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    24 October 1992, Volume 13 Issue 10
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    Articles
    Synthesis of Adducts Between Alkaline Earth Dodecatungstophosphates with DMF and EtOH and Determination of the Heats of Addition Reaction
    WANG Ai-Min, ZHU Jing, GU Yi-Dong
    1992, 13(10):  1193-1196. 
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    Adducts,Ca2/3(PW12O40)·9DMF·EtOH,Sr2/3(PW12O40)·8DMF·EtOH and Ba2/3(PW12O40)·9DMF were synthesized in non-aqueous solutions,Their compositions and Keggin structures were characterized by elemental analysis and IRspectrometry.The heats of addition reactions between calcium dodecatungstophosphate,strontium dodecatungstophosphate and barium dodecatungstophosphate with DMF and EtOH were respectively determined by solution calorimetry.The values were -207.4±2.3 kJ/mol,-197.1±5.4 kJ/mol and -270,9±2.4 kJ/mol at 30℃,respectively.
    Syntheses and Spectroscopic Properties of Ternary Complex (这里有图片19921002-1197-1.gif)
    ZHAI Ying-Li, WANG Xiu-Jian, WANG Qiu-Ying
    1992, 13(10):  1197-1200. 
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    The ternary complex of monomolybdenum   was synthesized in methanol with o-mercaptophenol and benzoylhydrazine as the ligand and (Bu4N[Mo8O26] as the parent The properties of the complex were characterized by elemental analysis,molar conductivity,electronic spectra,infrared spectra,1H NMR spectra and TG-DTA,The most possible structure is proposed on the basis of the spectral data and the IR spectra show that the complex has not terminal oxygen atoms,
    Synthesis and Crystal Structure of Complexes of Rare Earth(Ⅲ) Isothiocyanate with N-(p-chlorophenyl)aza-15-Crown-5
    LUO Lan, WEI Ming-Li, YAN Shi-Ping, WANG Geng-Lin, WANG Hong-Gen, YAO Xin-Kan
    1992, 13(10):  1201-1204. 
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    Twelve 1:1 complexes of rare earth(Ⅲ) isothiocyanate with N-(p-chlorophenyl)aza 15-crown-5 were synthesized and characterized by elementary analyses,conductivity measurements,UVspectra,IRspectra and TG-DATanalyses.The crystal and molecular structures of C19H24N4O4S3ClSm were determined by single-crystal X-ray diffraction.The unit-cell is triclinic,space group P1 with a=0.8422(3) nm,b=0.9056(1) nm,c=1.7041(6) nm,α=93.88(1)°β=102.25(3)°,γ=98.85(2)°,V=1.2482 nm3,M=654.34,Z=2,Dx=1.74 g/cm3,R=0.045,Rw=0.056.The Sm3+ deviates from the plane of the four ether oxygens by 0.1482 (±0.006) nm and is coordinated to every hetero-atom in the polyether ring,and is also coordination to the nitrogen atoms of three isothiocyanates,and the average bond distance is as follows:Sm-O(ether)0.2500 nm,Sm-N(SCN)0.2390 nm,Sm-N 0.2712(5) nm.The coordination number of Sm3+ ion is eight.
    Studies on the Solid State Reactions of Coordination Compounds (LVI)——The Solid-Solid State Reaction of Salicylaldoxime with Anhydrous Nickel Acetate at Room Temperature
    ZHENG Li-Min, ZHANG Wei-Hua, XIN Xin-Quan
    1992, 13(10):  1205-1208. 
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    Solid-solid state reaction of salicylaldoxime with anhydrous nickel acetate results in the formation of trans-[Ni(SAO)2] The process can be completed by putting the mixture at 30℃ for 4 hours,with a high yield of 99%.XRD,IR and elemental analysis are used to charaterize the solid product.The kinetics of the reaction is investigated by using the electrical conductivity measurement
    Synthesis of Zeolite NaX by Microwave Radiation
    SONG Tian-You, XU Jia-Ning, XU Wen-Guo, MENG Xian-Ping, FENG Hong, LIU Xi-Sheng, ZHOU Feng-Qi, XU Ru-Ren
    1992, 13(10):  1209-1210. 
