showed that with the addition of Pb2+, the emission peak of DNA at about 419 nm did not have obvious changes, but the intensity of fluorescence reduced gradually, showing that Pb2+ has quenching effect on the DNA endogenous fluorescence. Pb2+ has 0.8 binding sites to DNA, and the fluorescence quenching of DNA caused by Pb2+ belongs to static quenching. The binding constants of binding sites are 6.08×104 L·mol-1 and 2.82×104 L·mol-1 from the Lineweaver-Burk plot. The experiments of ultraviolet and fluorescence spectra showed that exogenous Pb2+ could cause some changes to the conformation of DNA, but analysis of electrophoresis proved that exogenous Pb2+ at different concentration did not result in DNA breakage.
2005 Vol. 25 (03): 424-427 [Abstract] ( 1023 ) PDF (1502 KB)  ( 372 )
428 Synthesis, Characterization and Fluorescence Properties of Binary and Ternary Rare Earth Complexes with N-Phenylanthranilic Acid and 1,10-Phenanthroline
WANG Xi-gui1, WU Hong-ying1, ZHAO Hui1, ZHAO Si-qin1, WENG Shi-fu2, WU Jin-guang2
Some novel binary and ternary complexes of rare earth (Tb) with N-phenylanthranilic acid and 1,10-phenanthroline were synthesized and their compositions were characterized by elemental analysis. The compositions of the complexes have been confirmed to be TbL3·4H2O and TbL3phen·2H2O (L: N-phenylanthranilic acid, phen: 1,10-phenanthroline). The spectroscopic properties of the complexes were discussed. The result shows that the luminescence intensities of binary and ternary complexes were decreased by N-phenylanthranilic acid and 1,10-phenanthroline. It is indicated that the intensity of Tb depends on the structure of ligands. The structure, energy transfer and energy matching were studied, and it is concluded that the structure of complex affects the luminescence properties of the complexes.
2005 Vol. 25 (03): 428-431 [Abstract] ( 977 ) PDF (917 KB)  ( 501 )
432 Spectral Study and Determination of Metoclopramide and Procaine Hydrochloride by Sequential Injection Analysis
WANG Ai-jun, FAN Jing*, FENG Su-ling,CUI Feng-ling
A sequential injection spectrophotometric method is proposed for the determination of metoclopramide or procaine hydrochloride, based on the reactions of metoclopramide and procaine hydrochloride with cerium(Ⅳ) in sulfuric acid medium. Red intermediate products were observed and were found unstable so that their analytical use is only possible by sequential injection technology. For metoclopramide, the detection limit is 6.5 μg·mL-1, and the linear range of determination is 9.7-116.6 μg·mL-1 with a sampling frequency of 45 h-1. For procaine hydrochloride, the detection limit is 7.4 μg·mL-1, and the linear range of the determination is 10.0-130.0 μg·mL-1 with a sampling frequency of 45 h-1. The method has been applied to the determination of metoclopramide and procaine hydrochloride in tablets and injections with satisfactory results as compared with standard method.
2005 Vol. 25 (03): 432-435 [Abstract] ( 1591 ) PDF (784 KB)  ( 376 )
436 Direct Determination of Ammonia in Plasma with Indophenol Method
DENG Jian1, XU Jin-sheng2, FAN Hua1, YUAN Ya-li1, LIU Chuan-xiang1
A new method for direct determination of ammonia in plasmas with indophenol reagent is described. It is shown that using sodium citrate as anticoagulant in phosphate buffer within pH 10.5-11.2, indophenol reagent reacts sensitively with ammonia in the plasmas to form a stable blue compound with a maximum absorption at 630 nm with low interference. The apparent molor absorptivity is 2.48×104 L·mol-1·cm-1，and the linear range 0-1 500 μmol·L-1 (r=0.999 9) with a detection limit of 1.7 μmol·L-1. The relative standard deviation is 1.13%(n=11) and the recoveries are in the range of 93.6%-101.6% with an average recovery of 97.0%. The proposed method has been applied to detect ammonia in the plasmas from 43 healthy persons and 97 patients who suffered from liver diseases with satisfactory results.
2005 Vol. 25 (03): 436-438 [Abstract] ( 584 ) PDF (764 KB)  ( 373 )
439 Experimental Testing of Micro Biochemical Analytical System
CHEN Gang1，WEN Zhi-yu1，WEN Zhong-quan1，XU Yi2，LI Xia1，JIANG Zi-ping1
A micro biochemical analytical system based on a micro fiber spectrometer is introduced. Experiment was carried out to calibrate and test the analysis system. In the experiment, the absorption spectra of Fe2+-ferroin solution bodies with different concentrations were obtained. The working curve shows a fine linearity of the analysis system. The authors also compared the experimental results obtained from 722-spectrometer and those from our analysis system. It was shown that their system can meet the requirement of practical use. This system also has many advantages, such as real-time whole spectrum analyzing and small volume, and is an ideal instrument for biochemical analysis.
