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    24 October 1988, Volume 9 Issue 10
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    Articles
    Synthesis of Molybdenum 4,4′, 4", 4'"-Tetrasulfophthalocyanine and Its Fluorescence
    Huang peili, Liu Huoan, Liu Chenxi
    1988, 9(10):  983-986. 
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    A solid Phase synthetic method for Molybdenum 4,4′,4",4′"tetrasulfo-phthalocyanine and its fluorecsence spectra are given in detail. It was synthesised with triammonium 4-sulfophthalate,urea and Mo(V) hydroxide, boric acid and ammonium chloride were used as catalysts. Anal, calcd. for(C8H3N2SO3Na)4MoO2·4H2O: C34.28; H1.78; N 10.00; Mo 8.57, found C33.58; H 1.70; N 9.58; Mo 8.4. Confirmations from visual and infra-red spectra were made. The yield was 15%. Its fluorescence spectrum and effects of solvent and surfactant on the spectra were also studied. Its fluorescence quantum yield (φF 0.803) was found to be higher than that of znic tetrasulfophthalocyanine and is the highest one in all known transition metals. Hence the Molybdenum compound could play an important role in forming light energy conversion systems and fluorescent materials.
    Synthesis of B-ZSM-5 Zeolites in Slightly Acidic Medium
    Qiu Shilun, Pang Wenqin, Zhao Daqing
    1988, 9(10):  987-992. 
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    B-ZSM-5 type molecular sieve was synthesized by hydrothermal crystallization at 150-200℃ from mixture containing NH4F and tetrapropyl-ammonium bromide (TPABr) as template. pHvalues were 5~7. Because of the lack of alkaline metal hydroxide, NH4-form precursors were obtained and H-form B-ZSM-5 was directly yielded after calcination. After adsorption of pyridin the IRspectra showed the presence of both Lewis and Bronsted acid sites. SEManalysis indicated that the formation of large B-ZSM-5 crystals and its growth were pe'r-fect. Si substitution by Bled to a decrease of crystal size and of the length/width ratio. XRD, IR, XPS, DTAstudies on B-ZSM-5 proved that boron atom did situate in ZSM-5 framework.
    Successive Approximation Correction Method for Interelement Interferences in ICP-AES
    Tan Jinzong, Chen Xinkun, Ma Jinqiu
    1988, 9(10):  993-997. 
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    Various interelement interferences usually exist in the analysis of complex, multi- component samples by ICP-AES.The problem is how to look for an ideal course to correct them. Anew method named "Successive Approximation Correction Method" (SACM) is advanced in this paper. SACM is based on K-coefficient correction method, and can be described with the equation  Good results, whether major or trace elements, can be gained by the use of SACM. In the article SACMis proven, checked and evaluated.
    A Study of the Ultra-Sensitive Colour Reaction for Determining Trace Amounts of Silicon
    Li Shihe, Li Shengquan, Liu Changsong
    1988, 9(10):  998-1001. 
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    An ultra-sensitive colour reaction based on the multicomponent complex, of siliconvanadomolybdate blue-Rhodamine Bin aqueous phase has been investigated. The maximum absorption wavelength of the complex is at 595nm. Beer's law is obeyed for silicon in the range from o to 0.7μg/25mL. The apparent molar absorptivity is 1.10 ×106L·mol-1·cm-1 at 595nm. This method has been applied to,the determination of trace amount of silicon in different water with satisfactory results.
    Principle of A. C. Oscillo-Bipotentiometric Titrations(J)——The Theoretical Equation of the Fluorescent Potential Line
    Xu Weijian, Gao Hong(H. Kao)
    1988, 9(10):  1002-1005. 
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    The theoretical principle of A. C. oscillo-bipotentiometric titration is discussed. The theoretical equation of the fluorescent potential line has been derived for the case of a reversible couple titrated with another reversible couple on two similar Pt electrodes. Theoretical predictions consist with experimental results.