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    In this paper the synthesis of zeolite NaX by means of microwave radiation is reported firstly in China.The pure product was obtained in 30min.The crystal size on SEM pictures is smaller and more regular than that obtained under the conditions of conventional synthetic method.
    Studies on Dual Carbon Fiber Microelectrodes and Its Application to Detection of Dopamine
    ZHANG Xue-Ji, B. J. Seddon, WANG Chang-Fa, ZHOU Xing-Yao, ZHAO Zao-Fan
    1992, 13(10):  1211-1213. 
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    The present paper covers the investigation and application of dual microelectrodes.Dopamine is detected with the electrodes from the ascorbic acid background.Electrode reaction mechanism is studied.Collector current is proportional to concentration of dopamine in the range over 5.0×10-4 mol/L to 5.0×10-6 mol/Land ramains independent of ascorbic acid concentration to approximately 5.0×10-4 mol/L.
    Simultaneous Determination of Trace Fluorene, Acenaphthylene,Anthracene and Perylene by Polarization-Synchronization Spectrofluorimetry
    GU Li-Zhong, WENG Yi-Bin, HUANG Xian-Zhi, CHEN Guo-Zhen
    1992, 13(10):  1214-1216. 
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    The present paper contains a new method of polarization-synchronization spectrofluo-rimetry for the simultaneous determination of trace fluorene.acenaphthylene,anthracene and perylene.The use of this technique can effectively suppress the effect of scatteredlight during synchronous scanning,and hence enhance sensitivity.The detection limits of fluorene,acenaph-thene anthracene and perylene were(ng/mL):1.1,10.0,1.8 and 0.26,respectively.The relative standard deviation was less than 4.2%.
    Single-Sweep Polarographic Investigation of Ni(Ⅱ)-Bilirubin and Ni(Ⅱ)-2,2' Bipyridyl-Bilirubin
    WANG Ju-Li, JIANG Mian, ZHOU Xing-Yao
    1992, 13(10):  1217-1220. 
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    The single-sweep polarographic behavior and mechanisms of Ni (Ⅱ)-bilirubin(BR) and Ni(Ⅱ)-2,2' bipyridyl(Bipy)-bilirubin were investigated.In pH 7.5 phosphate buffer solution,Ni(Ⅱ)-BRexhibited a catalytic prewave with cathodic peak potential-1.0 V(vs.SCE) and Ni(Ⅱ)-Bipy-BRproduced a sensitive catalytic hydrogen wave with cathodic peak potential-1.5 V(vs.SCE).These waves can be used to determine trace bilirubin,the heights of derivative peak are linear with bilirubin over the ranges of 1×10-6～5×10-6 mol/Land 2×10-7～8×10-6 mol/L respectively.
    Extracting Two-dimensional Pure Spectra from Mixture Spectra with Inverse Neural Model
    CONG Pei-Sheng, LI Tong-Hua, LIU Bing, LIU Dong-Xiang
    1992, 13(10):  1221-1224. 
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    An inverse neural model which consists of less input nodes and more output nodes is proposed in this paper.The unique weights of the neural model can be obtained when the number of training samples is greater than the number of input nodes of the model,and they are the pure spectra of components of the mixtures in our experiments.The obtained pure spectra which were extracted from the excitation-emission matrix of anthracene phenanthrene and pyrene multi-sample mixture were compared to the experimental pure spectra.Both obtained and experimental pure spectra were used as calibration in rank annihilation to predict the concentrations of components in the unknown mixtures.The results show that the obtained pure spectra were more suit-able for calibration and the average predictive errors were decreased from 7%,8.5% and 7,8% to 2.3%,5.0%,and 3.5% for anthracene,phenanthrene and pyrene respectively.
    Studies on Photochemical Fluorimetric Method(Ⅷ)——Wave Scanning-Differential Rate Method
    GUO Xiang-Qun, XU Jin-Gou, ZHAO Yi-Bing, CHEN Guo-Zhen
    1992, 13(10):  1225-1228. 