2005 Vol. 25 (03): 439-443 [Abstract] ( 913 ) PDF (1500 KB)  ( 369 )
444 Nanometer-Size Titanium Dioxide Separation/Preconcentration and ICP-AES for the Determination of Cd, Co and Zn
SHI Ta-qing1, LIANG Pei2*, LI Jing2, LU Han-bing2
The adsorption behavior of Cd, Co and Zn on nanometer-size TiO2 was investigated. At pH 9.0, Cd, Co and Zn were retained on the nanometer-size TiO2, then eluted with 0.1 mol·L-1 HNO3 and determined by ICP-AES. The adsorption capacities of nanometer TiO2 were found to be 8.1, 6.9 and 15.1 mg·g-1 for Cd, Co and Zn respectively. The detection limits (3σ) for Cd, Co and Zn are 5.1, 3.4 and 2.9 ng·mL-1 respectively. The proposed method has been applied to the determination of trace Cd, Co and Zn in environmental samples with satisfactory results.
2005 Vol. 25 (03): 444-446 [Abstract] ( 1402 ) PDF (762 KB)  ( 360 )
447 Study on Analytic Precision of Laser Microemission Spectral Analysis in Argon Atmosphere at Reduced Pressure
GUO Qing-lin1 , ZHANG Bo1, ZHANG Jin-ping1, WANG Lan-xun2, CHEN Jin-zhong1
According to mathematic statistics, data for laser microemission spectroscopic analysis were selected, which were collected with the use of CCD (charge-coupled device) in argon atmosphere at reduced pressure. By selection, the effects of some factors, such as the difference of bore ablated on the sample surface by the laser, the distribution nonuniformity of element in the sample, and the fluctuation of output energy of the laser, etc. were reduced. The method that improves analytic precision of laser microemission spectroscopic analysis was studied. And quantitative analysis of Cu, Zn and Mg in aluminum alloy standard samples was performed, using the Cu(Ⅰ) line at 324.7 nm , the Zn(Ⅰ) line at 334.5 nm, and the Mg(Ⅰ) line at 383.8 nm. The results show that the RSDs of relative intensity of the spectral lines of Cu, Zn, Mg are 1.80%，4.35% and 6.29% respectively, and the RSDs of quantitative analysis of them are 10.1%, 6.98% and 8.17% respectively. The relative errors of the average of analysis of them are -3.76%，3.62% and -1.62% respectively.
2005 Vol. 25 (03): 447-449 [Abstract] ( 1985 ) PDF (791 KB)  ( 359 )
450 Research on the Transformation of GBC-918 Spectrophotometric Data into Text Data
YE Zhi-xiang1，CHENG Guo-zhong2，YANG Ying-chun1
This paper introduces the principle of designing resident program which can be used to obtain GBCUV screen pictures. First, the spectrophotometric data of refinery waste water, phenol and aniline were obtained by using GBCUV software. Second, the data mentioned above were transformed into text data with TXTSR.COM and TXZH.EXE. Finally, after the text data of refinery waste water were processed by Kalman filtering, the recoveries of phenol and aniline were in the range of 99.0%-103.8% and 97.8%-100.6% respectively. In conclusion, using this software can enlarge the application of GBC-918 and meet the need of modern spectral analysis.
2005 Vol. 25 (03): 450-452 [Abstract] ( 1468 ) PDF (758 KB)  ( 544 )
453 Soft X-Ray Reflectometer with Laser Produced Plasma Source
CHEN Bo, NI Qi-liang, CAO Ji-hong
A soft X-ray reflectometor with laser-produced plasma source developed in the authorial lab is presented for the measurements of efficiencies of gratings, transmission of filter and reflectance of multilayer coatings. The reflectometer is composed of a soft X-ray laser-produced plasma source, a grazing incidence monochromator with a constant deviation angle, a vacuum chamber, a sample table, a photo-electronic unit and a computer controlling unit. The working wavelength is from 8 to 30 nm and the maximum sample size is 130 mm long by 120 mm wide by 120 mm high. In order to test the performances of the reflectometer, the reflectivity of multilayer coatings was obtained by using this device. The measured results agree well with the theoretical calculation. The reproducibility of measured reflectance is ±0.6%.
2005 Vol. 25 (03): 453-455 [Abstract] ( 1041 ) PDF (791 KB)  ( 376 )
456 X-Ray Microanalysis of the Activity of Immobilized Urease on Chitosan Membrane
MA Xiao-li, YAO Zi-hua*
The localization of the activity of immobilized urease on chitosan membrane was studied by X-ray microanalysis. BaCl2 and urea were selected as the capture and substrate respectively. The substrate was hydrolyzed by immobilized urease to produce NH3 and CO2 in Tris-HCl buffer(pH 7.0), and the latter was captured by BaCl2 to form precipitate. The precipite was deposited on the active site of immobilized urease. It is shown that the method is practicable and reliable. The optimum condition for the localization of activity of immobilized urease was studied.
