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2004 Vol. 24, No. 06
Published: 2004-06-26
 
       光谱学与光谱分析
641 Laser Fluorescence Excited Spectrum of NO via A2Σ←X2Π Transition
ZHANG Lian-shui，ZHANG Gui-yin，ZHAO Xiao-hui，YANG Xiao-dong，LI Yi
Two-photon fluorescence excited spectrum of NO induced by Nd:YAG laser pumped optical parameter generator/amplifier as excitation source was obtained in the range of 420-472 nm. With this technique, the structure of the energy levels of NO molecule in A2Σ electronic state was investigated. The peaks of the spectrum were attributed to A2Σ(v′=0,1)←X2Π(v″=0) transition. The near square dependence of fluorescence signal on the laser intensity indicates a two-photon process. The ground-vibrational-state oscillation frequency and the force constant of A2Σ state were calculated. The fluorescence lifetime of A2Σ(v′=0) state under the pressure of 266 Pa was also obtained by measuring fluorescence decay curve of A2Σ(v′=0) states. It is about 53.76 ns. Fitting the curve of the fluorescence radiant lifetime versus pressure, the spontaneous radiant lifetimes and the rate coefficient of nonradiative transition relaxation of A2Σ(v′=0, 1) states were deduced.
2004 Vol. 24 (06): 641-643 [Abstract] ( 995 ) PDF (972 KB)  ( 329 )
644 Photoluminescent and Electroluminescent Properties of a New Rare Earth Terbium Complex
WANG Li1, ZHANG Xi-qing1，LIN Peng1, XIONG De-ping1, HUANG Shi-hua1，YU Tian-zhi2
Pure green and narrow bandwidth emission from an organic electroluminescent device was presented by using a new rare earth terbium (Ⅲ) complex as the emissive layer. The structure of the device was ITO/PVK/Tb/PBD/LiF/Al. It was proved that this new kind of rare earth complex has excellent photoluminescent and electroluminescent properties. The electroluminescent spectrum of the device was very similar to that of the terbium (Ⅲ) complex film. The electroluminescent mechanism of the device was proposed by measuring and analyzing the spectra and electroluminescent property of the device. It is proposed that the excited carriers of PVK and PBD were captured by Tb3+ and light was emitted when the electrons and holes recombined at Tb3+.
2004 Vol. 24 (06): 644-646 [Abstract] ( 1594 ) PDF (844 KB)  ( 485 )
647 Fluorescence Spectra and Fluorescence Quantum Yield of Sulfosalicylic Acid
WEI Yong-ju, LI Na, QIN Shen-jun
Fluorescence spectra and fluorescence quantum yield of sulfosalicylic acid (SSA) have been studied. Under the condition of pH＜2, SSA has no fluorescence. With the increase in pH value, fluorescence intensity of SSA increases. In the range of pH 5-10.5, SSA gives a strong and steady fluorescence with a maximum emission wavelength at 402 nm and excitation wavelengths at 212, 238 and 297 nm, respectively. In strong alkaline solutions with pH＞13, SSA exists as another fluorescence species with a maximum excitation wavelength at 261 nm and a maximum emission wavelength at 390 nm. The excitation spectrum of SSA changes when its concentration is relatively higher, but the emission spectrum remains unchanged. There is an excellent linear relationship between fluorescence intensity and the concentration of SSA under neutral condition. The linear range is 5-250 ng·mL-1, and the detection limit is 5 ng·mL-1. Using quinine bisulphate as a reference, fluorescence quantum yields of SSA at different wavelengths were measured. At the maximum excitation wavelength 297 nm, fluorescence quantum yield of SSA is 0.54.
2004 Vol. 24 (06): 647-651 [Abstract] ( 1446 ) PDF (949 KB)  ( 801 )
652 Spectral Evidences for Aggregation of Sulfonated Naphthalocyanine Zinc(Ⅱ) and Cobalt(Ⅱ)
LIU Ying1, 2，LIU Yue1, ZUO Xia2, WU Yi-qun2
When the naphthalocyanines were sulfonated to give sulfonated naphthalocyanine cobalt (Ⅱ) and sulfonated naphthalocyanine zinc (Ⅱ), enhanced aggregation tendency was observed. The Q band of the fluorescence emission spectra and electronic absorption spectra for sulfonated naphthalocyanine zinc (Ⅱ) and sulfonated naphthalocyanine cobalt (Ⅱ) in the solutions of DMF and ethanol showed that the excimer or the aggregation form coexists with the monomer, that the aggregation form dissociates into its monomer when the excimer releases a photon or the ground aggregation form absorbs a photon, and that mirror symmetry exists between the fluorescence emission spectrum of the excimer and the electronic absorption spectrum of the corresponding ground aggregation form. There is a red shift for the excimer in the fluorescence emission spectrum and a blue shift for the aggregation form in the electronic absorption spectrum of the Q band. The quenching effect in fluorescence emission spectrum is large when the concentration of sulfonated naphthalocyanine cobalt (Ⅱ) is high.
