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2004 Vol. 24, No. 03
Published: 2004-03-26
 
       光谱学与光谱分析
257 Spectral Study of Three Compounds of Tungstosilicic Salt with Keggin Structure
CHEN Yi-ping1，ZHAO Shi-long1，ZHANG Han-hui1，2*，SUN Rui-qing1，YANG Qi-yu1
Three compounds of tungstosilicic acid and tungstosilicic salt: K3H[SiWⅥ12O40]·3H2O(Ⅰ), (H3O)4[H3SiWⅥ9WⅤ3O40]·2H2O(Ⅱ) and [(CH3)4N]4[SiWⅥ12O40]·4.5H2O(Ⅲ), with Keggin structure, have been synthesized. The relationship between their properties and structures was studied by using FTIR, NIR FT-Raman, UV-Vis and flurescence etc. They possess isolated [SiW12O40] cage anion, which combines with cation and water by static electric action and weak hydrogen bond; The study of their FTIR and Raman spectra shows that the vibrational frequencies of the group are related to the structure of the materials. For the compoundⅡ, the vibrational frequency of νas(WOd) decreases as part of W6+ are reduced to W5+, and the charges of anion group affect νas(W—Oc—W)，νas(Si—Oa) and δ(Oa—Si—Oa) etc. apparently. In UV-Vis spectra of compound Ⅰ and Ⅱ, there are two characteristic peaks at 200 and 260 nm，respectively. The fluorescence spectra of compound Ⅰ were studied, and showed that the emission peak is at 350, 440，520 and 675 nm excited by 220, 350 and 440 nm.
2004 Vol. 24 (03): 257-260 [Abstract] ( 1450 ) PDF (1103 KB)  ( 357 )
261 Spectral Studies on Nano-sized SO2-4/ TiO2 Photocatalyst Prepared by Hydrothermal Heating the Solution of Ti(SO4)2
YE Zhao, ZHANG Han-hui, PAN Hai-bo
In this paper, the nano-sized SO2-4/ TiO2 solid superacid photocatalysts have been prepared by the method of hydrothermal heating the mixed solution of Ti(SO4)2 and urea, heating-decomposing, wet impregnating-calcining. The middle products and the ultimate products have been characterized by XRD, BET, FTIR, DRS and FS. The degradation of rhodamine B by photocatalyst was regarded as a model reaction. The optimum condition of preparing SO2-4/ TiO2 photocatalysts has been chosen. The results show that hydrothermal treating the solution of Ti(SO4)2 can get the anatase nano-sized TiO2 in the weak alkalinity medium; at 300℃ by-products of hydrothermal reaction, such as (NH4)2SO4 and so on, can be decomposed by calcining for 4 hours, avoiding much loss of H2SO4; the most important factors that imfluence the photocatalystic activities of SO2-4/ TiO2 are the concentration of SO2-4 on TiO2 and the calcination time. SO2-4/ TiO2 photocatalysts have the best photocatalystic activities, up to the level of P-25 photocatalyst, when the concentration of SO2-4 on TiO2 is 11% and the calcination temperature is 450℃.
2004 Vol. 24 (03): 261-265 [Abstract] ( 1626 ) PDF (1063 KB)  ( 360 )
266 Nonlinear Optical Absorption Characteristics of a Novel Organic Material ZnTBP/CA/PhR
LI Lu-ying，ZHAO You-yuan，YU Shi-rui，ZHENG Rui-zhi
The measurement of optical absorption spectrum in visible light range of a novel organic material Zn-tetrabenzoporphin-crotonic acid/phenoxy resin (ZnTBP/CA/PhR) is reported in this paper. The nonlinear absorption property of the sample illuminated by lasers with different wavelengths was studied. And the absorption alteration and kinetic process of the major spectrum bands were observed. The saturation absorption (SA) and reverse saturation absorption (RSA) appeared as the input fluence increased，and re-reverse saturation absorption process of the material was demonstrated in the experiment. These properties occurred in a broad range of visible spectrum. The paper qualitatively analyses the physical mechanism during the whole course. Based on the nonlinear absorption characteristics, we showed some applications in photonics field of ZnTBP/CA/PhR.
2004 Vol. 24 (03): 266-269 [Abstract] ( 958 ) PDF (948 KB)  ( 288 )
270 Solid Phase Extraction and Room Temperature Phosphorimetry Coupling Technique and Its Application
SU Wen-bin，ZHU Ruo-hua，QIANG Hong，GU Xue-xin
The principle and application in the environmental analysis of Solid Phase Extraction (SPE) combined with Room Temperature Phosphorescence (RTP) analysis were reviewed. The principle, device, separation modes, operation procedures and application of SPE were commented. The merits and shortages in the operation procedure and quantitative analysis of classic RTP were also summarized. The potential application in the trace sample analysis and the advantage of coupling technique of SPE and RTP were indicated. The sensitivity and selectivity of the coupling technique could be greatly increased because of the strong enrichment ability of the SPE materials and the high selectivity of RTP. So far the technique has been successfully used in the analysis of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and polychlorinated dibenzofurans (PClDBFs) in the environmental samples according to their phosphorescence emission after preconcentration on the Whatman 1PS filter paper and C18 or C8 SPE membranes.
