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    24 February 1988, Volume 9 Issue 2
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    Articles
    The Synthesis and Properties of Novel Molecular Sieves CFAP-5 and CFSAPO-5
    He Heyong, Long Yingcai
    1988, 9(2):  103-107. 
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    A novel type of A1PO4 molecular sieves named CFAP-5 and silicophosphoalu-minate molecular sieves named CFSAPO-5 were synthesised hydro thermally in the system of Pr32O3-P2O5-H2Oand Pr3N-Al2O3-P2O5-SiO2-H2Orespectively. The molar composition of reactants is. Pr3N:Al2O3:P2O5:H2O = 1:(1~1.2):1:(40-80) for CFAP-5 and Pr3N:Al2O3 :P2O5:SiO2:H2O =1:(1~1.2): 1: (0.5-2): (40-80) for CFSAPO-5. Dipropylamine can also be used as "template". According to the study of XRD, 1R, TG, DTAand adsorption, the original product of CFAP-5 was changed into a form of molecular sieve after cal-cined at a range of 300-450℃ and CFSAPO-5 at a range of 300-600℃ respectively. The largest free dimension of adsorption window is 4.4-4.9A.
    Kinetic Studies On the Extraction of Uranium(Ⅳ) from Hydrochloric Acid Solutions with HDEHP
    Zhou Zuming, Mao Jiajun, Zhi Min, Qin Qizong
    1988, 9(2):  108-112. 
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    The kineties of extraction of uranium (Ⅳ) from hydrochloric acid solutions with HDEHPin cyclohexane have been investigated using the single drop technique. The effects of the concentrations of U(Ⅳ),H+ and HDEHP on the extraction rate for U(Ⅳ) have been examined. It is found that the extraction rate is proportional to [U(Ⅳ)] and [(HDEHP)2](0)1/2 but there is no effect with hydrogen-icn concentration in the aqueous solution.The extraction rate was found to increase with the increasing temperature and the apparent activation energy is 41.7 kJ·mol-1 between 10~40℃.It is suggested that the rate-controlling step may be the chemical reaction of U4+ with HDEHP monomer at the liquid-liquid interface.
    Syntheses and Structures of Rare Earth Picrate Hydrates
    Tian Yongchi, Liang Yingqiu, Ni Jiazan
    1988, 9(2):  113-117. 
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    Fifteen rare earth picrate hydrates have been synthesized in the reaction of RE2O3 with picric acid. Some results of elemental analysis, vibrational spectra, XPS, thermal analysis and lattic parameters are reported, and molecular structures and properties have been discussed.
    Atomic Absorption Spectrophotometry for Indirect Determination of Trace Iodide by Solvent Extraction of Neocuproine-Copper(Ⅰ)·Ⅰ-System
    Hou Yonggen, Lin Shuchang, Chi Xizeng
    1988, 9(2):  118-122. 
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    The formation and solvent extraction conditions of bis(neocuproine)-copper (Ⅰ)·Ⅰ- ion-pair as well as the composition of ion-pair and its effect on determination sensitivity were studied. Furthermore; we investigated origin of the absorption peaks and the composition of ion-pair was proved by using the solvent extraction spectrophotometry. It was applied to the determination of trace iodide in normal human serum and boiled kelp solution. The results are satisfactory.
    The Adsorptive-Complex Wave of Gopper(Ⅱ)-Imidazole System
    Lin Sauchang, Hu Naifei
    1988, 9(2):  123-127. 
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    A new system of Cu(Ⅱ)-Imidazole for the determination of trace copper by polarography is proposed.In a supporting electrolyte containing 0.2mol/L NaOH,a sensitive adsorptive-complex wave of this system was obtained by single-sweep polarography.The peak potential of the polarographic wave was -0.59V vs.SCE. The linear relationship between v/ave height and the concentration of coppre held in the range of 3.1×10-8~1.6×10-6mol/L.This method has a better selectivity for it is satisfactory in the determination of trace copper in waste water or surface water.The character of the polarographic wave was studied by cyclic voltammetry, normal pulse polarography and some other methods. The results indicated that the polarographic wave is an adsorptive wave of complex with weakly adsorbed reactant. The .adsorptive species is Cu(Imid)32+, which was inferred from contrast experiment with the. theoretical calculation.
    Preface
    Study on Organo-Iodoso Compounds(Ⅲ)——The Correlation Analysis of IR Vibration Frequency of IO Group in the Substituted lodosobenzene to the Substituent Constant
    Zhu Shenjie, Zhang Chunhao
    1988, 9(2):  128-133. 