2004 Vol. 24 (06): 652-654 [Abstract] ( 1003 ) PDF (841 KB)  ( 369 )
655 Study on White Light Diffuse Reflection Spectrum of Chinese Herbal Medicine
CHEN Mao-xin
The white light diffuse reflection spectra of 57 kinds of Chinese herbal medicines were measured. Each of these spectra has some characteristics feature individually different from others. The spectra of those Chinese herbal medicines，whose medicinal sections are above ground (growing under sunlight)，have a larger absorption peak in the region 650-690 nm than those under ground and inside herbal medicine body (growing isn’t under sunlight, for example, the seeds). It was demonstrated that the white light diffuse reflection spectrum may be used to examine or distinguish Chinese herbal medicines as additional method and to control cultivation or growth of some Chinese herbal medicines.
2004 Vol. 24 (06): 655-658 [Abstract] ( 1355 ) PDF (885 KB)  ( 335 )
659 Frequency Stabilization of Diode Laser Using Zeeman Spectra
JIANG Kai-jun，WANG Jin，LI Ke，HE Ming，TU Xian-hua, ZHAN Ming-sheng
Zeeman split takes place for the hyperfine level structure of neutral atoms where magnetic field exists. In addition, being excited by right circularly polarized light and left circularly polarized light, atoms obey different transition rules. So, the absorption peak between the hyperfine Zeeman level shifts with respect to the absorption peak without magnetic field. Accordingly, the authors demonstrated a kind of simple and flexible method to stabilize the frequency of diode laser. The linewidth of diode laser was reduced to less than 1 MHz using this method. Through analyzing the experiment results, the authors found that when the sum of both shifts of the hyperfine level of atoms excited by right circularly polarized light and left circularly polarized light was equal to the FWHM(Full Width at Half Maｘimum) of the saturated absorption peak, the laser frequency was stabilized best.
2004 Vol. 24 (06): 659-662 [Abstract] ( 193 ) PDF (888 KB)  ( 368 )
663 Pressure-Tuning Infrared Spectral Study on the Single-Molecule-Magnet Manganese Complexes
XU Zhen-hua1，CHEN Zhi-da1, Ian S Butler2
The infrared spectra (IR) of single-molecule-magnet manganese complexes [Mn12O12(O2CC6H4-3-Cl)16(H2O)3(3Cl-C6H4CO2H)]·(3-Cl-C6H4CO2H)(Ⅰ) and [Mn12O12(O2CCH2Br)16(H2O)4]·4(CH2Cl2)(Ⅱ) were studied at high external pressure. The different pressure-induced phase transition pressures were observed for both complexes (complex Ⅰ, 25-29 kbar) and (complex Ⅱ, 29-35 kbar). Both were second-order pressure-induced phase transition. The possible changes from higher spin to lower spin happened near the phase transition pressure following the changes of their structures when undergoing the high pressures. The average value of pressure sensitivities in the low-pressure phase is unusually smaller (0.19 cm-1·kbar-1) than in the high-pressure phase (0.29 cm-1·kbar-1) in the complex Ⅰ. On the contrary, the average value of the pressure sensitivities in the low-pressure phase is higher (0.34 cm-1·kbar-1) than in the high-pressure phase (0.23 cm-1·kbar-1) in the complex Ⅱ as usually, which means that the possibility of compression is lower in the high-pressure phase than in the low-pressure phase.
2004 Vol. 24 (06): 663-665 [Abstract] ( 165 ) PDF (842 KB)  ( 356 )
666 Developing Robust Near Infrared Calibration Models
CHU Xiao-li，YUAN Hong-fu，WANG Yan-bin，LU Wan-zhen
There are three approaches to developing robust near infrared calibration models, including spectral pretreatment such as differentiation, Piecewise Multiplicative Scatter Correction(PMSC), Finite Impulse Response(FIR), and Orthogonal Signal Correction(OSC), to remove external variations, selecting wavelengths which are insensitive to external variations, and constructing temperature-hybrid calibration models. In this paper, these three strategies were investigated based on reforming gasoline NIR spectra collected at different temperatures in order to develop robust RON and benzene calibration models against temperature. It has been found that with only spectral pretreatment even OSC method fails to obtain satisfactory results, which could not remove the effects caused by temperature fluctuation. Selecting wavelengths by genetic algorithms and constructing temperature-hybrid calibration models, in which spectra measured at different temperature are combined into one calibration set, are both good approaches to developing robust NIR calibration models against temperature. The latter seems better because it needs no special knowledge and extra software, but the non-linear effects should be considered in practical applications.
