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1993 Volume 10 Issue 4
1993, 10(4): 1-4
Abstract:
In the polymerization of butyl methacrylate catalyzed by Nd(Oct)3-Al(i-Bu)3, the conversion in hexane and petroleum ether was found to be higher than that observed in toluene and tetrahydrofuran. The combination of Al(i-Bu)3 with Nd(Oct)3 gave the polymer of higher molecular weight than other Nd-complexes:Nd(P204)3, Nd(P507)3 and Nd(naph)3. Kinetics study showed that the rate of polymerization is first order with respect to the monomer and catalyst concentration. The activation energy of polymerization of butyl methacrylate is 47.4kJ/mol.
In the polymerization of butyl methacrylate catalyzed by Nd(Oct)3-Al(i-Bu)3, the conversion in hexane and petroleum ether was found to be higher than that observed in toluene and tetrahydrofuran. The combination of Al(i-Bu)3 with Nd(Oct)3 gave the polymer of higher molecular weight than other Nd-complexes:Nd(P204)3, Nd(P507)3 and Nd(naph)3. Kinetics study showed that the rate of polymerization is first order with respect to the monomer and catalyst concentration. The activation energy of polymerization of butyl methacrylate is 47.4kJ/mol.
1993, 10(4): 5-9
Abstract:
It was found that H3PMo12O40 was an excellent passivator in comparison with H4SiMo12O40, H3PW12O40, H4SiW12O40 and chromates. The optimium conditions of passivation with H3PMo12O40 on the zinc-plating coating as follows:H3PMo12O40 5g/L, pH 1.1, passivation time 35s, passivation temperature 15℃, retention time in air 10s, confinement temperature 100℃(water). The surface appearence, composition and possible structure of the passivated film were determined by scanning electron microscopy, X-ray photoelectron spectroscopy, Auger electron spectroscopy, IR and Raman spectrometry. The results showed that a dense corrosion-resistant film was formed on the zinc surface consisting of P, Mo, O and Zn. Molybdenum existed in Mo (Ⅵ), Mo (Ⅴ) and Mo(Ⅵ) in the film with a P/Mo ratio 1:3.0. A certain complex passivated film, Znx(PMo3)yOx/ZnO/Zn is assumed to be formed.
It was found that H3PMo12O40 was an excellent passivator in comparison with H4SiMo12O40, H3PW12O40, H4SiW12O40 and chromates. The optimium conditions of passivation with H3PMo12O40 on the zinc-plating coating as follows:H3PMo12O40 5g/L, pH 1.1, passivation time 35s, passivation temperature 15℃, retention time in air 10s, confinement temperature 100℃(water). The surface appearence, composition and possible structure of the passivated film were determined by scanning electron microscopy, X-ray photoelectron spectroscopy, Auger electron spectroscopy, IR and Raman spectrometry. The results showed that a dense corrosion-resistant film was formed on the zinc surface consisting of P, Mo, O and Zn. Molybdenum existed in Mo (Ⅵ), Mo (Ⅴ) and Mo(Ⅵ) in the film with a P/Mo ratio 1:3.0. A certain complex passivated film, Znx(PMo3)yOx/ZnO/Zn is assumed to be formed.
1993, 10(4): 10-12
Abstract:
Sixteen cornplexes of rare earth (RE=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Y) with 1-pheny-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP) and 1-nitroso-2-naphthol (NN) have been synthesized and characterized by elemental analysis, IR 1H NMR and DTA measurements. The ternary complexes have a general formula RE:PMBP:NN=1:3:1(1:4:1 when RE=Ce(Ⅳ)). All the complexes are crystal in gray-violet colour. They are soluble in ethanol, acetone and benzene, insoluble in water, and air-stable at room temperature.
Sixteen cornplexes of rare earth (RE=La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Y) with 1-pheny-3-methyl-4-benzoyl-pyrazolone-5 (HPMBP) and 1-nitroso-2-naphthol (NN) have been synthesized and characterized by elemental analysis, IR 1H NMR and DTA measurements. The ternary complexes have a general formula RE:PMBP:NN=1:3:1(1:4:1 when RE=Ce(Ⅳ)). All the complexes are crystal in gray-violet colour. They are soluble in ethanol, acetone and benzene, insoluble in water, and air-stable at room temperature.