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    Two characteristic absorption peaks for I-O group of some substituted iodosobcn-zencs were identified in the region 320-625cm-1 by comparing the IR spectra of the substituted iodosobenzenes with corresponding substituted iodobenzen.es. These two peaks could be assigned to asymmetric vibration vas and symmetric vibration vs of group in the polymeric structure of these iodosocompoumds. The cor-relation of vIO to the substituent constants σ1,σR0 and Es was studied by linear regression analysis. The linear regression equations of the para substituent and meta substituent were obbtained as follows:para: vIO= ρ1σ1+ρRσR0+C meta: vIO= ρ1σ1+ρRσR0+SEs+C
    Articles
    The Synthesis of 2-Amino-1-Phenylpropanes
    Su Jingyu, Zheng Yishen, Wu Jianqing, Tang Ganming, Zeng Longmei
    1988, 9(2):  134-139. 
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    2-Amino-1-phenylpropanes are useful ideal appetite depressants. Among them, 2-N-ethylamino-1-(m-trifluorornethyl)pheny]propanc (Fenfluramine) is most important.Aconvenient method for the syntheses of these compounds is described in this paper. With benzyl methyl ketone as intermediate, the target compounds were successfully obtained from reductive amination reaction in quite reasonable yields. According to the 1HNMR,it was found that the product yielded by the approach of Y.A.Larionova[4] was :not 2-N-ethylamino-1-(m-trifluoromethyl)phcnylpropane but its rearranged isomer. The stepwise rearrangement products was carefully examined by 1HNMRand some improvement in amination was reported.
    Study on the Kinetics of β-Cyclodextrin-Catalyzed Hydrolysis of Phenolic Esters Containing a Ferrocenyl Group——A Probe to the Substituent Effects
    Zhang Daodao, Liang Guibai
    1988, 9(2):  140-143. 
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    In this work, we have determined the pKα valuc of 4-nitro-2, 3, 5, 6-tetrafl-uorophenol and studied the relationship between pKα and the acceleration rales of β-cyclodextrin-catalyzed hydrolysis of subslituled phcnyl esters of trans-fcrrocenc-acrylic acid and ferrocenylcyclopropanccarboxylic acid.It has been found that the acceleration rates are dependent on the electronic nature of the substituents. It obeys Hammett linear free-energy relationship since the phcnyl. groups of subslratcs do not enter but the fcrroccnyl groups enter the cavities of the β-cyclodextrin.
    A Theoretical Study of the Electronic Structures and Stabilitieis of Transition Metal Triple-Decker Sandwich Complexes
    Yu Hengtai, Yang Zhongzhi, Wang Zhizhong, Zhu Yukui
    1988, 9(2):  144-148. 
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    The relationship between electronic structrucs and stabilities of transition metal triple-decker sandwich complexes was analysed and discussed.By the use of the level of metal dxz (or dyz) orbital in combination of the fragment CpMM'Cp as a standard value, if the HOMO πlevel in the penta- or hexa-coordination ring is near to or higher than this value, the complex would exist stably; on the contrary, if this π level is lower than this value,the complex would not exist stably. The results arc satisfactory for 8 different middle coordination rings. The effects of substituent group in the middle coordination ring are also discussed. We hope that these conclusions are able to guide further the syntheses of transition metal triple-decker sandwich complexes.
    An Ab Initio Study on the Structures and Properties of the Series of Methylenimine in Gas-Phase
    Dai Shushan, Ma Zhongxin, Wang Meixing
    1988, 9(2):  149-152. 
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    The series of methylenimine (H2C=NR) in gas-phase was studies by the Hartree-Fock SCFab initio method. Based on the 3-21Gor STO-3Gbasis sets, we optimized the geometries of those molecules. Upon the optimized geometries, molecular energies, charge distribution and acidity were calculated on the bases of 3-21G. For certain related reaction, we approximate the enthalpy change (△H) by energy change (△E) of the RHF/3-21Gand CID/3-2lG。 the calculated results are found to be very close to the thermochemical data and experimental acidity.
    Surface Acidity of Chromia-Promoted Magnetite Shift Catalyst
    Yang Shangrun, Xu Weixing, Fu Xiancai
    1988, 9(2):  153-156. 
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    The surface acidity of chromia-promoted magnetite shift catalyst, (Fe,Cr)3O4, was studied by TPDtechnique. The experimental results revealed the variability of surface structure of the catalyst. The adsorption of pyridine rearranges the surface structure and accelerates the establishment of a stable adsorption state of pyridine on the surface.There exist mainly two kinds of acidic site, α and β,on the surface of catalyst. The content of surface oxygen of the catalyst treated by COat higher temperature will be lower and the TPDpeaks of pyridine absorbed on the catalyst, which had been treated by COat different temperatures, varied regularly: the higher the treated temperature, the taller the peak α and the shorter the peakβ. This fact in combination with the shape and the position of peaks α and β had led to the conclusion that the peaks α and βare relative to Fe2+ site snd Fe3+ site, respectively.The activation energy of desorption of pyridine, Ed on the site βhas been determined by consulting table method. Its value is 278.8 + 13.8kJ/mol.