2004 Vol. 24 (06): 666-671 [Abstract] ( 991 ) PDF (920 KB)  ( 498 )
672 Research on the Nonlinear Model of Near Infrared Spectroscopy and the Total Sugar of Tobacco Samples
CHEN Da, WANG Fang, SHAO Xue-guang, SU Qing-de
Near infrared spectroscopy (NIR) is an instrumental method applied for rapidly measuring the NIR spectra of pulverized tobacco samples and computing the chemical compositions from the spectral data. In the present paper, a mixed algorithm was employed for building the nonlinear model of NIR and the total sugar of tobacco samples. The mixed algorithm was combined with Partial Least Squares (PLS) method and Artificial Neural Network (ANN). The model based on the mixed algorithm was divided into two parts: linear part and nonlinear part, and the corresponding model of each part was built respectively. Compared with the classical multivariate calibration methods such as Principle Component Regression (PCR), PLS and nonlinear PLS (NPLS), the proposed procedure performed much better. The results showed that the mixed algorithm could be used for the quantitative analysis of the total sugar in tobacco samples.
2004 Vol. 24 (06): 672-674 [Abstract] ( 1111 ) PDF (877 KB)  ( 614 )
675 Research on Model and Wavelength Selection of Near Infrared Spectral Information
ZHENG Yong-mei1, ZHANG Jun2, CHEN Xing-dan2, SHEN Xuan-guo1, ZHANG Tie-qiang1
Based on stepwise linear regression, and according to the theory of near infrared absorbption, spectrum(1 000-2 500 nm) obtained by detector was divided into three ranges, which were Ⅰ(1 000-1 400 nm) and Ⅱ(1 400-1 860 nm) and Ⅲ(1 860—2 500 nm). In each range the regression wavelengths of different wavelength gaps were picked up stepwise. Regression coefficients and parameters were calculated by Matlab5.3 Program. Regression models were built up in different ranges with different wavelength gaps. Best models could be determined． Prediction results of protein content of ground wheat were displayed in scatter plots. Different results were discussed and compared，which has referencemeaning for application.
2004 Vol. 24 (06): 675-678 [Abstract] ( 1099 ) PDF (872 KB)  ( 587 )
679 A Rapid Method for Identification of Genus Lycium by FTIR Spectroscopy
PENG Yong1, SUN Su-qin2*, ZHAO Zhong-zhen1, LEUNG Hei-wun1
In this article, a method of using Fourier-transform infrared spectroscopy (FTIR) to identify 7 species and 3 variations of genus lycium (Gouqi) in China is described. This method is based on the additive IR absorptions of the chemical components and the differences of their relative contents in various Gouqi. These differences are reflected in the FTIR spectra. The method provides a novel fingerprinting technique for the identification and differentiation of traditional Chinese medicine. Such technique can serve as a rapid, simple, reliable and non-destructive analytical method for Gouqi as a Chinese material medication.
2004 Vol. 24 (06): 679-681 [Abstract] ( 957 ) PDF (896 KB)  ( 380 )
682 SERS Mechanism for Rhodium Electrode in the Ultraviolet Region
YANG Zhi-lin1, 2, WU De-yin1, REN Bin1, ZHOU Hai-guang2, TIAN Zhong-qun1*
Stable and good quality of Surface-Enhanced Raman Scattering (SERS) signal from net rhodium electrode in the ultraviolet region was observed for the first time by our group recently. In this paper, both qualitative and quantitative analyses are given to interpret the new experimental results mainly based on the electromagnetic field theory. The mechanisms of SERS for rhodium electrode in the ultraviolet region are mainly attributed to the lightning rod effect together with the weak surface plasmon resonance. According to the calculation, the surface-averaged enhancement factor (SEF) for rhodium electrode in the ultraviolet region is about two orders of magnitude when the surface of the substrate is roughened properly, which is in good agreement with the experimental results. The authors also give a comparative study to show why silver, which is the best SERS active substrate in the visible and near infrared region, can’t give any SERS signal when the 325 nm excitation line is used.
2004 Vol. 24 (06): 682-685 [Abstract] ( 988 ) PDF (867 KB)  ( 524 )
686 IR and Raman Spectroscopic Studies on the Complexes of Ytterbium with Pyran Derivatives
YUAN Ya-xian, GU Jian-sheng*, REN Zhi-gang, GU Ren-ao
The complexes of ytterbium(Yb) with 3-hydroxy-2-methyl-γ-pyrone(HL) and 3-hydroxyflavone(HL′) have been prepared respectively in the non-aqueous solution by direct electrochemical oxidation of sacrificial metal anodes, and their IR and Raman spectra have been measured. They provided the complemental information for deducing their structure. By comparing the spectra of the ligands and their complexes, the stretching vibrational band of —OH disappeared in the complexes, and the frequency shifts of some relevant bands of the ligands were observed, particularly for the stretching vibration of CO. In the low frequency region, new bands at 300-500 cm-1 were detected in YbL3 and YbL′3 respectively, which could be assigned to the stretching vibrational mode of Yb—O. All the obvious change in the IR and Raman spectra revealed that CO and —OH were coordinated with Yb center through oxygen atoms. Based on the IR and Raman results, the structures of the two complexes were proposed.
