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    24 April 1983, Volume 4 Issue 2
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    Articles
    SYNTHESIS AND PROPERTIES OF NEW CHELATING REAGENT-1-PHENY L-3-METHYL -4-HEPTAFLUOROBUTYRYLPYRAZOLONE-5
    Li Juyuan, Yang Rudong
    1983, 4(2):  141-144. 
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    New chela ting reagent-l-phenyl-3-methyl-4-heptafluorobutyrylpyrazo-lone-5 was synthesized and characterized by elemental analysis,mass spectra, infrared and ultraviolet spectra as well as thermogravimetric and differential thermal analysis.The dissociation constant has also been determinated.
    STUDY ON THE SYNTHESIS AND PROPERTIES OF THE SOLID COMPLEX COMPOUNDS OF RARE EARTH ELEMENTS WITH1-PHENYL-3-METHYL-4- HEPTAFLUROBUTYRYL-PYRAZOLONE-5
    Li Juyuan, Yang Rudong
    1983, 4(2):  145-151. 
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    The complexes of rare earth elements (except Pm) and 1-phenyl-3-methyl-4-heptaflurobutyryl-pyrazolone-5 have been prepared in solid state and characterized by elemental analysis,infrared and ultraviolet spectra, as well as thermogravimetric (TG) and differential thermal analysis (DTA). Their composition is LnA3·HA (LnA3 for Lu). Besides, the possibility of some other solid complex compounds has also been tried as a shift reagent in nuclear magnetic resonance spectrum.
    EXTRACTION OF CALCIUM AND COBALT (Ⅱ) FROM SULPHATE SOLUTION WITH HDEHP IN VARIOUS DILUENTS
    Fu Xun, Jiang Dehua, Shen Jinglan
    1983, 4(2):  152-158. 
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    The distribution of Ca, Co (Ⅱ) between aqueous sulphate solution and HDEHPin n-hexane, kerosene, cyclohexane, carbon tetrachloride, methyl isobutyl ketone, toluene, benzene and chloroform has been studied at 25±1℃ respectively. The composition of the extracted species and the extraction constants were calculated and tabulated for different diluents. The distribution ratios decrease in the following order of diluents. n-hexane>kerosene >cyclohexane > carbon tetrachloride > methyl isobutyl ketone >toluene> benzene>chloroform.The results were discussed with the Lewis acidity and the solubility parameter of the diluents respectively.
    A STUDY ON THE PHASE DIAGRAM OF TERNARY SALT SYSTEM BeSO4-Al2 (S04)3-Na2SO4
    P. I. Fedorov, Zhang Qiyun
    1983, 4(2):  159-162. 
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    Astudy has been made of ternary salt system BeSO4-Al2(SO4)3-Na2SO4 by the thermal analysis method. A ternary peritectic point containing BeSO4 18.8 Wt%, Al2(SO4)3 15.0%, Na2O4 66.2%, melting at 490℃and a ternary eutectic point containing BeSO4 20.0%, Al2(SO4)3 11.2%, Na2SO4 68.8%, melting at 475℃, were found in this system. The composition of the other ternary eutectic point melting at 595℃has not been exactly determined. No evidence was found about any ternary compound existing in the system.
    A STUDY ON THE BINARY SALTS SYSTEMS Li2SO4-MgSO4 AND LiNO3-Mg(NO3)2
    Zhang Qiyun, Lu Jingzhi, Sun Shuren
    1983, 4(2):  163-166. 
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    Astudy has been made of the binary salts systems Li2SO4-MgSO4 and LiNO3-Mg(NO3)2 by the visual polythermal and DTA methods. An incon-gruently melting compound Li2SO4·2MgSO4 occurring at 832℃ was found in the Li2SO4-MgSO4 system. The eutectic point between Li3SO4 and Li2SO4·2MgSO4 occurring at 647℃ lies in the composition of 23.6 Wt% MgSO4. The values of eutectoid are 4.2% MgSO4 and at 552℃. The system LiNO3-Mg(NO3)2 is of a simple eutectic type, the eutectic point occurring at 200℃ contains 47.3% Mg(NO3)2. No solid solution existed on the both sides of LiNO3 and Mg(NO3)2.
