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2007 Vol. 27, No. 06
Published: 2007-06-26
 
       光谱学与光谱分析
1041 Spectral Studies on Liquid Crystal Photoalignment Film of Photosensitive Monomer with Fluorinated Groups
FEI Chun-hong1,2,ZHANG Ling-li1,2,YAO Li-shuang1,2,LÜ Feng-zhen1,2,PENG Zeng-hui1,XUAN Li1*
2,2,3,3,4,4-hexafluoro-1,5-pentanediol dicinnamate ester, which could be crosslinked under irradiation of linearly polarized ultraviolet light, was synthesized in the present work. UV-Visible spectra and FTIR spectra revealed that [2+2] cycloaddition was the main reaction of the monomer, but there was no clear morphological anisotropy on the surface of the obtained photoalignment film through atomic force microscopic analysis. The photoalignment film could induce homogenous alignment of liquid crystal and the alignment is uniform. It was found that the pretilt angle of the photoalignment film is 1°-2°.
2007 Vol. 27 (06): 1041-1043 [Abstract] ( 1491 ) PDF (1070 KB)  ( 414 )
1044 Energy Transfer in Cs(6P)+(Ne, N2) Collisions
WANG Shu-ying,SUN Mao-zhu,DAI Kang,SHEN Yi-fan*
The collisional energy transfer process Cs(6P3/2)+M,where M＝Ne, N2,under gas cell conditions has been investigated. The Cs(6P3/2) state was excited by a diode laser. The direct 6P3/2→6S1/2 fluorescence and the sensitized 6P1/2→6S1/2 fluorescence as a function of quenching gas pressure were measured. For quenching by Ne only energy transfer from the electronic to translational is possible. However, in the N2 case, energy transfer from the electronic to vibrational or rotational is important. Using a two-state rate equation model, the quenching rate coefficients for Cs(6P3/2) were obtained. The fine structure energy transfer rate coefficient for Ne is 1.45×10-12 cm3·s-1. By comparing the relative fluorescence intensities for Ne and N2 case, the authors estimate that the rate coefficient for 6P3/2→6P1/2 transfer in collision with N2 is 1.64×10-12 cm3·s-1. The quenching rate coefficient for the 6P state is 4.88×10-12 cm3·s-1.
2007 Vol. 27 (06): 1044-1046 [Abstract] ( 1045 ) PDF (526 KB)  ( 412 )
1047 Effects of Argon Atmosphere at High Pressure on Electron Temperature of Laser-Induced Cu Plasmas
CHEN Jin-zhong, SHI Jin-chao, GUO Qing-lin, HUAI Su-fang, WEI Yan-hong
Copper plasma was induced with a high energy neodymium glass laser(0-25J) beam ablating the Cu target in argon atmosphere. It was observed that the line intensity of the emission spectra increases when the ambient pressure(0.1-0.5 MPa) rises. In order to study the enhancement mechanism, with the model of local thermodynamic equilibrium, the electron temperature was measured in argon atmosphere. The experimental results showed that electron temperature increases as the pressure rises. In addition, spatially resolved electron temperature was measured in Ar atmosphere at 0.1, 0.3, 0.5 MPa.
2007 Vol. 27 (06): 1047-1050 [Abstract] ( 1678 ) PDF (1253 KB)  ( 456 )
1051 High Contrast Organic Light-Emitting Diodes Using Pb-LiF as Cathode
CONG Yang,CHEN Zhi-jian*,GONG Qi-huang*
A metal-insulator complex film made by co-evaporating metal Pb and transparent insulator LiF was tested as a low-reflecting cathode to realize high contrast organic light-emitting diodes (OLED). The optical reflectivity and electrical characteristic of the high contrast OLED were studied as compared with the device based on Al as the cathode. The reflectivity of the Pb-LiF complex cathode is 18% only, about 5 times lower than that of Al cathode. The experimental result shows that the high contrast and the conventional OLEDs are similar in terms of the electroluminescent property.
2007 Vol. 27 (06): 1051-1053 [Abstract] ( 1032 ) PDF (666 KB)  ( 437 )
1054 Effects of Zn2+ Doping on the Structural and Luminescent Properties of GdTaO4∶Eu3+ Phosphors
XIAO Li-hong,GU Mu*,LIU Xiao-lin,ZHANG Rui,LIU Bing-jie,XU Xin
GdTaO4∶Eu0.1 phosphors with different concentrations of Zn2+ dopant were synthesized by the solid-state reaction at high temperature. The present paper mainly focused on the effects of Zn2+ on the crystallization behavior, morphology and photoluminescence (PL) properties of GdTaO4∶Eu3+. The synthesized materials were characterized by X-ray diffraction (XRD), scanning electronic microscopy (SEM), PL excitation and emission spectra, decay time curves, etc. Results suggested that the co-doping of Zn2+ could remarkably improve the PL intensity of GdTaO4∶Eu0.1,and there were two maxima in the curve of Eu3+ PL intensity at 611 nm vs Zn2+doping concentration x. When x=0.01 the intensity was improved up to 2.7 times that of pure GdTaO4∶Eu3+,which could be attributed to the creation of oxygen vacancies for the charge neutrality and the alternation of the local environment of activator Eu3+ions resulting from the incorporation of Zn2+ ions; the other was enhanced up to 3.2 times at x=0.13 which was due to the flux effect of Zn2+ ions. But ZnO and GdTa7O19 were observed in an excessive Zn2+ doping range (x>0.13), which resulted in the decrease in the PL brightness and lengthening of decay time. Meanwhile, primary results indicated that the PL intensity of GdTaO4∶Eu0.1,Zn0.13 could be further strengthened by the co-doping of Li+ and K+ ions.
2007 Vol. 27 (06): 1054-1057 [Abstract] ( 1124 ) PDF (1310 KB)  ( 466 )
1058 Hydrothermal Synthesis and Luminescence of One-Dimensional Mn2+-Doped CdS Nanocrystals
YUAN Qiu-li1,ZHAO Jin-tao1,NIE Qiu-lin1,2
One-dimensional Mn2+-doped CdS nanocrystals were synthesized by the hydrothermal route. The products were characterized by SEM, EDS, XRD, TEM, HRTEM and PL, respectively. The results revealed that dopant Mn2+ completely substitutes Cd2+ in CdS nanocrystals, and the product was of good crystallite. Further more, a complete suppression of the emission from surface states at room temperature when doping with ions Mn2+ has been observed.
2007 Vol. 27 (06): 1058-1061 [Abstract] ( 2246 ) PDF (1196 KB)  ( 489 )
1062 Rapid Prediction of Annual Ring Density of Paulownia elongate Standing Tress Using Near Infrared Spectroscopy
JIANG Ze-hui1,WANG Yu-rong1*,FEI Ben-hua1,FU Feng1,HSE Chung-yun2
Rapid prediction of annual ring density of Paulownia elongate standing trees using near infrared spectroscopy was studied. It was non-destructive to collect the samples for trees, that is, the wood cores 5 mm in diameter were unthreaded at the breast height of standing trees instead of fallen trees. Then the spectra data were collected by autoscan method of NIR. The annual ring density was determined by mercury immersion. And the models were made and analyzed by the partial least square (PLS) and full cross validation in the 350-2 500 nm wavelength range. The results showed that high coefficients were obtained between the annual ring and the NIR fitted data. The correlation coefficient of prediction model was 0.88 and 0.91 in the middle diameter and bigger diameter, respectively. Moreover, high coefficients of correlation were also obtained between annual ring density laboratory-determined and the NIR fitted data in the middle diameter of Paulownia elongate standing trees, the correlation coefficient of calibration model and prediction model were 0.90 and 0.83, and the standard errors of calibration(SEC) and standard errors of prediction(SEP) were 0.012 and 0.016, respectively. The method can simply, rapidly and non-destructively estimate the annual ring density of the Paulownia elongate standing trees close to the cutting age.