    Studies on New Inorganic Ion Exchangers Containing Phosphorous(Ⅵ)——The Study of the Radial Distribution Function of an Amorphous Stannic Hexametaphosphate
    Yao Xingdong, Yao Songnian, Liu Jinchun, Liu Liangbin, Cheng Jieke
    1988, 9(10):  1006-1010. 
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    The structure of an amorphous inorganic ion exchanger-stannic hexametaphosphate is postulated with radial distribution function (RDF) by X-ray diffraction. The ion exchange characteristic of the exchanger is; explained in accordance with this structural model.
    Research on the Formation of Excimer and Exciplex and the Solvent Effect
    Zhou Yimin, Wang Shenxiu, Gao Zhenheng
    1988, 9(10):  1011-1015. 
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    The fluorescence spectra of 4-(5′-p-biphenylyl oxadiazolyl-2′-) benzyl ω-biphenylyl polymethylene carboxylate (compounds 1-4) and their corresponding model compound 2-p-methylphenyl-5-biphenylyl-1, 3,4-oxadiazole have been determined. The-intensities of fluorescence increase as the increasing of concentration at first, then the intensities of fluorescence"decrease as the increasing of concentration. This phenomenon demonstrates that these compounds can form excimer. The experimental results show that they can form not only inter-molecular excimer but also intramolecular exciplex and triple exciplex.The fluoiesoence spectra of compounds. 1~4 in the solvents of different polarity, such as toluene, dioxane, and dichloro-methane, have been determined. The results of determination show that the intramolecular exciplex and the triple exciplex are readily formed as the increasing of the solvent polarity.
    1,3,2-Oxazaphospholidine Derivatives(Ⅱ)——Studies on Synthesis and Properties of 2-Diethylamino 3-Substituted Formyl-1,3,2-Oxazaphospholidines
    Yang Huazheng, Shao Jiushu, Wang Huilin, Chen Ruyu
    1988, 9(10):  1016-1022. 
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    Aseries of new 2-diethylamino 3-substituted formyl-1,3,2-oxazaphospho-lidine derivatives (Ⅰ) have been prepared by the reaction of tris (diethylamino) phosphine with N-(β-hydroxyethyl) substituted amides. When (Ⅰ) was refluxed with sulfur in benzene, its 2-thione derivative (Ⅱ) was obtained. Compound(Ⅱ) can also be synthesized directly in one pot without the separation and purification of intermediate (Ⅰ). The IR, 1HNMRand MSspectra of these compounds have been discussed.
    Studies on the Free Radicals Formed in the UV Photolysis Processes of Ferrocene and Its Amino-Methyl Substituted Derivatives
    Chen Dewen, Zhou Jianwei, Xu Guangzhi, Hong Renfang, Sun Lijun, Shi Shujian
    1988, 9(10):  1023-1028. 
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    Active radicals formed in the UVphotolysis of ferrocene and its amino-methyl substituted derivatives in CCl4 solution have been studied by means of spin trapp-ing-ESRtechnique. The results show that Ferrocene and substituted ferrocene are very sensitive to UVirradiation. As NDis used as trapping agent,the strong ESRsignals can be detected in photoreaction systems irradiated by UVfor only 1~3 min,but the strength of ESRsignals decay and disappear rapidly during less than 8 min and then the residual weak signal with 6 lines may be observed;when irradiation term is more than 3 min, noly 6 simple peaks may be observed.Therefore, The primary photolysis processes of ferrocene and its derivatives should produce free radicals(C5H5Fe)·, C5H5· and (C5H5Fe)·, (RC5H4)·, respectively. The active intermediate (C5H5Fe)· may be further decomposed to form C5H5· and Fe. The ESRspectrum with 25 linesmaybe is the signal of spin adducts (C5H5Fe-ND)·. The values of splitting con-stants for the spin adducts (RC5H4-ND)·, which may show ESRspectra with 6 lines, are nearly the same as for the spin adducts (C5H5-ND)·, then it can be concluded that the effect of substituent on the superfine splitting can't be observed. At the same time, three of the substituted ferrocenes can give out triplet ESRpeaks besides those 6 peaks, it means that there are two structural forms for spin adducts (RC5H4ND)·:
    Studies on the Synthesis of 5-(Substituted Phenyl) Thio-2,4- Diaminopyrimidines and Their QSAR of the Inhibition to E. coli DHFR
    Zhang Wensheng, Li Renli, Zhang Jundong, Martin Poe
    1988, 9(10):  1029-1034. 