    THE MECHANISM OF THE FORMATION AND THE CRYSTAL GROWTH OF MOLECULAR-SIEVE-ZEOLITE (Ⅵ) ——Liquid Phase Mechanism Followed arid the Heterogeneity of Compositions Si-Al Ratio in the Course of the Formation of NaY Type Zeolite
    Xu Ruren, Zhao Jingping
    1983, 4(2):  167-172. 
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    The changes in concentrations of the components SiO2 and Al3O3 and in weight average molecular weight (Mw) of SiO2 as a function of the crystallization time in the liquid phase of gel were investigated by using chemical analysis and low angle laser light scattering methods respectively. Results have shown that the formation of NaYtype zeolite follows the liquid phase mechanism. The existence of the microcrystal of NaY type zeolite in the liquid phase of gel in the course of the crystallization of NaYtype zeolite was proved by the experiment of electron diffraction.By means of determining by X-ray powder diffraction the silica-alumina ratio and its change of NaYtype zeolite presented in the crystal phase at the intervals of crystallization time, it has been found that the silica-alumina ratio of the NaYtype zeolite formed in the course of crystallization decreases gradually with the rucleation and crystal growth of NaYtype zeolite, which show the heterogeneity of the composition silica-alumina ratio of the NaYtype zeolite formed in the course of crystallization.
    POLAROGRAPHIC ADSORPTIVE WAVE OF CADMIUM-MESO-TETRA (4-TRIMETHYLAMMON-IUMPHENYL) PORPHINE COMPLEX
    Luo Dengbai, Gao Jinsong, Wu Xuanjie, Zhao Zaofan
    1983, 4(2):  173-178. 
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    The polarographic adsorptive wave of cadmium-meso-tetra(4-trimethyl-ammoniumphenyl) porphine (TTAPP) complex in sodium hydroxide solution has been studied. Ep=-1.23V (vs.SCE). The detection limit is 2×10-8M. The peak height is linearly proportional to cadmium concentration over a range of 0.002 to 0.8μg ml-1. In the presence of masking agents tartrate and ethylenediamine, more than 30 species of ions at certain concentration range do not interfere the determination. This method has been applied to the determination of trace amounts of Cd in fresh water, electroplating waste water and aluminium alloys. The mechanism of adsorptive wave has been discussed. The composition of Cd-TTAPPcomplex has been studied by "polarographic mole-ratio method". The results show that the Cd:TTAPPin complex is 1:1, the conditional stability constant of complex is β'= (7.7±0.6)×107. It agrees well with the results of spectrophotometry which Cd; TTAPP = 1:1 and β'=9.2×l07.
    ATOMIC ABSORPTION SPECTROSCOPIC ANALYSIS OF Cu, Zn, Cd IN NATURAL WATER USING PAN- POLYURETHANE FOAM FOR PRECONCENTRATION
    Zhou Zhirui
    1983, 4(2):  179-184. 
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    This paper describes a method of solid-liquid extraction to replace the conventional solvent extraction, using FANloaded polyurethane foams in batch and column operation for preconcentration of the trace Cu, Zn, Cd in aqueous solution. The effects of pH, various anions in batch method and flow-rate in column process on the extraction behavior of Cu, Zn, Cd have been investigated. Preconcentration of Cu, Zn, Cd ions from natural water is successful.
    STUDIES ON MECHANISM OF INTERREACTION OF SOME CYANOFORMAZAN DERIVATIVES WITH SURFACTANTS
    Yu Ruqin, Feng Yaping
    1983, 4(2):  185-188. 
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    The effect of surfactants on the absorption spectra of 1,5-bis-(2-hydroxy-5-chlorophenyl)-3-cyanoformazan (HCPCF) and l,5-bis-(2-hydroxy-5-sulfo-phenyl)-3-cyanoformazan (HSPCF) and their metallic ion complexes has been investigated. The mechanism of the difference in the interreaction of HCPCFand HSPCFand the corresponding complexes has been interpreted by analysing phenomena concerning electrophoresis and phase separation. For HCPCFand its complexes, the direction of migration under electric field is determined by the charge of the micelle. The presence of Tween-80 has no effect on the migration direction of HSPCFand its complexes, while TPCreverses the migration direction of HSPCFand its metallic complexes. On the basis of these phenomena it has been shown that HCPCFand its complexes can enter into the micellar phase of both cationic and nonionic surfactants, on the other hand HSPCFas well as its complexes can not enter into the micelle of nonionic surfactants. This conclusion has been confirmed by phase separation experiments above the cloud point. The effect of surfactant micelles on the complex formation reaction rate has also been discussed.