2007 Vol. 27 (06): 1062-1065 [Abstract] ( 1200 ) PDF (520 KB)  ( 451 )
1066 Distribution of Nitrogen and Hydrogen in Diamond and Its Significance to Nucleation and Growth of Diamond
YANG Zhi-jun,PENG Ming-sheng,MENG Yu-fei,YUAN Zhi-zhong,SU Yu-wei,LI Hong-zhong
From the center to the rim of natural diamond there are differences in nitrogen and C—H bond contents, suggesting that diamond was formed under varying substance conditions. Both the nitrogen and C—H bond contents tend to decrease from the center to the rim as a whole, indicaing that nitrogen and hydrogen are expended little by little during the formation of diamond. But in the middle area of the sample both the nitrogen and C—H bond contents have a tendency to increase. This implies that nitrogen and hydrogen are added into the environment of diamond formation. meanwhile nitrogen is added earlier. So the procedure of diamond formation may be divided into three stages, namely nucleation and growth in the early stage, growth in the middle stage and in the late stage. In the early and late stages nitrogen and hydrogen are consumed in the environment of diamond formation. In the middle stage nitrogen and hydrogen must be replenished for the growth of diamond, and nitrogen should be replenished earlier than hydrogen. Hydrogen is useful to the nucleation and growth of diamond. During the formation of diamond the compounds of nitrogen and hydrogen do not exist. So we must avoid the formation of compounds of nitrogen and hydrogen for the nucleation and growth of diamond if we plan to introduce hydrogen to the synthesis of diamond at high temperature and high pressure (HPHT). Implanted hydrogen in graphite for the HPHT synthesis of diamond is a good choice.
2007 Vol. 27 (06): 1066-1070 [Abstract] ( 1192 ) PDF (810 KB)  ( 510 )
1071 Phase Transitions of Surface-Stabilized Liquid Crystal Studied by Temperature-Dependent FTIR Spectroscopy
CHENG Yu-chuan1,SUN Li1,ZHAO Chun2,WANG Xu1,XU Wei-qing1,ZHAO Bing1*
The FTIR spectra were measured for liquid crystal molecules in CaF2 cell over a temperature range of 40-150 ℃. The alkyl chain transformed from ordered zigzag-dominated conformation to disordered gaucheness-dominated conformation with increasing temperature. Meanwhile, the degree of freedom of the rotation of the carbonyl group increased, the co-plane interaction between the carbonyl group and the phenyl ring broke, and the conjugation between the CO bond and the phenyl ring was reduced at the SCA*→SA phase transition point, followed by the increase of the plane angle between the two phenyl rings. Due to the surface stability effect of the LC cell, there existed on the cell surface a layer whose structure was independent of the temperature and LC phase. Therefore, the molecules still retained its originally phase property even at temperatures near and above the transition point.
2007 Vol. 27 (06): 1071-1073 [Abstract] ( 2362 ) PDF (989 KB)  ( 425 )
1074 The Analysis of Vital Reaction Following Skin Injury Close to Death in Mouse by FTIR
HUANG Ping1,YANG Guang-de3,TUO Ya1,2,WANG Zhen-yuan1*
Fourier transform infrared spectroscopy (FTIR) was applied to study the difference of vital reaction following skin injury close to death in mouse and provided the evidence for forensic practice. The results demonstrated that vital 5 min, postmortem and normal groups showed significant differences in the wave form and intensity: (1) The intensity at 3 007 and 1 745 cm-1 related to lipid for the vital injury was higher than that for the postmortem; (2) The intensity at 1 160 cm-1 related to carbohydrate for the vital injure increased more compared to the postmortem; (3) The intensity of the band at 1 640 cm-1 related to amideⅠband for the injury groups was higher than the normal, but it was the lowest for the vital injury. These results show that it will be possible for FTIR to become an effective method to determine the vital reaction of injury close to death in forensic practice.
2007 Vol. 27 (06): 1074-1076 [Abstract] ( 1571 ) PDF (606 KB)  ( 417 )
1077 Processing of Interferogram Symmetrization in Optical Fiber Fourier Spectrometer
LI Bao-sheng1,LIU Yong2,WANG An2
The asymmetry of an interferogram is caused by off-center sampling or defects in the fiber interferometer, and the spectra from Fourier cosine transformations of one-sided interferogram have phase errors. A method was firstly applied to symmetrizing interferogram by using the convolution technique in optical fiber Fourier spectrometer (FFTS). The phase error can be derived from the central portion of the interferogram. Symmetrization function was obtained from the Fourier transform of the phase error. Thus in spatial domain the symmetrization function convolved with original interferogram, and the spectra with correction of phase errors resulted from the symmetrized interferogram. Experimental study shows that the method efficiently corrects the phase error in FFTS. The method not only overcomes the disadvantages of two-sided interferogram, but also has better accuracy of the results.
2007 Vol. 27 (06): 1077-1080 [Abstract] ( 2322 ) PDF (994 KB)  ( 504 )
1081 The Rapid and Nondestructive Identification and Infrared Spectra Visualization of Banlangen Granule
LI Yan1,WU Ran-ran1,YU Bai-hua1,HU Lan-ping1,2,WANG Jun-de1
Banlangen granule is the main medicament of Banlangen, and is widely used for the prevention and cure of flu and viral infection. In the present article, Fourier transform infrared (FTIR) spectroscopy was used in the identification and analysis of the traditional Chinese medicine, Banlangen granule. The FTIR spectra of Banlangen granule samples coming from different companies and different batches of the same company were obtained. The curves of original absorbance and the second derivatives of the absorbance were analyzed for identification, and compared with those of indigowoad root and indigowoad leaf, which are their raw medicine materials. In addition, the infrared fingerprint spectra were visualized in the form of color bar figure. Results showed that characteristic fingerprint spectra of Banlangen Granule could be picked up effectively, and the products quality of different pharmaceutical factories and the spectra of different batch numbers from the same factory could be revealed directly by FTIR spectroscopy combined with the second derivative spectrum and fingerprint spectrum visualization of analytical data. Thus they were differentiated conveniently, accurately, quickly and directly with this method, providing a simple and effective technique in supervising and examining the quality of the traditional Chinese medicine.
2007 Vol. 27 (06): 1081-1085 [Abstract] ( 1640 ) PDF (849 KB)  ( 453 )
1086 Investigation of Amanitaceae Mushrooms by Fourier Transform Infrared Spectroscopy
ZHAO De-zhang1,LIU Gang1*,SONG Ding-shan2,LIU Jian-hong3,ZHOU Yi-lan4,OU Jia-ming1,SUN Shi-zhong3
In the present paper, FTIR was used for obtaining vibrational spectra of untreated Amanitaceae mushrooms harvested in the mountains of Yunnan province, Southwest of China. The results show that the spectra of fruiting body and spore exhibit obvious differences. In the spectra of fruiting body, the strongest absorption band appears at about 1 655 cm-1,which is described as amide Ⅰ. There are two strong absorption bands at 1 077 and 1 042 cm-1 which are assigned to C—O stretching in carbohydrate. The vibrational spectra indicate that the main compositions of the Amanitaceae mushrooms are protein and carbohydrate. The spectrum of spore of Amanita fritillaria shows strong bands at 2 926, 2 855 and 1 747 cm-1,which can be assigned to the absorption of lipids. The spectra of fruiting body exhibit complicated patterns in the interval between 1 800 and 750 cm-1,which may be used to discriminate different species of Amanitaceae mushrooms. In addition, FTIR spectral differences were observed between different parts of Amanita manginiana. The result suggests that the chemical constituents are various in different parts of fruiting bodies. It is showed that FTIR spectroscopic method is a valuable tool for rapid and nondestructive identification of Amanita mushrooms.
2007 Vol. 27 (06): 1086-1089 [Abstract] ( 1553 ) PDF (849 KB)  ( 445 )
1090 Study on Infrared Absorption Spectra of High Cholesterol Blood Sample
YAO Hong-bing1,YE Xia1,ZHAO Zhi-min2
The research on the technology of infrared absorption spectrum and its application plays an important role in the development of technology of optical measurement. The analysis technology of blood infrared absorption spectrum is presented in the present paper. By comparison between and analyzing the infrared absorption spectra of the normal blood sample and the high cholesterol blood sample, the differences were obtained. The infrared absorption spectra of normal blood serum and high cholesterol blood serum were detected, and the differences between the spectra are presented. The analysis results indicate that the differences of the absorptivity, the absorption peak position and the absorptivity ratio between the normal blood sample and the high cholesterol blood sample can be taken as a criterion to check the normal and abnormal blood sample. This work, valuable for application, provides an important reference for the diagnosis of diseases.