2004 Vol. 24 (03): 270-273 [Abstract] ( 955 ) PDF (907 KB)  ( 452 )
274 Studies on Photoluminescence Characteristics of Curcumin in Acrylamide Polymer
WANG Sui, CHANG Xi-jun*, GONG Guo-quan
A photoluminescence polymer was prepared using acrylamide as a monomer, a large excess of ethyleneglycol dimethacrylate as the cross-linking agent, and curcumin as a fluorescence additive. The polymer was ground into powder and screened in order to get even powder, whose diameter was from 40 to 75 μm. The emission spectra of curcumin in solid powder polymer show a strong blue shift compared with that of curcumin in C2H5OH solution. Meanwhile, rhodamine 6G, tetraiodofluorescein and phloxin have the same phenomenon of blue shift. Based on these facts, we speculate that the mechanism is probably single molecular luminescence because of the limit effect in three dimension space of the polymer. The molecule fluorescence peak was also depending on its environment because the surrounding electron field affected the molecule luminescence in polymer.
2004 Vol. 24 (03): 274-277 [Abstract] ( 612 ) PDF (904 KB)  ( 402 )
278 Chemiluminescence Method for Determination of Dipyridamole
RAO Zhi-ming, ZHANG Wang-hua, LI Qiu-zhong, XIE Guo-ping, YANG Hui-qin
A new system for the determination of dipyridamole with flow injection chemiluminescence was described. It is based on the chemiluminescence reaction of dipyridamole-potassium permanganate with rhodamine B. Tween-80 was found to be an enhancer of the chemiluminescence reaction. A method based on the enhanced chemiluminescence for dipyridamole determination has been developed. The method has high sensitivity, selectivity and good repeatability with a linear concentration range of 5.0×10-8-5.0×10-5 g·mL-1，a detection limit of 1.7×10-8 g·mL-1 and a RSD of 1.1％(n=11, cs=1.0×10-6 g·mL-1).
2004 Vol. 24 (03): 278-280 [Abstract] ( 1059 ) PDF (939 KB)  ( 406 )
281 Electron Spectra of Chemical Assembly Mesoporous MCM-41 with Transition Metal Complexes
HUO Yong-qian, LI Jun, WANG Wei, GONG Ya-qiong, ZHANG Feng-xing*
In the paper the complexes of metal cobalt(Ⅲ), manganese(Ⅲ), iron(Ⅲ) and copper(Ⅱ) with Schiff-base N,N-ethylenebis(salicylideneaminnato) have been synthesized and characterized. The nanosized porous material MCM-41 has been functionalized by the modification of the internal pore surface with γ-aminopropyl and was assembled by the modification groups with metal complex of Schiff-base. These metal complexes and functionalized nanosized porous materials were charcterized by XRD, IR and UV-Vis. It is indicated by spectral analysis that the synthesized nanosized porous materials have been confirmed to be MCM-41 with hexagon bores, and the γ-aminopropyls have been bonded on their internal pore surface. And the complexes of metal cobalt(Ⅲ), manganese(Ⅲ), iron(Ⅲ) and copper(Ⅱ) with Schiff-base N,N-ethylenebis(salicylideneaminnato) were assembled into MCM-41. The IR spectra of these samples show that there were characteristic absorptions of the amino and the Schiff base groups, and the absorption of amino shifted to longer wavelength.
2004 Vol. 24 (03): 281-284 [Abstract] ( 1628 ) PDF (963 KB)  ( 312 )
285 Approximate Calculation of L-S Coupling of Aluminum 3p Electronic Angular Momentums
LI Zun-ying，ZHAO Ru-jian
Al plasma was obtained by a pulsed laser beam, which was produced from a Nd:YAG laser set with Q-switch, ablating metal target Al in Ar. Based on the plasma, radiation of the plasma was recorded with time- and space-resolved technology, so Al characteristic radiation spectra were obtained. According to the spectra, the coupling of aluminum 3p electronic angular momentums was simplified as quasi-hydrogen particle. At the same time, the main quantum and orbit angular quantum shielding coefficients of aluminum nucleus, signed as α and s respectively, were carefully figured out with related theories of quantum mechanics. With our experiment, the resonance double lines of aluminum were scaled up at 396.15 and 394.40 nm respectively. As a result of our calculation, the main quantum shielding coefficient of aluminum nucleus was σ＝10.850 359, and the orbit angular quantum one was s＝7.332 875. Their values were reasonable in terms of the order of magnitude.
2004 Vol. 24 (03): 285-287 [Abstract] ( 1052 ) PDF (921 KB)  ( 309 )
288 NⅡ Ion Spectra Related to Lightning Discharges
YUAN Ping1, 2, LIU Xin-sheng1, ZHANG Yi-jun1
Appling the atomic structure theory to the research field of physical processes of lightning discharges, parameters such as wavelengths, oscillator strengths, transition probabilities and excitation energy of upper levels have been calculated for the transitions of NⅡ ions related to lightning discharges. Large-scale multi-configuration Dirac-Fock wavefunctions were applied to include the most important effects of relativity, correlation, and rearrangement of the electron density within the same (computational) model. More detailed identification than ever for lightning spectra has been done, and reference data have been provided for further theoretic and experimental works on the physical mechanism of lightning discharges.