    EXTRACTION OF NOBLE METALS WITH BIS- (n-OCTYLSULFIDE) ETHANE——STUDY ON THE EXTRACTION OF PALLADIUM AND ITS MECHANISM
    Shao Pinxi, Chao Chengchun, Gui Mingde, Can Weitang
    1983, 4(2):  189-193. 
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    In this paper the extraction of palladium with bis (n-octylsulfide) ethane [C8H17S(CH2)2SC8H17) has been studied. The effect of concentration of hydrochloric acid and diluent has been discussed. It was shown that bis (n-octylsulfide) ethane is highly effective extractant of palladium from hydrochloric acid medium. Compostion of extracted complex was established by method of isomolar series and of saturation, Asmus's me -thod and chemical analysis of solid complex and found to be Pd: bis (n-octylsulfide) ethane = 1:1. Study on the nuclear magnetic resonance spectrum and infrared spectrum indicated that bis (n-octylsulfide) ethane is coordinated to palladium through sulphur to form five-membered neutral chelate complex.
    STUDIES OF LIQUID CRYSTALS USED AS STATIONARY PHASES IN GAS CHROMATOGRAPHY(Ⅱ) ——CHROMATOGRAPHIC BEHAVIOR OF SOME MIXED LIQUID CRYSTALS
    Chen Yaozu, Chen Shizhi, Ma Xueyi
    1983, 4(2):  194-200. 
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    In present paper, chromatographic behavior of mixed liquid crystals used as stationary phases in GC has been studied. Their dependency on the temperature, the stability of supercooled state were compared with those of the homo-liquid crystals. The phase constants, relative polarity of some liquid crystals and their mixtures were determined. In general, the resolving powers of mixed liquid crystals are better than that of corresponding homo-liquid crystals.On the packed and the glass capillary columns coated with a mixed liquid crystal, some natural essential oil and synthetic mixtures have been separated.
    N-MANNICH BASES OF NORCANTHARIDINIMIDE AND ANALOGS
    Chen Guangxu, Zhao Xinqi
    1983, 4(2):  201-206. 
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    Norcantharidinimide, 7-oxabicyclo [2, 2, 1] heptane-2,3-dicarboximide and its deaydroderivative, 7-oxabicyclo [2,2,l]-hept-5-ene-2, 3-dicarboxi-mide, were found to readily undergo Mannich reaction with primary or secondary amine to form N-Mannich bases in good yields. Thirty-five N-Mannich bases of this type were prepared from both aliphatic and aromatic amines.
    Preface
    SYNTHESIS OF SOME NEW N-STYRYL UREA AND N-BENZYL THIOUREA DERIVATIVES
    Chen Ruyu, Yang Huazheng, Wang Fu
    1983, 4(2):  207-212. 
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    Six new substituted compounds of urea of the general formula -CH=CHNHNR1R2(R1=H, R2=C1-3 alkyl, or R1=R2=C1-3 alkyl) have beenprepared by the reactions of a styrylisocyanate with appropriate alkyl-amines. The yields of these compounds are mostly over ninety percent.By the reactions of α-methylbenzyl or p-chloro-α-methylbenzyl isothio-cyanates with different alkylamines, twelve new substituted thioureas havebeen synthesized. Their general formula is X-NR1R2 (R1 and R2 are the same as above; X=Cl, H). The yields of most of the products are over eighty percent.An attempt has been made to synthesize the above substituted thioureas by means of One Step Method, namely, the direct reaction of substituted benzylamine,alkylamine and carbon disulfide. The result shows that whereas dimethylamine can react successfully with the benzyl- or substituted benzylamine and carbon disulfide to give the corresponding substituted thioureas with yields of about seventy percent. Methylamine did not react normally, and the products are mainly sym-dibenzyl or sym-di-substituted benzyl thioureas.Bioassay for these compounds shows that they have herbicidal activi-ties, some of which rank higher than HERBICIDE No. 1 Cl-(CH3)2.