2004 Vol. 24 (06): 686-689 [Abstract] ( 978 ) PDF (858 KB)  ( 437 )
690 Infrared Spectroscopic Study of Changbaishan Diatomite
XIAO Wan-sheng, PENG Wen-shi, WANG Guan-xin, WANG Fu-ya, WENG Ke-nan
Changbaishan diatomite was treated under the conditions of temperature from 100 to 1 330 ℃, and examined by infrared spectroscopy applying the KBr-technique. In the range from 250 to 1 500 cm-1, the spectra of the samples at 100 to 1 100 ℃ show the same three characteristic broad bands at 1 100, 801 and 471 cm-1, which are similar to amorphous silica. Besides the above three broad bands, the spectra of 1 200 and 1 330 ℃ treated samples eｘhibit three new bands at 618, 386 and 301 cm-1, which indicate that the diatomite transforms into cristobalite. While all of the eleven samples show an asymmetric broad band at 3 440 cm-1 in the range from 3 000 to 4 000 cm-1, the spectrum of 500 ℃ treated sample begins to eｘhibit a 3 745 cm-1 band assigning to isolated Si—OH group stretching vibration. The 3 745 cm-1 band shows the highest intensity at 900 ℃, and disappears at 1 200 ℃. According to the absorbance of the 3 745 cm-1 band of different temperature treated samples, the H2O content in the form of Si—OH group was calculated semi-quantitatively, which indicates that the Si—OH group exists at the internal structure defects in addition to eｘisting at the surface. The transform mechanism of diatomite into cristobalite was also discussed.
2004 Vol. 24 (06): 690-693 [Abstract] ( 969 ) PDF (866 KB)  ( 470 )
694 Hydrothermal Synthesis and Spectra Properties of Compound Mn5(PO3(OH))2(PO4)2(H2O)4
WU Xiao-yuan1，ZHANG Han-hui1，2*，HUANG Chang-cang1，SUN Rui-qing1，YANG Qi-yu1，LIN Zhi-hua1
The title compound Mn5(PO3(OH))2(PO4)2(H2O)4 was synthesized under hydrothermal condition. Its crystal structure was determined by single-crystal X-ray diffraction. DRS, IR, fluorescence and TGA spectra were used to characterize the title compound. As a result, the compound is formed by linking with PO4 and MnO6, and the oxygen in it can be divided to three categories,so in IR spectra the characteristic peaks of Mn—O and P—O are separated in to three，respectively. In DRS there are two peaks at 210 and 250 nm coresponding Od→Mn and O<sub>b, c→Mn. In fluorescence spectra the emission peaks are located at 354 and 413 nm when excited at 218 and 310 nm. Besides，thermal behavior of the compound is discussed by TGA diagrams. Finally, quantum chemistry calculation is performed to explain the structure characteristic. HF=-4 558.659 555 1 a.u, HOMO(Alpha)=-0.280 80a.u，LOMO(Alpha)=0.015 27a.u，ΔE(Alpha)= 0.296 07 a.u;HOMO(Beta)=-0.259 19 a.u，LOMO(Beta)=0.001 08 a.u，ΔE(Beta)=0.260 72 a.u and Dipole=4.208 2 Debye。
2004 Vol. 24 (06): 694-697 [Abstract] ( 1622 ) PDF (950 KB)  ( 415 )
698 Study on Measuring Host-Guest Ratio of Inclusion Compound of β-CD-Permethrin by IR
SHAO Qiong-fang1, DONG Ming2*, XIE Xiao-hong1, ZENG Lan-ping1, LENG Lei-bao1
Permethrin is one of the agrochemicals used in tea gardens currently with the characteristic of being easily decomposed in light. Permethrin with β-cyclodextrin(CD) made into Inclusion Compound (IC) can increase its stability and reduce dosage to remain on the tea. Host/guest ratio is one of the important parameters of IC. The IC of permethrin with β-CD was prepared by means of liquid phase method and characterized by using IR. The result of the IR proves that the characteristic absorption peaks of the host and guest are not changed by forming their IC. The host/guest ratio of the IC measured by IR is 1∶1. Potassium sulfocyanate(KSCN) was chosen as an inside mark material, because it has only one strong absorption peak at 2 100 cm-1 and the peak was chosen as a quantitative peak of KSCN. The peak at 580 cm-1 is the characteristic absorption of the wreath vibration of β-CD and was chosen as a quantitative peak of β-CD. KSCN and β-CD were mixed with a certain quantity ratio and the mixture was analyzed by IR. The work curve of IR was established. A kind of new experimental method of measuring host/guest ratio of the IC was provided.