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    The present paper deals with a differential rate kinetic photochemical fluorimetric technique,wave scanning-differential rate method,for simultaneous determination of two compounds.The principle for this method as well as the experimental technique by which the in situ photochemical fluorimetry is able to carry out by use of commercial fluorescence spectropho-tometer is described.A wave scanning-differential rate method for the simultaneous determination of riboflavin and menadione based on their photochemical reaction,used as an example of this technique,is proposed,The calibration graph was rectilinear from 0.0 ng/mLto 1.20μg/mLfor riboflavin (r=0.999) and from 0.0 ng/mL to 2.70 /ng/mL for menadione (r=0.998).The limits of detection were 0.22 ng/mL riboflavin and 2.6 ng/mLmenadione.The average recoveries were 101% and 99%,respectively.The standard deviations were 2.5% for riboflavin and 2.8% for menadione
    The Theory of Reversible Wave at Ultramicrodisk Electrodes in Staircase Sweep Voltammetry
    YU Jun-Sheng, ZHANG Zu-Xun
    1992, 13(10):  1229-1232. 
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    An equation is derived for the current response of a reversible electron transfer reaction for staircase sweep voltammetry at uhramicrodisk electrodes and verified experimentally.Characters of its current potential curves are discussed.Experimental results for oxidation of K4Fe(CN)6 at uhramicrodisk platinum electrodes agree well with the theory.
    Rapid Alkaline Degradation Determination of Trace Chlorotetracycline by Flow Injection Fluorimetry
    ZHAO Yi-Bing, YU Zhi-Xiong, GUO Xiang-Qun, XU Jin-Gou, CHEN Guo-Zhen
    1992, 13(10):  1233-1236. 
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    The present paper covers a new flow injection fluorimetric method for the determination of trace chlorotetracycline.Chlorotetracycline reacts rapidly with 0.25 mol/L NaOHin a reaction tube and produces strong fluorescent species detected by fluorimetry in a flow cell.The fluorescence intensity of the product is proportional to the concentration of chlorotetracycline over the range of 10-8～10-5 mol/L.Coexisting tetracycline and anhydrochlorotetracycline do not interfere with the determination of chlorotetracycline.This method can be used not only for the quality detection of chlorotetracycline medicine but also for the determination of chlorotetracycline in tetracyline medicine.The determination of chlorotetracyciine in urine and serum is successful with satisfactory recoveries.
    Studies on Structure and Properties of Organic Reagents(Ⅹ)——Study of Structure and Absorption Spectrum of Azobenzene Derivatives
    TONG Shen-Yang, ZENG Wei
    1992, 13(10):  1237-1240. 
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    In order to study the relationship among absorption spectra of organic reagents,the calculation of π-electronic excitation energies of azobenzene derivatives has been carried out by means of PPP-SCF-CI method.The intramolecular charge-transfer character of the first π-π transition was found,Agood agreement was obtained between the observed and calculated values for the first π-π excitation.The effect of substituents on the absorption spectrum was studied on the basis of these calculated results.
    A Study on Determination of Copper by Microwave Induced Plasma Atomic Absorption Spectrometry(MIP-AAS)
    DUAN Yi-Xiang, LU Hui, HOU Ming-Yi, ZHANG Han-Qi, JIN Qin-Han
    1992, 13(10):  1241-1243. 
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    The determination of copper by MIP-AAS was studied systematically.The sample solution was introduced from an ultrasonic nebulizer and the solvent was removed by both a condenser and a concentrated H2SO4 desiccator.The experimental parameters which affect the determination of copper were examined in detail.The characteristic concentration for copper was shown to be 0.008μg/mL,and a good accuracy was also achieved.
    Simultaneous Determination of Five Synthetic Food Colorants in Their Mixed Systems by On-line Kalman Filtering Spectrophotometry
    ZHUO Zong-Liang, LIU Xin-An, LIN Ai-Hua, SHI Le-Ming
    1992, 13(10):  1244-1246. 
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    Mixed samples containing amaranth,new coccine,tartrazine,sunset-yellow and brilliant blue were analyzed with an on-line Kalman filtering system composed of a Varian DMS 200 UV/VIS spectrophotometer,an IBM PC/AT micro-computer and the relevant supporting software.The simultaneous determination of five individual components was successfully completed without prior separation and with a good accuracy and high speed.