2004 Vol. 24 (03): 288-291 [Abstract] ( 947 ) PDF (900 KB)  ( 436 )
292 Study on the Spectroscopy of Paramagnetic Compounds [{Cu(bipy) [C6H4(COO)2]}2·H2O]n and [Cu(phen)[C6H4(COO)2]]n
CHEN Rui-ping, YANG Bing-ping, ZENG Hui-yi, ZHENG Yu，DONG Zhen-chao
The cluster compounds with d9-d9 magnetic system were investigated because of their magnetic character. Some of the copper(Ⅱ) compounds with terephthalato as bridged unit, [{Cu(bipy)[C6H4(COO)2]}2·H2O]n and [Cu(phen)[C6H4(COO)2]]n, have been synthesized through a solvothermal reaction, and their crystal structures have been determined by X-ray diffraction. Their shape looks like zigzag-chain. In this paper, the molecular vibration spectra of the title complexes have been studied in detail. The middle and far-infrared spectra，and Raman spectra of the compounds have been reported and their assignments have been made experientially. The characteristic carbonyl absorption of terephthalato group at 1 688 cm-1 disappeared while the complexes formed. The characteristic peaks of COO- group were splited into two peaks respectively that appeared at 1 603, 1 574 cm-1(νasCOO) and 1 369, 1 356 cm-1 (νsCOO) in [{Cu(bipy)[C6H4(COO)2]}2·H2O]n, and at 1 614, 1 605 cm-1(νasCOO) and 1 373, 1 344 cm-1(νsCOO) in [Cu(phen)[C6H4(COO)2]]n. The relationship between the structures of the compounds and the spectra has been discussed as well. The coincidence between experiential assignments and the theoretic calculation will be confirmed.
2004 Vol. 24 (03): 292-294 [Abstract] ( 1009 ) PDF (912 KB)  ( 359 )
295 Time-resolved FTIR Study of Amorphous Process of Nylon 6 with Calcium Chloride
CHENG Xu，HE Qi-jia，ZHANG Ai-min
The influence of calcium chloride on the crystallinity of nylon 6 was studied by means of time-resolved FTIR, WADX and DSC. The results show that the crystallinity of nylon 6 decreased with the increase of CaCl2, and finally nylon 6 changed from crystal phase to amorphous phase. Because hydrogen bond is the main reason that nylon has three-dimensional ordered structure and forms crystalline phase, we further studied the changes of wave number of NH, amideⅠand amideⅡ related to hydrogen bond in CaCl2/PA6 complexes by time-resolved FTIR. These studies indicate that in the chloroethanol solution of nylon 6 and calcium chloride, complex bonds between calcium cation and oxygen atom of carbonyl group gradually form, and calcium cations are inserted into the molecular chains of nylon 6, which weaken the hydrogen bonds between the molecular chains of nylon 6 and damage the three-dimensional ordered structure of nylon 6, so the crystallinity of nylon 6 decreases and nylon 6 changes from crystalline to amorphous phase.
2004 Vol. 24 (03): 295-298 [Abstract] ( 1604 ) PDF (960 KB)  ( 463 )
299 In Situ Raman Spectroscopic Study on the Oxidation of HCHO on a Roughened Platinum Electrode
WANG Xiao-cong1，2，SU Xiao-qiong2，ZHONG Qi-ling2*，HUANG Xi-gen2，REN Bin3，XIANG Juan3，TIAN Zhong-qun3
The electrooxidation behavior of HCHO on a roughened platinum electrode was studied by cyclic voltammetry． Two factors that influence the electrooxidation behavior of HCHO，i． e． the concentration of the supporting electrolyte and the structure of the electrode surface were taken into account． The dissociative adsorption behavior of HCHO on a roughened platinum electrode was investigated by confocal microprobe Raman spectroscopy in-situ, and the spontaneous dissociative adsorption behavior of HCHO on a roughened platinum electrode was found by CV and was confirmed at the molecule level by in-situ Raman spectra.
2004 Vol. 24 (03): 299-302 [Abstract] ( 513 ) PDF (998 KB)  ( 502 )
303 Infrared Absorption Spectroscopy of Optical Waveguide in Proton-exchanged LiNbO3
FU Yun-liang1, 3，JIN Guo-liang2，YUAN Yi-fang3，HE Meng-xiong4，DENG Guang-qiang4
Z-cut proton-eｘchanged LiNbO3 optical waveguides eｘchanged with different proton sources miｘed with adipic acid and benzoic acid in different mol ratios were analyzed by infrared absorption spectroscopy. The result shows that there is an absorption peak of OH- free group at 3 500 cm-1with the characteristic of substitute protons, and the absorption peak of H-bond is nearby 700 cm-1 with the characteristic of packing protons. The different miｘing ratios and different concentrations of H＋ in the proton source，result in different proton-eｘchanged velocities and bring on the change in these absorption peaｋs. It is very important to study the change in these absorption peaｋs for maｋing high ｑuality LiNbO3 optical waveguide.
2004 Vol. 24 (03): 303-304 [Abstract] ( 1968 ) PDF (884 KB)  ( 325 )
305 Preparation and Properties of Complex of Europium Lanthanum with Crown Ether and p-phthalic Acid
ZHAO Yong-liang1，2, ZHAO Feng-ying3，HAO Zhong-xi1
Two complexes of crown ether europium(EuL) and crown ether lanthanum(LaL) were synthesized by europium perchlorate and lanthanum perchlorate with 18-crown-6(18-C-6) respectively. The heternuclear complexes of europium-lanthanum p-phthalic acid crown ether were prepared by the two complexes (EuL and LaL) with p-phthalic acid. The elemental analysis shows that its composition is EuLaL2L′(ClO4)4·6H2O(L＝18-C-6 and L′=p-C6H4(COO)2). The IR spectra, UV-spectra and molar conductor indicate that both ligands(L and L′) coordinate rare earth ions (Eu3＋ and La3＋), but perchlorate group is free. The fluorescence spectra show that the fluorescence intensities of the complex of heternuclear (EuLaL2L′(ClO4)4·6H2O) are more than eight times that of the crown ether europium complex. It was shown that the linked ligand (p-phthalic acid) can transfer the absorbed energy of Lanthanum-crown ether to europium-crown ether with high efficiency.