1993, 10(4): 13-17
Abstract:
The catalytic species,water-soluble sulfonated-triphenylphosphine-rhodium complexes have been supported on SiO2 surface to form heterogenized-homogeneous catalysts denoted supported aque ous phase catalysts (SAPC). The SAPC possesses high catalytic activities even in the presence of excessive phosphine ligand owing to its high surface area. Hydroformylation of methyl 10-undecenoate and 1-hexene are easily carried out in an autoclave or fixed bed reactor over SAPC. With fixed bed reactor,aldehyde selectivities of up to 95% can be achieved in 4.0 MPa of CO/H2 (1/1, V/V) at 100℃; and the ratios of normal to isomcr aldehyde (n/i) were found to be increased with the increase of P/Rh ratios. It is also found that the reaction rate decreased and the n/i ratios of aldehydes were almost unchanged,when P/Rh ratios were over 15.
The catalytic species,water-soluble sulfonated-triphenylphosphine-rhodium complexes have been supported on SiO2 surface to form heterogenized-homogeneous catalysts denoted supported aque ous phase catalysts (SAPC). The SAPC possesses high catalytic activities even in the presence of excessive phosphine ligand owing to its high surface area. Hydroformylation of methyl 10-undecenoate and 1-hexene are easily carried out in an autoclave or fixed bed reactor over SAPC. With fixed bed reactor,aldehyde selectivities of up to 95% can be achieved in 4.0 MPa of CO/H2 (1/1, V/V) at 100℃; and the ratios of normal to isomcr aldehyde (n/i) were found to be increased with the increase of P/Rh ratios. It is also found that the reaction rate decreased and the n/i ratios of aldehydes were almost unchanged,when P/Rh ratios were over 15.
1993, 10(4): 18-21
Abstract:
The synergistic extraction of uranium (Ⅵ) by 1,10-bis (1'-phenyl-3'-methyl-5'-oxopyra-zol-4'-y1)-1, 10-decanedione(H2A) and some asymmetric sulfoxides (n-butyloctyl-,n-pentylhexyl-,and ethyl-n-dodecyl sulfoxide,n-BOSO,n-PHSO, and n-EDSO, respectively) has been studied, By using slope analysis method the formula of the extraction complexes were shown to be UO2A·B(Brepresents sufoxide). The synergistic extraction eqilibrium constants were calculated. The solid extracted complexes have been characterized by elemental analyses, UV and IR spectroscopy.
The synergistic extraction of uranium (Ⅵ) by 1,10-bis (1'-phenyl-3'-methyl-5'-oxopyra-zol-4'-y1)-1, 10-decanedione(H2A) and some asymmetric sulfoxides (n-butyloctyl-,n-pentylhexyl-,and ethyl-n-dodecyl sulfoxide,n-BOSO,n-PHSO, and n-EDSO, respectively) has been studied, By using slope analysis method the formula of the extraction complexes were shown to be UO2A·B(Brepresents sufoxide). The synergistic extraction eqilibrium constants were calculated. The solid extracted complexes have been characterized by elemental analyses, UV and IR spectroscopy.
1993, 10(4): 22-25
Abstract:
The synthesis and characterization of a new bis-N-functionalized diaza-dioxa maeroeycle 1,2-his(1, 12-diaza-3, 4:9,10-dibenzo-5, 8-dioxaeyclopentadeeane-N-aeetie aeid) ethane (H2L2) are reported. Eight lanthanide (La, Pr, Nd, Sm, Eu, Gd, Dy, Yb) complexes with this ligand have been prepared in methanol solution by the reaction of H2L2 with rare earth nitrate respectively. These complexes have a general formula of Ln2L2(NO3)4·nH2O. Their coordination properties are discussed.
The synthesis and characterization of a new bis-N-functionalized diaza-dioxa maeroeycle 1,2-his(1, 12-diaza-3, 4:9,10-dibenzo-5, 8-dioxaeyclopentadeeane-N-aeetie aeid) ethane (H2L2) are reported. Eight lanthanide (La, Pr, Nd, Sm, Eu, Gd, Dy, Yb) complexes with this ligand have been prepared in methanol solution by the reaction of H2L2 with rare earth nitrate respectively. These complexes have a general formula of Ln2L2(NO3)4·nH2O. Their coordination properties are discussed.