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    Eight dihydrofolate reductase inhibitors, 5-(X-phenyl) thio-2,4-diamino-pyrimidines (X = 4′-NH2 and its hydrochloride; 4′-Ihydrochloride;4′-NHCOCH3; 4′-OH, 4′,-NNSCH3; 3′,5′- (Br)2,4′ -NH2 hydrochloride, 4′-OCH2CH3; 4′-OCH2CH2CH3), have been synthesized from 5-(4′-nitrophenyl) thio-2,4-diamino pyrimidine. Their inhibitory activities to E.coli MB 1428 DHFRhave been tested. All sixteen thiophenyl pyrimidines (eight of them were reported previously) have been correlated with Hansch analyses. The correlation equation shows that their inhibitory activities are linearly correlated with MR3,4,5 and bilinearly correlated with π3,4,5. MR′is, defined with a maximum value cf 0.79 which means the MRvalues of substitvents have to te trurcaled at the value of 0.79 when the substituent is larger than methoxy group, similar to the definition in the correlation of benzylpyrimidines.
    Kinetics and Mechanism of Oxygen Atom Transfer Reactions to Os3(CO)12 and Its Phosphine Substituted Derivatives
    Shen Jiankun, Gao Yici, Shi Qizhen, Fred Basolo
    1988, 9(10):  1035-1040. 
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    Detailed kinetic data are reported for the reactions of COsubstitution of Os3(CO)12 and Os3(CO)11L (where L = PPh3, AsPh3, P(n-Bu)3) in CH2Cl2-C2H5OH and CH2Cl2 respectively in the presence of Me3NO. The results indicate that the reactions follow associative rate law, that is, r = k2[complex][Me3NO], and are independent of entering ligand concentration. The effect of C2H5OH as solvent on the reactions has been investigated quantitatively. Reaction mechanism, structures of transition states and intermediates have been proposed. The ligand effects on the reactions have been discussed as well.
    A Study of UV Spectra of Ph-(SiMe2)n-Ph with π→π* Transitions
    Li Zhiru, Zeng Jun, Tang Yanbin, Sun Chiachung
    1988, 9(10):  1041-1046. 
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    The UV Spectra of Ph(SiMe2)nPh with n = 1,2,3,4,5,6 are analyzed by means of the EHMO-CI-SPIN-FREE method with four-orbital models.The first and the second absorption bands arise in essence from the π→π* transitions. Furthermore, the d atomic orbitals of silicon chain, which may play an important role in the red shift of first absoption bands, are discussed.
    A Study on the Interaction of Spectral Sensitizing Dye with Silver Bromide by Chronopotentionietry
    Shi Junying, Lu Hongqi, Yang Linchu
    1988, 9(10):  1047-1051. 
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    A chronopotentiometry technique for studying the interaction of spectral sensitive dye with silver bromide is described. This method is based on the principle that the transition time of the silver bromide will be reduced with increasing the amount of sensitizing dye-silver bromide inert compound.The experiment indicates that transition time and reduce potential of silver bromide are decreased by addition of the spectral sensitizing dye. The equilibirum constant of the spectral sensitive' dye-silver bromide inert compounds is computed.There are some relation sbetween the amount of the inert compound and the characteristic increasing emulsion sensitivity of the dyes.
    Studies of Copolymerization of Methyl Methacryl-aterMMA) and N-p-Tolylmethacrylamides(N-p-TMA)
    Dbg Youjun, Qi Daquan, Wang Xindeng
    1988, 9(10):  1052-1056. 
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    The N-p-Tolylmethacrylamide(N-p-TMA)was synthesized by the reaction of p-methylaniline with methacryloyl chloride in the presence of triethylamine.