2005 Vol. 25 (03): 456-459 [Abstract] ( 1373 ) PDF (834 KB)  ( 346 )
460 X-Ray Fluorescence Spectrometric Determination of High Rhenium Content in Rhenium-Tungsten Alloys Used in Traveling Wave Tube
BAO Sheng-xiang1，WANG Shou-xu1，MA Li-li1，ZHAO Deng-hua2，FAN Rong-kui2，LI Jian2
The matrix effect, spectral overlap and background were investigated for X-ray fluorescence (XRF) spectrometric determination of rhenium content according to the analysis requirement of rhenium-tungsten alloys, a key material used in traveling wave tube. The reason for causing the calibration curve nonlinear was explained theoretically when binary ratio technique of XRF was used. Both theoretical and experimental results show that linear calibration curve can be obtained if the curve is plotted by Re% vs. Re Lα X-ray intensity instead of binary ratio technique. The method is rapid and accurate and the results obtained in this work are in good agreement with those of chemical analysis. The method has been successfully applied to product quality control.
2005 Vol. 25 (03): 460-462 [Abstract] ( 1495 ) PDF (755 KB)  ( 409 )
463 Study on the Reaction Mechanism of Chloroacetanilide Herbicides with Urease Using Fluorescence Spectrum and High-Performance Liquid Chromatography
LIU Hui-jun1，ZHAN Xiu-ming1，LI Ke-bin2，LIU Wei-ping1*
The relationship between excess thermodynamic function and binding to urease of four chloroacetanilide herbicides was studied using high-performance liquid chromatography and fluorescence spectrum. The linear relationship between the composition of mobile phase of RP-HPLC and the capacity factor of chloroacetanilide herbicides has been obtained. The excess thermodynamic enthalpy (Δ*) of acetochlor, pretilachlor, butachlor and metolachlor was determined, and the binding constant K and the number of binding sites with urease were calculated. The relationship between excess thermodynamic function and the binding constant K was suggested.
2005 Vol. 25 (03): 463-466 [Abstract] ( 1425 ) PDF (837 KB)  ( 509 )
467 Synthesis and Character of Megastigmatrienone
WANG Jian-lin,YANG Shao-long,XU Yan-mei, ZHAO Qing-hua, QIAN Lan
In this synthetic route, the raw materials are obtained easily and the conditions of reactions are smoothly. The products in some main procedures of the route have high yieds. This synthetic route is a new way of the compound，there hasn’t been reported anywhere. It needs further studies to be practically applied. According to this synthetic routes, the authors studied technolygical conditions of the reactions of every step. Some products are analyzed by refractive index, IR, HNMR, and MS and confirmed its structure.
2005 Vol. 25 (03): 467-469 [Abstract] ( 1405 ) PDF (815 KB)  ( 522 )
470 Grafting Reaction of Tetrabutyltin on the MCM-41 Surface and Characterization of the Grafted Product
XU Hai-bing, WANG Xu-xu*, FU Xian-zhi
MCM-41 modified with tetrabutyltin and Sn-O-MCM-41 obtained from calcination of the modified MCM-41 in pure oxygen were characterized by XRD，FTIR，UV-Vis DRS, and TG analysis. It was found that the hydrothermal stability, surface acidity, and coordinative states of tin atoms on both samples were evidently different. After calcination, the surface tin atoms of sample remained in the tetrahedronal structure, and the hydrothermal stability and surface acidity were improved. According to the results, the reason for the enhancement of catalytic activity of Sn-O-MCM-41 was discussed.
2005 Vol. 25 (03): 470-472 [Abstract] ( 982 ) PDF (788 KB)  ( 454 )
473 Experimental Study on Harmonic Detection of Methane by Use of a Digital Lock-In Amplifier
DONG Lei, MA Wei-guang, YIN Wang-bao, LI Chang-yong, JIA Suo-tang
The harmonic detection of methane at 6 105.369 4 cm-1 was measured by use of a digital lock-in amplifier (SR830) remotely controlled by a computer. The programme was written by Visual Basic 6.0 because it has strong function and a friendly appearance. The experimental results are in agreement with theoretical analysis, which fully confirms that a better signal-to-noise ratio (SNR) can be achieved in the high-harmonics detection of trace gases by the digital lock-in amplifier. The method can be applicable to the highly sensitive detection of pollution gases.
2005 Vol. 25 (03): 473-476 [Abstract] ( 1668 ) PDF (1027 KB)  ( 743 )
477 Determination of Trace Pb in Whole Blood by Zeeman-GFAAS
CHEN Xiao-hong，YU Xiao-yu
The determination method for trace Pb in whole blood was studied, which was diluted by 0.5% HNO3. In the measurement, Zeeman-GFAAS was used and the relative condition was discussed. This method shows that the detection limit was 10.0 pg, the relative standard deviation of standards (RSD) was 0.36%-1.8%，the relative standard deviation of samples (RSD) was 1.4%-2.3%, and the recovery rate was 96.0%-101.7%. The concurrent interference was low. This method is simple and rapid. It is an ideal method to determine trace Pb in whole blood.
2005 Vol. 25 (03): 477-478 [Abstract] ( 996 ) PDF (796 KB)  ( 367 )

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