2007 Vol. 27 (06): 1090-1092 [Abstract] ( 581 ) PDF (526 KB)  ( 509 )
1093 Progress in Application of Infrared Spectroscopy and Comparative Study of Chromatographic Fingerprints
LIU Yan1,LIU Shun-hang1,WANG Jun-quan1,SUN Su-qin2*
The newest development of applications of IR techniques to the identification of Chinese herbs, the discrimination of folk medicine herbs, Chinese herbs processing and Chinese traditional injection, which involving enhancing computer analysis depth, intensifying the pre-treatment of Chinese herb and using 2D-IR correlation spectroscopy for processing control, was elaborated in the present paper. Meanwhile, the establishment of multi-component determination analysis system of chromatographic fingerprint diagram was shown. And the sameness and difference of the IR spectroscopy and chromatography fingerprint diagram techniques were analyzed, and a comparison was made in terms of quality control of Chinese herbal medicine.
2007 Vol. 27 (06): 1093-1097 [Abstract] ( 2594 ) PDF (797 KB)  ( 448 )
1098 Nondestructive Quantitative Analysis of Cofrel Medicines by Improved Partial Least Squares-NIR Spectroscopy
LIU Ming-yang1,MENG Yu2,REN Yu-lin1,ZHANG Han-qi1
In the present paper，improved partial least squares(PLS) method was used to parse near infrared(NIR) reflectance spectrum of Cofrel medicine. The contents of benproperine phosphate，a availability pharmaceutical in Cofrel medicine，were accurately nondestructively quantitatively predicted. The best number of principal components (PC) was designed by scores plot of samples in PC. The effects of the wavelength range，conventional spectra，first-derivative spectra and second-derivative spectra on the results were discussed respectively. Comparing the results with those of HPLC，the relative errors(RE%) of benproperine phosphate were less than 0.42%. The analytical results were sufficient for practical manufacture of Cofrel medicine.
2007 Vol. 27 (06): 1098-1101 [Abstract] ( 1175 ) PDF (855 KB)  ( 476 )
1102 The Surface Adsorption and Selective Catalytic Reaction of NO on Cu-ZSM-5 Using In situ DRIFTS
ZHANG Ping1,WANG Le-fu2,CHEN Yong-heng1
The prepared Cu-ZSM-5 catalyst presents higher activity at low temperature during the selective catalytic reduction (SCR) of NO, and the conversion from NO to N2 is 70.6% at 613 K. The in situ diffuse reflectance FTIR spectroscopy (in situ DRIFTS) is an important method for studying surface adsorption of catalyst and mechanism of catalytic reaction, and was used to study the surface adsorbed species and the selective catalytic reduction reaction of NO on Cu-ZSM-5 catalyst in the presence of propene as reductant, with excess O2 and at 298-773 K. Based on the in-situ DRIFTS, a reaction mechanism is proposed that on Cu-ZSM-5, NO is first transformed to a series of NOx surface adsorbates, then these species react with the activating species of propene (CxHy or CxHyOz) to form organo-intermediates, including a process from organo-NH to organo-CN again to organo-NOx (organo-nitro or organo-nitrito), and finally these key intermediates react to form nitrogen. The role of Cu is to promote NOx content. Propene is easily activated on Cu-ZSM-5 with oxygen, and furthermore, the presence of oxygen is necessary to form organo-NOx intermediates.
2007 Vol. 27 (06): 1102-1105 [Abstract] ( 2302 ) PDF (1194 KB)  ( 574 )
1106 Spectral Analysis of the Effect of Different Polymerization Potential on Electrosynthesized Poly (5-Nitroindole) Films
ZHOU Wei-qiang1,2,XU Jing-kun2,WANG Jing-wu1*,PU Shou-zhi2
High quality poly (5-nitroindole) (PNI) films can be synthesized electrochemically by direct anodic oxidation of 5-nitroindole (NI) in boron trifluoride diethyl etherate (BFEE) at different polymerization potential in the range of 1.23-2.23 V (vs. SCE). To the best of our knowledge, this is the first time that high quality polymer films of nitro group substituted conducting polymers were electrodeposited. The oxidation onset potential of NI was only 1.04 V vs. SCE in this medium. Chronoamperometric response of NI, FTIR and 1H NMR indicated that the polymerization potential had a great effect on the quality of PNI films. Lower potential is helpful for the electrochemical polymerization of NI and the extension of the conjugation length of PNI. On the other hand, a higher potential led to side reactions and poor polymer film quality. The structural characterization of PNI films by FTIR and 1H NMR indicated that the electrochemical polymerization of NI occurred at C2 and C3 positions.
2007 Vol. 27 (06): 1106-1109 [Abstract] ( 2128 ) PDF (1098 KB)  ( 466 )
1110 Identification of Sulphur Residue in Chrysanthemum by Fourier Transform Infrared Spectroscopy
ZHAO Hua-rong, WEN Shu-min, FENG Ya-qi, WANG Xiao-yan, CHEN Guan-hua
Qi and Huai chrysanthemum samples processed in different ways were discriminated by means of Fourier transform infrared (FTIR) spectroscopy. It was shown that different processing methods may result in the variation of relative content of effective components in chrysanthemum. The variation of chemical structure may also occur. And the variations can be reflected differently on the transform infrared spectra. The dry chrysanthemum smoked with sulphur had different characters in the vibration frequency and shape of IR from other samples at 1 600 and 1 060 cm-1,and showed static characteristic absorptions at 922, 818 and 777 cm-1,which were stronger than others. The chrysanthemum processed in different ways showed differences in the Fourier transform infrared spectra. The sulphur residue in chrysanthemum can be identified by FTIR without separation and abstraction. This method is not only quick and precise but also convenient and direct. Different sorts of chrysanthemum can be identified in this way.
2007 Vol. 27 (06): 1110-1112 [Abstract] ( 435 ) PDF (667 KB)  ( 504 )
1113 Study on Predicting Firmness of Watermelon by Vis/NIR Diffuse Transmittance Technique
TIAN Hai-qing,YING Yi-bin*,LU Hui-shan,XU Hui-rong,XIE Li-juan,FU Xia-ping,YU Hai-yan
Watermelon is a popular fruit in the world and firmness (FM) is one of the major characteristics used for assessing watermelon quality. The objective of the present research was to study the potential of visible/near Infrared (Vis/NIR) diffuse transmittance spectroscopy as a way for the nondestructive measurement of FM of watermelon. Statistical models between the spectra and FM were developed using partial least square (PLS) and principle component regression (PCR) methods. Performance of different models was assessed in terms of correlation coefficients (r) of validation set of samples and root mean square errors of prediction (RMSEP). Models for three kinds of mathematical treatments of spectra (original, first derivative and second derivative) were established. Savitsky-Goaly filter smoothing method was used for spectra data smoothing. The PLS model of the second derivative spectra gave the best prediction of FM, with a correlation coefficient (r) of 0.974 and root mean square errors of prediction (RMSEP) of 0.589 N using Savitsky-Goaly filter smoothing method. The results of this study indicate that NIR diffuse transmittance spectroscopy can be used to predict the FM of watermelon. The Vis/NIR diffuse transmittance technique will be valuable for the nandestructive detection large shape and thick peel fruits’.