1993, 10(4): 26-29
Abstract:
Superconductors of type YBa2Cu3-xMxO7-y(My=V,Nb,Ta;x=0.0~0.7) have been prepared. No phase-transition from orthorhombie to tetragonal for x≤0.6 were found by X-ray diffractometry. The lattice parameters of the system vary with the number of x. The D.C. resistivities and the values of Hall effect measured at room temperature showed a progressive increase, but the concentration and the mobility of the carrier decreased gradually with the increase of x. This reveals that the partial substitution by the element of the V B group affects the electronic structure of the superconductor. The change of the electronic structure has been discussed in terms of the crystal field theory.
Superconductors of type YBa2Cu3-xMxO7-y(My=V,Nb,Ta;x=0.0~0.7) have been prepared. No phase-transition from orthorhombie to tetragonal for x≤0.6 were found by X-ray diffractometry. The lattice parameters of the system vary with the number of x. The D.C. resistivities and the values of Hall effect measured at room temperature showed a progressive increase, but the concentration and the mobility of the carrier decreased gradually with the increase of x. This reveals that the partial substitution by the element of the V B group affects the electronic structure of the superconductor. The change of the electronic structure has been discussed in terms of the crystal field theory.
1993, 10(4): 30-34
Abstract:
Six new solid complexes of rare earth with 1-naphthaleneaeetie acid(NAA) and 1,10-phenanthroline (Phen) were prepared. These complexes all have the compsition of RE(NAA)3·Phen (RE=Y, La, Nd, Sm, Eu, Er). The compositions, properties and bonding specificity between RE3+ and ligands have been confirmed by elemental analysis,molar conductance, IR, UV-Vis, H-NMR,XPS spectra and TG-DTA measurements.
Six new solid complexes of rare earth with 1-naphthaleneaeetie acid(NAA) and 1,10-phenanthroline (Phen) were prepared. These complexes all have the compsition of RE(NAA)3·Phen (RE=Y, La, Nd, Sm, Eu, Er). The compositions, properties and bonding specificity between RE3+ and ligands have been confirmed by elemental analysis,molar conductance, IR, UV-Vis, H-NMR,XPS spectra and TG-DTA measurements.
1993, 10(4): 35-38
Abstract:
Fourteen new derivatives of steviol have been synthesized through structural modification.Among them the compound 4 appeared the best bioactivity in relation to bud sprout and growth of cotton plant.
Fourteen new derivatives of steviol have been synthesized through structural modification.Among them the compound 4 appeared the best bioactivity in relation to bud sprout and growth of cotton plant.
1993, 10(4): 39-42
Abstract:
The MPcs (M=Fe2+, Co2+, Cu2+; Pc=phthalocyanine) were coordinated with -(CH2)3N(C2H5)2 group of SiO2,which had been linked with above group through organic synthesis.The UV-Vis diffuse reflection spectra revealed this supporting. ESR result indicated that only the supported CoPe and FePc were capable of reacting with O2 producing O2-.
The MPcs (M=Fe2+, Co2+, Cu2+; Pc=phthalocyanine) were coordinated with -(CH2)3N(C2H5)2 group of SiO2,which had been linked with above group through organic synthesis.The UV-Vis diffuse reflection spectra revealed this supporting. ESR result indicated that only the supported CoPe and FePc were capable of reacting with O2 producing O2-.
1993, 10(4): 43-46
Abstract:
The glass-transition temperatures of the side chain liquid crystalline polyacrylates containing para-nitro azobenzene have been studied by DSC. It was found that the Tg value decreased with increasing the length of the spacer and MA content in the copolymers. But for the copolymers containing acrylic acid the Tg is higher than that of the corresponding homopolymers owing to the presence of hydrogen bond.
The glass-transition temperatures of the side chain liquid crystalline polyacrylates containing para-nitro azobenzene have been studied by DSC. It was found that the Tg value decreased with increasing the length of the spacer and MA content in the copolymers. But for the copolymers containing acrylic acid the Tg is higher than that of the corresponding homopolymers owing to the presence of hydrogen bond.