2004 Vol. 24 (06): 698-700 [Abstract] ( 586 ) PDF (842 KB)  ( 392 )
701 Study on the Degradation of Polymer Light-Emitting Diodes by In-Situ Micro-Raman Spectroscopy
LIN Hai-bo1, XU Xiao-xuan1, WU Hong-bin2，WU Zhong-chen1, YU Gang3, XU Jing-jun1, ZHANG Cun-zhou1*
The authors report Raman degradation study of polymer light-emitting devices under ambient conditions. In order to investigate the chemical degradation reaction in polymer light-emitting diode (PLEDs) devices, the chemical structure of the poly (2-(4-Ethylhexyl) phenyl-1, 4-phenylene vinylene) (P-PPV) polymer was analyzed by micro-Ramam spectroscopy during the lifetime of the devices. The evidence for the reduction of conjugation length is provided by Raman spectroscopy. This reduction of the conjugation length，which dramatically increases the resistance and cuts off the current density，was the main reason for the failure of lighting. These findings provide an important insight into the intrinsic degradation mechanisms of the polymer LEDs and help in the development of even more stable devices.
2004 Vol. 24 (06): 701-703 [Abstract] ( 1457 ) PDF (960 KB)  ( 386 )
704 Synthesis，Spectra, Nonlinear Optical Properties and Theoretical Calculations of Metal Complexes Containing Phenothiazine Ligand
XUE Zhao-ming1, ZHANG Xuan-jun1, TIAN Yu-peng1,2
A new ligand, S-benzyl-(-N-[10-ethylphenothiazinyl-3yl]-methylene] dithiocarbazate ( abbreviated as HL)，and its complexes ML2 (M=Co and Hg) have been synthesized and fully characterized by elemental analyses, EI-MS, 1H NMR, IR, UV-Vis spectra, and photoluminescence measurement. All of the compounds emit an olivine color in DMF solution. The emission maximum (λemmax), and fluorescence quantum(Φf) of each compound were measured. Nonlinear Optical properties of the HL and ML2 were studied by z-scan technique. Nonlinear absorption coefficient β were measured to be 0.71，0.19 and 0.395 cm·GW-1. Theoretical calculations (RHF/PM3) were consistent with the experimental results.
2004 Vol. 24 (06): 704-707 [Abstract] ( 1500 ) PDF (942 KB)  ( 412 )
708 Study on the Transition of Green，Yellow Fluorescence of Ternary Complexes of Tb-Benzoic Acid-1,10-Phenanthroline
WANG Xi-gui1，WU Hong-ying1，YAO Guang-qing2，WENG Shi-fu2，WU Jin-guang2
In this paper, ternary solid complexes of Tb-benzioc acid-1,10-phenanthroline have been synthesized. Compared with binary complexes of Tb-benzioc acid, their properties were investigated. The results showed that the second ligand-phenanthroline enhanced the fluorescence intensities of Tb3+, and shortened its fluorescence lifetime, and it was found that the aggregative state influenced the luminescence properties of ternary complexes. When particulates dispersed to a certain degree, the probability of 5D4→7F5 transition of Tb3+ was great, so, green fluorescence was observed for the complexes. With the aggregation of particles, the probability of 5D4→7F5 transition of Tb3+ decreased, while the probability of 5D4→7F3 transition increased. Therefore, ternary complexes of Tb-benzoic acid-1,10-phenanthroline eｘhibited yellow fluorescence. In addition, spectroscopic properties of the complexes were investigated.
2004 Vol. 24 (06): 708-712 [Abstract] ( 210 ) PDF (905 KB)  ( 525 )
713 Synthesis of 2-(2,5-Dihydroxyphenyl)-Tetraphenylporphrin and Its Structure Identification
CHEN Shi-qing, CHEN Zhang-ping*, HUANG Qi-mao, JIANG Zhong-xing
2-(2,5-dihydroxyphenyl)-tetraphenylporphrin 1′, 2-(2,5-dihydroxyphenyl)-tetraphenylporphyrinato Cu(Ⅱ)2′, Ni(Ⅱ)3′ and Zn(Ⅱ)4′ were synthesized by direct reaction of 2-nitro-5,10,15, 20-tetraphenylporphrin 1 or its metallic complexes 2, 3, 4 with hydroquinone under heating without solvent. The yields were about 81%, 71%, 61% and 40% respectively for 1′, 2′, 3′ and 4′. Their structures were determined by 1 H NMR, 2D NMR, IR, MS and UV-Vis spectra. It is shown that the hydroquinone connects with pyrrole ring through carbon-carbon bond, and is located in the same plane of porphyrin. One of the hydroxy group of hydroquinone is located in the deshield area of porphyrin and its proton shift occurs downfield at δ＝7.52. Another one is located in the shield area of meso benzene, and the proton shift occurs upfield at δ＝4.18. Also the 6 proton shift of hydroquinone occurs upfield at δ＝4.93.