2007 Vol. 27 (06): 1113-1117 [Abstract] ( 1735 ) PDF (686 KB)  ( 515 )
1118 Influence of Optical Path Length on NIR Analysis Results for Trace Metal Determination in Chinese Rice Wine
YU Hai-yan,YING Yi-bin*,XIE Li-juan,FU Xia-ping
The prediction performance of near infrared (NIR) spectra with different optical path-length for trace metal (potassium, calcium, magnesium, zincum, and iron) determination was investigated. NIR transmission spectra of Chinese rice wine were collected in rectangular quartz cuvette with different optical path lengths (1,2, 5 and 10 mm) using Fourier transform near infrared (FT-NIR) spectrometer in the wavelength range of 800-2 500 nm with air as the reference. The reference data for potassium, calcium, magnesium, zincum, and iron were determined by atomic absorption spectroscopy (AAS). Calibration models were developed by partial least squares (PLS) regression. The PLS models of NIR spectra group with 5 mm path length gave the best calibration result. The determination coefficients (r2) for potassium, calcium, magnesium, zincum, and iron were 0.93, 0.85, 0.93, 0.72, and 0.66, respectively, and the root mean square error of cross validation (RMSECV) for the five elements were 26.5, 35.6, 4.63, 0.26, and 0.64 mg·L-1,respectively, whereas the models established by NIR spectra group of 10 mm path-length was the worst. And the r2 values for potassium, calcium, magnesium, zincum, and iron were 0.61, 0.65, 0.63, 0.09, and 0.25, respectively. The results indicated that the optical path length has an influence on the NIR analysis results for trace metal determination in Chinese rice wine, and that the appropriate path length for the NIR analysis should be determined by comparison analysis.
2007 Vol. 27 (06): 1118-1120 [Abstract] ( 1157 ) PDF (480 KB)  ( 437 )
1121 Determination of Citric Acid Mono Polyethyleneoxide Nonyl Phenyl Ether Amber Diehylene Glycoldinitrate Diglycollic Amide by IR
WANG Wen-bo1,SHEN Shu-chang1,ZHANG Li-yuan2,AN Hong1
In the present paper, citric acid, acetic anhydride, polyethyleneoxide nonyl phenyl ether and diethanolamine were used as raw materials. The raw materials were purified, and the intermediate products were synthesized. Finally, the citric acid mono polyethyleneoxide nonyl phenyl ether amber diehylene glycol dinitrate diglycollic amide was made. The acidamide of the product synthesized was determined by IR. There is a characteristic peak of CO in acidamide at 1 642.39 cm-1. Using potassium rhodanate as a internal standard, and according to Lambert-Beer law, a method to determine the citric acid mono polyethyleneoxide nonyl phenyl ether amber diehylene glycol dinitrate diglycollic amide was developed. The linear regression equation is A=0.007 6m+0.325 6 with a correlation coefficient (r2) of 0.998 9. The experimental results of the precisions and recoveries are satisfied. The method is very necessary for confirming the reaction extent and controlling quality of citric acid mono polyethyleneoxide nonyl phenyl ether amber diehylene glycol dinitrate diglycollic amide. So, the synthesis process conditions were right according to the IR data.
2007 Vol. 27 (06): 1121-1123 [Abstract] ( 214 ) PDF (459 KB)  ( 428 )
1124 Application of Pyroelectric Infrared Sensor to Radio Control Alarm System
WANG Song-de,LIANG Hui-qin,ZHANG Xu-xin,ZHU Xiao-long
A radio control alarm system was developed, which is composed of a pyroelectric infrared detecting module, a radio receiving/transmitting module, a digital encoding/decoding IC, and a voice recoding/playing module. When somebody enters the surveillance area, the infrared sensor will receive and transform the radiant energy into electric signal, which is amplified by internal circuits, and then generates a control signal to start transmitting system. As the encoded pulse is modulated by the transmitting module, a radio control signal will be spread to space; When received, the signal will be demodulated, amplified, shaped and decoded to trigger the recoding/playing circuits, which play the recoded voice to awake watch people. The system mainly adopts the RDP-18 pyroelectric infrared detecting module, which has full function from signal receiving to output control. The whole device is a module configuration. It has the advantage of frequency stable, work reliable, no debugging, and a remote control distance of 1 000 m, and is suitable for use in many kinds of demands.
2007 Vol. 27 (06): 1124-1126 [Abstract] ( 1618 ) PDF (417 KB)  ( 469 )
1127 Double-Layer Partial Least Squares Method and Its Application to NIR Spectroscopic Quantitative Analysis
CHENG Zhong
Aiming at the near infrared spectroscopy (NIR) with local effect sensitivity, numerous predictor variables with serious multicollinearity and having nonlinear quantitative relationship with the chemical compositions from the spectral data, a double-layer partial least squares (DNPLS) algorithm was constructed based on the error feedback-weighting correction. The model based on this proposed algorithm was divided into two parts: the outer part that embedded the nonlinear mapping between each pair of partial least square components into the regression framework of the partial least squares(PLS)method and the inner part that estimated the increment of weight vector by linear PLS method. Subsequently, to increase PLS components interpretative capability，the error-based weights updating procedure in the PLS input outer model was deduced and implemented in the DNPLS regression framework, Finally, the application to the corn sample water content modeling of the proposed DNPLS method was presented with a comparison to some other methods. The DNPLS method not only held a fine learning ability but also improved the prediction performance and steady capability.
2007 Vol. 27 (06): 1127-1130 [Abstract] ( 2366 ) PDF (1037 KB)  ( 491 )
1131 Application of Near Infrared Spectroscopy Technique to Nondestructive Measurement of Vegetable Quality
XIE Li-juan,YING Yi-bin*,YU Hai-yan,FU Xia-ping
Nondestructive detection techniques of vegetable include electrical properties, optical reflectance and transmission, sonic vibration, nuclear magnetic resonance (NMR), machine vision, aromatic volatile emission, vibration characteristics and others. The most widely employed and successful technique is to use its optical property. Near infrared spectroscopy technique is extremely fast, highly efficient, cheap to implement, of good recurrence and no sample preparation, and is a rapid and non-destructive modern measuring technique that has been widely used in many fields. In the present paper, the application of near infrared spectroscopy technique to nondestructive measurement of vegetable quality was briefly introduced. Some considerable aspects existing in the application were also discussed, and it is pointed out that because of vegetable’s diversity and rot-proneness, automation analysis machine should be developed to improve the speed of quality detection, and cooperating with several other nondestructive techniques, such as NMR and machine vision, is the research trend.
2007 Vol. 27 (06): 1131-1135 [Abstract] ( 657 ) PDF (1066 KB)  ( 543 )
1136 Surface-Enhanced Raman Spectroscopic Studies on the Thiophenol Adsorbed on Novel Ag-Au Alloy Nanoparticles
WANG Mei,YAO Jian-lin,GU Ren-ao*
Ag-Au alloy seeds were prepared by the simultaneous reduction of Ag and Au salts. The seeds were grown via NH2OH·HCl-growth method to obtain novel Ag-Au alloy nanoparticles with diameters of 40-60 nm. The nanoseeds and novel nanoparticles were characterized by UV-Vis spectroscopy and TEM respectively. The observation of one surface plasma resonance absorption band, the redshift in their frequencies, and the uniform color of the nanoparticles shown in TEM images indicated the formation of alloy structure for both the nanoseeds and the novel nanoparticles. By using thiophenol(TP) as probe molecules, SERS studies were performed on the novel nanoparticles. The absorption bands of the nanoparticles red shifted with the addition of TP, and new bands were detected in the near infrared region, which were attributed to the aggregation of TP covered nanoparticles. With the excitation line of 632.8 nm, the SERS intensity of TP on Au was most largely enhanced, and that on alloy nanoparticles were increased as xAu increased.
2007 Vol. 27 (06): 1136-1139 [Abstract] ( 1613 ) PDF (895 KB)  ( 477 )
1140 Surface-Enhanced Raman Spectra of Oxidation Damnification of Fetal Bovine Serum by Ozone
ZOU Zu-quan1,3,LIU Yan-nan2，3,WU Ying5,LI Qi-nan2,3,CHEN Mei-zong1,3,SUN Hai-ying1,3,Lee Imshik1,3,4
Fetal bovine serum was treated by ozone for 1 hour and 3 hours before getting its surface-enhanced Raman spectra from 200 to 1 800 cm-1. Treated with ozone for 1 hour, it shows a significant decrease in band intensity. Treated with ozone for 3 hours, the band intensity has a further decrease but not so obviously, which means that oxidation of ozone is short lived. Treated with ozone, the orderly conformations of main chains in protein such as α-helix, β-sheet and β-corner are damaged seriously. Aromatic side chains and C─S of Cys and Met also are damnified greatly. All this means that strong oxidation of ozone results in denaturation, conformational changes and even degradation in protein.