    Solid Phase Synthesis and Biological Activities of α-h-ANF and Its Analogs
    ZHANG Ran, WANG Yu-Hong, ZHU Zhi-Hua, GUO Li-Li, XU Jian-Ping, WANG Zong-Mu, LI Wei
    1992, 13(10):  1247-1250. 
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    Based upon a structural working model for ANF's functioning mechanism,two analogs of α-h-ANF were designed.Using Fmoc-AA-Pfp as monomer,α-h-ANFand its analogs cited above were synthesized by a solid phase procedure with a high yield and purity.The biological activity study of rabbit aorta shows that one of the analogs is twice and another about one and a half times more active than α-h-ANF itself.
    Research on Bond-Linked Bisoxazoles(Ⅱ)——Studies on the Structures and Optical Properties of 4,4'-bis[2"-(5"-Substituted Phenyl Oxazolyl)]-1,1'-Biphenyl and 5,5'-bis(Dimethylphenyl)-2,2'-Bioxazole
    WANG Ming-Zhen, ZHANG Wen-Qin, GAO Zhen-Heng
    1992, 13(10):  1251-1254. 
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    Nine of 4,4'-bis[2"-(5"-substituted phenyl oxazolyl)]-1,1'-biphenyl and three of 5,5'-bis(dimethyl phenyl)-2,2'-bioxazole were synthesized.Eight of them are new compounds.The relationships between the structures of these compounds and their electron spectra,laser conversion efficiencies were discussed.Some valuable conclusions were summarized.
    The Conformation of trans 1,2-Bis[5-(substituted phenyl)-oxazol-2-yl]ethylene
    XUE Jie-You, ZHANG Wen-Qin, WANG Ming-Zhen, LI Hui-Jie, GAO Zhen-Heng, LU Xiang-Jun, LIN Shao-Fan
    1992, 13(10):  1255-1257. 
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    Trans -1,2-bis[5-(2,4,6-trimethylphenyl)oxazol-2-yl]ethylene has been synthesized.The calculation of molecular mechanic force field (MMX program) for POEOP,2,5-dirnethyl-POEOP and 2,4,6-trimethyl-POEOPhas been performed.The structural parameters of POEOPdetermined consist with the MMXcalculation.Both two oxazole ring moieties are arranged in an-ti conformation which is stable than the syn one by 4.6 kJ/mol and the rotation energy barrier is ca.lculation 20.9 kj/mol.Besides,the relationship between the conformation and UVspectra of POEOPsystem has been discussed.
    Studies on Chemical Constituents of Artemisia Subdigitata Mattf
    SHI Yan-Ping, LI Yu, ZHANG Hui-Chang
    1992, 13(10):  1258-1261. 
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    Seventeen compounds were separated from the whole dried part of Arteisia subdigitata Mattf.and their structures were identified by spectrometry.Four of them are new flavanoids;5,8,3',5'-tetrahydroxy flavanone (1),5,8,2'-trihydroxy-5'-methoxyflavanone(2),5,7,4'-tri-hydroxy-3',5'-dimethoxyflavanone(3),3-(3-hydroxy)phenoxy-2-propenal(6);The others are known compounds;Tricin(4),Quercetin-3-rhamnoside (5).ethyl 2,5-dihydroxy cinnamiate (7),8-hydroxy-6,7-dimethoxy coumarin (8),2,4-hexadiyn-l-one (9),α-amyrin (10),β-amyrin (11),α-amyrin acetate (12),α-amyrone (13),fridelin (14),β-sitosterol (15),Te-tracosanoic acid(16) and n-butyl palmitate(17).
    Synthesis of Arylpyrazolinylvinyloxazolidinodihydroindoles and Their Chromophoric Properties
    MA Yin-Min, LI Zhong-Jie
    1992, 13(10):  1262-1264. 