    Articles
    SYNTHESIS OF ALIPHATIC α-AMINO ACIDS FROM CHLOROFORM, ALIPHATIC ALDEHYDES (OR KETONES) AND AQUEOUS AMMONIA UNDER TWO-PHASE CONDITIONS
    Yu Lingchong, Yan Meirong
    1983, 4(2):  213-217. 
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    The reaction of chloroform, aliphatic aldehydes (or ketones) and aqueous ammonia in the presence of triethylbenzyl ammonium chloride and lithium chloride under two-phase conditions was studied.Optimum reaction conditions were determined with cyclohexanone. Under these conditions straightchain aliphatic aldehydes also undergo the reaction. Nine aliphatic α-amino acids were prepared and the yields range from 21.4% to 52.4%.The isolation of by-product a-amino amide (2-amino-2-methyl-n-valer-amide) demonstrates that the reaction involves the formation of an intermediate epoxide followed by the opening of the epoxide ring by ammonia.
    Preface
    THERMODYNAMIC INVESTIGATION OF THE EXTRACTION SYSTEM(Ⅰ) ——DETERMINATION OF THE ACTIVITY COEFFICIENTS OF BINARY SYSTEMS OF TBP-DILUENT BY ~(32)P-LABELED TBP DISTRIBUTION METHOD
    Gao Hongcheng, Peng Qixiu, Peng Lie, Wang Wenqing, Hsu Kwang-hsien
    1983, 4(2):  218-222. 
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    The activity coefficients of TBPin various diluents have been determined by 32P-labeled TBP distribution method. 33P-labeled TBPhas been preparedby Higgin's method.It was dissolved in various diluents-benzene,hexane,carbon tetrachloride, chloroform and odourless kerosene. The composition of TBPsolutions could be varied with a wide range from 1 to 98 volume%. This method is simpler, more rapid and the range of cnocentration studied is broader than other physico-chemical methods.The radioactivities of aqueous phase equilibrated with 32P-labeled TBPand its solutions were first measured, then the ratios A2 of the radioactivities were calculated therefrom. The thermodynamic equilibrium constant λ0 is equal to the ratio of the activities of TBPbetween the two phases.As the solubility of TBPin water is low, the activity coefficient of TBPin water can be assumed to be equal to unity. Pure TBPis used as the standard state of solute for the determination of f2 which is the activity coefficient of the solute TBP. Let The effect of different solvents on the activity coefficients thus measured has been discussed from the point of view of intermolecular interactions. As an alternate approach we choos ean infinitely dilute solution of TBPas the reference state so that the activity coefficients at infinitely dilute solution were taken to be unity. The standard state of the solute TBPwas obtained by extrapolating the Henry's law line to N2→ and it is a hypothetical state.
    Articles
    CNDO CALCULATIONS ON TRANSITION METAL COMPOUNDS (Ⅱ) ——ACTIVE CENTER MOBELS OF N2 ABSORPTION ON α-Fe(111) PLANE CLUSTERS
    Wang Zhizhong, Ding Dezeng, Tang Aoqing
    1983, 4(2):  223-229. 
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    In this paper we have studied active center models of N3 adsorption on α-Fe(lll) plane clusters by the CNDO method. Obtained conclusions are following:(l)The end-on and the side-on complexes activate dinitrogen by coordination through mainly weakening π-bond in the N2 molecules. (2) For N2 adsorptions on the Fe4 clusters, the bomb-laying type activates the triple bond of the N2 molecules more than the perpendicular-insertion type. (3) For N2 adsorptions on the Fe7 clusters, the perpendicular-insertion type activates the triple bond of dinitrogen more than the bomb-laying type. In general, Fe7 clusters activate triple bond of dinitrogen more than the Fe4 clusters. (4) When we consider the charges on the adsorpted dinitrogen in all perpendicular-insertion models sn atom N placing far from adsorbent atom Fe is carried more negatively. The Hδ+ attaches the outside Natom favorably, but for all bomb-laying adsorption types this is not true.