2004 Vol. 24 (06): 713-716 [Abstract] ( 177 ) PDF (862 KB)  ( 442 )
717 Fluorescence Characteristics of Tb3+-Pefeoxacin and Determination of Pefeoxacin
ZHOU Jing, DU Li-ming*, CHEN Cai-ping
Terbium(Ⅲ) can react with Pefeoxacin(PEFX) to form 1∶2 coordination compound in a near neutral medium. Based on this reaction, we proposed a simple, rapid, and sensitive new method for the fluorimetric determination of Pefeoxacin and investigated the reaction conditions in detail;meanwhile we discussed the efficiency and mechanism of the intramolecular energy transfer. The results show that in the range of 0.01-1.67 μg·mL-1, there is a linear relationship between the concentration of PEFX and its fluorescence intensity, and the regression equation is F=120.01 C+2.608，with the detection limit of 0.01 μg·mL-1, the recovery within the range of 95.2%-101.7%，and the RSD of 2.9%-3.0%. This method has been successfully applied to the determination of Pefeoxacin in untreated human serum and gelatine capsule.
2004 Vol. 24 (06): 717-719 [Abstract] ( 928 ) PDF (889 KB)  ( 346 )
720 First Derivative Spetrophotometric Direct Determination of 2-Hydroxy-4-Methoxybenzo Phenone in Polyester Resin by Computer Assistant
WEI Xian-jun，SUN Rui-xia
2-hydroxy-4-methoxybenzo phenone (UV-9 ) is one of general auxiliary reagents used in paint resin and plastics, which can delay the material degradation and ageing of high polymer. Direct determination of high polymer by ultraviolet spectrum has not been reported. We selected an efficient solvent that can dissolve the resin of high polymer, and got an even，transparent and steady mensuration system. The first derivative absorption data of 2-hydroxy-4-methoxybenzo phenone(UV-9) were treated many times with smooth handing by Origin 6.1，a famous data analysis software. At a certain wavelength, the results accord with Beer′s law from 1.000 to 20.00 μg·mL-1, thus UV-9 can be measured directly. Its absorptivity is 5.7×104 L·mol-1·cm-1. The results of synthetic samples determined by this method showed that the relative standard deviation and the relative error of UV-9 are less than 5.25% and 4.75% respectively，and the UV-9 recovery rate is 98.88%-102.04%.
2004 Vol. 24 (06): 720-722 [Abstract] ( 1562 ) PDF (830 KB)  ( 334 )
723 Inhibitory Kinetic-Synchronous Fluorimetric Determination of Trace Aniline
ZHANG Ai-mei, JIA Li-ping
A novel kinetic-synchronous fluorimetric method is reported for the determination of trace aniline. The method is based on the inhibitory effect of aniline on the oxidation of fluorescein by potassium bromate in the presence of surfactant -CTMAB in the acid medium. Fluorescein’s oxidized product produces strong fluorescence. But its excitation and emission spectra overlap seriously. So this article adopted synchronous fluorimetric spectra to diminish spectra overlap and obtained very good sensitivity and selectivity. The detection limit for aniline is 0.3 μg·L-1, and the linear range is 0-10 μg·L-1. The proposed method has been applied to the determination of trace aniline in waste water and laboratory water with satisfactory results.
2004 Vol. 24 (06): 723-725 [Abstract] ( 1043 ) PDF (890 KB)  ( 343 )
726 Photo-Fenton Oxidation Processes Used in the Degradation of Rhodamine B
ZHENG Huai-li, XIANG Xin-yi
Photo-Fenton method, the combination of Fenton reagent with light, is an efficient method for waste water treatment. In this paper, the degradation of rhodamine B (a kind of organic dye) using this method was researched. Through numerous experiments, the influences of five parameters including light source, pH, reaction time, dosage of Fenton reagent，and initial dye concentration were investigated intensively. In this paper, the mechanisms of this reaction have also been probed. It is concluded from the experiments that the irradiations of 450 W high-pressure mercury lamp and sun light can both accelerate the process of degradation effectively. Under optimal conditions, the overall color removal was more than 99.9% within 45 min; COD can be removed effectively at the same time.