2004 Vol. 24 (03): 305-307 [Abstract] ( 1594 ) PDF (897 KB)  ( 381 )
308 Identification of Gastrodia Elata Blume by Fourier Transform Infrared Spectroscopy
LIU Gang1, DONG Qin2, YU Fan2, LIU Jian-hong3, SUN Shi-zhong3
In this paper, a method of rapid and undamaged identification of wild and cultivated Gastrodia elata Blume, and one of its fakes by Fourier transform infrared spectroscopy (FTIR) is reported. The results show that Gastrodia elata Blume and its fake have different characteristic infrared spectra, by which Gastrodia elata Blume can be identified from its fake. Wild winter, wild spring, and cultivated Gastrodia elata Blume can be discriminated by FTIR, according to the differences of their spectral peaks and absorbance ratios. By the differences of absorbance ratios of several peaks, different grade of Gastrodia elata Blume may be classified. FTIR has proved to be a rapid, simple and nondestructive method for the identification of Gastrodia elata Blume.
2004 Vol. 24 (03): 308-310 [Abstract] ( 1623 ) PDF (902 KB)  ( 504 )
311 Study on the Identification of Dangguitou and Dangguiwei by Two-dimensional Infrared Correlation Spectroscopy
Lü Guang-hua1，SUN Su-qin2, LEUNG Hi-wun1, CHAN Kelvin K C1
Fourier transform infrared spectroscopy (FTIR) combined with two-dimensional correlation spectroscopy was used to identify the different parts of Danggui in this paper. Guitou and Guiwei are two parts of the same officinal plant, and similar to each other in normal. FTIR spectra revealed the comparabilities of these two parts in herbal characters, organizing structure and alkaloid components. However, variance in amino acids and naphtha contents, which is aroused by the different parts of the angelica, could be identified easily and clearly in 2D FTIR spectra. Thus the fast and accurate property of 2D FTIR spectroscopy makes it a powerful and new approach to evaluating the medicinal herbs impersonally.
2004 Vol. 24 (03): 311-314 [Abstract] ( 1543 ) PDF (1242 KB)  ( 451 )
315 FTIR of Adipose Tissue of Ming Dynasty Mummy
YANG Hai-feng, YU Ying-hao
The Fourier transform infrared spectra (FTIR) of adipose tissue of Ming dynasty GUCONGLI mummy were investigated by chloroform-methanol extracttion and two ways of infrared sample preparation. The results show that the triglycide in the adipose tissue was hydrolyzed into free fatty acids, and both the octdecenic acid and saturated fatty acids existed.
2004 Vol. 24 (03): 315-316 [Abstract] ( 1086 ) PDF (865 KB)  ( 338 )
317 Application and Progress of Fourier Transform Attenuated Total Reflection Infrared Spectroscopy
XU Lin, WANG Nai-yan, BA Shu-hong, WANG Yun-long
With the application of Fourier transform infrared spectrograph and the development of chemical metrology, Fourier Transform Attenuated Total Reflection Infrared spectroscopy (ATR-FTIR) has become a kind of beneficial tool and means for analyzing samples, for which traditional transmission way does not work quite effectively, and for analyzing surface layer structure. ATR-FTIR has been applied to every realm such as spinning and weaving, quality testing, public security and so on. At present, people are launching applied study based on specific property of ATR-FTIR. Therefore, this paper mainly introduced the present study situation and development situation of ATR-FTIR, including theoretical development for depth profiling, qualitative analysis of material surface, quantitative analysis of mixture and solution component, and the application of fiber as ATR appurtenance. In addition, some special fields were also involved, such as inspecting hollow cored fiber’s structure and change of orientation, and studying effective mechanism about skin promoter.
2004 Vol. 24 (03): 317-319 [Abstract] ( 1055 ) PDF (876 KB)  ( 684 )
317 Application and Progress of Fourier Transform Attenuated Total Reflection Infrared Spectroscopy
XU Lin, WANG Nai-yan, BA Shu-hong, WANG Yun-long
With the application of Fourier transform infrared spectrograph and the development of chemical metrology, Fourier Transform Attenuated Total Reflection Infrared spectroscopy (ATR-FTIR) has become a kind of beneficial tool and means for analyzing samples, for which traditional transmission way does not work quite effectively, and for analyzing surface layer structure. ATR-FTIR has been applied to every realm such as spinning and weaving, quality testing, public security and so on. At present, people are launching applied study based on specific property of ATR-FTIR. Therefore, this paper mainly introduced the present study situation and development situation of ATR-FTIR, including theoretical development for depth profiling, qualitative analysis of material surface, quantitative analysis of mixture and solution component, and the application of fiber as ATR appurtenance. In addition, some special fields were also involved, such as inspecting hollow cored fiber’s structure and change of orientation, and studying effective mechanism about skin promoter.