    THE STUDY OF THE CONSTRUCTION OF HIGH PRECISION SATURATED CADMIUM SULFATE STANDARD CELLS
    Zhu Xunzhi(Hsun-chih Chu), Qu Jin, You Quansheng, Fan Longfei
    1983, 4(2):  230-236. 
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    This paper describes the method for the preparation and purification of materials used in construction of high precision saturated cadmium sulfate standard cells from general technical grade chemicals. Forty acid cells (0.049 N H2SO4) were studied, readings of emf were taken at intervals during the period of 1973 to 1979, the average change in emf is 0.33μVper year.Various factors are briefly discussed in the article. The following processes will take place during the aging period of the cells: the dissolution of alkali constituents from the inner surface of the glass container into the cells and the slight reaction of cadmium in the negative electrode with the acid in the solution, both these two processes will cause the increase of the emf. While another process, the gradual growth of the crystal sizes of the mercurous sulfate, will decrease the emf of the cells. Experimental data are given for these two factors.
    THE CORRELATION BETWEEN THE CONFORMATIONAL ANALYSES OF THE5-SUBSTITUTED ISOPROPYLIDENE MALONATES AND THE PRINCIPLE OF THE STRUCTURAL ADAPTABILITY
    Jin Songshou, Huang Xian, Chen Cheng-chu
    1983, 4(2):  237-243. 
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    In this paper, the conformation of the 5-substituted isopropylidene malonates was analyzed in detail according to the principle of the structural adaptability for the interreaction between the groups of molecules. The results agreed with their nuclear magnetic resonance spectra.(1) It was evident that the isopropylidene malonate had two energetically favoured chair conformations which could rapidly interconvert one another,(2) If the 5-substituted group contained aromatic group, such as phe-nyl, furfyl, the favoured conformation was that the aromatic ring tended to be parallel with the plane containing the two ester-groups. Here the boat conformation might be favourable. Therefore, the long range shielding effect of the aromatic ring toward the 2-methyl group could be shown. It means that the chemical shifts would move to higher magnetic field.(3) If the 5-substituted group was a carbonylmethyl group, the oxygen atom in carbonyl group approached to the three hydrogen atoms of the 2-methyl group. At that time a long range deshielding effect of the carbonyl group appeared.
    HIGH INHIBITION EFFECT OF 2,2,6,6-TETRA- METHYL-4-HYDROXYL-PIPERIDINE- 1-OXYL ON ACRYLIC ACID
    Zhang Ziyi, Wei Xiuying
    1983, 4(2):  244-247. 
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    The high inhibition effect of 2,2,6,6-tetra-methyl-4-hydroxyl piperi-dine-oxyi (TMHPO.) on radical polymerization of acrylic acid, initiated by benzoylperoxide, has been studied. The results showed that the inhibition effect was predominant when the amounts of TMHPO. were approximately equal to 0.1-0.3% of those of acrylic acid, and became more prominent especially when TMHPO. was the incorporated with 1,4-benzo-quinone and phenothiazine. For presumably, these were a synergistic action between TMHPO. and other inhibitors such as 1,4-benzoquinone and phe-nothazine.
    CONTROL OF 1,2-CONTENT OF POLYBUTADIENE IN ANIONIC POLYMERIZATION FOR PREPARING POLYBUTADIENE AND BLOCK COPOLYMER SBS
    Lu Yi, Xu Ruiqing, Jin Guantai
    1983, 4(2):  248-252. 
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    Here was studied the influence of tetrahydrofuran on the 1,2-content of polybutadiene in anionic polymerizaton for preparing polybutadiene and block copolymer SBS by using n-butyl lithium as initiator in solution of cyclohexane.The experiments showed that at given temperatures the 1,2-content of polybutadiene is a exponential function of the concentration of THF,so the 1,2-content of polybutadiene can be controlled by changing the concentration of THFat given temperature of polymerization.
    DETERMINATION OF METHYLMERCURY IN HUMAN HAIR BY COMBINED GAS CHROMATOGRAPH- MERCURY ANALYZER
    Zhang Xie
    1983, 4(2):  253-256. 
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    Amethod for determining methylmercury in human hair is described. The sample is digested by hydrochloric acid and extracted with benzene, The concentrated extract is then injected into the gas chromatograph, where methylmercury is directly reduced to the elemental mercury in the hydrogen atmosphere and the mercury vapor is finally measured by Mercury-Analyzer.This method is simple and rapid with a detection limit of 1×10-11 g Hg and a relative standard deviation of 2.3%. The method is satisfactory for the analysis of human hair samples.