    A Study on Component of Anionic Copolymerization of a-Methylstyrene and Butadiene
    Guo Shaohua, Zhou Kejian, Gao Ying, Ying Shengkang
    1988, 9(10):  1057-1062. 
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    The component of anionic copolymerization of α-methylstyrene (M1) and butadiene (M2), initiated -by BuEi-THF in cyclohexane, were investigated in detail. The copolymerization equation in the presence of various species, accompanied with depropagation during copolymerization,was derived. Both apparent monomer reactivity ratios γ1 and γ2,were dependent on [THF], and γ2 >>γ1,for example, γ1=0.049 and γ2=350 when [THF] =0.801M; γ1 =0.001 and γ2=220 when[THF]=0.06mol/L.
    Fluorescence Studies of Excimer Formation of Polyethersulphone (PES) Under Irradiating of Ultraviolet Light
    Zhang Lifang, Ma Rongjiu, Wu Zhongwen
    1988, 9(10):  1063-1067. 
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    This paper studied fluorescence spectra of polyethersulphone (PES) in N,N'-Dimethyl formamide. It is found that there is only normal monomer fluorescence peak in the range of concentration from 0.0004mg/mLto 1 mg/mLunder normal case. Whereas excimer can be formed when it was irradiated by 280nm light beam, and Ic/Im is dependent on the irradiating time.
    Complexes of Schiff-base-bis-Crown with the Lanthanoid Nitrates: Synthesis and Characterization
    Lu Yugang, Pan Ruiqi, Ren Dehou, Jiang Haiying, Yin Cuimei, Ma Jiangsheng
    1988, 9(10):  1068-1070. 
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    The behaviour of complexes formed betweeu 15, 15' -dimethylenedinitril-odimethylidynebis(2,3,5,6,8,9,11,12-octahydro-1,4,7,10,13-benzopentaoxacyclo-pentadecm) and lanthanoid nitrates Ln(NO3)3·nH2O(Ln = Y,Eu,Gd,Dy,Er,Tm,Yb,:Lu;n=3-4) have been investigated. The solid complexes having stoichio metric formula 3Ln(NO3)3·L·9H2O have been characterized by elemental analysis, IR, UV, TGand DSC. Their probable structures were conjectured.
    Studies on the Polisilicate Anions in the Liquid Phase During the Formation of ZSM-5 Type Zeolite
    Ma Shujie, Zhao Xuewei, Song Tianyou, Ding Hong
    1988, 9(10):  1071-1073. 
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    In the system of 15Na2O·Al2O3-50 SiO2·5TPABr·3000H2O, in which water glass was put as a source of SiO2. The changes in concentration of SiO2, and Al2O3 in the liquid phase of gel were investigated by the chemical analysis and ICP. The variations of amounts for various polysilicate anions in the liquid phase during the crystallzation of zeolite ZSM-5 were investigated by TMS-GLCand TMS-GPC. We used the electron micrograph to study particle size of solid phase. According to these results, liquid phase mechanism during the formation of ZSM-5 type zeolite has been proposed.
    Studies on Aminoalkylferrocene Derivatives (Ⅱ)--The Reactions for Palladium complex of N,N- Diefhylaminomethylferrocene with Olefins
    Zhang Lun, Xiang Jinfu, Wang Shuangli, Wang Jiying
    1988, 9(10):  1074-1076. 
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    In this communication we report on the synthesis of the palladium complex of N,N-diethylaminomethylferrocene, di-μ-chloro-bis(2-(diethylaminometh-yl)ferrocenyl)dipalladium, and its reactions with styrene, methyl propenate, and 2-ferrocenylpfopene. The palladium complex and all the reaction products, which have been identified by elemental analyses, IR, 1H NMRspectra, are 1,2-disubsti-tuted ferrocene.
    Spectrophotometric Determination of Trace Cobalt with the New Reagent 2-(2-Thiazolylazo)-5-diethylaminobenzoic Acid
    Shen Hanxi, Li lianjun
    1988, 9(10):  1077-1079. 