    Several Conclusions Concerning Diffuse Functions
    Liu Chengbu, Deng Conghao
    1988, 9(2):  157-162. 
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    Several conclusions drawn from the useg of diffuse functions in the ab initio study of molecular ations have been discussed .The orbital exponents of the diffuse functions for some basis sets have been determined by using the method of linear fitting. These values are nearly identical with those obtained by method of optimization.
    The Breakage Mechanism Study of Containing Oxygen Organic Compound by IR Laser
    Guo Guangsheng, Gu Yuezhu, Guo Ypngyou, Yin Yongjia
    1988, 9(2):  163-167. 
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    Using TEA CO2 laser as excitation source, we have studied the processes of multiphoton dissociation of propylene oxide (PO), tetrahydrofuran (THF)and diallyl ether (DAE). It was obtained that the dependence of dissociation yield on laser energy-density. We propose a mechanism involving breakage of the C-Obond in PO, THFand DAE. We found that the initiative step of dissociation in these moleculae is breakage of the weaker C-Obond. The threshold energy is about 0.8J/cm2.
    The Application of FT-IR-EMS Method in the Study of the Dynamics of PEP/PU IPN Formation
    Ma Song, Tang Daxin, Li Yuwei, Zhang Jun, Zhang Donghua, Tang Xinyi
    1988, 9(2):  168-171. 
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    The FT-IR emission spectra(FT-IR EMS) of IPN during polymerizationunder 140℃ are measured using modified 5DX FT-IR spectrometer. The reactionextents and kinetic constants are calculated by peak-area ratio method. "The results show that both the polymerization of EPOand the formation of PUare firstorder reaction and kepo=0.035, kepo in IPN= 0.10, and kPU=0.15. The relation between reaction and structure is discussed. The results show that FT-IR EMSis an effective technique in the study of polymer reaction kinetic.
    Free Radical Ring-Opening Polymerization of 4-Methylene-1,3-Dioxolane and It's Derivatives (Ⅰ)——The Investigation of Polymerization Mechanism of 4-Methylene-2-Phenyl-1 ,3-Dioxolane
    Pan Caiyuan, Wu Zheng, Huang Weiyuan
    1988, 9(2):  172-177. 
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    This paper describes the synthesis of the monomer,4-methylene-2-phenyl-1 ,3-dioxolane. Unlike 4-methylene-1 ,3-dioxolane and it's derivatives, it can be initiated by free radical initiators, such as DTBP, BPOand AIBN. Upon the investigation of JR, 1H NMRand 13C NMR spectra of the polymer, it is found that a copolymer with repeating units Ⅳ,Ⅴ and Ⅵ is obtained. Based on this study, the polymerization mechanism of the monomer is discussed.
    Studies on Segmented Polyester Polyurethane Block Copolymers and Their Zwitterionomers
    Yang Changzheng, Gu Xuerong, Mao Xiaoli, Lu Xingjun, Chen Nandou
    1988, 9(2):  178-183. 
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    Aseries of segmented polyester polyurethanc block copolymers based on poly (ethylene-prOpy]ene)adipate(PEPA),4,4' -methylene diphenylere diisocyanate (MDJ) and N-methyl-diethanolamine were synthesized. Their zwittcrionomers in different degrees of ionization were prepared by quaternization of the tertiary arrine with γ-propane sultone. The effects of hard segmente contents and degrees of ionization on the extent of microphase separation and physical properties were studied by IRspectrometry, differential scanning calorimetry, dynamic mechanical spectroscopy, dielectric measurement and stress-stain analysis.The reason which causes the change of morphology was discussed.
    The Growth of Large Single Crystals of Molecular Sieves ZAPO-5 and MnAPO-5
    Han Shuyun, Yang Chuncai, Zhou Jianrong
    1988, 9(2):  184-185. 
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    The large single crystals of molecular sieves ZAPO-5 and MnAPO-5 were synthesized in the presence of fluride ions.The growthes of ZAPO-5 and MnAPO-5 arge single crystals were investigated in the systems of F--C6H15NO-P2O5-Al2O3-ZnO-H2O and F--C6H15NO-P2O5-Al2O3-MnO-H2O.
    Synthesis and Characterization of a Novel Crystalline AlPO4 Molecular Sieve CFAP-6
    Long Yingcai, Dong Lingzhen, He Heyong
    1988, 9(2):  186-188. 