1993, 10(4): 47-50
Abstract:
The thermal decomposition of a series of polyanilines with different oxidation degrees and poly-o-toluidine was studied by Direct Pyrolysis Mass Spectrometry (DPMS) and Pyrolysis Gas Chromatograph/Mass Spectrometry(PGC/MS). The techniques of Collision Induced Decomposition (CID) and Tandem Mass Spectrometry have been used to investigate the mechanism of the chain cleavage.The results showed that the series of ions containing several units of polyaniline can be divided into two sources:benzene-diamine and guinone-deirnine units in polyaniline and its derivatines. The ratios of relative abandances of above ions were strongly influenced by the oxidation degrees. The mechanism of thermal decomposition of polyanilines and their derivatives was discussed.
The thermal decomposition of a series of polyanilines with different oxidation degrees and poly-o-toluidine was studied by Direct Pyrolysis Mass Spectrometry (DPMS) and Pyrolysis Gas Chromatograph/Mass Spectrometry(PGC/MS). The techniques of Collision Induced Decomposition (CID) and Tandem Mass Spectrometry have been used to investigate the mechanism of the chain cleavage.The results showed that the series of ions containing several units of polyaniline can be divided into two sources:benzene-diamine and guinone-deirnine units in polyaniline and its derivatines. The ratios of relative abandances of above ions were strongly influenced by the oxidation degrees. The mechanism of thermal decomposition of polyanilines and their derivatives was discussed.
1993, 10(4): 51-54
Abstract:
The emulsifier-free emulsion copolymerization of MMA with St has been carried out. At 70℃,[KPS]=5.55×10-3mol/L,[MMA]=0.51mol/L and[St]=0.49mol/L a higher conversion, smaller emulsion particles and greater concentration of particles can be obtained. A homogeneous nucleation mechanism has been proposed on the basis of the molecular weight and its distribution measurements in the course of the copolymrization. When the value of conversion exeessed 30.9%, the agglutination degree of the emulsion particles surpassed the formation speed of the particles. Radicles formed from KPS on decomposition appeared to stabilize the emulsion.
The emulsifier-free emulsion copolymerization of MMA with St has been carried out. At 70℃,[KPS]=5.55×10-3mol/L,[MMA]=0.51mol/L and[St]=0.49mol/L a higher conversion, smaller emulsion particles and greater concentration of particles can be obtained. A homogeneous nucleation mechanism has been proposed on the basis of the molecular weight and its distribution measurements in the course of the copolymrization. When the value of conversion exeessed 30.9%, the agglutination degree of the emulsion particles surpassed the formation speed of the particles. Radicles formed from KPS on decomposition appeared to stabilize the emulsion.
1993, 10(4): 55-57
Abstract:
Pd micropartieles modified by polyaniline (PAN (Pd)) which was obtained by using H6P4O13 as supporting electrolyte exhibited a considerably higher catalytic activity in oxidation of formic acid than the bare Pd electrode. Incorporation of Pd microparticles in PAN films were made by potential cycling between-0.2V and 0.5V(vs. SCE) in 0.01mol/L PdCl42- in about 15 Min. The catalytic activity was found in dependence on the size of the Pd particles, affected by the morphology of PAN film used. The XPS and electrochemical results reveal that the electrocatalytie mechanisms are different at the PAN(Pd) and bare Pd electrodes.
Pd micropartieles modified by polyaniline (PAN (Pd)) which was obtained by using H6P4O13 as supporting electrolyte exhibited a considerably higher catalytic activity in oxidation of formic acid than the bare Pd electrode. Incorporation of Pd microparticles in PAN films were made by potential cycling between-0.2V and 0.5V(vs. SCE) in 0.01mol/L PdCl42- in about 15 Min. The catalytic activity was found in dependence on the size of the Pd particles, affected by the morphology of PAN film used. The XPS and electrochemical results reveal that the electrocatalytie mechanisms are different at the PAN(Pd) and bare Pd electrodes.
1993, 10(4): 58-60
Abstract:
The galvanic cell type SOx(x=2,3) gas sensors consisting of with Ag-β"-alumina as solid electrolyte and porous Pt as working electrode and Ag as reference electrode have been constructed and tested. The electric motion force(EMF) responses were in good agreement with theoretical values for the SOx(x=2,3) partial pressures over a range from 10 ppm to 104 ppm at the temperature 550~750℃. And CO,CO2 and NO2 having the concentrations more than 10 times of SOx didn't disturb the measurement.