2004 Vol. 24 (06): 726-729 [Abstract] ( 1043 ) PDF (889 KB)  ( 389 )
730 Simultaneous Determination of Copper and Iron by Catalytic Kinetic Spectrophotometry
HE Chi-yang, WU Gen-hua, CHENG Qiong, CHEN You-cun
A simultaneous catalytic effect copper(Ⅱ) and iron(Ⅲ) on the oxidation of acid chrome blue K by potassium bromate in dilute sulfuric acid medium was observed. But there was an obvious difference in their reaction rates，and the ratio of the reaction constant changed with time. And their spectral addiitive properties were not satisfactory. The simultaneous determination of copper and iron by catalytic kinetic spectrophotometric method was realized by using a three-layer Levenberg-Marｑuardt BP neural network to cope with the eｘperimental data. The optimum conditions of reaction and determination were studied. The calculation results of the determination in synthetic samples and human hair were satisfactory.
2004 Vol. 24 (06): 730-732 [Abstract] ( 952 ) PDF (890 KB)  ( 349 )
733 Determination of the Content of Wear Metal in Lubrication Oil by ICP-AES
ZHAO Jin-wei1, 2，CHENG Wei2，FENG Ya-hui2
An analytical method for determining wear metal elements directly by ICP-AES was proposed in this paper. The optimum condition was selected. The Conostan S-21 and Conostan 75 (oil-base standard samples) prepared by multi-element oil-base reserved standard samples were applied to make calibration curve. Oil samples were diluted 5 times by kerosene. The contents of wear metals in lubrication oil were determined by ICP-AES. The relative standard deviation (RSD) of all elements was less than 1%. In addition, the authors represented the analytical efficacy of Leeman labs multi-track profile ICP, and its rapid and accurate characters of simultaneous multi-element measurement.
2004 Vol. 24 (06): 733-736 [Abstract] ( 1608 ) PDF (839 KB)  ( 381 )
737 Determination of Inorganic Elements in Plantago by ICP-AES
FU Zhi-hong，XIE Ming-yong*，ZHANG Zhi-ming，GUO Lan
In this paper, the contents of elements Se, Zn, Mn, Cu, Mg, Fe, Al and Be in the plantago, originating from different places and produced with various methods, were determined by ICP-AES technique. Its recovery ratio obtained by standard addition method ranged between 80.4% and 119.7%, and its RSD was lower than 6%. The results of the determination show that the seeds in plantago are rich in the inorganic elements such as Mg, Fe, Al and Zn essential to human health.
2004 Vol. 24 (06): 737-740 [Abstract] ( 1606 ) PDF (972 KB)  ( 376 )
741 Determination of Trace Copper and Zinc in Hypertension Complicated with Hyperlipemia by Atomic Absorption Spectrophotometry
HE Bang-ping1, LI Dong-fang2, MA Jian-wei3, CHEN Jie1, LIU Xiao-yu1, ZHANG Xin-rong1, XU Jian-ming1
The serum levels of Zn, Cu, cholesterol (Ch) and triglyceride (TG) were determined in 44 patients with hypertension complicated with hyperlipemia, 42 patients with hypertension(HP) and 30 healthy controls by atomic absorption spectrophotometry and automatic biochemical analytical instrument of reagent kit. It was found that the contents of Zn, Ch, TG and Zn/Cu ratio in hypertension complicated with hyperlipemia were significantly higher than in HP and control, while Cu in hypertension complicated with hyperlipemia was significantly lower than in HP and control. The contents of Zn, Ch, TG and Zn/Cu ratio in hypertension were significantly increased. It is suggested that hypertension complicated with hyperlipemia is closely related with Zn and Cu.
2004 Vol. 24 (06): 741-743 [Abstract] ( 410 ) PDF (871 KB)  ( 465 )
744 The Research to the Optimal Calibration Model for Discrete Scanning Spectrometers
LU Yong-jun, QU Yan-ling, ZHANG Jun, PIAO Ren-guan
For spectrometers which don’t operate in consistently scanning mode such as fixed-filter spectrometer, diode arrays spectrometer and so on，how to find an optimal wavelengths combination rapidly and accurately has always been a key problem in NIR so far. The conventional methods to choose the optimal wavelengths for calibration are Forward Stepwise multiple linear Regression(FSR) and Backward Stepwise Regression(BSR), which choose the optimal wavelengths based on the t test result of all the calibration wavelengths. However, maybe the wavelength eliminated is very useful in application and the wavelength chosen may not be so useful as expected, as a result it is compulsory to make more tests to verify the truly applicable wavelength combination for calibration. In this paper the combination of the combination-making algorithm in combinatorics and computer languages which operate facing matrix is used to choose the optimal combination of wavelengths for calibration automatically and efficiently by computer. The most robust calibration equation can be obtained by making analysis of calibration regression that operates to find the minimum root mean standard error of calibration.