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    The reactions of DMF/POCl3 with 1,5-diphenylpyrazoline,1,3,5-triphenylpyrazoline and l,5-diphenyl-3-styrylpyrazoline respectively afford three anticipated formylated compounds,which condense with l-hydroxyethyl-2,3,3-trimethyl-3H-indolium iodide,then are treated with base to give IVa,IVb and IVc,which have not been found in literature.The primary experiments show that the arylpyrazolinyl styryloxazolidino [3,2-a]dihydroindoles have halochromic and piezochromic property.The properties make them suitable for manufacturing the acid-sensitive film and using as the pressure-sensitive pigment.
    Studies on the Chemical Constituents of the Marine Mollusc, Siphonaria Japonia(Ⅰ)
    ZENG Long-Mei, YANG Dong-Bo, FU Xiong, SU Jing-Yu, WANG Qi-Wen
    1992, 13(10):  1265-1267. 
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    Four compounds,siphonarin A(1),glyerol-1-hexadecyl ether(2),cholesterol and oc-tadecylic acid,isolated from the marine pulmonate mollusc of Siphonaria japonia,were identified on the basis of the spectral data.These compounds are known but were found for the first time in the Siphonaria japonia.
    Studies of Tri (Substituted Silyl methylene)tin Unsaturated Carboxylates
    XIE Qing-Lan, XU Xiao-Hua, XIE Xiao-Juan, CHEN Chuan-Feng
    1992, 13(10):  1268-1270. 
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    Fourteen tri[(phenyidimethylsilyl)methylene]-(Ⅰ) and tri[(diphenylmethyisilyl) methylene]tin(Ⅱ) unsaturated carboxylates were synthesized by the reaction of corresponding bis(silylmethylene) stannoxanes with unsaturated carboxylic acids.The IR.1H NMR,119Sn NMR and 29Si NMR spectra of these compounds were studied.The data of IRand 119Sn NMRindicate that these compounds are four-coordinated monomeric organotin compounds.The miticide activities of these compounds depended on the substituted silylgroups.Compounds (Ⅰ) have a good acaricidal activity,but which become zero for compounds(Ⅱ).
    Phase Transfer Catalytic Conjugated Addition of α-Carbanion Contaning Phosphorus
    LIU Zeng-Xun, LIU Shun-Yao
    1992, 13(10):  1271-1273. 
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    This paper reports the formation of a-carbanions containing phosphorus from ethoxy carbonylmethyl phenyl phosphonate(I) and cyanomethylphenylphosphonate(I) under the conditions of solid-liquid phase tranfer catalysis,and thirteen new compounds synthesized by the conjugated addition between the carbanions and unsaturated carboxylates,as well as unsaturated cyanides.The structures of the new compounds were determined by elementary analysis and 1H NMR.The synthetic method is considered convenient and practicable for introducing desired functional groups through the conjugated addition of the compounds containg phosphorus as the acceptors under mild conditions.
    Acid-Base and Catalytic Properties of (K,Na)ZSM-5 Zeolites
    TAO Ke-Yi, GAO Feng, WEN Lang-You, CHEN Zhong-Ming, ZANG Ya-Ru, LI He-Xuan
    1992, 13(10):  1274-1278. 
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    The acid-base properties of a series of (K,Na)ZSM-5 zeolites with various contents Kwere investigated by IR,TPD,Hammett-Indicator non-aqueous titration and measurement of catalytic properties.The KOHexchanged ZSM-5 zeolites have moderate Lewis acid sites(cation,Na+,K+) and two different kinds of base sites,the weak ones (AlO4-or framework oxygen ions) and the strong ones(OH-).The acidity decreases while the basicity increases with increasing the concentrations of exchanging KOHsolutions.The samples exhibit higher catalytic activities for the dehydrogenation and dehydration of isopropanol.The catalytic properties correlate well with the acid-base properties.
    Structure and Pyroelectric Behavior of Azobenzene Derivative Langmuir-BIodgett Films
    YANG Jun, WANG Rong, WANG Hui, DONG Xi-Juan, TANG Da-Xin, JIANG Lei, LI Tie-Jin, ZHANG Bao-Wen, CAO Yi
    1992, 13(10):  1279-1282. 
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    Amphiphilic azobenzene derivative mono-molecular layer and multilayer were deposited on the glass substrate electroplated with metal film and the nonmetal CaF2 monocrystailine substrate by using Langmuir-Blodgett method.The orientations of transition moment and long axes of the molecule were studied by using infrared linear dichroic spectra.Orderly period structure of the films was researched by using X-ray diffraction method.The results obtained show that the high pyroelectric activity was related to the bi-period structure of the LBfilms was discussed.