The galvanic cell type SOx(x=2,3) gas sensors consisting of with Ag-β"-alumina as solid electrolyte and porous Pt as working electrode and Ag as reference electrode have been constructed and tested. The electric motion force(EMF) responses were in good agreement with theoretical values for the SOx(x=2,3) partial pressures over a range from 10 ppm to 104 ppm at the temperature 550~750℃. And CO,CO2 and NO2 having the concentrations more than 10 times of SOx didn't disturb the measurement.
1993, 10(4): 61-63
Abstract:
The electrochemical performances of MLNi4-xMnAlx hydrogen storage alloys with different Al content have been studied. The results showed that the discharge capacity,fast discharge ability,overpotentials and cycle life of the MLNi4-xMnAlx electrodes were affected by Al contents. The cyclic voltarnmetry of MH electrodes exhibited a good linear relationship between Ip and v1/2,suggesting MH electrode reaction being controlled by diffusion process.
The electrochemical performances of MLNi4-xMnAlx hydrogen storage alloys with different Al content have been studied. The results showed that the discharge capacity,fast discharge ability,overpotentials and cycle life of the MLNi4-xMnAlx electrodes were affected by Al contents. The cyclic voltarnmetry of MH electrodes exhibited a good linear relationship between Ip and v1/2,suggesting MH electrode reaction being controlled by diffusion process.
1993, 10(4): 64-66
Abstract:
The neutral red/montmorillonite/SnO2 chemical modified electrode prepared had a higher electroactivity and stability. In comparison with the bare SnO2 electrode, the diffusion coefficients of neutral red determined by thin-layer spectroelectrochemical methods in the interface of the montmorillonite film were reduced by four order of magnitude, but the peak currents in cyclic voltammograms were increased.
The neutral red/montmorillonite/SnO2 chemical modified electrode prepared had a higher electroactivity and stability. In comparison with the bare SnO2 electrode, the diffusion coefficients of neutral red determined by thin-layer spectroelectrochemical methods in the interface of the montmorillonite film were reduced by four order of magnitude, but the peak currents in cyclic voltammograms were increased.
1993, 10(4): 67-69
Abstract:
In the blends of high impact polystyene (HIPS) with styrene-butadiene triblock copolymer (SBS) the SBS can be considered as both toughening angent of HIPS and compatibilizer for PS and PB phases in the HIPS. Addition of SBS into HIPS resulted in a marked increase of impact resistance of the latter.
In the blends of high impact polystyene (HIPS) with styrene-butadiene triblock copolymer (SBS) the SBS can be considered as both toughening angent of HIPS and compatibilizer for PS and PB phases in the HIPS. Addition of SBS into HIPS resulted in a marked increase of impact resistance of the latter.
1993, 10(4): 70-71
Abstract:
A technical procedure has been described for preparation of powder coating from waste PET resin. It consists of degradation of PET resin in the presence of propylene glycol and glycerin at 533K and ultilization of isocyanato-terminated precursor as latent curing agent. The coating shows a satisfactory result in physical and chemical properties.
A technical procedure has been described for preparation of powder coating from waste PET resin. It consists of degradation of PET resin in the presence of propylene glycol and glycerin at 533K and ultilization of isocyanato-terminated precursor as latent curing agent. The coating shows a satisfactory result in physical and chemical properties.
1993, 10(4): 72-74
Abstract:
The extraction behavior of trivalent rare-earth ions (except Sc, Pm) in hydrochloric acid solution using a n-octane solution containing his(2,4,4-trimethylpentyl) phosphinic acid(HBTMPP) was studied. The mean separation factor (βzz+1) for the system was found to be 3.24. The system showed an advantage of higher selectivity and easier stripping ever that With HEH/EHP. The extraction mechanism for Er(Ⅲ) and Tm(Ⅲ) ions has been investigated by the method,of solpe analysis.The equilibrium constants of the extraction have been calculated and the IR and 1H NMR spectra of the Er (Ⅲ) complex have been discussed.