2004 Vol. 24 (03): 317-319 [Abstract] ( 963 ) PDF (876 KB)  ( 398 )
320 Detection of Organic Autotrophic Particles by FCM(Flow Cytometry) in an Oligotrophic Lake
GUO Pei-yong, ZHU Yin-mei
Organic autotrophic particles were detected by flow cytometry(FCM) in an oligotrophic lake. Utilizing scattering signals and fluorescence of their natural pigments, different populations could be rapidly discriminated and enumerated. We found that they belonged to three populations. R1 were the smallest population, while R3 were the largest one. R1 contained phycoerythrin but lacked chlorophyll. On the contrary, R3 contained a large amount of chlorophyll but lacked phycoerythrin. R2 contained not only chlorophyll but also a great deal of phycoerythrin. Organic autotrophic particles account for the most proportion of the total particles that were smaller than 50 μm. They represented 70.24% of the total particles. In this study, we found that flow cytometry is particularly suited to the analysis of organic autotrophic particles that are difficult to study with traditional methods.
2004 Vol. 24 (03): 320-322 [Abstract] ( 208 ) PDF (945 KB)  ( 298 )
323 Study of the Effect of Aliphatic Alcohol on the Inclusion Interaction of Qucertin-cyclodextrin Complexes
LIU Xiu-ping, ZHANG Guo-mei, YANG Yu, DONG Chuan, SHUANG Shao-min
The inclusion interaction of qucertin with β-cyclodextrin and its derivatives was studied by fluorimetry. The formation constants of their inclusion complexes were determined, and the stoichiometry ratio on the formation of the inclusion complexes was determined by equimolar continueous variation method. The effect of aliphatic alcohols with short chains on inclusion process was discussed. The results showed that the inclusion ability of β-CD and its derivatives was in the order: HP-β-CD＞M-β-CD＞β-CD. The effect of aliphatic alcohol on complexes was related to the carbon number and volume of alcohol molecules.
2004 Vol. 24 (03): 323-326 [Abstract] ( 1004 ) PDF (958 KB)  ( 361 )
323 Study of the Effect of Aliphatic Alcohol on the Inclusion Interaction of Qucertin-cyclodextrin Complexes
LIU Xiu-ping, ZHANG Guo-mei, YANG Yu, DONG Chuan, SHUANG Shao-min
The inclusion interaction of qucertin with β-cyclodextrin and its derivatives was studied by fluorimetry. The formation constants of their inclusion complexes were determined, and the stoichiometry ratio on the formation of the inclusion complexes was determined by equimolar continueous variation method. The effect of aliphatic alcohols with short chains on inclusion process was discussed. The results showed that the inclusion ability of β-CD and its derivatives was in the order: HP-β-CD＞M-β-CD＞β-CD. The effect of aliphatic alcohol on complexes was related to the carbon number and volume of alcohol molecules.
2004 Vol. 24 (03): 323-326 [Abstract] ( 1391 ) PDF (958 KB)  ( 315 )
327 Synthesis of Mixed Complexes of Lanthanum with 2,2-Bipyridyl and 1,10-Phenanthroline and Suudy of the Interaction of the Complexes with DNA
FANG Guang-rong，LI Ling, CAI Zhao-ｘia，LIU Li-ming，SONG Gong-wu
A mixed complex of La with 2,2-bipyridyl (dpy) and 1,10-phenanthroline(phen) was synthesized. Elemental analysis, IR and TGA of the complex were investigated, thus it was proved that the conformation of it was La(dpy)(phen)Cl3. The interaction of the complex with DNA has been studied also. The spectra showed that the interaction between La(dpy)(phen)Cl3 and DNA experienced intercalation of long-range self-assembly. The study made it clear that the synthesized mixed complex La(dpy)(phen)Cl3 can interact with DNA, and La(dpy)(phen)Cl3 can be used for probing a nucleic acid.
2004 Vol. 24 (03): 327-329 [Abstract] ( 1573 ) PDF (956 KB)  ( 321 )
330 Color Reaction of New Tailed Porphyrin-pyridine Quaternary Ammonium Salts with Copper (Ⅱ)
HAN Shi-tian，LIU Yan-qin*，DENG Hui
Color reactions of Cu2+ with three new different-chain-length tailed porphyrin-pyridine quaternary ammonium salts were studied. The Soret bands of complexes lie at (Ⅰ)，(Ⅱ)413 nm and (Ⅲ)414 nm, which are separated from those of the diacid forms (Ⅰ)443.5 nm，(Ⅱ)444 nm and (Ⅲ)446 nm. The contrast is about 30 nm. The ratio of Cu2+: reagent in the complexes is 1∶1． The apparent molar absorptivities of complexes are(Ⅰ)3.4×105，(Ⅱ)2.9×105 and(Ⅲ)2.5×105 L·mol-1·cm-1, and Beer’s law is obeyed in the ranges of (Ⅰ)0-0.5 μg·(10 mL)-1，(Ⅱ)0-0.6 μg·(10 mL)-1 and (Ⅲ)0-1 .0 μg·(10 mL)-1 for Cu2+. This method can be used for the determination of trace Cu2+.
2004 Vol. 24 (03): 330-332 [Abstract] ( 984 ) PDF (946 KB)  ( 362 )
333 The Reformation of Tomato Ecology Using Photo-ecology Film
MENG Ji-wu1, 2, 3, ZHENG Rong-er1, ZHANG Yun-dong2, CAO Bai-qing3，LI Wei3
The action spectrum of photosynthesis of tomato was studied with excitation and fluorescence spectra of its leaf. To simulate action spectrum of tomato the fluorescent auxiliary was specially prepared and used to make the photo-ecology film. The film was used to cover the roof of greenhouses for planting tomatoes in Jianguo village of Xinfa town, Daoli district, Harbin. The survey of ecology conditions, tomato growth and yield has been made in comparison with those in the greenhouse using normal film. It is shown that the yield of tomato in the photo-ecology film greenhouse has increased by 53.7 %, which leads to a production value rise of 61.4%.