2004 Vol. 24 (06): 744-747 [Abstract] ( 1034 ) PDF (823 KB)  ( 503 )
748 1H NMR Analysis of Rice Wine Treated by Electric Field
ZENG Xin-an，FU Xiong, LI Guo-ji，YU Shu-juan
This paper studied the 1H NMR spectrum change of Guangdong rice wine. Three kinds of rice wine were studied: raw wine, finished product wine and electric-field-treated wine(40 kV·m-1, 50 Hz, 180 min). Results showed that many weak peaks appeared in raw wine’s CH3— and —CH2— peaks in contrast to the other two samples, reflecting that single molecules and various kinds of hydrogen-bonded clusters coexisted in the raw wine, and many kinds of organic compounds also contributed to forming peaks. As to the peaks of hydroxide H, the peak forms of the three samples were level, single sharp and irregular，respectively(raw, finished product and electric-field-treated wine). The level peak of raw wine inferved that there were two kinds of hydroxide H existed, one was involved in forming hydrogen bonds，while the other was not. The single sharp peak of finished product wine showed that single stable large hydrogen-bonded clusters were formed in the wine, and the irregular peak of electric-field- treated wine illustrated that there might exist various kinds of hydrogen-bonded clusters, whose main structure was similar to that of the finished product wine.
2004 Vol. 24 (06): 748-751 [Abstract] ( 938 ) PDF (944 KB)  ( 350 )
752 EXAFS Study on the Stripping Mechanism in N263/Alkaline Cyanide Gold Solution/Sulfuric Thiourea System
TANG Hong-ping1, YANG Ming-de1, HE Pei-jiong1，HU Tian-dou2, ZHANG Jing2, XIE Ya-ning2
Quaternary ammonium salt has strong affinity with gold in cyanide solutions, but it is not readily stripped. Stripping with acidic thiourea solutions and air sparging shows promise. There are some reports on the process of thiourea stripping, but little about its mechanism. In this paper, the stripping mechanism of N263/sulphuric thiourea/alkaline cyanide gold solution is studied by EXAFS. According to the experiments, sulphuric acid, thiourea and gold-thiourea complex can be extracted by N263 as a neutral molecule, and the stripping process can be described as following: (1) Sulphuric acid and thiourea are extracted by N263; (2) In organic phase, gold-cyanide complex is converted to gold-thiourea complex, which exists as Au[SC(NH2)2]2HSO4, and CN- forms HCN with acid at the same time; (3) HCN is removed by air sparging, and Au[SC(NH2)2]2HSO4 is distributed between organic phase and liquor phase, most of which transfers to liquor phase and is stripped.
2004 Vol. 24 (06): 752-755 [Abstract] ( 983 ) PDF (905 KB)  ( 361 )
756 Study on the Eu-containing Coordination Polymer Ⅰ.Structural Characterization of Eu(Ⅲ)-thienyltrifluroacetone-poly (Styrene-acrylic acid)
XIAO Li-ren, GAO Feng, TANG Jie-yuan, ZHANG Wen-gong*
Three samples (a), (b) and (c) of luminescent Eu-containing copolymer (NaEu(Ⅲ)-TTA-PSAA) were synthesized through the reaction of copolymer of acrylic acid and styrene (Mw＝3 000) with metalorganic complex (NaEu(TTA)4) obtained from Eu and thienyltrifluroacetone. These samples of coordination polymers were characterized by FTIR, UV and XPS, and their composition and structures were determined. The results of electrical conductivity methods and elemental analysis indicated that there were different compositions and structures of these coordination polymers in different pH. The results of elemental analysis also showed that the content of Eu3+ in sample (a), (b) and (c) was 11.89%，12.55% and 13.41%, respectively.
2004 Vol. 24 (06): 756-761 [Abstract] ( 393 ) PDF (969 KB)  ( 497 )
762 Study on the Reaction between Cobalt Tetrasulphonated Phthalocyanine and Sodium Sulfide
LIU Wei，YE Tao，GUO Rong
A new method which uses multi-wave number and double-parameter to analyse the UV-Vis. spectra is proposed to determine the composition and stabilization constants of coordination compounds. With this method, the reaction of cobalt tetrasulphonated phthalcyanine[CoTsPc] and sodium sulfide[Na2S] was studied. The result shows that pH of the medium has great effect on the reaction. A five coordinated compound Co(Ⅱ)TsPc(HS) was formed at pH=7.0. The equilibrium constants and thermodynamics are reported for the reaction under that condition. At higher pH, a redox-reaction took place and a five coordinated compound with the oxidation number Ⅰ for cobalt [SCo(Ⅰ)TsPc] was found.
2004 Vol. 24 (06): 762-767 [Abstract] ( 1394 ) PDF (961 KB)  ( 385 )

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