The extraction behavior of trivalent rare-earth ions (except Sc, Pm) in hydrochloric acid solution using a n-octane solution containing his(2,4,4-trimethylpentyl) phosphinic acid(HBTMPP) was studied. The mean separation factor (βzz+1) for the system was found to be 3.24. The system showed an advantage of higher selectivity and easier stripping ever that With HEH/EHP. The extraction mechanism for Er(Ⅲ) and Tm(Ⅲ) ions has been investigated by the method,of solpe analysis.The equilibrium constants of the extraction have been calculated and the IR and 1H NMR spectra of the Er (Ⅲ) complex have been discussed.
1993, 10(4): 75-76
Abstract:
Under phase transfer catalytic conditions, eight alanine optical isomers were synthesized with optical yields ranging from 0~52.1%. An obvious effect of the double asymmetric induction was observed.
Under phase transfer catalytic conditions, eight alanine optical isomers were synthesized with optical yields ranging from 0~52.1%. An obvious effect of the double asymmetric induction was observed.
1993, 10(4): 77-78
Abstract:
A novel amorphous polymer with NLO chromophores (p-nitroaniline) in the main-chain was synthesized. The structure was characterized by IR, 1H NMR spectra. The glass transition ternperature was 123℃. The poling and relaxation of NLO chromophore containing in polymer film have been discussed by of UV-Vis Spectra.
A novel amorphous polymer with NLO chromophores (p-nitroaniline) in the main-chain was synthesized. The structure was characterized by IR, 1H NMR spectra. The glass transition ternperature was 123℃. The poling and relaxation of NLO chromophore containing in polymer film have been discussed by of UV-Vis Spectra.
1993, 10(4): 79-81
Abstract:
The strong-acid type ion-exchange resin supported trasition metal (Co2+,Cu2+,Ni2+) catalysts were prepared. The effects of the amount of the catalyst, solvent, and temperature on the addition reaction of alcohols on the alkene ethers have been investigated.
The strong-acid type ion-exchange resin supported trasition metal (Co2+,Cu2+,Ni2+) catalysts were prepared. The effects of the amount of the catalyst, solvent, and temperature on the addition reaction of alcohols on the alkene ethers have been investigated.
1993, 10(4): 82-83
Abstract:
It is reported for the first time that carbazole, a compound with only one functional group,can accelerate the electrochemical reaction of cytochrome c. The results are favorable to understand the promotion mechanism.
It is reported for the first time that carbazole, a compound with only one functional group,can accelerate the electrochemical reaction of cytochrome c. The results are favorable to understand the promotion mechanism.
1993, 10(4): 84-85
Abstract:
Some N-alkyl imidazole derivatives have been prepared from imidazole and alkyl halides in the presence of potassium hydroxides impregnated on alumina. The preparation was carried out at mild condition and in good yields and the supported reagent could be reused after recovery without loss of its activity.
Some N-alkyl imidazole derivatives have been prepared from imidazole and alkyl halides in the presence of potassium hydroxides impregnated on alumina. The preparation was carried out at mild condition and in good yields and the supported reagent could be reused after recovery without loss of its activity.
1993, 10(4): 86-88
Abstract:
A polyether reverse osmosis composite membrane "PFT" was prepared. The supporting membrane was an asymmetric ultrafiltrate membrane made from polyetheretherketone "PEK-C". The active layer was a sulfonated closslinked polycondensate made by in-situ polymerization of furfuryl alcohol and tris-(2-hydroxyethyl)isocyanurate. The constitution of the casting solution of PEK-C and the additives to the composite membrane solution on the performance of PFT membrane have been discussed. The title membrane gave over 99.6% salt rejection and 0.30m3/m2 per day Water flux at pressure of 4.9MPa with 1.5% NaCl aqueous solution.
A polyether reverse osmosis composite membrane "PFT" was prepared. The supporting membrane was an asymmetric ultrafiltrate membrane made from polyetheretherketone "PEK-C". The active layer was a sulfonated closslinked polycondensate made by in-situ polymerization of furfuryl alcohol and tris-(2-hydroxyethyl)isocyanurate. The constitution of the casting solution of PEK-C and the additives to the composite membrane solution on the performance of PFT membrane have been discussed. The title membrane gave over 99.6% salt rejection and 0.30m3/m2 per day Water flux at pressure of 4.9MPa with 1.5% NaCl aqueous solution.