2004 Vol. 24 (03): 333-335 [Abstract] ( 1640 ) PDF (914 KB)  ( 531 )
336 Synthesis and Spectral Characterization of Boron Complexes of Bis-schiff Base from Acylpyrazolone
LI Jin-zhou，AN Yu-mei，WANG Lu，YU Wen-jin
Three novel bis-schiff base complexes [B(PMαFP)2en]Ac, [B(PMαFP)2pen]Ac and [B(PMTHP)2en]Ac have been synthesized, where (HPMαFP)2en=N,N′-bis[(1-phenyl-3-methyl-5-oxo-4-pyrazolinyl)α-furylmethylidyne]ethylenediimine, (HPMαFP)2pen=N,N′-bis[(1-phenyl-3-methyl-5-oxo-4-pyrazolinyl) α-furylmethylidyne]-o-phenylenediimine and (HPMTHP)2en=N,N′-bis[(1-phenyl-3-methyl-5-oxo-4-pyrazolinyl)-2-thenoylmethylidyne] ethylenediimine. They were characterized by elemental analysis, IR, UV-Vis, 1H NMR, 13C NMR，and molar conductance measurements. The results show that the bis-schiff base is a quadridentate ligand and boron is four-coordinated in the complexes.
2004 Vol. 24 (03): 336-338 [Abstract] ( 1081 ) PDF (880 KB)  ( 372 )
339 Study on the Fluorescence Spectra of LaL3 with DNA
WANG Xing-min1，SONG Yu-min2*，TENG Xiu-lan2, GENG Zhi-yuan2, YANG Pei-ju2, YANG Mei-ling2
A fluorescence method is presented for the determination of DNA.The method is based on the interaction of LaL3 [L=morin(2′, 3, 4′, 5, 7-Pentahydroxyflavone), 2′-OH group deprotonated] with DNA in NH3·H2O-NH4Cl buffer of pH=8.0, with λex at 387 nm, and λem at 535 nm. Enhanced fluorescence was observed for LaL3 in the presence of DNA and in the presence of buffer solution of 10%(φ) and ethanol of 10%(φ). The linear range of determination was between 0 and 15 μg·mL-11 for DNA.The method proved to be simple, easy and sensitive for the determination of DNA. The mechanism of enhancing and the reasons for the effects of acid were also discussed.
2004 Vol. 24 (03): 339-341 [Abstract] ( 1586 ) PDF (904 KB)  ( 432 )
342 Catalysis-fluorescence Determination of Trace Nitrite Based on the Oxidation of Acridine Orange by Potassium Bromate
BAO Suo-yan1 ，LIU Wei-jie1, 2，HU Han-fang1
Acridine orange can be oxidized with discoloring and fluorescence quenching by potassium bromate in phosphoric acid medium, but the reaction rate is very low. The presence of trace nitrite can catalyze this reaction to improve the sensitivity of it apparently and to make the net fluorescence value of the system decrease greatly. Based on the above investigation, a new catalysis-fluorescence determination method of trace nitrite has been proposed. The method described is very sensitive and selective. The catalysis reaction is under the conditions of λeｘ/λem＝446/505 nm, 55 ℃ and 10 min for the reaction time. The method permits the existence of more than 20 common foreign ions. There isn’t interference by the same quantity of Fe3+, Br- and I-. The detection limit is 0.012 ng·mL-1. The linear range of determination is 0.05-5 ng·mL-1. The method has been used for the determination of trace nitrite in water and soil samples with satisfactory results.
2004 Vol. 24 (03): 342-344 [Abstract] ( 1488 ) PDF (961 KB)  ( 351 )
345 Ion Floatation-spectrophotometric Determination of Palladium(Ⅱ) Content in Acetaldehyde Catalyst
DONG Hui-ru，ZHANG Jing-chang，HU Shao-cheng
The nature of palladium (Ⅱ) and copper (Ⅱ) is very similar, so it is very difficult to determine trace palladium (Ⅱ) in the coexistence of a great quantity of copper (Ⅱ). This paper applied ion floatation-spectrophotometric principle, using 1-( 2-pyridylazo)-2-naphthol (PAN) as collector, and through controlling pH of the solution and determination wavelength, without separation to determine palladium (Ⅱ) content in acetaldehyde catalyst with a great quantity of copper (Ⅱ)． The relative error was 0.61%，and RSD was 2.33%. The results were satisfactory.
2004 Vol. 24 (03): 345-347 [Abstract] ( 1014 ) PDF (937 KB)  ( 322 )
348 Study on the Method for Determination of Sulfate in Fe-catalyst by Inductively Coupled Plasma Atomic Emission Spectrometry
LIU Dong-yan，GUI Guo-qing
A direct method was reported for the determination of sulfate in iron-catalyst by inductively coupled plasma atomic emission spectrometry (ICP-AES). The samples were dissolved with hydrochloric acid. The interference factors of hydrochloric acid and iron were studied. The results showed that the effect of iron on the test of sulfate was not only to cause background interference but also to depress the intensity of sulfur seriously as well，and the effect increased with the increment of iron amount． Due to the physical in terference，a high concentration of HCl also depresesed the intensity of sulfur． Matrix effect from iron and HCl were corrected by matrix matching method. The recommended method is simple and rapid，and show satisfying precision and accuracy. The recoveries were more than 97%, and the relative standard deviations of six samples were less than 3%.