    Studies on the Theory of Solvation Thermodynamics(Ⅴ)——A Theoretical Calculation of Solubility Product for AgCl and AgBrO3 in Mixed Solvents Containing Water
    WANG Feng-Yun, YE Jing-Xian, ZHANG Wei-Quan
    1992, 13(10):  1283-1286. 
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    By improving the formula about the dissociation equilibrium and the calculation process developed in the previous researches,we took the dissociation equilibrium of AgCl and AgBrO3 in a series of MeOH-H2O,EtOH-H2O,PrOH-H2O,Me2CO-H2O and DMSOH2O mixed solvents for examples in this article,and calculated the solubility product constants of the slightly soluble salts.The obtained values are in good accordance with those from literatures,
    Preparation of Nanocrystalline Materials of NiO by Colloidal-Method
    WANG Zi-Chen, ZHANG Li-Hua, Li Xi, XU Bao-Kun, ZHAO Mu-Yu
    1992, 13(10):  1287-1290. 
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    NiOnanocrystalline materials were prepared from NiCl2 and NaOHby the colloidal chemicai method.The most favourable experiment conditions for the preparation of NiOultrafine particles(UFP) were studied.XRD,IR,TG,DTAand TEMexaminations were used to characterize the samples.The spherical UFPparticle NiOis cubic crystal with an average diameter of 6.0 nm.
    Oxygen Atom Transfer Reactions of Metal Carbonyl Compounds——Kinetics of CO Substitution Reactions of Cr(CO)6 in the Presence of Substituted Iodosylbenzenes
    JIAO Xiang-Dong, FAN Wen-Ge, GAO Yi-Ci, SHI Qi-Zhen
    1992, 13(10):  1291-1294. 
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    The kinetic data are reported for the reactions between Cr(CO)6 and the entering lin-gands L(where L=CH3CN,PPh3) in the presence of substituted iodosylbenzenes R-C6H4IO to form Cr(CO)5L.The results indicate that the steric hindrance of substituents of R-C6H4IO increases the rate of the reactions,the reactivities decreases in the order;o-substituted>m-substi-tuted>p-substituted>unsubstituted.There is a good linear correlation between the rate of O-a-torn transfer reactions and the electronic factors of p-substituted iodosylbenzenes,and the electron-withdrawing substituents make the reaction faster,the reactivities of R-C6H4IO increase with weakening the I-Obond strengths at the similar steric hindrance.
    Studies on Thermokinetics(ⅩⅩⅢ)——Selected Peak-Height Method for the First Order Reaction
    WANG Rui-Lin, DUAN Zhi-Hua, ZENG Xian-Cheng, DENG Yu
    1992, 13(10):  1295-1298. 
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    In this paper in the light of a theoretical thermogram curve equation of the first order reaction,a novel data processing method is proposed,in which the rate constant is calculated from both selected peak-height without using any peak-area and other data.Therefore the problems arisen from the peak-area-computation or from the error in reading can be avoided.In order to test the validity of this novel method,the kinetics of the reaction between tri-ethylamine and ethyl iodide are investigated in DMSO,The rate constant calculated with this novel method is in agreement with those in the literature,and therefore the basic pnciples of this selected peak-height method are believed to be correct.
    The Characterization for Geometric Texture and Catalytic Properties of V-series Catalysts by Using Method of Fractal Dimension
    DUAN Shi-Duo, LIN Qiang, WANG Ji-Fen, ZHU Bin
    1992, 13(10):  1299-1301. 
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    The surface texture of heterogeneous catalysts was characterized by using the fractal theory method,computer image texture analysis technique,the catalyst for the oxidation of naphthalene to phthalic anhydride as the sample,and by changing the content of promoter K2SO4 and P2O5 in this paper.The experimental results show that the fractal dimension value Dchanged with the variation of the promoter contents and the yield of phthalic anhydride reached the highest value when Dvalue was maximum.