1993, 10(4): 89-91
Abstract:
In this paper, the two coordination compounds of copper perchlorate with 4'-bromo(or 4',5'-dibromo)-benzo=15-crown-5 have been prepared in acetone medium, the composition of the new coordination compounds have been determined as Cu(ClO4)2·L·3H2O(L=4'-bromobenzo-15-crown-5 or 4', 5'-dibromo-benzo-15-crown-5), the IR, UV, TG-DTA,X-ray powder diffraction analysis and molar conductance of these coordination compounds have also been studied. It shows that coordination number of the coordination compounds is 9.
In this paper, the two coordination compounds of copper perchlorate with 4'-bromo(or 4',5'-dibromo)-benzo=15-crown-5 have been prepared in acetone medium, the composition of the new coordination compounds have been determined as Cu(ClO4)2·L·3H2O(L=4'-bromobenzo-15-crown-5 or 4', 5'-dibromo-benzo-15-crown-5), the IR, UV, TG-DTA,X-ray powder diffraction analysis and molar conductance of these coordination compounds have also been studied. It shows that coordination number of the coordination compounds is 9.
1993, 10(4): 92-94
Abstract:
A novel route for dihydrojasmone synthesis is reported. The main strategy inolves the nucleophilic substitution using ethyl α-cyanoheptyl carbonate (2) as acyl-anion(
=O) equivalents to bromide (3),following by hydrolysis to give the undecane-2,5-dione (5) which by base cyclization afforded dihydrojasmone (6). The method is simple and carried out in mild reaction conditions.
A novel route for dihydrojasmone synthesis is reported. The main strategy inolves the nucleophilic substitution using ethyl α-cyanoheptyl carbonate (2) as acyl-anion(
=O) equivalents to bromide (3),following by hydrolysis to give the undecane-2,5-dione (5) which by base cyclization afforded dihydrojasmone (6). The method is simple and carried out in mild reaction conditions.
1993, 10(4): 95-97
Abstract:
Verapamil is an electroinactive cationic drug. This paper describes the method for determination of trace verapamil on the Nafion-modified glassy carbon electrode. The peak current of dopamine is decreased when verapamil is added to an electrolyte solution containing electroactive dopamine. A good linear relationship was found between the extent of the decrease in the peak current and the logarithmic concentration of verapamil in the range of 5×10-7~1×10-5mol/L. The detection limit of the method was 2.5×10-7mol/L. The recovery was 96.2~105.7%, and the relative standard deviation was 3.2% (n=10).
Verapamil is an electroinactive cationic drug. This paper describes the method for determination of trace verapamil on the Nafion-modified glassy carbon electrode. The peak current of dopamine is decreased when verapamil is added to an electrolyte solution containing electroactive dopamine. A good linear relationship was found between the extent of the decrease in the peak current and the logarithmic concentration of verapamil in the range of 5×10-7~1×10-5mol/L. The detection limit of the method was 2.5×10-7mol/L. The recovery was 96.2~105.7%, and the relative standard deviation was 3.2% (n=10).
1993, 10(4): 98-100
Abstract:
Several triearbocyanine and tetramethinestyryl-cyanine dyes containing indole end group were synthesized from trimethylindoline quaternary salt. The structures of the dyes were confirmed by elemental analyses, IR spectra and 1H NMR spectroscopy. Some indotricarbocyanines with N,N-diphenyl amino group on the meso positions of the bridges of heptamethine chains are well soluble in 1,2-dichloroethane.
Several triearbocyanine and tetramethinestyryl-cyanine dyes containing indole end group were synthesized from trimethylindoline quaternary salt. The structures of the dyes were confirmed by elemental analyses, IR spectra and 1H NMR spectroscopy. Some indotricarbocyanines with N,N-diphenyl amino group on the meso positions of the bridges of heptamethine chains are well soluble in 1,2-dichloroethane.
1993, 10(4): 101-103
Abstract:
The cyclized random copolymers of cis-1,4-butadiene and isoprene have been investigated by using pyrolysis-gas chromatography. The results show that the amount of main pyrolysis products changes regularly with the degree of cyclization. Both units of butadiene and isoprene participate in cyclization, but the butadiene units are less liable to be cyclized.