2004 Vol. 24 (03): 348-350 [Abstract] ( 1513 ) PDF (943 KB)  ( 324 )
351 Determination of Trace Selenium in Coal By Microwave Digestion and Hydride Generation ICP-AES
LIU Jing，ZHENG Chu-guang，ZHANG Jun-ying，XU Jie-ying
A method for determining trace Se in coal by microwave digestion and hydride generation ICP-AES is reported. The digestion system of HNO3-HCl-HF was evaluated. The hydride generation occurred in 3 mol·L-1 hydrochloric acid media with 1% sodium tetrahydroborate as a reduction reagent. The experimental conditions of microwave digestion, prereduction，and interferences were investigated. This method is simple and rapid. The treatment method was applicable to Se and gave results that were in good agreement with the certified values of the standard reference material. Testing results showed that the detection limit was 0.3 μg·L-1 and RSD was below 5%.
2004 Vol. 24 (03): 351-353 [Abstract] ( 1612 ) PDF (938 KB)  ( 440 )
354 Determination of Micro-Elements in Couplers by Inductively Coupled Plasma Atomic Emission Spectrometry
DU Bao-an1 ，WANG Xiang-yan2
By ICP-AES, we established a method to quantitatively determine the micro-elements in couplers. We processed the unknown sample with wet digesting method. Nine micro-elements in the couplers can be quantitatively determined at the same time. Using the powerful chem.-station, we have discussed the method to eliminate physical interference and background correction. The results of the experiment showed that the method is accurate, quick, of high performance，and with all RSDs≤1.00%. The linear correlation coefficient of the tested elements is over 0.999 9.
2004 Vol. 24 (03): 354-356 [Abstract] ( 1579 ) PDF (931 KB)  ( 393 )
357 Determination of Trace Elements in Flowers and Tests of Conditions
LI Jia-xin1，MAI Yong-fu2，KUANG Zu-yan2，WANG Yue-hua2
The optimum conditions，such as the ratio of fuel gas to combustion-supporting gas，burnerheight，lamp current and band pass，for the determination of trace elements such as calcium，magnesium，cobalt and potassium in flowers were studied by flame atomic absorption spectrophotometry(AAS)． The eｘperimental results showed that Beers law was obeyed in the range of 0-50 μg·mL-1 for Ca，0-80 μg·mL-1for Mg，0-4 μg·mL-1 for Co，and 0-120 μg·mL-1 for K． The correlation coefficients were in the range of 0.99７ 5-0.999 5 under the seleced conditions． Applied to the determination in rose & Chinese rose the method proved to be simple，rapid and selective with satisfactory recovery of 9７％-104％ and relative standard devition of 1.2％-2.3％.
2004 Vol. 24 (03): 357-359 [Abstract] ( 1611 ) PDF (887 KB)  ( 352 )
360 Analysis of the Contents of K, Na, Ca, Mg, Zn, Cu, Fe and Mn in Serum of Middle and Old-Aged Hypertension Patients
LIU Wei-ming, ZHU Zhi-guo, LENG Hong-xia
Atomic absorption method was used to detect the contents of K, Na, Ca, Mg, Zn, Cu, Fe and Mn in serum of 48 hypertension patients and 52 healthy people. The results show that the contents of Na, Mg, Zn, Fe and Mn in hypertension were higher than healthy control, while K, Ca and Cu were lower. Na/K were higher, but Ca/Mg and Cu/Zn were lower, than healthy control. These suggested that we should add K, Ca, Mg and Cu properly, reduce Na, scientifically control the increase of Zn, Fe and Mn, pay attention to the balance relation of Na/K, Ca/Mg and Cu/Zn, reduce Na/K, raise Cu/Zn, and add Ca with Mg properly. This can be useful for preventing and treating hypertension.
2004 Vol. 24 (03): 360-362 [Abstract] ( 982 ) PDF (982 KB)  ( 548 )
363 Determination of Zinc in Mineral by FAAS after Phase Separation and Extraction
YANG Xiang，HAN Hong-yin，CHEN Wen-wu，ZHANG Xin-hua，TANG Zhi-yong，JIN Ze-xiang
Non-ion surface active agent can be separated from its solution of water by heating to its cloud point. A new method for the determination of zinc in mineral samples by flame atomic absorption spectrophotometer after phase separation and extraction making use of its cloud point was studied in this paper. The conditions of phase separation and extraction such as using Triton X-100 as phase separation agent, and octanol to drop the cloud point, and the influence of acidity and the number of times for oscillating were discussed. The detection limit was 0.005 μg·mL-1. This method has been applied to the determination of zinc in ores with satisfactory results.
2004 Vol. 24 (03): 363-365 [Abstract] ( 384 ) PDF (885 KB)  ( 355 )
366 Determination of Trace Elements in Shenrong Heixi Wan
ZHANG Qi-feng, LIU Qin, YAO Xing
Shenrong Heiｘi Wan is a pure traditional Jiangｘi medicine which has been mainly used to cure coma in clinic as its main function is resuscitation． In this paper，four trace elements in Shenrong Heiｘi Wan and other five traditional Chinese medicines have been determined and contrasted by AAS. The results show that there are abundant benificial trace elements in Shenrong Heiｘi Wan while pernicious trace elements such as Hg，Cd etc. are low. So the medicine is safe to taｋe.