    Conversion of Methane and Carbon Dioxide into Synthesis Gas Rich in Carbon Monoxide
    SUN Xi-Xian, LI Xin-Min, LI Jian-Hua, FAN Ye-Mei, XU Heng-Yong, SU Yu, SHI Ke-Ying, XU Guo-Lin, HUANG Ren-Cai, ZHOU Pei-Heng, LIU Jin-Xiang
    1992, 13(10):  1302-1306. 
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    The thermodynamic properties of the conversion of methane and carbon dioxide were studied.The equilibrium constant of the reaction and the theoretical distributions of products were calculated in order to determine the operating conditions needed to inhibit carbon deposition.The catalytic activity of the conversion of CH4 and CO2 into synthesis gas over Ni/Al2O3 catalyst was examined by using a fixed-bed flow apparatus.It is found that CH4 and CO2 over Ni/Al2O3-3 catalyst has reached the theoretical equilibrium conversions,and the synthesis gas also reached the theoretical yield.The results indicate that Ni/Al2O3-3 catalyst has a high activity,selectivity and stability.
    Treating Extraction of Acetic Acid Aqueous Solution with Calcium Alginate Capsule
    ZHANG He-Zhe, WU Zi-Sheng, CHENG Ya-Ling
    1992, 13(10):  1307-1309. 
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    This paper reports the extraction of acetic acid from its aqueous solution by using calcium alginate capsule.The results show that this method has the advantage of quick extraction.However,it is revealed that the Kvalue is comparatively small and the capacity of extrection is limited.
    Kinetic Study of Substitution Reaction of Co2(μ-C2ph2)(CO)6
    JIANG Fa-Ming, WANG Be-Kang, XU Cong-Ying, HE Jin-An, CHEN Han-Wen, DAI An-Bang
    1992, 13(10):  1310-1312. 
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    The kinetics of substitution reaction for Co2(μ-C2ph2)(CO)6 with P(OBu)3 and PCy3 in decalin at 55° was studied.It is found that the reactions under the atmosphere of N2 follow two different mechanisms: dissociation and association mechanism,and the reaction rate can be represented by the equation: kobs=k1+k2[L].In addition,the dependence oi lgk2 on the basicity and the size of entering ligands is also discussed.
    Characterization of the Surface Texture of Catalysts for Naphthalene Oxidation to Phthalic Anhydride(PA) and Exploration of Surface Texture Model
    DUAN Shi-Duo, YANG Kui
    1992, 13(10):  1313-1314. 
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    The catalyst texture is one of the important features for characterizing catalyst properties.In this paper,the Image Texture Analysis Technique is introduced to analyze the SEM images of PAcatalysts in order to obtain the catalyst texture information.It is found that the texture entropy feature(F9) is in close relation with the activity of catalysts.An appropriate surface texture model corresponding to the high activity catalysts for the oxidation of naphthalene to PA is deduced as: The model is consistent with the results of activity evaluation andphysical chemistry analysis such as XRD,TPD-MS,ESR.
    Studies on Polysilyl-Arylene Siloxane(Ⅱ)——Synthesis of Poly(tetramethyl-p-silphenyiene Siioxane)
    LIN Si-Cong, LIU Xiao-Ning, WANG Zhi-Liu, TU Xiang-Tong
    1992, 13(10):  1315-1318. 
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    Poly(tetramethyl-p-silphenylene siloxane) (PMSPS) with Mw of 6.6×105 was synthesized by the ring-opening polymerization of dodecametliyl-cyeio-p-silphenylene trisiloxane (MSPTS) at 160℃ with potassium silanolate (0.01%)as the catalyst.The relationship between conversion of monomer or Mw of PMSPS and polymerization time indicates that under the mentioned polymerization condition,the MSPTSis active enough to polymerize and the ring-opening polymerization ss basically completed within half an hour.In addition,some properties of PMSPS,characterized by GPC,FTIR,1H NMR,13C NMR and TGA are also reported.The TGAresult shows that PMSPS has a much higher thermal stability than that of polydimethylsiloxane mrtety.