The cyclized random copolymers of cis-1,4-butadiene and isoprene have been investigated by using pyrolysis-gas chromatography. The results show that the amount of main pyrolysis products changes regularly with the degree of cyclization. Both units of butadiene and isoprene participate in cyclization, but the butadiene units are less liable to be cyclized.
1993, 10(4): 104-106
Abstract:
Five lanthanoid complexes of salicylidene ethylenediamine (L) have been synthesized and characterized by elemental analysis, IR. UV, DTA-TG, molar conductance, X-ray diffraction analysis. The compositions of the complexes were confirmed to be[Ln2L3(NO3)3](NO3)3·2H2O (Ln=Eu,Tb,Ho,Tm,Lu).
Five lanthanoid complexes of salicylidene ethylenediamine (L) have been synthesized and characterized by elemental analysis, IR. UV, DTA-TG, molar conductance, X-ray diffraction analysis. The compositions of the complexes were confirmed to be[Ln2L3(NO3)3](NO3)3·2H2O (Ln=Eu,Tb,Ho,Tm,Lu).
1993, 10(4): 107-109
Abstract:
The effect of heat treatment of carbon fiber cloth on its surface properties and electrode performance has been investigated. In the absence of noble metal as catalyst the activity of carbon fiber cloth electrode was obviously increased after heat treatment. The activation by heat treatment was studied by ESCA.
The effect of heat treatment of carbon fiber cloth on its surface properties and electrode performance has been investigated. In the absence of noble metal as catalyst the activity of carbon fiber cloth electrode was obviously increased after heat treatment. The activation by heat treatment was studied by ESCA.
1993, 10(4): 110-113
Abstract:
The title complex has been synthesized and characterized by FT-IR spectrometry. The crystal of the complex, determined by X-ray diffraction method, belongs to orthorhombic with space group Pnn2 and cell parameters a=1.4433(1)nm, b=2.0169(3)nm, c=1.8489(2)nm and Z=4.The two Sm ions are connected by four carboxyl groups forming a dinuclear complex. Four water molecules are coordinated to cach Sm ion in this dinuclear complex. Therefore, there are 8 oxygen atoms coordinated to each Sm ion assuming a bicapped trigonal prism. The N atoms of NH3+ groups in the complex does not coordinate to Smions. The two Sm ions are spaced in 0.4443nm, thus no metalmetal bonds could be formed in the complex.
The title complex has been synthesized and characterized by FT-IR spectrometry. The crystal of the complex, determined by X-ray diffraction method, belongs to orthorhombic with space group Pnn2 and cell parameters a=1.4433(1)nm, b=2.0169(3)nm, c=1.8489(2)nm and Z=4.The two Sm ions are connected by four carboxyl groups forming a dinuclear complex. Four water molecules are coordinated to cach Sm ion in this dinuclear complex. Therefore, there are 8 oxygen atoms coordinated to each Sm ion assuming a bicapped trigonal prism. The N atoms of NH3+ groups in the complex does not coordinate to Smions. The two Sm ions are spaced in 0.4443nm, thus no metalmetal bonds could be formed in the complex.
1993, 10(4): 114-115
Abstract:
The title compound has been synthesized by using 4-Aminoantipyrine and methylisthiocyanate as raw materials in 67% yield. The use of poisonous thiophosgene has been avioded. The compound was characterized by elemental analysis, IR, UV, and MS measurements.
The title compound has been synthesized by using 4-Aminoantipyrine and methylisthiocyanate as raw materials in 67% yield. The use of poisonous thiophosgene has been avioded. The compound was characterized by elemental analysis, IR, UV, and MS measurements.
1993, 10(4): 116-118
Abstract:
Silver (Ⅱ) and cadmium(Ⅱ) tetra-4-oxy(2-ethylbehenate) phenyl porphyrin were synthesized. The LB films of the complexes gave the collapse pressures over 60mN/m. Visible spectra were recorded for the solution and multilayer and IR and ESR spectra for the solid.
Silver (Ⅱ) and cadmium(Ⅱ) tetra-4-oxy(2-ethylbehenate) phenyl porphyrin were synthesized. The LB films of the complexes gave the collapse pressures over 60mN/m. Visible spectra were recorded for the solution and multilayer and IR and ESR spectra for the solid.