2004 Vol. 24 (03): 366-367 [Abstract] ( 1410 ) PDF (858 KB)  ( 316 )
368 Studies on Sequential Injection Spectrophotometric System Using A Reflective Flow Cell for Process Analysis
FAN Shi-hua, WANG Shi-li, FAN Xiao-feng, WANG Fu-ren, FANG Zhao-lun
A reflective flow cell was developed and coupled to a sequential injection system and optical fiber photometric detection system based on emitting diode light source. A multistrand bifurcated optical fiber was coupled with incident light, detector and flow cell. Optical fibers were used to carry light from the electronics unit to a reflective flow-through cell and back. The liquid flow path through the cell is linear with a large exit aperture such that bubbles are not trapped in the optical path. The optical arrangement is such that the incident light crosses the liquid flow orthogonally and is reflected back to the receiver fiber. This arrangement reduces the reflective index sensitivity by an order of magnitude relative to a conventional flow cell. The cell showed good immunity to refractive index and air bubble effects. The chromogenic reaction of chloride ion with mercury thiocyanate-iron(Ⅲ) was used as a model reaction to optimize the experiment system and check the optical system. The reflectance of the reaction was monitored with blue emitting diode. The linear range was 0—100 mg·L-1 Cl-. A detection limit (3σ) of 1.2 mg·L-1, precision of 1.5% (n=11), and a throughput of 30 samples per hour were achieved.
2004 Vol. 24 (03): 368-371 [Abstract] ( 436 ) PDF (972 KB)  ( 431 )
372 The Depolarization Characteristic of Quartz Depolarizer in UV-VUV Spectral Region
LIU Ying1, FU Shao-jun1，LI Fu-tian2
The quartz depolarizer consisting of two wedge-shaped quartz crystals was designed based on the Lyot depolarizer. The quartz depolarizer is used to reduce the polarization response of spectral instruments. The residual degree of polarization of the quartz depolarizer was derived by the method of matrix optics, so the variation regularity of its depolarization characteristic was analysed concerning its center thickness and the status of the incident radiation in the UV-VUV spectral range. Its depolarization effect was obvious for the radiation with some spectral bandwidth. Also, the depolarization characteristic of the quartz depolarizer was studied experimentally with 1-meter Seya-Namioka UV-VUV spectrometer, using LiF crystals as the polarizer and analyzer. The residual degree of polarization of the quartz depolarizer was less than 1%. Both the theoretical analysis and experimental results show that the quartz depolarizer we designed is appropriate to the spectral measurement with high accuracy.
2004 Vol. 24 (03): 372-375 [Abstract] ( 1909 ) PDF (920 KB)  ( 366 )
376 Mathematical Model of Dispersive Infrared Gas Analyzer Based on Pyroelectric Detector
ZHANG Yong-huai，LIU Jun-hua
This paper analyzes the characteristics of the pyroelectric detector based on its working principle. The input and output mathematical model of DIGA (Dispersive Infrared Gas Analyzer) system with pyroelectric detector was established according to the design principle of DIGA. We have manufactured a novel multi-gas DIGA on the basis of this model, then pointed out several problems that should be taken into account in the design. Application indicates that this model is of considerable practical value for the design, study, performance analysis and further improvement of DIGA.
2004 Vol. 24 (03): 376-378 [Abstract] ( 940 ) PDF (903 KB)  ( 326 )
379 Study on the Phosphorylaions Reaction between Ethyl Salicylate and DEPH
CHEN Xiao-lan1，LIAO Xin-cheng1，LU Jian-sha1，GUO Lei1，QU Ling-bo1，ZHAO Yu-fen1，2
Atherton-Todd reaction has been extensively applied to the synthesis of phosphates and phosphoroamidates. Under Atherton-Todd reaction conditions, dialkyl phosphites were probably transformed into diakyl phosphorochloridates. We have tried to use Atherton-Todd reaction to synthesize phosphate of salicylic-acid. But when the —COOH of salicylic acid was under unprotected, the yield was quite low. It was found that the —COOH possibly participated in the reaction. The competitive reaction between the —COOH and —OH of salicylic acid probably existed. In order to understand the detail mechanism, ethyl-salicylate was selected to be phosphorylated. In the end, ethyl-salicylate successfully phosphorylated by modification of the classical Atherton-Todd procedure through dropping the DEPH and tetrachloromethane into the mixed solution of ethyl-salicylate, triethylamine and dioxane with good yields. The structures were elucidated by NMR and ESI/MS/MS data.
2004 Vol. 24 (03): 379-380 [Abstract] ( 1526 ) PDF (935 KB)  ( 336 )
381 Coordination Bonding Driving Supramolecular Self-assembly of Tetraphenylporphyrinatozinc(Ⅱ) with Imidazolyl Tailed Porphyrinatoiron(Ⅲ) Studied by Fluorescence Spectra and 1H NMR
HU Shu-guang, HUANG Jin-wang, MA Li, LUO Hai-ying, JI Liang-nian
Coordination bonding driving supramolecular self-assembly of Zn(TPP) with Fe(p-ImEPTPP)Cl was investigated by fluorescence spectra and 1H NMR. The results indicate that an obvious fluorescence quenching observed from Zn(TPP) by addition of Fe(p-ImEPTPP)Cl is due to the coordination of the terminal imidazolyl group of Fe(p-ImEQTPP)Cl to Zn2+ of Zn(TPP). The change of fluorescence spectra of Zn(TPP) / Fe(p-ImEPTPP)Cl system by adding some Lewis bases，such as piperidine, imidazole and pyridine，as well as 1H NMR further supported this coordination.
2004 Vol. 24 (03): 381-383 [Abstract] ( 1006 ) PDF (913 KB)  ( 457 )

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