    STUDIES ON NITROXIDES (Ⅳ) ——OXIDATION OF CYSTEINE BY 2,2,6,6-TETRAMETHYL-4- HYDROXYPIPERIDINE-1-OXYL
    Liu Youcheng, Wang Xiuzhi, Liu Zhongli
    1983, 4(2):  257-259. 
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    The redox reaction of 2,2,6, 6-tetramethyl-4-hydroxypiperidine-1-oxyl radical with dl-cysteine in buffer solution of different pHhas been studied at room temperature under free of oxygen in the dark.It was found that in acidic buffer the oxidation product of cysteine was cysteic acid, in neutral buffer the product was cystine accompanied by a small amount of cysteic acid, whereas in basic buffer the product was cystine only. The reduction product of the nitroxide was identified as the corresponding hydroxylamine in all these cases.
    SPECTROPHOTOMETRIC DETERMINATION OF ULTRATRACEAMOUNTS COPPER (Ⅱ) BY A NEW AND HIGH SENSITIVELY CATALYTIC REACTION
    Yuan Dawen, Chen Siqing, Peng Shanshan
    1983, 4(2):  260-262. 
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    In this paper, varieous conditions,suitable for determining ultratracea-mounts of Cu2+ when mixed reductant of sulphanilic acid and α-naphthyl-amine is oxidized by H2O2 using as a catalytic reaction,have been examined in detail. The sensitivity of this method presented as apparent molar absorptivity equals 1.25×107. The interference of many common ions can be separated by precipitating with ammonia. Trace amounts of Cu2+ in some high-purity reagents, such as NaCl, LiCl·H2O, were determined by this method with satisfactory results.
    THE REASON FOR BRINGING ON TWO SETS OF PI-BOND ENERGY DATA
    Luo Yuran
    1983, 4(2):  263-265. 
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    The assumption that the bond energies in the free radicals are equal to ones in the parent molecules is the reason for bringing on two sets of pi-bond energy data. If the assumption is not accepted, the same values of pi-bond energies can be estimated from thermochemical and kinetic data. The theoretical base and the error range for Benson-O'Neal empirical rule for estimating activation energies of thermal cis-trans isomerization have been discussed.
    STUDIES ON THE CHANGES OF SOME CRYSTALLINE PHASES OF Fe-Pb PHOSPHATE CATALYSTS
    Zhen Kaiji, Bi Yingli
    1983, 4(2):  266-268. 
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    In this paper, changes of some crystalline phases of Fe-Pb phosphate catalysts were investigated using X-ray diffraction and TDA methods.Obtained results may provide some further information about the oxi-dative dehydrogenation reaction of isobutylic acid on the given catalysts.
    ANALYSIS OF TRACE AMOUNTS OF RARE EARTH ELEMENTS IN CROPS BY POLAROGRAPHIC CATALYTIC WAVES
    Gao Xiaoxia, Jiao Kui, Zhang Manping
    1983, 4(2):  269-270. 
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    Recently, in China the application of small amount of rare-earth nitrates or chlorides to the field has proved that REenhanced the growth and development of crops and increased yields. In order to understand the functions of rare earth elements in plant growth, we must first of all establish a sensitive analytical method for the determination of trace amounts of RE in the plants. In the present investigation we have used the sensitive single-sweep polarographic waves suggested by our research group to determine the RE contents in spinach, tea and pineleaves taken from different districts. The results showed that those plants growing near the RE mines (Jiangxi) have higher content of RE (ranging from 1.7 to 37.8 μg/g dry material basis) than those from other places. Wu Zhaoming et al of Institute of Botany, Academic Sinica, applied La-nitrate in water culture of cucumber and cut down the leaves from different parts of the plant for analysis. We found that the contents of La in the young leaves are much more than that in the old leaves. This result is in accordance with general role of distribution, that is more nutrient elements gathering in the growing center of the plant. This preliminary information is very useful for further study to find out whether RE is an essential nutrient element or not and what is its physiological function in the growth of the plant.
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