2007 Vol. 27 (06): 1140-1142 [Abstract] ( 1630 ) PDF (673 KB)  ( 493 )
1143 Ab Initio Calculation of Hyperfine Structure and Raman Spectra of Binary Alkali Metal Silicates
ZENG Hao,YOU Jing-lin*,CHEN Hui,JIANG Guo-chang
Ab initio calculation method of quantum chemistry was used to optimize several typical binary alkali metals silicates model clusters under restricted Hartree-Fock method with 6-31G(d) basis sets. The symmetric stretching vibrational frequency of non-bridging oxygen in the high frequency range, its Raman optical activity (ROA) and the influence of different cations of those model clusters were also calculated and evaluated with the concept of hyperfine micro-structure. It was shown that the symmetric stretching vibrational frequency of non-bridging oxygen in the high frequency range is related closely to the environmental hyperfine micro-structure，and ROA enhancement of Q3 species occurs as Q4 species is its nearest neighbor. It can be inferred that the Raman scattering properties of silicates might be predominantly determined by hyperfine micro-structure instead of crude SiO4 tetrahedron as primary micro-structure. It was found that large cation can enhance ROA of the symmetric stretching vibration of non-bridging oxygen by charge transfer mechanism, while ROA weakening effect can be expected on small model clusters due to the excessive charge transfer.
2007 Vol. 27 (06): 1143-1147 [Abstract] ( 2311 ) PDF (1147 KB)  ( 422 )
1148 Analysis of Different Methods for Denoising of High Temperature Raman Spectra
CHEN Hui,JIANG Guo-chang,YOU Jing-lin*,WU Yong-quan
Combined with time accumulated resolution and space resolution the SU-HTRS(T/S) set has been realized at Shanghai University. It is impossible to avoid noise at high temperature, so different mathematic methods, such as Savitzky-Golay method, FFT and wavelet methods have been adopted for denoising. For various noise levels, the effects of three methods on the peak location, intensity and covering area as well as the smoothing degree of the reduced spectra were analyzed. It can be concluded that Savitzky-Golay method is simple and quick, while wavelet method offers the best results in denoising process.
2007 Vol. 27 (06): 1148-1151 [Abstract] ( 608 ) PDF (671 KB)  ( 544 )
1152 Spectroscopy and XPS Studies on Molecular Recognition of a Molecularly Imprinted Cotinine-Specific Polymer
YANG Jun1,2,ZHU Xiao-lan1,2,SU Qing-de1,2*,CAI Ji-bao1,2,HU Yan1,GAO Yun2
In the present study, molecular imprinting technique was used to develop a method based on noncovalent interaction for the systhesis of a cotinine-specific polymer. The molecular recognition characteristics of the template polymer were evaluated by UV, IR, XPS and 1H NMR. The results indicated that the interactions should be cooperative hydrogen bonds produced by self-assembling of the template and the monomer. The stoichiometric mole ratio of COT-MAA complex is 1∶2. Furthermore, nitrogen atom of the pyridine ring and oxygen atom of the lactam group in cotinine molecular are hydrogen-bond acceptors, being the predominant binding sites interacting with the functional monomer.
2007 Vol. 27 (06): 1152-1155 [Abstract] ( 1948 ) PDF (1217 KB)  ( 443 )
1156 Investigation on the Fluorescence Spectroscopy of Normal and Malignant Rectum Tissues
MENG Tao1,XU Duan-fu1,XU Yi-zhuang2,ZHAO Ying1,WANG Du-jin1,WU Jin-guang2*
In the present article the fluorescence characteristics of normal and malignant rectum organ tissues of 12 samples were investigated in vitro using UV (200-400 nm) fluorescence spectroscopy and compared with the results of the infrared spectra of normal and malignant rectum organ tissues. The results showed that the fluorescence intensity of normal rectal tissue was higher than that of rectal malignant tissue. The difference in fluorescence intensity at 492 and 544 nm between normal rectal tissue and malignant tissue may be considered as a detection criterion.
2007 Vol. 27 (06): 1156-1160 [Abstract] ( 612 ) PDF (1240 KB)  ( 436 )
1161 Fluorescence Properties of C60-Glucocorticoids
LIU Rui-li,YIN Juan-juan,MA Ji-fei,LI Qing-nuan,LI Wen-xin*
C60 and its derivatives have become a research hotspot because of their unique structures, physical and chemical properties. The fluorescence properties of C60 and its derivatives are an important research embranchment of the fullerene science field. In the present paper the fluorescence properties of C60-glucocorticoids were firstly investigated. When excited with the wavelength of 350 nm at room temperature, C60-glucocorticoids displayed the fluorescence emission in chloroform at 447 nm. The sixty carbon atoms of C60 molecule are equivalent, belonging to the Ih group, and presenting high symmetry. It is difficult to observe the fluorescence of C60 under the same condition because of the high symmetry of C60 molecule. The fluorescence emission of C60-glucocorticoids is probably due to the decrease in the high symmetry of C60 molecule. Moreover, the fluorescence emission at 447 nm of a series of concentrations (10-13 μmol·L-1) of C60-glucocorticoids chloroform solutions excited at 350 nm was determined, and the result indicated that the C60-glucocorticoids in chloroform could quench itself′s fluorescence intensity. Within the concentration range of 10-64 μmol·L-1,the fluorescence intensity increased along with the accretion of the concentration. When the concentration of C60-glucocorticoids was greater than 64 μmol·L-1 the fluorescence intensity decreased gradually.
2007 Vol. 27 (06): 1161-1163 [Abstract] ( 2356 ) PDF (769 KB)  ( 377 )
1164 Preparation of Lomefloxacin-Tb3+ Nanoparticles Modified by PVP via Microwave-Assistance and Its Properties of Fluorescence
HE Hua1,2,YE Hai-ying1,LIU Xuhui3
Polyvinylpyrrolidone(PVP)-modified LFLX-Tb3+ nanoparticles were prepared by microwave radiation method. The obtained products were characterized by means of SEM, FTIR and fluorescence spectra. The surface-modified LFLX-Tb3+ nanoparticles showed a narrow size distribution and enhanced luminescence property compared with that of the unmodified ones. These results were attibuted to the surface passivation of the LFLX-Tb3+ nanoparticles by the PVP molecules. It is confirmed that the addition dosage of PVP is an important factor in the preparation of the LFLX-Tb3+ nanoparticles. The reasons for luminescence enhancement were discussed.
2007 Vol. 27 (06): 1164-1167 [Abstract] ( 418 ) PDF (1142 KB)  ( 412 )
1168 Study on the Interaction of Hemoglobin and Cu(Ⅱ)-ARS Complex
WU Xiao-hua,MIAO Ji-gen,MIAO Yu-qing,CHEN Jian-rong
The reaction of hemoglobin (Hb) with copper(Ⅱ)-Alizarin red S (ARS) complex was studied in H3PO4-KH2PO4 buffer solution (pH 4.2) by ultraviolet-visible spectrophotometry. The results show that the interaction of Hb and Cu(Ⅱ)-ARS complex produces red ionic association complex with its maximum absorption peak at 537 nm. At the maximum absorption, the composition of the complex was determined to be nHb∶nCu(Ⅱ)∶nARS=1∶4∶8, and the apparent molar absorptivity was 1.52×105 L·mol-1·cm-1. The concentration of Hb is linear with the absorbency in the range of 1.0×10-7-2.0×10-6 mol·L-1 and the regression equation was established as A=0.026 9+151 675ｃ(mol·L-1) with the coefficient r=0.997 2. The effects of solution acidity, reagent amount, reaction time, temperature, ionic strength and the added surfactant were examined on the formation of the Hb-Cu(Ⅱ)-ARS complex. A preliminary investigation was carried out to elucidate the reaction mechanism, and it could be concluded that the Hb and Cu(Ⅱ)-ARS complex are combined mainly by electrostatic attraction. Further investigation was also undertaken to find out the effects of common amino acids and metallic ions on the formation of Hb-Cu(Ⅱ)-ARS complex.