    Inhibiting Effect of Radical Polymerization of Vinyl Monomers(ⅩⅤ)——Studies on the Behaviour of Some Substituted Hydroxyl amines in the Copolymerization of Styrene with Aeryloititrile
    ZHANG Zi-Yi, LI Zhao-Long, YANG Mao-Lin
    1992, 13(10):  1319-1322. 
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    The behaviour of N,N'-diethylhydroxylamine (DEHA),N,N'-diisopropyl-hydroxylamine(DIPHA) and 4-hydroxylmorpholine(MPHA) as inhibitors of the copolymerization of styrene(M1) with acrylonitrile(M2) initiated by benzoyl peroxide,at 60℃ was investigated.The result showed that the three kinds of hydroxyiamines were proved to be the very efficient inhibitors and their relative inhibiting order was DEHA>MPHA>DIPHA.It was also found that the reactivity radios of St and ANare different for various inhibitors.When the a-mount of hydroxyiamines is about 500 ppm,r1 decreases and r2 increases and the azeotropic point of copolymerization of St-AN decreases from 0.62 to 0.55,0,54 and 0,57 for DEHA,DIPHA and MPHA respectively,showing an increasing tendency toward alternating copolymerization.
    Studies on Acrylamide-Dicyanodiamide Maeromer and Its Copolymer with Styrene(Ⅱ)——The Interactions of Copolymer with Methyl Orange and Its Homologue
    ZANG Qing-Da, LI Zhuo-Mei
    1992, 13(10):  1323-1326. 
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    The binding of amphiphilic copolymer P-M-St which consists of hydrophobic groups aiongs the mam chain and hydrophilic groups along the graft side chain and the condensation polymer of dicyanodiamide and formaldehyde D-Fwith methyl orange (MO) as well as the binding of P-M-St with MOhomologue ethyl orange (EO) and orange-W (Q-IV ) were studied thermodynamically by the method of equilibrium dialysis at 25,35,45℃ and 55℃.The equilibrium constant K1 and △H,△S,△G were obtained.It has been found that the binding ability of P-M-St is stronger than that of D-Fsince the former contains hydrophobic groups.The binding ability of dyes with P-M-St is in the order; O-IV>EO>MO,i.e.,the larger the hydrophobic group in dyes,the stronger is the binding ability.When urea or methanol is added,the hydro-phobic interaction of copolymer and dyes is destroyed,resulting in weakening the polymer-dye binding.After dyes interact with polymers,the λmax shifts to ultraviolet region.The stronger the hydrophobicity of environments in which dyes lie,the greater the displacement.
    Studies on the Rigid-Rigid Block Copolymers(Ⅰ)——The Structure and Properties of PEEK-PES Block Copolymers
    CAO Jun-Kui, SU Wen-Cheng, PIAO Ming-Jun, LIU Xin-Yu, WU Zhong-Wen
    1992, 13(10):  1327-1330. 
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    A series of block copolymers of polyetheretherketone (PEEK) and polyethersuifone (PES) were prepared by polycondensation of two oligomers.Some properties of the copolymers were investigated by DSC,TGA,WAXD,and dynamic viscoelastic measurement.The results show that for the copolymers in this study no phase separation is observed.The copolymers are crystalline polymers similar to PEEK,moreover Tg of a copolymer is about 20℃higher than that of PEEK,and they also have a better high temperature mechanical property.
    Synthesis of Silica-Bound Dithia-Aza Crown Ether Platinum Complex and Its Catalytic Property for Hydrosilylation of Olefins
    CHEN Yuan-Yin, MENG Ling-Zhi, LI Li-Ping
    1992, 13(10):  1331-1334. 
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    Di-(β-chloroethyl)allylarnine reacted with 3,6-dioxa-1,8-octamethylene dimercaptan in the presence of sodium ethoxide as condensating agent via.cyclizative condensation to give N-aliyl-l,7-dithia-4-aza-10,13-dioxa-cyclopentadecane.The latter was subjected to hydrosilylation with triethoxysilane,immobilization on furned silican,in sequence,and then reacted with potassium chloroplatinite.Anew type of organosilicon polymer-supported thia-aza crown ether and its platinum complex were obtained.It was found that this platinum complex was an efficient catalyst for the hydrosilylation of olefins with triethoxysilane.
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