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    2-(2-Thiazolylazo)-5-diethylaminobenzoic acid (TAEB) was synthesized and studied as a new reagent for the spectrophotometric determination of trace amount of cobalt. Its acid dissociation constants both in the absence and in the presence of Triton X-100 were determined. In a pH2.6~4.8 medium TAEBreacts with cobalt (Ⅲ) ions to form a stable complex, exhibiting an absorption maximum at 672nm. The molar absorptivity was found to be 1.26×105dm3·mol-1·cm-1. The constituent of the complex was established as Co:TAEB =1:3. Interference from copper, nickel, iron and chromium ions and etc. can be eliminated by acidification with HCl after cobalt complex is formed. The method has been used for the determination of trace cobalt in steel and iron directly with satisfactory results.
    Simultaneous Differential Reaction-Rate Determination of Micro Phosphorus and Arsenic by the Method of Proportional Equations
    Zi Mingxian, Liu Hailan, Zhao Qinglan
    1988, 9(10):  1080-1082. 
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    The article describes a method of simultaneous determination of micro phosphorus and arsenic by differential reaction-rate method. The proportional coefficients of K3min(P),K3min(As), K9min(P) and K9min(As) in solutions containing 0.3755mol·L-1 of sulphuric acid and 0.4% ammonium molybdate at 65℃ are reported. The method described is suitable for simultaneous determination of phosphorus and arsenic in a ratio of (P:As) more than 1.5. The relative error and relative standard deviation are within 1.0%.
    Studies on Fluorination of Halopyridazinones
    Pei Wen, Lin Chengji, Tian Guanrong
    1988, 9(10):  1083-1084. 
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    This article reports a new method for preparing 4-fluoro-1,2-dihydro-pyridazinedione and the reaction of 4,5-dichloro-1-aryl-6(1H)-pyridazinones with KFin aprotic polar solvent. Ten new compounds of 4-fluoro-5-chloro-1-aryl-6(1H)-pyridazinones have been prepared.
    Heat Capacity and Phase Transitions of 2,2-Dimethyl-1,3-Propanediol Between 270 and 440K
    Zhang Zhiying, Zou Hong, Yang Menglin
    1988, 9(10):  1085-1087. 
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    The heat capacity of 2,2-dimethyl-1,3-propanediol was measured over the temperature range 270 to 440Kby means of an automated adiabatic calorimeter. Asolid-solid and a solid-liquid phase transitions were found at (314.8 ± 0.1) Kand(403.3±0.1)K.The enthalpies and entropies of these transitions were determined to be (12.41±0.1) kJ·mol-1 and (39.4±0.3)JK-1·mol-1 for the solid -solid transition, and(4.44 ±0.1) kJ·mol-1 and (10.5±0.1)JK-1·mol-1 for the solid-liquid transition. Cp,m at 298.15Kis 183.18 JK-1mol-1.
    Researches on Reduction of Sulfur in Organic Medium by Controlled Potential Coulometry
    Xie Naixian, Huang Yixiang
    1988, 9(10):  1088-1090. 
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    The controlled "potential coulometry is suitable for examining the effects of slower reactions coupled to the electron transfer process such as in sulfur-DMSOsystem, since the time window of this method is longer. The theorietical treatment for the first step of sulfur reduction was completed, while the working curve of T1/2 -lgr that allowst he determination of apparent rate constant for reaction S82-= S62-+ (1/4)S8 with a value of k=6×10-3s-1 was given. In the second step of sulfur reduction, the electrolysis curve with almost a horizontal at begining and a wave shape at some later were found. The experimental phenomena were explained on the base of results obtained previously.
    Quantum Chemical Studies(PPP Method) of Some Properties of Organic Reagents(Ⅱ)
    Li Menglong, Zhang Kaicheng
    1988, 9(10):  1091-1093. 
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    Fluorone photometric reagent series have been studied with a computer program of PPPmethod for the electronic structures, and photometric properties of the organic reagents determined by experiments were compared with the calculated results and a good agreement was found. Some rules were presented by analyzing the calculated results. The conclusion indicated that substituent effects on the photometric properties of reagents and their metal complexes are not obvious.
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