2007 Vol. 27 (06): 1168-1171 [Abstract] ( 2500 ) PDF (772 KB)  ( 409 )
1172 Studies on the Anion Recognition of N-Aryl-N′-(4-Ethyloxybenzoyl) Thioureas Derivatives by Spectroscopy
HU Jing-han1,XU Wei-xia2,WEI Tai-bao2
The interactions of N-aryl-N′-(4-ethyloxybenzoyl) thioureas derivatives and anions such as F-,Cl-,Br-,I-,CH3COO-,H2PO-4,HSO-4 and NO-3 in DMSO were investigated by UV-Vis and 1H NMR spectroscopy. The results showed that hydrogen-bonding complexes were formed between receptors and the three anions such as F-,CH3COO- and H2PO-4,and the solutions turned light yellow from colorlessness, but there had no evident binding with Cl-,Br-,I-,HSO-4 and NO-3. It was regular that the two receptors had different binding ability with F-,CH3COO- and H2PO-4. For the same anion, the association constants followed the trend: receptor 1a> receptor 1b. The UV-Vis data indicated that a 1∶1 stoichiometry complex was formed.
2007 Vol. 27 (06): 1172-1175 [Abstract] ( 1608 ) PDF (569 KB)  ( 450 )
1176 Synthesis and Study on the Interaction of Rare Earth Complexes of N′,N-Bis(2-Pyridinecarboxamide)-1,2-Ethane with DNA
LU Xiao-hong1,LIN Qiu-yue1,2*,HU Rui-ding1,2,LIU Wei-dong1,2,FENG Jie1
Four rare earth complexes of N′,N-bis(2-pyridinecarboxamide)-1,2-ethane were synthesized and characterized by elemental analysis, conductivity measurement, thermal studies, IR and electronic spectra. The composition of the four complexes is [Ln(H2L)(NO3)2](NO3)·3H2O (Ln=Sm, Eu, Gd, Tb). Results of spectral measurements indicate that the oxygen of carbonyl and the nitrogen of pyridyl coordinate with Ln(Ⅲ) respectively, and the NO-3 shows bidentate coordination. So the four complexes are 1∶1 chelated complexes. The interaction between [Sm(H2L)(NO3)2](NO3)·3H2O and DNA was studied by employing UV-Visible (UV-Vis) spectra, fluorescence spectra and SERS spectra. Experimental results show that with the incremental addition of DNA, the bands at 265 nm show hypochromism accompanied by a small red shift and the binding constant Kb obtained is 1.24×105. Meanwhile fluorescence spectra show that the addition of [Sm(H2L)(NO3)2](NO3)·3H2O to DNA pretreated with EB causes an appreciable reduction in fluorescence intensity，indicating that the complex competes with ethidium bromide in binding to DNA, and free ethidium bromide increases. The addition of DNA causes the SERS signals of the complex to weaken and the band at 1 282 cm-1 to disappear, which suggests that the planar pyridine molecule of the ligand may partly be inserted into the double-stranded helix plane in DNA, making π electronic density of aromatic rings in complex change. The above phenomena indicate that [Sm(H2L)(NO3)2](NO3)·3H2O interacts intensively with DNA.
2007 Vol. 27 (06): 1176-1180 [Abstract] ( 897 ) PDF (939 KB)  ( 436 )
1181 Studies on the Interaction between RNA with Neutral Red and Determination of RNA by Spectrophotometry
SI Wen-hui
An analytical method for the determination of ribonucleic acid by spectrophotometry was established. At the maximum absorption wavelength for neutral red in B-R buffer solution, and under the best conditions, the decrease in the absorbance was linear with the amount of ribonucleic acid. The linearity range was 0.0-9.0 μg·mL-1,the detection limit was 0.52 μg·mL-1,and the correlation coeffient was 0.999 8. This method was simple, rapid, and selective. So its application to the determination of ribonucleic acid was satisfactory. The reaction mechanism was that the electrostatic interaction leads to molecular association of RNA with neutral red, resulting in anti-ion permutation and bonding reaction.
2007 Vol. 27 (06): 1181-1184 [Abstract] ( 2051 ) PDF (806 KB)  ( 427 )
1185 Preparation and Spectral Analysis of Coordination Compounds of Chitosan with Ce(Ⅲ)，Zr(Ⅳ)，Pb(Ⅱ) and Cd(Ⅱ)
DING Chun-mei,YUE Wen-jin,SU Yun,LI Guo-yan,GUO Li,CHEN Liang
Coordination compounds of chistosan (CTS) with Ce(Ⅲ), Zr(Ⅳ)，Pb(Ⅱ) and Cd(Ⅱ) (M-CTS) were prepared, which were synthesized by the reaction of CTS with cerium nitrate, zirconium nitrate, cadmium sulfate, and lead nitrate in acid systems. The coordination compounds were characterized by infrared spectrum (IR), X-ray diffraction spectrum (XRD) and X-ray photoelectron spectrum (XPS). The results showed that the N atom in amidogen of CTS coordinates with Cd in the coordination compounds of Cd-CTS, while in the coordination compounds of Ce-CTS, Zr-CTS and Pb-CTS, the N atom in amidogen and O atom in hydroxyl of CTS participate in the coordination reaction. It is suggested that the coordination bonds are different with the change of heavy metal ions.
2007 Vol. 27 (06): 1185-1187 [Abstract] ( 2614 ) PDF (555 KB)  ( 494 )
1188 Simultaneous Determination of Iron, Copper and Cobalt in Food Samples by Diode Array Detection-Flow Injection Analysis Using Partial Least Squares Calibration Model
MI Jian-ping1,LI Yuan-qian1*,ZOU Xiao-li1,ZHENG Bo1,YANG Jing-guo2
A flow injection-CCD-diode array detection spectrophotometric method using partial least squares (PLS) algorithm for the simultaneous determination of iron, copper and cobalt in food samples has been established. The method was based on the chromogenic reaction between metallic ions and 5-Br-PADAP in the presence of acetic acid-acetic sodium buffer solution (pH 5) containing 30 g·L-1 ascorbic acid and 2%(φ) Triton X-100. The overlapped spectra of these complexes were collected by CCD diode array detector and the multi-wavelength absorbance data were processed using partial least squares algorithm. The reaction conditions and analytical parameters of FIA were investigated. The food samples can be analyzed without any separation after digestion，and the sampling rate was 45·h-1. The linear ranges of Fe2+,Cu+ and Co2+ were 0.2-10.0 μg·mL-1,0.1-5.0 μg·mL-1,and 0.01-1.0 μg·mL-1 and the detection limits were 0.2, 0.1 and 0.01 μg·mL-1,respectively. The average recoveries of spiked samples were 89.4%-110.8% for the three elements. The relative standard deviation (RSD) of samples was in the range of 1.1%-12.1%. Comparing the proposed method with ICP-AES, the relative error was below 12.1%. Above all, this method is simple, quick, sensitive, selective, and easy to be apply and generalize.
2007 Vol. 27 (06): 1188-1191 [Abstract] ( 591 ) PDF (742 KB)  ( 472 )
1192 Determination of Trace Impurities in High Purity Titanium Dioxide by High Resolution Inductively Coupled Plasma Mass Spectrometry
HE Xiao-mei1,XIE Hua-lin1,NIE Xi-du1,TANG You-gen2
An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for the rapid simultaneous determination of twenty six elements (Be, Na, Mg, Al, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, As, Mo, Cd, Sn, Sb, Ba, Ce, Nd, Sm, Pt, Pb and Bi) in high purity titanium dioxide was described. Samples were decomposed by (NH4)2SO4 and H2SO4. Most of the spectral interferences could be avoided by measuring in the high-resolution mode. The matrix effects due to the presence of excess sulfuric acid and Ti were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits are 0.004-0.63 μg·g-1,the recovery ratio is 87.6%-106.4%, and the RSD is less than 3.5%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity titanium dioxide with satisfactory results.