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    A novel crystalline aluminophosphate CFAP-6 was synthesized hydro thermally in a system of di-n-butylamine-(NH4)2O-P2O5-Al2O3-H2O, the P2O5 and Al2O3 sources of which were (NH4)3PO4·3H2Oand Al2(SO4)3 aqueous solutionrespectively.The mole ratio composition of rcactant was: di-n-butylamine/(NH4)2O/P2O5/Al2O3/H2O = (1~1.2)/(3~3.6)/(l~1.2)/l/67.The reaction is conducted at 200℃. Investigations of DTA, XRD, IRand the adsorption experiment show that transformation of the raw powder (phase a) into more stable crystal form (phase b) with properties of molecular sieve, on heating at 350℃ and giving H2O and amine(or ampnia) off. Isotherms for the adsorption of H2O and CH3OH at 23℃ indicate that the dimension of the adsorption window of CFAP-6 is between 4.3 and 4.9Å and the. capacity about 0.07mL/g.
    A Graphic and Regressive Method for Linear Titration with Computer
    Xu Shushen, An Zhe, Li Feng, Liu Sidong
    1988, 9(2):  189-191. 
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    In the linear titrations, two methods arc commonly used, the graphic method and the calculating method. The present paper describes a new method on the basis of the graphic method, namely, graphic regressive method. According to this mcthod, the graphs are drawn by microcomputer, and the results are obtained by the use of linear regression equations. Thus, the present method saves both time and labour compared with the former two methods. By appling this method to determine several very weak acids and weak acid mixture,we obtained satisfactory results in all cases.
    Studies on Atomization Process in Graphite Furnace Atomizer (Ⅲ)--Atomization Mechanism of Germanium in Graphite Furnace
    Zheng Yansheng, Zhang Dalei
    1988, 9(2):  192-194. 
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    The atomization mechanism of germanium is discussed on the basis of observation of atomization behavior of germanium and enhancement effects of HNO3, HClO4 and organic compounds on absorption signal of Ge in graphite furnace. It is affirmed that two types of reduction reaction in atomization process are existed.GeO2(s)+C→GeO(g)+CO and GeO2(s)+CO→GeO(g) +CO2 .The appearancetemperature of Ge experimentally was measured to be 2150K.The △H° value of Ge is 138.5 kcal/mol calculated by using △H° =γTapp.It is corresponding to the dissociation energy of the Ge-Obond(l58.8 kcal/mol). The germanium atoms in vapor phase are formed which is due to the thermal decomposition of GeO(g).
    Determination of Micro Organo-Fluorides in Waste water by Head-Space Gas Chromatography
    Jin Xinrong, Shen Shujuan, He Ping, Chang Wenjuan
    1988, 9(2):  195-197. 
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    In this paper, Head-Space Gas Chromatography is used to determine micro organo-fluorides in wastewater. We designed an equilibrium bottle and inspected the influences of salt effect, equilibrium time and equilibrium temperature on the result. Minimum detectable concentration for octafluorobutylene is 0.01 ppm. Qualitative determination of organo-fluorides in wastewater was performed with GC/MS.
    Studies on the Constituents of Saussurea Involucrata Kar. et Kin(Ⅳ)
    Jia Zhongjian, He Kangwei, Du Mei, Li Yu, Chu Tse-Tsin
    1988, 9(2):  198-200. 
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    Two crystals have been obtained from soussitrea involucrata Kar. et Kin. These were identified as 11α, 13-dihydrodesacylcynaropicrin and quercetin-3-O-α-L-rhamnoside.
    The Catalytic Effect of Bis-(Acetylacetonato) Cobalt in Organic Reactions (Ⅲ)——The Reaction of α,α,α-Trichlorotoluene with Alcohol
    Chen Weixing, Fu Heliang, Shang Yun, Hu Hongwen
    1988, 9(2):  201-202. 
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    In the presence of catalytic amount of bis-(acelvlacetonato) cobalt α, α,α-trichlorotoluene reacis with alcohols to give alkyl benzoates and chlorides in 92.7-53.8% and 97-32.6% yields, respectively.
    A New Synthesis of 4-Hydroxyindole
    Liu zhibin, Yang Shiying, Zhu Chunsheng, Gao Jiyu(Kao Tsiyu)
    1988, 9(2):  203-205. 
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    4-Hydroxyindole is an important intermediate in the synthesis of psilo-cyben(Ⅰ) and psilocin(Ⅱ), Anew synthesis of 4-hydroxyindole has been accomplished. This synthetic route leaving out the decarboxylation step gives much better yield.
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