2007 Vol. 27 (06): 1192-1196 [Abstract] ( 1758 ) PDF (928 KB)  ( 438 )
1197 Determination of Trace Heavy Metal Elements in Cortex Phellodendri Chinensis by ICP-MS after Microwave-Assisted Digestion
KOU Xing-ming1,XU Min2,GU Yong-zuo1
An inductively coupled plasma mass spectrometry (ICP-MS) for determination of the contents of 8 trace heavy metal elements in cortex phellodendri chinensis after microwave-assisted digestion of the sample has been developed. The accuracy of the method was evaluated by the analysis of corresponding trace heavy metal elements in standard reference materials (GBW 07604 and GBW 07605). By applying the proposed method, the contents of 8 trace heavy metal elements in cortex phellodendri chinensis cultivated in different areas (in Bazhong, Yibin and Yingjing, respectively) of Sichuan and different growth period (6, 8 and 10 years of samples from Yingjing) were determined. The relative standard deviation (RSD) is in the range of 3.2％-17.8％ and the recoveries of standard addition are in the range of 70％-120％. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of 8 trace heavy metal elements in cortex phellodendri chinensis. The results also show that the concentrations of 4 harmful trace heavy metal elements As, Cd, Hg and Pb in cortex phellodendri chinensis are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation. Therefore, the cortex phellodendri chinensis is fit for use as medicine and export.
2007 Vol. 27 (06): 1197-1200 [Abstract] ( 2305 ) PDF (429 KB)  ( 458 )
1201 Application of ICP-MS to Detection of Heavy Metals in Soil from Different Cropping Systems
RUI Yu-kui,KONG Xiang-bin*,QIN Jing
With the rapid development of the society，more and more attention has been paid to the influence of human activity on environment and food pollution. Soils of different cropping systems, sampled from Daxing district of Beijing, were analyzed in terms of the contents of heavy metals (Ti, Cr, Mn, Ni, Cu, Zn, As, Cd and Pb) by the method of ICP-MS to determine the influence of cropping system on environment. The results showed that the contents of nine heavy metals in soils from the cropping systems (fruits and maize/wheat) were several times higher than those from vegetable system. Contents of Cr, Mn, Ni, Cu, Zn, As and Cd were the highest in soils from fruit system, while Ti and Pb the highest in soils from maize/wheat system. The causes of the above differences could be the different harvest organs for different crops.
2007 Vol. 27 (06): 1201-1203 [Abstract] ( 652 ) PDF (293 KB)  ( 513 )
1204 Study on the Determinations of Ni, Fe, Mo, Mn and B in Ti/TiC Composite Material by Atomic Emission Spectrometry
LI Hui-zhi,ZHAI Dian-tang,XU Chong-juan,PEI Mei-shan
The present paper describes the determination of trace Ni, Fe, Mo , Mn and B in Ti/TiC composite material using carbon powder, calcium carbonate, cupric oxide and beryllium oxide as buffer by atomic emission spectrometry(ASE). Be 298.61 nm was selected as internal standard line. Sample separation and chemistry treatment were not requirel. The sample was directly loaded into ordinary electrode. The method is simple, rapid and accurate. The requirement of determination, and factors of influence were studied. A new method has developed for the determination of Ni, Fe, Mo, Mn and B. The analysis lines of Ni, Fe, Mo, Mn and B are 300.36, 248.33, 315.82, 260.57 and 249.68 nm respectively. The internal standard line of Be is 298.61 nm. The linear ranges of the determination of Ni, Fe, Mo, Mn and B are 0.003%-0.30%, 0.001%-0.20%, 0.003%-0.30%, 0.001%-0.20%, 0.001%-0.20% respectively. The detection limits of Ni, Fe, Mo, Mn and B are 0.003%;0.001%, 0.003%, 0.001% and 0.001% respectively. The ranges of the recovery of Ni, Fe, Mo, Mn and B are 95.80%-104.8%, and the standard relative deviations(RSD) are less than 5.0%(n=9). The method has been applied to the determination of Ni, Fe, Mo , Mn and B with satisfactory results.
2007 Vol. 27 (06): 1204-1206 [Abstract] ( 1699 ) PDF (509 KB)  ( 469 )
1207 Study on Phase Distribution and Release of Heavy Metal in Pyrite Using Sequential Extraction Procedure and ICP-MS
ZHANG Ping1,2,QI Jian-ying1,2,YANG Chun-xia1,CHEN Yong-heng1*
Heavy metal elements of V, Cr, Mn, Co, Ni, Cu, Zn, Sr, Mo, Cd, Sb, Ba and Pb were determined by ICP-MS. The linear ranges of determination for these elements were obtained, and the correlation coefficients were larger than 0.997. The detection limit ranges were from 0.005 to 0.01 μg·L-1 and the RSDs were lower than 5%. Phase distributions of heavy metals in pyrite were analyzed by ICP-MS with sequential extraction procedure. The result showed that Pb was the main heavy metal in pyrite and its total content was 830 mg·kg-1. Pb existed mostly in carbonate or galena (PbS) phase of pyrite and the proportion was 56.9%. Pb existed less in iron oxides with 29.7% in proportion, and least in sulfide and silicate with 3.5% and 9.9%, respectively. The release of Pb in pyrite was primary in natural environment, but the release of Cr and Cd was not be ignorable, too.
2007 Vol. 27 (06): 1207-1209 [Abstract] ( 1762 ) PDF (351 KB)  ( 463 )
1210 Determination of 27 Elements in Tobacco by ICP-MS Using Microwave Digestion for Sample Preparation
HU Qing-yuan1,2,LI Li3,SHI Jie4,CHEN Zai-gen2,WANG Fang2, WANG An1
While the organic and biologically active components in tobacco smoke are well characterized, it is also important to know which inorganic elements are contained in tobacco. In the present paper, the determination of Be, Na, Mg, K, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Ag, Cd, Sn, Cs, Ba, Hg, Tl, Pb, Th and U in tobacco leaves was studied by inductively coupled plasma mass spectrometry. Samples were digested in a mixture of nitric acid and hydrogen peroxide by closed-vessel microwave digestion. The instrumental operating conditions were optimized for the measurement of above 17 elements. Ge, In and Bi were used as internal standard elements to compensate matrix effect and signal drift. The precision of measurement ranges from 1.28% to 9.18% in terms of relative standard deviation. The recoveries for spiking tobacco samples and the limits of detection are in the range of 93.64%-108.9% and 0.356 3 ng·L-1-1.725 μg·L-1,respectively. The results of experiment show that the method can meet the requirements of trace analysis.
2007 Vol. 27 (06): 1210-1213 [Abstract] ( 1961 ) PDF (456 KB)  ( 498 )
1214 Determination of Harmful Elements in Various Fish Tissues by ICP-AES
HE Jin-zhe1,LIU Wen-han2,YANG Kai1,WU Hao1
Twelve kinds of fish tissues were wetly decomposed and the harmful elements of Cd, As, Pb and Hg were determined by ICP-AES method in the present paper. The techniques for operating ICP instrument were optimized, spectral interference for elements in special wavelength range was studied, and the correction factor of IECs model was established. The results indicated that the signal to noise ratio and detection limit for elements with higher ionization potential energy may be improved by increasing the radio generator power properly and reducing the nebulizer pressure. There were Cr, Cu, As, Sn and Na elements that mainly disturbed the determined elements such as As(189.042 nm), Pb(220.353 nm), Cd(228.802 nm ) and Hg(184.950 nm). The primary contaminating elements in tissues of freshwater fish and seawater fish were Pb and As respectively.
2007 Vol. 27 (06): 1214-1217 [Abstract] ( 1135 ) PDF (1242 KB)  ( 451 )
1218 Determination of Trace Elements in Radix Ophiopogonis by HG-ICP-AES
LOU Qi-zheng1,XU Run-sheng2
In this paper, a method of microwave digestion technique for the contents determination of trace elements Ni，Zn，Mn，Cu，Mg，Fe，Ca and Pb in radix ophiopogonis by hydride generation inductively coupled plasma atomic emition spectrometry (HG-ICP-AES) was reported. Its recovery ratio obtained by standard addition method ranged between 97.8% and 102.5%, and its RSD was lower than 4.0%. The results of the determination show that radix ophiopogonis is rich in the inorganic elements such as Fe, and the content of Zn in radix ophiopogonis of Zhejiang is much higher in radix ophiopogonis of Sichun. The result will provide scientific data for the study on the elements in radix ophiopogonis and on their relativity of medicine efficacy.
2007 Vol. 27 (06): 1218-1221 [Abstract] ( 1808 ) PDF (656 KB)  ( 475 )
1222 Study on Determination of Metal Elements in Honeysuckle by Carbon Pick-Up Acid Dissolvation Digestion with ICP-AES
ZHANG Sheng-bang1,LI Jin-yan2,GUO Yu-sheng1
Honeysuckle is a lonicera plant, commonly used traditional precious raw material for medicine in China, and is a commonly used Chinese native medicine and an important material for cold drink. Honeysuckle has the effect of alleviating fever and disintoxicating, and is used mainly to treat the carbuncular swelling, and cure boils, throat rheumatism, erysipelas, painfully hot sun blood dysentery, cold, and various diseases accompanied by fever. The simultaneous determination of multi-metal elements in honeysuckle was studied by inductively coupled plasma atomic emission spectrum (ICP-AES) after carbon pick-up acid dissolvation digestion. The average recovery of the method for Cu, Mn, Ni, Pb, Fe, Cr, Ca and Mg in honeysuckle was found to be 83.8%-115.6%, while RSD (n=10) is 1.1%-4.9% for the multi-elements in honeysuckle. The method was applied to the analysis of some practical samples and the results obtained were satisfactory. Fe and Mn are rather rich in honeysuckle. It is of important significance to assess the value of the food cooked with medicinal herbs by the determination of multi-trace elements.
2007 Vol. 27 (06): 1222-1224 [Abstract] ( 2129 ) PDF (309 KB)  ( 418 )
1225 Filter Coated with Phenyl Fluorone for Enrichment and Determination of Indium by GFAAS
LI Xing-yang,WEI Xiao-ling,GONG Qi*
The filter fiber column coated with phenyl fluorone was extended to pre-concentrate trace amount of indium determined by GFAAS. The optimized condition for filter fiber coated with phenyl fluorone was obtained. The enrichment condition was achieved when the pregnant solution at pH 5 flowed through the filter fiber column at the rate of less than 2.0 mL·min-1,then 8mL HNO3 of 5.00 mol·L-1 was used as an eluent. With a general graphite tube coated with tungsten and silver as matrix modifier, the sensitivity was enhanced with GFAAS. The method was validated by the determination of trace indium in water, artificial zinc, and aluminium samples. The detection limit of the method was 0.32 ng·mL-1,the recovery was in the range of 95.0%-101%, and the RSD was between 1.8% and 7.0％.
2007 Vol. 27 (06): 1225-1228 [Abstract] ( 1555 ) PDF (546 KB)  ( 414 )
1229 Determination of Inorganic Elements in Different Parts of Sonchus Oleraceus L by Flame Atomic Absorption Spectrometry
WANG Nai-xing,CUI Xue-gui,DU Ai-qin,MAO Hong-zhi
Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (μg·g-1) for the 13 kinds of metal elements is as follows: leaf (77 213.72)＞flower (47 927.15)＞stem(42 280.99)＞root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.
2007 Vol. 27 (06): 1229-1230 [Abstract] ( 1665 ) PDF (293 KB)  ( 491 )
1231 Study on Different Digestion Methods for Determination of Twelve Metal Elements in the Plant Platycodon Grandiflorum (Jacq.) A. DC.by FAAS
XUE Guo-qing1,HAN Yu-qi1,SONG Hai1,DI Duo-long2
In the present paper the effects of different digestion methods on determining the amount of metal elements in the plant platycodon grandiflorum (Jacq.) A. DC. by flame atomic absorption spectrophotometry(FAAS) are reported. FAAS method was established for the determination of K, Mg, Ca, Cu, Zn, Mn, Fe, Co, Ni, Cd and Cr and Pb in the plant platycodon grandiflorum (Jacq.) A. DC. The samples were incinerated and followed by digestion with HNO3-HClO4(φ,4∶1) at 90-95 ℃ and normal pressure. In the meantime, the optimum parameters of FAAS and effects of solution medium on the results were discussed. The analytical results of K, Mg, Ca, Mn, Fe, Cu and Zn were 13 226.32, 922.57, 1 710.72, 9.23, 336.66, 8.75 and 19.62 μg·g-1 respectively, while Co, Ni, Cd, Cr and Pb were not checked out in the samples. The results showed that the recovery of standard addition was 95.45%～105.50% and the relative standard deviation (n=9) was 0.34%～5.78%. The method is quick, simple and convenient, and the results are satisfactory.
2007 Vol. 27 (06): 1231-1234 [Abstract] ( 496 ) PDF (480 KB)  ( 474 )
1235 Determination of the Amount of 13 Metal Elements in the Rape Pollen from Different Regions by Flame Atomic Absorption Spectrophotometry
CHANG Yan-hong1,2,XUE Guo-qing1*,SONG Hai1,DI Duo-long3
The objective of the present paper was to determine the amount of metal elements in the rape pollen from different regions by flame atomic absorption spectrophotometry (FAAS). FAAS method was established for the determination of K, Na, Ca, Mg, Fe, Co, Ni, Cu, Zn, Mn, Cd, Cr and Pb in the rape pollen. The samples were incinerated and then digested with HNO3-HClO4(V∶V=4∶1) at 90-95 ℃ and under normal pressure. In the meantime, the optimum parameters of FAAS and the effects of solution medium on the results were studied. The analytical results of K, Na, Ca, Mg, Fe, Cu, Zn and Mn rape pollen from different habitats respectively were 4 248.00, 75.77, 312.10, 856.61, 599.53, 8.78, 27.82, 22.54 μg·g-1 and 7 585.75, 242.56, 287.88, 699.43, 1 020.65, 10.25, 40.44, 30.97 μg·g-1,while Co, Ni, Cd, Cr and Pb were not checked out in the samples. The results showed that the recovery of standard addition was 95.22%-105.49%, and the RSD(n=9) was 0.30%-5.00%. The characteristic method is quick, simple and convenient, and the results are satisfactory.
2007 Vol. 27 (06): 1235-1238 [Abstract] ( 1186 ) PDF (438 KB)  ( 457 )
1239 Spectral Measurement System and Laser Therapy Experiments for Port Wine Stains
ZHAO You-quan1,WANG Ya-li1,FAN Shi-fu1,ZHANG Li2,GU Ying2
To measure and analyze the spectrum of a small skin region for laser therapy of port wine stain is very useful for clinical doctor to understand the optical characters of patient’s pigmented skin, to adjust the output parameters of lasers and then to improve the therapy effects. Based on the analysis of the forming mechanism of port wine stains and clinical operation of the disease, the present paper presents an automatic spectral measurement and analysis system for port wine stain therapy. It can accomplish the spectral detection in the range from 380 to 780 nm, with a spectral resolution of 1 nm. Experiments were performed for patients with various age and pigment diseases; finally, some influencing factors and relevant solutions are enumerated and discussed.
2007 Vol. 27 (06): 1239-1242 [Abstract] ( 1851 ) PDF (918 KB)  ( 431 )
1243 Determination of Lead with GFAAS Using Online Flow Injection
CHEN Zhong-lan
A cheap, rapid and sensitive method for the determination of trace amount of lead in water samples by graphite furnace absorption spectrometry coupled with online flow injection preconcentration with ammonium pyrrolidine dithiocarboxylate chelating cellulose (CC-APDC) was developed. There were six steps in the preconcentration of flow injection: first, 0.15 mL nitric acid was used for a complete elution，which exceeded the volume of the graphite tube, so the 40 mL solution was removed before eluting. Secondly, 40 mL maximum concentration elution solution was added to GFAAS by fixed volume sampling to improve the accuracy. In addition, traditional stopping gas measurement was substituted with small flow gas atomization (30 mL·min-1,preconcention for 1 min) during the removal of high memory effect for ashing stage in graphite furnace, which develops tail-out phenomenon and makes blank value low and steady. Various parameters affecting the adsorption and elution, such as pH of the solution, eluent concentration, sample flow rate etc, were optimized. If miniflow in atomization step was used, the memory effect in the determination of lead by GFAAS could be removed. The CC-APDC was used for preparation and preconcentration. A good precision (RSD=1.4%, n=10), high enrichment factor (15) and sample throughput (50 h) with detection limit 0.12 μg·L-1 were obtained. This method has been successfully applied to the water sample for lead determination with a recovery of 95%-105%.
2007 Vol. 27 (06): 1243-1245 [Abstract] ( 535 ) PDF (550 KB)  ( 418 )

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